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Gemini VII 2390 Operator Manual V3.03

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®

Gemini VII
Operator’s Manual
V3.03

239-42828-01
Feb 2014
Adobe Acrobat Reader is a registered trademark of Adobe Systems, Inc.
Alconox is a registered trademark of the Alconox Company.
Micromeritics is a registered trademark of Micromeritics Instrument Corporation.
Microsoft, Windows, and Windows 7, and Windows Vista are registered trademarks of Microsoft Corporation.
Gemini is a registered trademark of Micromeritics Instrument Corporation.

© Micromeritics Instrument Corporation 2009-2014. All rights reserved. Printed in the U.S.A.
The software described in this manual is furnished under a license agreement and may be used or copied only in
accordance with the terms of the agreement.
WARRANTY
MICROMERITICS INSTRUMENT CORPORATION warrants for one year from the date of shipment each
instrument it manufactures to be free from defects in material and workmanship impairing its usefulness under
normal use and service conditions except as noted herein.

Our liability under this warranty is limited to repair, servicing and adjustment, free of charge at our plant, of any
instrument or defective parts when returned prepaid to us and which our examination discloses to have been
defective. The purchaser is responsible for all transportation charges involving the shipment of materials for
warranty repairs. Failure of any instrument or product due to operator error, improper installation, unauthorized
repair or alteration, failure of utilities, or environmental contamination will not constitute a warranty claim. The
materials of construction used in MICROMERITICS instruments and other products were chosen after extensive
testing and experience for their reliability and durability. However, these materials cannot be totally guaranteed
against wear and/or decomposition by chemical action (corrosion) as a result of normal use.

Repair parts are warranted to be free from defects in material and workmanship for 90 days from the date of
shipment.

No instrument or product shall be returned to MICROMERITICS prior to notification of alleged defect and
authorization to return the instrument or product. All repairs or replacements are made subject to factory
inspection of returned parts.

MICROMERITICS shall be released from all obligations under its warranty in the event repairs or modifications
are made by persons other than its own authorized service personnel unless such work is authorized in writing by
MICROMERITICS.

The obligations of this warranty will be limited under the following conditions:

1. Certain products sold by MICROMERITICS are the products of reputable manufacturers, sold
under their respective brand names or trade names. We, therefore, make no express or implied
warranty as to such products. We shall use our best efforts to obtain from the manufacturer, in
accordance with his customary practice, the repair or replacement of such of his products that may
prove defective in workmanship or materials. Service charges made by such manufacturer are the
responsibility of the ultimate purchaser. This states our entire liability in respect to such products,
except as an authorized person of MICROMERITICS may otherwise agree to in writing.
2. If an instrument or product is found defective during the warranty period, replacement parts may,
at the discretion of MICROMERITICS, be sent to be installed by the purchaser, e.g., printed
circuit boards, check valves, seals, etc.
3. Expendable items, e.g., sample tubes, detector source lamps, indicator lamps, fuses, valve plugs
(rotor) and stems, seals and O-rings, ferrules, etc., are excluded from this warranty except for
manufacturing defects. Such items which perform satisfactorily during the first 45 days after the
date of shipment are assumed to be free of manufacturing defects.
Purchaser agrees to hold MICROMERITICS harmless from any patent infringement action brought against
MICROMERITICS if, at the request of the purchaser, MICROMERITICS modifies a standard product or
manufactures a special product to the purchaser’s specifications.

MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of
its products other than the liability stated above. This warranty is in lieu of all other warranties, express or
implied, including, but not limited to, the implied warranties of merchantability or fitness for use.

4356 Communications Drive  Norcross, GA 30093-2901 Fax (770) 662-3696


Domestic Sales - (770) 662-3636 Domestic Repair Service - (770) 662-3666
International Sales - (770) 662-3660 Customer Service - (770) 662-3636

Form No. 008-42104-00


Rev. 12/95
Gemini VII Table of Contents

TABLE OF CONTENTS

1. GENERAL INFORMATION
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Organization of the Operator’s Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Equipment Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
Cryogen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-6
Degasser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-6
Vacuum Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-6
Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-7
User-defined Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-7
Report Features. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-7
Gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-7
Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-8

2. USER INTERFACE
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Instrument Components and Connectors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
Sample Compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
Turning the Analyzer On and Off . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Turning the Analyzer On . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Turning the Analyzer Off. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Using the Software. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Shortcut Menus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Shortcut Keys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
File Status and Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
File Name Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
Menu Structure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-9
Main Menu Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-10
Window Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-11
Help Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12

3. OPERATING PROCEDURES
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Specifying Sample Defaults. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Advanced Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Basic Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4
Restricted Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-5

239-42828-01 - Nov 2013 i


Table of Contents Gemini VII

Defining Sample Information Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6


Advanced Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6
Basic or Restricted Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-7
Opening Sample Information Files. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9
Opening Files with a Status of Complete, Analyzing, or Entered . . . . . . . . . . . . . . . . 3-9
Opening Files with a Status of Preparing, Prepared, or No Analysis . . . . . . . . . . . . . . 3-9
Defining Parameter Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-11
Degas Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12
Analysis Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-13
Adsorptive Properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-14
Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-15
Preparing for Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-16
Cleaning and Labeling Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-17
Determining the Sample Mass . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-18
Degassing the Sample. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-20
Installing the Sample Tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-21
Installing the Analysis Dewar. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-22
Performing an Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-24
Start Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-25
QuickStart Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-26
Blank Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-27
Generating Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-28
Printing Files. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-30
Listing Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-31
Exporting Isotherm Data. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-32
Format of Exported Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-33
Converting Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-34
Generating Graph Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-35
Multiple Sample Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-35
Multiple Graph Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-40

4. SOFTWARE AND SETUP MODIFICATIONS


Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
Installing the Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
Starting the Setup Program . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9
Installing Software Updates or Reverting to a Previous Version . . . . . . . . . . . . . . . . . . . . . 4-10
Adding an Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-13
Ethernet Switch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-13
Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-14
Moving an Analyzer from One PC to Another PC. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-16
Removing an Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-20
Changing the Analyzer Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-22
Reinstalling Calibration Files for an Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-24
Importing an Analyzer from a Previous Installation on this PC. . . . . . . . . . . . . . . . . . . . . . 4-27
Adding or Modifying SmartPrep . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-29
Uninstalling the Analysis Program. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-31

ii 239-42828-01 - Nov 2013


Gemini VII Table of Contents

5. FILE MENU
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
Common Fields and Buttons - File Menu Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
Open . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
Save . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
Save As. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5
Save As (t-Curve or Alpha-S Curve) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5
Save All . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Close. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Close All. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Print . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Export. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Convert. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7
Exit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7
Sample Information Files. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
Degas Conditions Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-10
Analysis Conditions Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11
Adsorptive Properties Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-17
Report Options Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-18
Summary Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-20
Isotherm Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-22
BET/Langmuir Surface Area Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-24
Freundlich Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-27
Temkin Isotherm Report Options. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-28
t-Plot Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-30
Alpha-S Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-33
f-Ratio Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-34
BJH Adsorption/Desorption Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-36
Tabular Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-38
Plot Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-40
Dollimore-Heal Adsorption/Desorption Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-41
Tabular Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-45
Plot Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-45
DFT Pore Size Report Options. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-46
DFT Surface Energy Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-49
Dubinin Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-49
Tabular Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-50
Transformed Isotherm Plot Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-51
Pore Volume Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-52
MP-Method Report Options. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-53
Tabular Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-54
Plot Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-54
Options Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-55
Sample Log Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-55
Validation Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-56
Entered or Collected Data File. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-57

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Table of Contents Gemini VII

6. UNIT MENU
Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1
Common Fields and Buttons - Unit Menu Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-2
Start Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-2
QuickStart Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-5
Start Po Measurement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-6
Blank Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-7
Enable Manual Control. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-8
Instrument Schematic Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-9
System Valves. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-10
Instrument Schematic Shortcut Menus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-11
Show Instrument Schematic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-12
Show Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-13
Show Instrument Log . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-15
Unit Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-16
Diagnostics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-17
Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-19
Zero Pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-20
Match Transducers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-20
Reset Pressure Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-21
Sample Servo . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-21
Balance Servo . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-21
Save to File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-22
Load from File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-23
Service Test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-23

7. REPORTS MENU
Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1
Common Fields and Buttons - Reports Menu Options. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-2
Start Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-2
Close Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-3
Open Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-3
SPC Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-3
Regression Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5
Control Chart . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-7
Heat of Adsorption Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-10
Report Features and Shortcuts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-12
Report Header . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-13
Report Tool Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-14
Report Shortcut Menus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-17
Report Header Shortcuts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-17
Tabular Reports Shortcuts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-18
Graph Shortcuts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-19
Other On-Screen Features. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-23
Zoom Feature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-23
Axis Cross-Hair . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-23
Report Examples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-24
Isotherm Linear Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-25

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BET Surface Area Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-26


BET Surface Area Plot. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-27
t-Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-28
BJH Adsorption Cumulative Pore Volume . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-29
BJH Adsorption dV/dlog(w) Pore Volume . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-30

8. OPTIONS MENU
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1
Option Presentation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1
Sample Defaults . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-2
Restricted Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-2
Units . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-3
Graph Grid Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-3
Service Test Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-4

9. TROUBLESHOOTING AND MAINTENANCE


Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1
Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1
Preventive Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-4
Recovering from a Power Failure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-4
Lubricating Elevator Drive Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-5
Cleaning the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-5
Cleaning the Analysis Dewar. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-5
Replacing Port Filter (Frit) and O-ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-6
Replacing the Sample Tube O-ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-7
Inspecting and Changing Vacuum Pump Oil. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-8
Inspecting the Oil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-8
Changing or Adding Oil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-8
Replacing the Alumina in the Oil Vapor Trap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-11
Changing the Vacuum Pump Exhaust Filter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-15
Performing a Leak Test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-16
Connecting Gases. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-18
Guidelines for Connecting Gases to the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-18
Disconnecting the Depleted Bottle. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-18
Connecting a Replacement Gas Bottle. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-19
Cleaning and Verifying the Gas Line. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-22
Performing a Blank Analysis for Diagnostic Purposes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-26
Performing a Reference Analysis. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-28
Analyzing Reference Material . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-29
Calibrating the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-30
Zero Pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-30
Match Transducers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-31
Sample Servo . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-31
Balance Servo. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-32

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Table of Contents Gemini VII

10. ORDERING INFORMATION

A. FORMS
Sample Data Worksheet . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-3

B. ERROR MESSAGES
2400 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-1
2500 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-7
4000 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-10
6000 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-22

C. CALCULATIONS
Saturation Pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-1
Relative Pressure Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-1
Quantity Adsorbed Calculations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-2
Free Space. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-2
Measured. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-2
Calculated . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-3
Equilibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-4
Thermal Transpiration Correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-5
BET Surface Area. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-6
Langmuir Surface Area. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-7
t-Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-8
BJH Pore Volume and Area Distribution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-10
Explanation of Terms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-10
Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-11
Compendium of Variables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-18
Horvath-Kawazoe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-19
Slit Pore Geometry (original HK). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-19
Cylinder Pore Geometry (Saito/Foley) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-20
Sphere Pore Geometry (Cheng/Yang) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-21
Cheng/Yang Correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-22
Interaction Parameter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-23
Additional Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-24
Interaction Parameter Components. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-25
Dubinin-Radushkevich . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-27
Dubinin-Astakhov. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-29
MP-Method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-33
Freundlich Isotherm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-35
Temkin Isotherm. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-35
DFT (Density Functional Theory) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-36
The Integral Equation of Adsorption . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-36
Application to Surface Energy Distribution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-37
Application to Pore Size Distribution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-37
Performing the Deconvolution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-38

vi 239-42828-01 - Nov 2013


Gemini VII Table of Contents

Regularization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-38
SPC Report Variables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-39
Regression Chart Variables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-39
Control Chart Variables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-40
Summary Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-40
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-42

D. ETHERNET CONFIGURATION
Configuring the Ethernet Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-1
Windows 7 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-1
Windows Vista . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-5

E. ANALYZING SAMPLES WITH TOTAL SURFACE AREA OF 1.0M2 OR LESS


Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-1
Using Glass Beads . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-1
Using Filler Rods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-3
Using Glass Beads and Filler Rods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-4

F. DFT MODELS
Models Based on Statistical Thermodynamics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-1
Theoretical Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-1
Molecular Simulation Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-2
Molecular Dynamics Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-2
Monte Carlo Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-2
Density Functional Formulation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-3
Models Included. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-7
Non-Local Density Functional Theory with Density-Independent Weights . . . . . . . . F-7
Non-Local Density Functional Theory with Density-Dependent Weights . . . . . . . . . F-7
Models Based on Classical Theories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-13
Surface Energy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-13
Pore Size. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-13
Models Included. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-14
Kelvin Equation with Halsey Thickness Curve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-14
Kelvin Equation with Harkins and Jura Thickness Curve . . . . . . . . . . . . . . . . . . . . . . F-15
Kelvin Equation with Broekhoff-de Boer Thickness Curve . . . . . . . . . . . . . . . . . . . . F-16
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-17

1. INDEX

Smart VacPrep Operator Manual

239-42828-01 - Nov 2013 vii


Table of Contents Gemini VII

viii 239-42828-01 - Nov 2013


Gemini VII Introduction

1. GENERAL INFORMATION

Introduction
This manual provides details on software installation, program menu options and operating instruc-
tions. This chapter contains information on the Gemini VII hardware and software components.

To help you use the analyzer system more efficiently, reference:

• Chapter 2, USER INTERFACE - prior to operating the analyzer and software

• Chapter 3, OPERATING PROCEDURES - for step-by-step instructions for common operations

• Chapter 4, SOFTWARE AND SETUP MODIFICATIONS - for instructions on software updates


and modifying analyzer configurations

Organization of the Operator’s Manual


This operator’s manual is organized as follows:

Chapter Description

Chapter 1 GENERAL INFORMATION


Provides a general description, features and specifications of the analyzer, and
organization of the manual.

Chapter 2 USER INTERFACE


Provides instrument and software interface.

Chapter 3 OPERATING PROCEDURES


Provides step-by-step procedures for the operations available using the Gemini VII
program.

Chapter 4 SOFTWARE AND SETUP MODIFICATIONS


Provides instructions for installing software updates and modifying analyzer setup
configurations.

Chapter 5 FILE MENU


Provides a description of the File menu options and field and button definitions.

Chapter 6 UNIT MENU


Provides a description of the Unit menu options and field and button definitions.

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Organization of the Operator’s Manual Gemini VII

Chapter Description (continued)

Chapter 7 REPORTS MENU


Provides a description of the Reports menu options and field and button
definitions.

Chapter 8 OPTIONS MENU


Provides a description of the Options menu options and field and button
definitions.

Chapter 9 TROUBLESHOOTING AND MAINTENANCE


Provides user maintenance and service information.

Chapter 10 ORDERING INFORMATION


Provides ordering information for the Gemini VII program and analyzer system
components.

Appendix A FORMS
Provides a sample information worksheet used to assist in obtaining a sample
mass.

Appendix B ERROR MESSAGES


Provides a list of program error messages, causes and actions.

Appendix C CALCULATIONS
Provides calculations used in reports.

Appendix D ETHERNET CONFIGURATION


Provides information on configuring an Ethernet port.

Appendix E ANALYZING SAMPLES WITH TOTAL SURFACE AREA OF 1.0M2 OR


LESS
Provides information on analyzing samples with a total surface area of 1.0 m2 or
less.

Appendix F DFT MODELS


Provides information on DFT models.

Index INDEX
Provides quick access to a subject matter.

1-2 239-42828-01 - Dec 2012


Gemini VII Equipment Description

Conventions
This manual uses the icons shown below to identify notes of importance, warnings and cautions.

Notes contain important information pertinent to the subject matter.

Warnings contain information to help prevent actions that may cause personal injury.

Cautions contain information to help prevent actions that may damage the analyzer or
components.

Equipment Description

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Equipment Description Gemini VII

The Gemini VII Series analyzers are easy to use, fully automatic, and provide single and multipoint
surface area and pore size measurements. Three models are available: the Gemini 2390a, 2390p, and
2390t.

The Gemini 2390a and 2390p are enclosed in the same size cabinet. The only physical difference is the
Po (saturation pressure) tube which is installed on the Gemini 2390p, allowing continuous measure-
ment of the saturation pressure.

The Gemini 2390t is in a slightly larger cabinet allowing the use of a larger Dewar and longer sample
tubes for extended analyses. This model also is equipped with a Po tube.

Most features are available on all three models, with the exception of a continuous Po measurement
and some reports. Refer to the following table for a brief summary of some of the model reports and
features.

The basic function of the Gemini analyzers is to determine the surface area of solid materials. Analyses
are performed using a static volumetric technique in which the adsorptive flows into a tube containing
the sample and into a balance tube simultaneously. The internal volume and the temperature surround-
ing both tubes are maintained at identical conditions. The only difference is the presence of the sample
in the sample tube.

Feature 2390a 2390p 2390t

Single and multipoint BET surface area   

Langmuir surface area   

Automatically generated pressure tables with user-selected points   

Total pore volume   

t-Plot method micropore volume and area   

Analysis log   

Statistical Process Control (SPC) reports   

Horvath-Kawazoe data reduction   

BJH pore size distribution using adsorption isotherm  

BJH pore size distribution using desorption isotherm 

Continuous measurement of saturation pressure (Po)  

Dubinin reports   

1-4 239-42828-01 - Dec 2012


Gemini VII Equipment Description

Feature (continued) 2390a 2390p 2390t

MP-Method reports   

DFT reports   

Operation
The sample and balance tubes are immersed in a single liquid nitrogen bath which maintains isother-
mal conditions for both tubes. The analysis gas is then delivered to the sample tube by a servo valve
mechanism. The delivery rate of analysis gas flow into the balance tube is controlled by another servo
valve connected to a differential pressure transducer. This differential pressure transducer measures the
pressure imbalance between the sample and balance tubes, which is caused by the adsorption of the
analysis gas onto the sample. As the sample adsorbs analysis gas, the pressure drops in the sample
tube. The servo valve continuously restores the pressure balance between the two tubes by admitting
more gas into the sample tube. The end result is that the Gemini maintains a constant pressure of anal-
ysis gas over the sample while varying the rate of analysis gas delivery to match exactly the rate at
which the sample can adsorb the gas.

The Gemini provides rapid and accurate sample analysis. As many as 50 data points can be collected
and reported in the BET, Langmuir, or t-Method range. The 2390p model of the Gemini VII Series can
report discrete point adsorption isotherms consisting of up to 1,000 adsorption points and, with the
Gemini 2390t, up to 1,000 adsorption and desorption isotherm points.

The Gemini requires only pure nitrogen as the analysis gas, even for most low surface area samples.
The analyzer requires no flow regulator, gas mixer, or mixed gases to operate. Surface areas as low as
0.01 m2/g are easily determined with excellent precision using nitrogen gas as the adsorbate. Option-
ally, helium may be used to determine any slight differences in volume between the balance tube and
the sample tube (differential free space). The Gemini uses this information to automatically compen-
sate even for these small differences in calculating analysis results.

The design of the Gemini avoids many errors which may occur with other surface area analysis
equipment:

• Any free space associated with the sample tube is offset by an identical amount in the balance tube.

• Any thermal gradient in the coolant bath is the same for both the sample and balance tubes and
produces a net effect of zero.

• Non-ideal gas behavior occurs in both the sample and balance tubes, cancelling negative effects on
sample analysis.

• Gas-mixture separation, which may occur in flowing-gas systems due to thermal diffusion, cannot
occur because mixed gases are not used.

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Equipment Description Gemini VII

Cryogen
Liquid nitrogen is used as the cryogen to cool the sample during analysis. An easy-to-use liquid nitro-
gen transfer system, the Model 021, eliminates the need to pressurize storage Dewars.

Degasser
Micromeritics has the following degassing units available for preparing samples:

• SmartPrep 065

The SmartPrep uses flowing-gas to remove adsorbed contaminants from the sample surface and
pores. It contains six sample ports, each one independently controlled for greater flexibility. It
contains two serial ports, one for connecting to the computer and a second for connecting an
additional SmartPrep. Up to four SmartPreps can be connected in sequence allowing the capability
of up to 24 preparation ports at one time.

The SmartPrep also can be controlled through the analyzer application and is the recommended
degassing unit for the analyzer.

• VacPrep 061

The VacPrep degasses up to six samples at up to 400 ºC with either flowing gas or evacuation.

• FlowPrep 060

The FlowPrep degasses up to six samples at up to 400 ºC with flowing gas.

Refer to ORDERING INFORMATION, page 10-1.

Vacuum Pump
An external vacuum pump equipped with an anti-suckback valve is required for sample analysis with
the Gemini analyzer. Any vacuum source achieving vacuums better than 20 x 10-3 mmHg at the instru-
ment inlet may be used.


A device to reduce oil vapor backstreaming is recommended.

The vacuum pump used with the Gemini must have an anti-suckback valve to prevent
oil from being admitted to the instrument should the power fail while the system is
under vacuum. Pumps available from Micromeritics are equipped with an anti-
suckback valve.

An oil-based or oil-free vacuum pump can be used with the Gemini analyzer. Appropriate vacuum
pumps are available from Micromeritics. Refer to ORDERING INFORMATION, page 10-1.

1-6 239-42828-01 - Dec 2012


Gemini VII Software

Software
The Gemini VII program allows other computer applications to run while an automatic operation is in
progress. The Help menu provides access to the online manual and instructional videos on using the
software.

The Gemini VII program offers a Windows interface with an easy way to collect, organize, archive and
reduce raw data and store sample information files for later use. The reports can be generated to
screen, paper, or exported for use in other applications. Cut and paste graphics, scalable and editable
graphs, and customized reports are easily generated.

User-defined Reports
Report options can be specified when creating the sample information file. When an analysis is run,
data gathered during the analysis process are compiled into the predefined reports. Reports can also be
defined and generated after an analysis has been run. Each selected report is displayed on its own tab
and reflects data collected during the analysis.

Report Features
• After analysis, reports can be viewed, printed, and/or copied and pasted into other documents.
• The report zoom feature provides the viewing of fine graph details and the ability to shift the axes.
• Reports can be customized with a choice of fonts and a logo added to the report header.

Gases
Compressed gases are required for sample analysis with the Gemini analyzer. Gas bottles and a rack
for storage of these bottles should be located near the analyzer. As an alternative, outlets from a central
source may be provided nearby. Gas sources must be able to supply flow rates of 4 liters per minute at
15 psig (103.4 kPa).

Appropriate two-stage regulators which have been leak-checked and specially cleaned are required.
Pressure relief valves should be set to no more than 30 psig. Gas regulators are available from
Micromeritics. Refer to ORDERING INFORMATION, page 10-1.

When helium is used for differential free-space measurement and nitrogen is used as the adsorbate gas,
they should be of the following purity or better:

• Helium - purity of 99.9% (For analysis of materials with very low surface areas, Micromeritics
recommends use of helium with purity of 99.995%.)

• Nitrogen - purity of 99.9% (For analysis of materials with very low surface areas, Micromeritics
recommends use of nitrogen with purity of 99.995%.)

239-42828-01 - Dec 2012 1-7


Specifications Gemini VII

Specifications
The analyzer has been designed and tested to meet the following specifications:

Characteristic Specification

Applicability

Surface Area: From 0.1 m2, total


From 0.01 m2/g, specific

Pore Volume: From 4 × 10-6 cm3/g

Pressure Measurement

Pressure Measurement 0 to 950 mmHg


Range:

P/Po Resolution: < 10-4

Relative Pressure Range: 0 to 1.0 P/Po (adsorption only)

Pressure Resolution: < 0.1 mmHg

Accuracy and Linearity: Better than ± 0.5% (full scale)


(Transducer manufacturer’s specification)

Vacuum System

External: Vacuum source achieving 20 × 10-3 mmHg (or better) at the instrument
inlet for oil-based or oil-free pumps.
For oil-based pumps, an anti-suckback valve is required to prevent oil
from being admitted into the Gemini should there be a power failure. A
device to reduce oil vapor backstreaming is also recommended.

Environment

Temperature: 10 to 35 ºC (50 to 96 ºF) operating


0 to 50 ºC (32 to 122 ºF) non-operating

Humidity: 20% to 80% relative, non-condensing

1-8 239-42828-01 - Dec 2012


Gemini VII Specifications

Characteristic Specification (continued)

Sample Tubes / Dewar

Standard Tube: • Gemini VII 2390a and 2390p


3/8 in (0.95 cm) OD, 6.1 in (15.5 cm) long with 6.5 cm3 of volume.
Sample capacity is approximately 2.0 cm3.

• Gemini VII 2390t: 3/8 in 


(0.95 cm) OD x 8.1 in (20.5 cm) long with 8.9 cm3 of volume.
Sample capacity is approximately 2.0 cm3.

Dewar: 8 hours; Gemini VII 2390a and 2390p 


> 24 hours; Gemini VII 2390t

Electrical

Voltage: 85 to 265 VAC

Power: 150 VA maximum

Frequency: 50 to 60 Hz

Gases

Adsorbate: Optimized for nitrogen in a liquid nitrogen sample bath. Gemini may
be used with non-corrosive adsorbate gases having vapor pressures at
both room and bath temperatures that are acceptably high relative to
the resolution of the 1,000 mmHg pressure transducer. Typically,
oxygen, argon, carbon dioxide, butane, methane, and other light
hydrocarbons will produce useful data above absolute pressures of a
few mmHg.

Physical

Height: 23 in (58 cm); Gemini VII 2390a and 2390p


29 in (74 cm); Gemini VII 2390t

Weight: 16 in (40 cm)

Depth: 20 in (51 cm)

239-42828-01 - Dec 2012 1-9


Specifications Gemini VII

Characteristic Specification (continued)

Computer

Minimum Requirements: • 1 GHz or faster 32-bit (x86) or 64-bit (x64) processor


• 2 GB RAM
• 40 GB minimum hard drive (formatted in NTFS) (one partition)
• Video Adapter capable of 1024 × 768 minimum resolution
• One RS-232 serial port
• Two USB ports
• One 10 BaseT Ethernet port (can be 10/100)
• CD-ROM drive
• Microsoft Windows 7 Professional
• Microsoft Vista **

** Windows 7 Professional is recommended for the best user


experience.

1-10 239-42828-01 - Dec 2012


Gemini VII Introduction

2. USER INTERFACE

Introduction
This chapter contains information on the analyzer hardware and software components of the 
Gemini VII.

• Shortcuts
• File name conventions
• Menu Structure

Instrument Components and Connectors

Component Description

Power indicator Blinks when power is applied to the analyzer; illuminates when analysis
program is initiated and ready for operation.

Sample compartment  Sliding door encloses the sample compartment.


door

239-42828-01 - Dec 2012 2-1


Instrument Components and Connectors Gemini VII

Front Panel

Power
Indicator

Sample compartment
door

Component Description

Power indicator Blinks when power is applied to the analyzer; illuminates when analysis
program is initiated and ready for operation.

Sample compartment  Sliding door encloses the sample compartment.


door

2-2 239-42828-01 - Dec 2012


Gemini VII Instrument Components and Connectors

Sample Compartment
Po port and tube (2390p and 2390t models)

Balance Port Sample port

Diagram of tube positions

Elevator

Component Description

Sample port For installing the sample tube.

Balance port For installing the balance tube.

Po port and tube The Po (saturation pressure) tube comes installed on the Gemini II 2390p
and 2390t.

Diagram Diagram of port numbers and locations as well as the positions of the
balance and sample tubes. The empty tube represents the balance tube
installed on the left port. The filled tube represents the sample tube
installed on the right port.

Elevator Allows placement of the Dewar around the sample and Po tubes. The
elevator raises automatically when the analysis is started and lowers
automatically upon completion. During analysis, the elevator lowers after
the free-space measurement to allow evacuation, then raises and continues
the analysis.

239-42828-01 - Dec 2012 2-3


Instrument Components and Connectors Gemini VII

Rear Panel

Helium inlet port

Adsorptive inlet port

Vacuum pump connector

Keypad connector

Ethernet port

USB ports

RS232 connector

On/Off Switch

Power connector

Component Description

Helium inlet port For attaching the helium gas supply.

Adsorptive inlet port For attaching the adsorptive (analysis) gas supply.

Vacuum pump For attaching the vacuum pump hose.


connector

Keypad connector Not used with the for Gemini VII version.

Ethernet port For connecting an Ethernet cable for communication between the analyzer
and the computer.

USB ports Not used with the Gemini VII version.

RS-232 connector Used by service personnel to perform calibration procedures.

On/Off switch For turning the analyzer on and off.

Power connector For connecting the analyzer to the power supply.

2-4 239-42828-01 - Dec 2012


Gemini VII Turning the Analyzer On and Off

Turning the Analyzer On and Off

Turning the Analyzer On


1. Place the computer, monitor and printer ON/OFF switches in the ON position.

2. Place the analyzer ON/OFF switch in the ON position. The pump will turn on automatically if it is
plugged into the electrical outlet.

Do not turn off the analyzer while initialization is in progress. Doing so may damage the
instrument.

3. Turn on the pump. The pump must warm for approximately two hours before performing
analyses. For analyses that require very precise results, allow the analyzer to warm up while the
sample is being prepared.

Turning the Analyzer Off


Always exit the analysis program before turning off the computer. Failure to do so
could result in loss of data.

It is recommended that the analyzer be powered on at all times. If it does become necessary to turn it
off, perform the following steps:

1. Select File > Exit from the analyzer program (or use the Alt+F4 keyboard shortcut).

If an analysis is in progress, the following message is displayed:

2459- An Instrument is busy. A delay in restarting this


application could result in loss of new data. Continue
program exit?

Yes No

Select Yes and the analysis program closes. The analysis continues and data continue to be
collected. Queued reports under the print manager will print. If a power failure occurs and an
uninterruptible power supply (UPS) is not attached to the analyzer, the data collected after exiting
the analysis program are lost.

2. Place the computer, monitor and printer ON/OFF switches in the OFF position.

3. Place the analyzer ON/OFF switch in the OFF position.

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Using the Software Gemini VII

Using the Software


The analysis program operates in the Windows environment and requires familiarity with standard
Windows operations, for example, using the mouse, menus and dialog boxes. While this manual pro-
vides brief instructions for such standard operations, if necessary, refer to Windows documentation or
its online help system to clarify any Windows functions.

Shortcut Menus
Shortcut menus are available for:

• the instrument schematic when Manual Control is enabled. Refer to


Enable Manual Control, page 6-8.

• onscreen graphs and tabular reports. Refer to Report Shortcut Menus, page 7-17.

Shortcut Keys
Shortcut keys can be used to activate some menu commands. Shortcut keys or key combinations (when
applicable) are listed to the right of the menu item.

Another shortcut method of accessing a menu or function is to use the Alt key plus the underlined let-
ter in the menu command. For example, to access the File menu, press Alt + F. Then press the
underlined letter on the submenu. For example, Alt + F opens the File menu; then press O to access the
Sample Information file option.

If the underscored letters do not display menus and dialogs, press the Alt key on the
keyboard.

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Gemini VII Using the Software

Shortcut Key(s) Function

F1 Access online operator’s manual

F2 Open a sample information file

F3 Open an analysis conditions file

F4 Open an adsorptive properties file

F5 Open a report options file

F6 Cascade windows

F7 Tile windows

F8 Start a report

F9 Close all open reports

F10 Generate a Heat of Adsorption report

Alt + F4 Exit the program

Shift + F2 List sample information files

Shift + F3 List analysis conditions files

Shift + F4 List adsorptive properties files

Shift + F5 List report options files

Shift + F9 Access shortcut menu of (1) selected component on instrument


schematic, or (2) onscreen reports

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Using the Software Gemini VII

Files

File Status and Description


In the Open File window, the Mic Status column and the Mic Description column display file status
and file description, respectively. Columns can be sorted by clicking the column header.

File Status Description

All All sample information files in the specified directory.

Analyzing Sample information files that are currently being used for analysis.

Complete Sample information files used in an analysis that has been completed.

Entered Sample information files containing manually entered data.

No Analysis Sample information files which have not been used to perform an analysis.

Prepared Sample information files used in an automatic degas operation but not for an
analysis.

Preparing Sample information files currently being used in an automatic degas operation.

File Name Conventions


For sample information files, a default file name (the next available sequence number) and a default
extension display. For Sample tube, Degas conditions, Analysis conditions, Adsorptive properties and
Report options, only a default extension displays.

The following table lists the default file extensions assigned to files in the Gemini VII
program:

File Type Default File Name Extension

Sample information .SMP

Sample tube .STB

Degas conditions .DEG

Analysis conditions .ANC

Adsorptive properties .ADP

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Gemini VII Menu Structure

File Type (continued) Default File Name Extension

Report options .RPO

Heat of Adsorption Report .HOA

Thickness curve .THK

Alpha-s curve .ALS

The following file types are available for reports saved from the Print window:

Report .REP

Spreadsheet .XLS

ASCII .TXT

Menu Structure
All program functions are located on menus accessed from the menu bar. Each menu contains com-
mands and, in some cases, a submenu. A submenu is indicated when the command is followed by an
arrow.
A SmartPrep menu option
displays on the menu bar if a
SmartPrep unit is used
with the analyzer.

Arrow indicates
a submenu is
available

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Menu Structure Gemini VII

Main Menu Bar


All functions are accessed from the main menu bar. The following table contains brief menu descrip-
tions and their locations:

Menu Item Description

File Use to manage files. Refer to FILE MENU, page 5-1.

Unit [n] Use to perform analyses, calibrations and other instrument operations.
Refer to UNIT MENU, page 6-1.

SmartPrep Displays only if a SmartPrep degassing unit is installed on the analyzer.


The options contained on this menu are explained in the SmartPrep
operator’s manual.

Reports Use to run reports and view the results. Refer to REPORTS MENU, page
7-1.

Options Use to edit sample defaults, specify system configuration and data
presentation formats. Refer to OPTIONS MENU, page 8-1.

Window Use to arrange the windows and icons on the computer screen and display
a list of open windows. Refer to Window Menu, page 2-11.

Help Use to access online operator’s manual, Micromeritics web page, and
videos. Refer to Help Menu, page 2-12.

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Gemini VII Menu Structure

Window Menu
The Window menu lists open files and provides the ability to rearrange the way open windows display.
A check mark appears to the left of the active window.

Window Menu
Description
Option

Cascade Stacks open windows in a fanned format so that each window title bar is
visible. F6 can also be used as a keyboard shortcut.

Tile Resizes open windows and arranges them horizontally so that multiple
windows can be viewed at once. F7 can also be used as a keyboard
shortcut.

Arrange Icons Arranges the symbols for all minimized windows.

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Menu Structure Gemini VII

Help Menu
The Help menu provides access to the online operator’s manual, the Micromeritics web page, online
instructional videos, and information about the analyzer.

Help Menu Option Description

Operator’s Manual Provides access to the online operator’s manual.

Micromeritics on the Provides a link to the Micromeritics web page: 


Web www.Micromeritics.com

Gemini VII on the Provides an Internet link to additional Gemini VII information: 
Web Gemini VII on the Web

Available Videos How To Prepare Samples


• Cleaning Sample Tubes
• Determining Sample Mass
• Degassing the Sample

How to Install Sample Tubes


How to Prepare a Dewar
How to Perform A Reference Analysis
• Creating a Reference Material Sample File
• Analyzing Reference Material

Evaluating Data

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Gemini VII Menu Structure

Help Menu Option Description (continued)

Available Videos Maintenance


(continued)
• Guidelines for Choosing Regulators
• Guidelines for Connecting Gases
• Connecting Gases
• Cleaning and Verifying Gas Lines
• Inspecting and Changing Vacuum Pump Oil
• Inspecting and Changing Alumina
• Changing the Vacuum Pump Exhaust Filter

About Gemini VII Provides the analysis program version number.

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Menu Structure Gemini VII

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Gemini VII Introduction

3. OPERATING PROCEDURES

Introduction
This chapter contains information on:

• specifying sample defaults


• creating sample files in Advanced, Basic and Restricted formats
• preparing samples and performing an analysis
• printing file contents, listing file statistics, exporting isotherm data, and converting sample files
• generating graph overlays

Specifying Sample Defaults


Sample information files include the information required by the analyzer to perform analyses and col-
lect data. When a sample information file is created, the system assigns the default values specified in
either Advanced or Basic format.

Format Description

Advanced Displays all parts of sample information and parameter files. Navigate to
parameter screens by clicking the tabs across the top of the window.

Basic Displays the entire sample information file in a single window with no tabs
across the top. This option is used once the parameter files have been created.
The previously entered or default parameter files are then accessible using
dropdown lists.

Restricted Displays the sample information file in a single window similar to the Basic
format with certain functions disabled. The Restricted format requires a
password when entering or exiting the Restricted format. It is typically used in
laboratories where analysis conditions must remain constant, for example, in the
pharmaceutical industry. The Advanced format is not available from the
Restricted format.

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Specifying Sample Defaults Gemini VII

Advanced Format
The values specified in the parameter portions of the default sample file (Degas Conditions, Analysis
Conditions, Adsorptive Properties, and Report Options) are saved as the defaults for new sample files.
To navigate from one set of parameters to another, click the parameter tab at the top of the window.

Perform the following steps to establish defaults for a sample information file in the Advanced format.

1. Go to Options > Sample Defaults.

2. In the Sequence Number alpha/numeric text box, specify a default file name string. The
Sequence Number field must contain a minimum of three (3) numbers. This number is
incrementally sequenced and displays in the File name text box in the File > Open > Sample
Information window.

3. The text box to the right of the Sample field, is used to enter a format for the sample
identification. Include the $ symbol to automatically include the Sequence Number field text as
part of the sample identification.

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Gemini VII Specifying Sample Defaults

4. Enter Operator, Submitter and Bar Code identification information in the respective text boxes.
To omit the field and information in the sample files, select the Omit checkbox to the right of the
field.

The field labels for the Sample, Operator, Submitter and Bar Code fields can be modified
by overwriting the default field labels.

5. In the Mass group box, enter default values for the sample’s mass and density. Both of these
values may be edited at the time of analysis. Refer to Sample Information Files, page 5-8.

6. In the Type of Data group box, select if data are to be automatically collected or manually
entered.

7. The optional user-defined fields in the User Parameters group box may be used to enter and
track information from another instrument or source, along with other statistical process control
data. Refer to Sample Information Files, page 5-8 .

8. After completing the Sample Description window, click the parameter tabs to edit other sample
information file parameters. The saved parameter defaults become the defaults for new parameter
files.

9. Click Save, then click Close.

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Specifying Sample Defaults Gemini VII

Basic Format
When specifying defaults in the Basic format, select from existing default parameters. The defaults
established in Basic format also serve as defaults for files created using the Restricted format.

To define parameter files before entering sample defaults in Basic format, refer to Defining Sample
Information Files, page 3-6.

Perform the following steps to establish defaults for a sample information file in the Basic format.

1. To change to Basic format, go to Options > Option Presentation > Basic.

2. Go to Options > Sample Defaults.

3. In the Sequence Number alpha/numeric text box, specify a default file name string. The
Sequence Number field must contain a minimum of three (3) numbers. This number is
incrementally sequenced and displays in the File name text box in the File > Open > Sample
Information window.

4. The text box to the right of the Sample field, is used to enter a format for the sample
identification. Include the $ symbol to automatically include the Sequence Number field text as
part of the sample identification.

The field label for the Sample field can be modified by overwriting the default field label.

5. In the Mass group box, enter default values for the sample’s mass and density. Both of these
values may be edited at the time of analysis. Refer to Sample Information Files, page 5-8.

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Gemini VII Specifying Sample Defaults

6. Select the dropdown arrow to the right of the Degas conditions, Analysis conditions, Adsorptive
properties, and Report options fields to select default parameter files that were saved while in
Advanced format and saved to the directory specified in Options > Parameter Files Directory.

7. Click Save, then click Close.

Restricted Format
Restricted format presents the sample information file in the same manner as the Basic format except
that the operator cannot switch to Advanced format. This format is password protected and is typically
used in laboratories where sample parameters must remain constant, for example, in pharmaceutical
laboratories.

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Defining Sample Information Files Gemini VII

Defining Sample Information Files


A sample information file must be created for each analysis. This file can be created in advance or at
the time of analysis. The sample information file identifies the sample, guides the analysis and speci-
fies report options.

A sample information file may be created in Restricted, Basic or Advanced format.

Advanced Format
1. Go to File > Open > Sample Information or use the F2 keyboard shortcut.

2. Accept the next sequenced file number or enter a new name in the File name text box. Click
Open.

3. Click OK to create the file.

Some text boxes


may not display if
omitted in Sample
Defaults.

4. Enter a sample description in the Sample text box.

5. Enter Operator, Submitter and Bar Code identification information in the respective text boxes.

6. In the Mass group box, enter default values for the sample’s mass and density. Both of these
values may be edited at the time of analysis. Refer to Sample Information Files, page 5-8.

7. In the Type of Data group box, select if data are to be automatically collected or manually
entered.

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Gemini VII Defining Sample Information Files

8. If SPC (Statistical Process Control) information is to be reported, enter appropriate information in


the User Parameters group box. These are user-definable parameters that can be entered and
tracked along with other statistical process control data.

9. After completing the Sample Description window, click the parameter tabs to edit other sample
information file parameters.

10. Click Save, then click Close.

Basic or Restricted Format


The Basic and Restricted formats use predefined parameter files to create a sample file. Refer to Spec-
ifying Sample Defaults, page 3-1.

• If using the Basic format, switch to the Advanced format to edit parameter file values.
• If using the Restricted format, parameter files cannot be edited. 

1. Go to File > Open > Sample Information or use the F2 keyboard shortcut.

2. In the File name field, accept the next sequenced file number or enter a new file name. Click
Open.

3. Click OK to create a new file. If Advanced displays in the dropdown list at the bottom of the
window and there are tabs across the top of the window, click the Advanced dropdown arrow and
select Basic to change to Basic format. If Advanced does not show in the dropdown list, then you
are in Restricted format.

The Restricted
format does not
show an
Advanced option.

4. In the Sample field, enter a sample description.

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Defining Sample Information Files Gemini VII

5. In the Mass group box, enter default values for the sample’s mass and density. Both of these
values may be edited at the time of analysis. Refer to Sample Information Files, page 5-8.

6. Click the dropdown arrows to select default parameter files for Degas conditions, Analysis
conditions, Adsorptive properties, and Report options.

If there is an existing sample file containing the values to be used in the current sample
file, click Replace All to choose the file and copy the values into the current file.

7. Click Save, then click Close.

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Gemini VII Defining Sample Information Files

Opening Sample Information Files


Be advised when working with an existing file that a copy of the file be used rather
than the original.

Opening Files with a Status of Complete, Analyzing, or Entered


1. Select File > Open > Sample Information.

2. To sort the file list by status, click the Mic Status column header. Select a file with a status of
Complete, Analyzing, or Entered and click Open (or double click the file name). The reporting
window displays.

3. Save the changes in the sample information file by clicking the Save button.

Opening Files with a Status of Preparing, Prepared, or No Analysis


1. Select File > Open > Sample Information.

2. To sort the file list by status, click the Mic Status column header.

3. Select the file to open in the Name column and click Open (or double click the file name).

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Defining Sample Information Files Gemini VII

4. The Sample Information window displays in the specified format (Advanced, Basic, or
Restricted). The following is shown in Advanced format.

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Gemini VII Defining Parameter Files

Defining Parameter Files


The following file types can exist as part of the sample information file as well as individual parameter
files:

• Degas conditions
• Analysis conditions
• Adsorptive properties
• Report options

Default parameter files can be used for multiple analyses without having to re-enter the values each
time an analysis is performed.

Predefined parameter files are included with the program and can be edited as needed or new parame-
ter files can be created. The Replace button can be used to replace values from an existing file to
overwrite values in the current file. Changes can be made as needed to the new file while the original
file remains unchanged.

New parameter files must be saved in the directory specified in Options > Parameter
Files Directory for the files to appear in dropdown lists in Basic and Restricted format.

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Defining Parameter Files Gemini VII

Degas Conditions
Degassing is a required step in preparation for the analysis; however, this section is
only applicable if using the SmartPrep Degasser. This section contains degassing
instructions that will be sent to the SmartPrep Degasser equipment.

Degas Conditions files contain degassing information for sample preparation.

1. Go to File > Open > Degas Conditions.

2. Enter a name in the File name text box. Click Open.

3. Click OK to create the file.

4. Enter a description in the Description text box.

5. Use the Insert button to enter up to five stages of degassing (soak temperature, ramp rate, and
soak time).

6. Click Save, then click Close. The file saves with a .DEG file extension.

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Gemini VII Defining Parameter Files

Analysis Conditions
Analysis conditions specify the data used to guide an analysis.

1. Go to File > Open > Analysis Conditions or use the F3 keyboard shortcut.

2. Enter a name in the File name text box. Click Open.

3. Click OK to create the file.

4. Enter a description in the Description text box.

5. Indicate the points for the pressure table. Use the Insert, Delete, Clear, and Append buttons to
assist in entering data.

6. Click the following buttons to specify:

Button Use to Specify

Preparation evacuation rate / time and leak test values

Free space how the free space is to be measured

Po and T how the saturation pressure (Po) is to be measured and the


analysis bath temperature

Analysis Method to enter equilibration time in seconds or enter the minimum


equilibration time for scanning in minutes

7. Click Save, then click Close. The file saves with a .ANC file extension.

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Defining Parameter Files Gemini VII

Adsorptive Properties
Adsorptive properties provide the adsorptive (analysis gas) characteristics for the analysis.

1. Go to File > Open > Adsorptive Properties or use the F4 keyboard shortcut.

2. Enter a name in the File name text box. Click Open.

3. Click OK to create the file.

4. Enter a description in the Adsorptive text box (for example, the gas and the temperature).

5. Enter the mnemonic for the Adsorptive gas (for example, CO2) in the Mnemonic text box.

6. Enter information in the following text boxes:

• Non-ideality factor
• Density conversion factor
• Molecular cross-sectional area

7. Click Save, then click Close. The file saves with a .ADP file extension.

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Gemini VII Defining Parameter Files

Report Options
Report Options files specify the type of reports that will be generated from an analysis or from manu-
ally entered data. They also contain report details, for example, axis scale, axis range and column
headings. Report options files may contain tabular reports, plots, or both, as well as user-defined report
tables.

Report options files may be defined to include overlay options. This system allows the overlay of up to
eight plots of different samples onto a ninth plot of the same type or overlay one plot type onto a differ-
ent plot type from the same analysis. Refer to Generating Graph Overlays, page 3-35.

1. Go to File > Open > Report Options or use the F5 keyboard shortcut.

2. Enter a name in the File name text box. Click Open.

3. Click OK to create the file.

4. Enter a description in the Description text box.

5. Select Show report title and enter a title to appear on the report header. Deselect this option to
omit a report title.

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Preparing for Analysis Gemini VII

6. Select the Show graphic checkbox to insert a graphic in the report header. Use the Browse button
to locate a .BMP or a .EMF file. Specify the graphic size in the Height and Width text fields.
Deselect this option to omit a report graphic.

7. The Selected Reports list box displays the reports that may be generated.

a.) Select the checkbox to the left of the report to include in this file. A selected box displays a
checkmark in the box.

b.) To specify report options, highlight the report in the Selected Reports list box and click
Edit. Makes changes as necessary. Click OK.

8. Click Save, then click Close. The file saves with a .RPO file extension.

Preparing for Analysis


The following table outlines the tasks to properly prepare for an analysis and the location of the task
procedure. It is recommended to perform the tasks in the following order:

Task Name and Location

Clean the sample tube Cleaning and Labeling Sample Tubes, page 3-17

Create the sample file Defining Sample Information Files, page 3-6

Weigh the sample Determining the Sample Mass, page 3-18

Degas the sample Degassing the Sample, page 3-20

Load sample on sample port Installing the Sample Tube, page 3-21

Fill Dewar and check LN2 level Installing the Analysis Dewar, page 3-22

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Gemini VII Preparing for Analysis

Cleaning and Labeling Sample Tubes


Sample tubes and filler rods must be clean and dry before samples are added and weighed. The follow-
ing table indicates which materials are supplied by Micromeritics and which are supplied by the user.
The procedures following the table are recommended.

Materials Supplied by Micromeritics Materials Supplied by User

• Sample tube • Drying oven


• Filler Rod (if used) • Ultrasonic cleaning unit
• Sample tube brush • Detergent
• Stopper for sample tube • Rubber gloves or lint-free cloth
• Sample tube rack • Acetone or isopropyl alcohol
• Sample weighing support • Safety glasses
• Sample data worksheet (copied from Appendix A • Waste container
of this manual) • Analytical balance
• Pipe cleaners

1. Preheat drying oven at 110 ºC.

2. Verify that the ultrasonic cleaning unit is clean.

3. Use 5 grams of Alconox (or other suitable detergent) per 500 mL of warm water and fill the
ultrasonic unit with enough water to cover the sample tubes and filler rods (if used). Ensure the
detergent is dissolved before placing the sample tubes and filler rods into the water. If too much
detergent is used, it may be difficult to rinse from the sample tubes.

4. Fill the sample tubes with warm water and place them in the ultrasonic cleaning unit. Then place
the filler rods in the unit. Turn on the ultrasonic cleaning unit for approximately fifteen minutes.

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Preparing for Analysis Gemini VII

5. Use rubber gloves to ensure no oils or residue are transferred to the clean tubes and filler rods and
remove the sample tubes and filler rods from the unit.

6. Clean the interior of the sample tubes with the brush supplied with the system.

7. Rinse the sample tubes and filler rods thoroughly with hot water. Then rinse again with isopropyl
alcohol or acetone. If isopropyl alcohol or acetone is not available, deionized water may be used.

8. Stand the sample tubes on the sample tube rack and place the filler rods in a basket or in the rack.
Bake in a vacuum oven for two hours at 110 °C.

9. Remove the sample tubes and filler rods from the oven and allow to cool.

Do not insert the filler rods at this time. Filler rods are inserted just before the sample
tube is installed on the analysis port.

10. Wipe a rubber stopper with a lint-free cloth.

11. Label the sample tube and stopper for identification.

Determining the Sample Mass


Analysis results are expressed in units of surface area per gram of sample; therefore, it is important the
true sample mass be known. The true mass is best calculated as:

• weigh the empty Sample Tube Set (sample tube and stopper or seal frit) before degas

• weigh the Sample Tube Set with sample before degas and subtract the weight of the empty Sample
Tube Set

• weigh the Sample Tube Set with sample after degas and subtract the weight of the empty Sample
Tube Set

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Gemini VII Preparing for Analysis

• weigh the Sample Tube Set with sample after analysis and subtract the weight of the empty Sample
Tube Set

A FORMS for recording the weights and calculating the mass is included in Appendix A. Make copies
as needed.

Use a copy of the Sample Data Worksheet to record the following:

1. Record the Sample Tube Identification.

2. Place the sample weighing support on the balance. Tare the balance and allow it to stabilize at
zero (0).

3. Place the sample tube set on the sample weighing support and place it on the balance.

4. Record the stabilized weight on the Sample Data Worksheet as [A] Mass for empty sample tube
set. Remove the sample weighing support and sample tube set from the balance.

Do not touch the sample with bare hands while performing the following steps. Doing
so could affect the accuracy of results.

5. Place a sample container on the balance and slowly pour the sample into the container.

6. Remove the rubber stopper (or seal frit) from the sample tube.

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Preparing for Analysis Gemini VII

7. Use the sample tube funnel (provided in the accessories kit) and pour the sample from the
weighing container into the sample tube.

Funnel

8. Replace the rubber stopper (or seal frit).

9. Weigh the sample tube set containing the sample and record the value on the Sample Data
Worksheet as [B] Sample tube set plus sample mass (Before Degas).

10. Subtract the [A] Mass for empty sample tube set from the [B] Mass of sample tube set plus sample
and record this value as the [C] Sample mass (Before Degas).

Degassing the Sample


After the sample has been weighed, use a degassing unit to remove any contaminants which may have
adsorbed to the surface or pores. Appropriate degassing units are available from Micromeritics. Refer
to ORDERING INFORMATION, page 10-1 for ordering information.

If using the SmartPrep degasser, a menu displays on the program menu bar. Degas the sample using
menu commands and information entered in the Degas Conditions window. Refer to the SmartPrep
operator’s manual for operating instructions.

After degassing is complete, perform the following steps:

1. Weigh the sample tube set containing the sample and record the weight on the Sample Data
Worksheet as [B] Sample tube set plus sample mass (After Degas).

2. Subtract the [A] Mass for empty sample tube set (Before Degas) from the [B] Sample tube set plus
sample mass (After Degas) to obtain the sample’s mass. Record this value as [C] Sample mass
(After Degas).

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Gemini VII Preparing for Analysis

Installing the Sample Tube


Follow the steps below to attach the sample tube to the analysis port and the balance tube to the bal-
ance port. Minimize sample exposure to air by completing the steps quickly.

1. Remove the sample tube stopper.

2. Place the connector nut, ferrule, and O-ring onto the sample tube stem.

O-ring

Ferrule

Connector nut

Sample tube

The sample tube ferrule is tapered slightly on one end. The ferrule may be installed onto the
sample tube with the tapered end in the up or down position.

If analyzing samples with a surface area of 1.0 m2 or less, use filler rods in the sample
and balance tubes. Refer to ANALYZING SAMPLES WITH TOTAL SURFACE
AREA OF 1.0M2 OR LESS, page E-1.

3. Attach the sample tube to the analysis port. Ensure it is fully in the port. Secure it in place by
screwing the connector nut onto the analysis port. Hand-tighten the connector nut.

4. If the balance tube is not installed, attach it to the balance port following the above procedures. If
a filler rod was used in the sample tube, one must be used in the balance tube.

It is not necessary to remove and replace the balance tube between analyses unless it
has been contaminated or if using a different size sample tube.

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Preparing for Analysis Gemini VII

5. Place the Dewar cover under the sample and balance tubes and slide upward until it is three inches
from sample nuts.

Installing the Analysis Dewar


Prepare the analysis Dewar after installing the sample tube.

Always handle glass Dewars with care. Any product incorporating a vacuum is a
potential safety hazard and should be treated with caution. Always observe the
precautions listed below.

When handling Dewars containing liquefied gases:

• Wear protection by using:


– goggles (or a face shield)
– an insulated or rubber apron
– insulated gloves

• When pouring liquefied gases from one container to another:


– cool the receiving container gradually to minimize thermal shock
– pour the liquefied gas slowly to prevent splashing
– vent the receiving container to the atmosphere

For glass Dewars:

• Use a plastic stirring rod when stirring substances in a Dewar containing liquefied gases (or other
materials of extremely low temperature). Do not use a glass or metal stirring rod unless it has a
protective coating.

• Do not remove the mesh covering from the Dewar flask. This covering helps to maintain a secure
grip on the Dewar.

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Gemini VII Preparing for Analysis

• Do not handle heavy objects above the Dewar. If unavoidable, place a protective cover over the
Dewar’s opening. If an object of sufficient weight is accidentally dropped into the Dewar, shattering
may occur.

For stainless steel Dewars:

• Use a plastic stirring rod when stirring substances in a Dewar containing liquefied gases (or other
materials of extremely low temperature).

• Do not handle heavy objects above the Dewar. If unavoidable, place a protective cover over the
Dewar’s opening.

To install the analysis Dewar:

1. Place the analysis Dewar onto the elevator.

2. Fill the Dewar with the analysis bath liquid (liquid nitrogen):

• Large Dewar - fill to about 5 cm (2 in) from the top.


• Small Dewar - fill to about 2 cm (3/4 in) from the top.

Incorrect fluid levels can lead to measurement errors. Check the level of the bath liquid
before each analysis.

3. Insert the dipstick into the Dewar and check the level of the analysis bath liquid. Condensation
should not exceed the Level Indicator mark.

Level indicator mark

Wetness or frozen 
condensation indicates
bath liquid level

4. For best results, if the Dewar has not been in use for a while, allow approximately 30 minutes for
the temperature of the Dewar to stabilize with the bath liquid. Then recheck the level of the bath
liquid. Add additional liquid if necessary.

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Performing an Analysis Gemini VII

Dewar support
(not used with
Gemini VII 2390t)

A Dewar support is not necessary for the larger Dewar used with the Gemini VII 2390t. Place the
Dewar directly on the elevator.

5. Close the sample compartment door.

Performing an Analysis
Begin analysis after the sample has been degassed and transferred to the analysis port. The system pro-
vides these types of analyses:

• Start Analysis (standard) - allows a single sample analysis


• QuickStart Analysis - allows multiple sample analyses using the same analysis conditions
• Blank Analysis - allows an analysis with an empty tube

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Gemini VII Performing an Analysis

Start Analysis
Ensure the analyzer compartment door is closed before beginning an analysis. If the
analyzer is operated at an excessive pressure, the sample or balance tube could
become dislodged from its port, possibly causing personal injury or damage to the
equipment.

1. Select Unit [n] > Start Analysis.

2. Click Browse to select a sample information file or accept the next sequenced number.

3. Verify the information populated into the sample identification, density and mass fields. This
information is pulled from the selected file. The density value is applicable only if using the
Calculate method for the free space determination.

4. Click Report after analysis to automatically generate reports when the analysis is complete. On
the Report Settings window, select the report destination. Click OK.

5. Click Start to start the analysis. A window displays data as they are collected. A short delay is
encountered before the port status changes from the Idle state at the bottom of the screen.

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Performing an Analysis Gemini VII

6. When the analysis is complete, remove the sample tube and store (or dispose) of the sample
material as applicable.

QuickStart Analysis
When using the QuickStart option, it is not necessary to prepare sample files in advance. Sample files
are assigned automatically and given default conditions. File contents can be replaced if necessary
using the Browse button.

1. Select Unit [n] > QuickStart Analysis.

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Gemini VII Performing an Analysis

2. File names are assigned automatically and given default conditions. To replace the parameters
with those in another sample information file, click Browse and select the sample file.

3. Verify the information populated into the sample identification, density, and mass fields. This
information is pulled from the selected sample file. The density value is applicable only if using
the Calculate method for the free space determination.

4. Click Report after analysis to automatically generate reports when the analysis is complete. On
the Report Settings window, select the report destination. Click OK.

5. Click Start to start the analysis. A window displays data as they are collected. A short delay is
encountered before the port status changes from the Idle state at the bottom of the screen.

6. When the analysis is complete, remove the sample tube and store (or dispose) of the sample
material as applicable.

Use caution when removing the sample tube if using a hanging filler rod. The sample
tube O-ring or Dewar cover may snag the filler rod retaining ring. Loosen the snag
gently; excessive force may break the tip of the filler rod.

Blank Analysis
Use this method to perform a blank analysis with no sample data. The blank analysis is used primarily
for diagnostic purposes to look for instrument problems. The blank analysis should result in zero
adsorptive. An amount other than zero could indicate a possible leak.

1. Open a new Sample Information file using Unit [n] > Blank Analysis.

2. Click Browse to select a sample information file.

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Generating Reports Gemini VII

3. Click Report after analysis to automatically generate reports when the analysis is complete. On
the Report Settings window, select the report destination. Click OK.

4. Click Start to start the analysis. A window displays data as they are collected. A short delay is
encountered before the port status changes from the Idle state at the bottom of the screen

When analysis is complete, remove the sample tube and store (or dispose) of the sample material as
applicable.

Use caution when removing the sample tube if using a hanging filler rod. The sample
tube O-ring or Dewar cover may snag the filler rod retaining ring. Loosen the snag
gently; excessive force may break the tip of the filler rod.

Generating Reports
Reports > Start Report > [file] (or use the F8 keyboard shortcut)

1. Select the report in the Name column. The selected report name appears in the File name text
box. To select more than one file, hold down the Ctrl key on the keyboard while selecting the
files. Click Open.

2. Select the report destination in the Report Settings window and click OK. Refer to Printing
Files, page 3-30.

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Gemini VII Generating Reports

3. If only one file was selected in step 1, the Select Reports window displays. Verify the reports to
generate and click OK. If multiple files were selected, this window does not display.

4. Click a tab across the top of the window to review each report.

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Printing Files Gemini VII

Printing Files
Provides the option to print the contents of one or more sample files to either the screen, a printer, or to
a file.

1. Go to File > Print > [file type] > [file].

2. From the Name column, select a file to print. To select more than one file, hold down the Ctrl key
on the keyboard while selecting the files. To sort a column, click the column header.

3. Click Open.

4. In the Report Settings window, select one of the following:

• Preview - to send the file to the screen.

• Print - to send the file to the default printer.

• Copies - select the number of copies to print. This field is only enabled when Print is selected.

• File - select the destination directory and enter a file name in the File name text box. Select to
save the file as a .REP, .XLS, or .TXT file format.

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Gemini VII Listing Files

5. Click Print. The following example shows a sample information file printed to the screen.

Listing Files
Provides the option to create a list of sample file information, for example, file name, date / time the
file was created or last edited, file identification and file status.

1. Go to File > List > [file type] > [file].

2. From the Name column, select a file to list. To select more than one file, hold down the Ctrl key
on the keyboard while selecting the files. To sort a column, click the column header.

3. Click List.

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Exporting Isotherm Data Gemini VII

4. In the Report Settings window, select one of the following:

• Preview - to send the file to the screen.

• Print - to send the file to the default printer.

• Copies - select the number of copies to print. This field is only enabled when Print is selected.

• File - select the destination directory and enter a file name in the File name text box. Select to
save the file as a .REP, .XLS, or .TXT file format.

5. Click OK. The following example shows a sample information file printed to the screen.

Exporting Isotherm Data


Provides the option to export isotherm data in a.TXT or .XLS file format. When saved to a file, the
data can be imported into other applications that read .TXT or .XLS file formats. The output file con-
tains elapsed time, absolute pressure, relative pressure and specific quantity adsorbed.

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Gemini VII Exporting Isotherm Data

Format of Exported Data


The output file consists of five columns containing elapsed time during analysis, absolute pressure, rel-
ative pressure, quantity adsorbed, and quantity dosed.

Description
Operator
Submitter
Sample Mass

* Type of Data
0 = automatically collected
1 = entered (relative pressures)
2 = entered (absolute pressures)

Elapsed Absolute Relative Quantity Quantity


Time during Pressure Pressure Adsorbed Dosed 
Analysis (mmHg) (cm3/g STP) (cm3/g STP)

1. Go to File > Export > [file].

2. From the Name column, select a file to export. To select more than one file, hold down the Ctrl
key on the keyboard while selecting the files. To sort a column, click the column header.

3. Click Open. The file is automatically converted to a .SMP file and the following window
displays.

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Converting Files Gemini VII

4. In the Export Settings window, select one of the following:

• Preview - to send the file to the screen.

• Print - to send the file to the default printer.

• Copies - select the number of copies to print. This field is only enabled when Print is selected.

• File - select the destination directory and enter a file name in the File name text box. Select to
save the file as a .REP, .XLS, or .TXT file format.

5. Click OK to close the window.

Converting Files
Converts StarDriver files (.MGD extension) to a sample information file with a .SMP file extension.
Only those files with a .MGD file extension display in the Name column. Multiple files can be
selected by holding down the Ctrl key on the keyboard while selecting the files.

1. Go to File > Convert > [file].

2. From the Name column, select a file to convert. To select more than one file, hold down the Ctrl
key on the keyboard while selecting the files. To sort a column, click the column header.

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Gemini VII Generating Graph Overlays

3. Click Open. The file is automatically converted to a .SMP file and the following window
displays.

4. Click OK to close the window.

Generating Graph Overlays


Use the graph overlay function to compare multiple graph options. Graphical lines are differentiated
by the use of varying symbols outlined on a legend. Overlays may be generated in two ways:

• Multiple Sample Overlays - overlay up to eight plots of the same type with that of the current plot.

• Multiple Graph Overlays - overlay two different types of plots from one sample. This type of
overlay is available only for:

– BJH Adsorption/Desorption
– DFT Pore Size/Surface Energy
– Dollimore-Heal Adsorption/Desorption
– Horvath-Kawazoe
– M-P Method

Only the Advanced format can be used to generate overlays. Select Options > Options Presentation >
Advanced to access the Advanced format or select Advanced from the dropdown list at the bottom of
the screen.

Multiple Sample Overlays


To overlay the same type of graph on multiple samples:

1. Go to File > Open > Sample Information.

If a file with a status other than Preparing, Prepared or No Analysis is selected, the Isotherm
plot displays. Select Advanced from the dropdown list at the bottom of the screen.

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Generating Graph Overlays Gemini VII

2. Click the Report Options tab at the top of the screen. Refer to the following table for instructions
for the selected report.

Highlight the report to


overlay, then click Edit.

If overlaying this type of


Then..
report...

a.) In the Selected Reports list box, highlight Isotherm and


click Edit.

• Isotherm b.) On the Isotherm Report Options window, select a plot in


the Selected Reports group box then click the Options
button to the right of the selected plot.

c.) On the Plot Options window, select the Overlay samples


checkbox and verify other fields. Click OK to save and close
the window.

d.) Click OK again on the Isotherm Report Options window to


return to the Report Options tab.

e.) Continue with Step 3.

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Gemini VII Generating Graph Overlays

If overlaying this type of


Then..
report... (continued)

• BET Surface Area a.) In the Selected Reports list box, highlight one of the report
• Langmuir Surface Area options shown on the left and click Edit.
• Freundlich
• Temkin b.) On the Report Options window, select the Overlay samples
• t-Plot checkbox for the Transform plot and/or the Isotherm plot.
• Alpha-S Verify other fields. Click OK to return to the Report Options
• f-Ratio tab.

c.) Continue with Step 3.

a.) In the Selected Reports list box, highlight one of the report
options shown on the left and click Edit.
• BJH Adsorption
• BJH Desorption
b.) Select the report variable from the Select Reports group box
• Dollimore-Heal
and click Edit.
Adsorption
• Dollimore-Heal c.) Click the dropdown arrow on the Overlay field and select the
Desorption Samples option. Verify other fields. Click OK to return to the
• MP-Method Report Options window.

d.) Click OK again to return to the Report Options tab.

e.) Continue with Step 3.

3. From the Report Options tab, click the Overlays button.

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Generating Graph Overlays Gemini VII

4. Click Browse to the right of the Sample [n] field. Select the file containing the graph to overlay
and click Open. After selecting up to eight files, click OK to return to the Report Options tab.

5. Click Save to save the selections to a new file name.

Be advised when working with an existing file that a copy of the file be used rather than
the original.

6. Select Reports > Start Report. The Start Report window displays with the name of the edited
and saved file in the File name text box. To select more than one file, hold down the Ctrl key on
the keyboard while selecting the files.

7. Click Open.

8. Select the report destination in the Report Settings window and click OK. Refer to
Printing Files, page 3-30.

9. If only one file was selected, the Selected Reports window displays. Verify the reports to
generate and click OK. If multiple files were selected, the following window will not display.

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Gemini VII Generating Graph Overlays

10. The report screen displays with tabs across the top of the screen. Click each tab to view the
reports.

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Generating Graph Overlays Gemini VII

Multiple Graph Overlays


Multiple graph overlays can only be generated for:

• BJH Adsorption
• BJH Desorption
• DFT Pore Size
• DFT Surface Energy
• Dollimore-Heal Adsorption
• Dollimore-Heal Desorption
• Horvath-Kawazoe
• MP-Method

The following instructions use BJH Adsorption as an example. Screen appearance will vary depending
on the selected report.

1. Go to File > Open > Sample Information.

2. Select a sample file to overlay graphs of other samples. To select more than one file, hold down
the Ctrl key on the keyboard while selecting the files. To sort a column, click the column header.
Click Open.

If a file with a status other than Preparing, Prepared or No Analysis is selected, the Isotherm
plot displays. Select Advanced from the dropdown list at the bottom of the screen.

3. Click the Report Options tab. In the Selected Reports list box, highlight the type of report to
overlay with a graph and click Edit.

Highlight the
report, then click
Edit.

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Gemini VII Generating Graph Overlays

4. From the Report Options window, in the Selected Reports list box, select a sub-report and click
and click Edit.

Select the report


variable

Click Edit

5. Click the dropdown arrow on the Overlay field and select a second variable to overlay. Click OK
to return to the Report Options window.

Displays the first report


variable

Select the second variable


from the dropdown list

6. Click OK again to return to the Report Options tab.

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Generating Graph Overlays Gemini VII

7. Click Save to save the selections.

Be advised when working with an existing file that a copy of the file be used rather
than the original.

8. Select Reports > Start Report. Select the file created in the previous steps and click Open. To
select more than one file, hold down the Ctrl key on the keyboard while selecting the files.

9. Click Open and select the report destination in the Report Settings window and click OK.

10. If only one file was selected in step 8, the Selected Reports window displays. Verify the reports
to generate and click OK. If multiple files were selected, the following window will not display.

11. The report screen displays with tabs across the top of the screen. Click each tab to view the
reports.

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Gemini VII Introduction

4. SOFTWARE AND SETUP MODIFICATIONS

Introduction
This chapter provides instructions for:

• installing the software


• installing software updates or reverting to a previous version
• adding an analyzer
• moving an analyzer from one PC to another PC
• removing an analyzer
• changing the analyzer setup (Ethernet port configuration)
• reinstalling calibration files
• importing an analyzer from a previous installation on this PC
• adding or modifying SmartPrep
• uninstalling the software

The analysis program can also be installed for offline data manipulation on a computer other than the
one controlling the analyzer. This allows:

• the creation or editing of sample and parameter files


• the generation of reports on completed sample files

Review the Micromeritics PROGRAM License Agreement for restrictions on the use of another copy
of the analysis program.


When finished working with the setup CD, store it in a safe location.

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Installing the Software Gemini VII

Installing the Software


The following prerequisites must be completed prior to installing the software:

• Configure an Ethernet port on the computer to communicate with the analyzer. Refer to
ETHERNET CONFIGURATION, page D-1.

• Attach the analyzer to the computer’s configured Ethernet port and turn on the power to the
analyzer.

If installing multiple analyzers, connect the Ethernet switch to the computer’s


configured port and connect the analyzers to the Ethernet switch. Refer to Ethernet
Switch, page 4-13. Then turn the analyzers on.

The application should not be installed on a network drive with shared access.
Multiple users cannot operate the application at the same time.

CDs containing calibration files end with a suffix of 99. Update CDs end with a suffix of 00.

1. Insert the installation CD into the CD-ROM drive. The program automatically starts the
installation. If the installation does not immediately start, navigate to the CD-Rom drive, locate
and double-click the setup.exe file.

System Installation videos for hardware components and verification of operation are available by
clicking the Click here to view the system installation videos link on the Ethernet Introduction
screen.

2. The Welcome screen displays. Click Next.

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Gemini VII Installing the Software

3. On the Ethernet Introduction screen, verify that the prerequisites have all been met. If not, click
Cancel and complete the steps, then restart the installation program. Do not proceed with
installation until these tasks have been completed. If the prerequisites have been met, click Next.

4. On the Choose Users screen, select one of the following, then click Next:

• Install for anyone using this computer - anyone who logs onto this computer will have
access to the analyzer program.

• Install just for me - only the person logged onto the computer at the time of installation will
have access to the analyzer program.

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Installing the Software Gemini VII

5. On the Choose Install Location screen, verify that enough disk space is available to continue the
installation. If not, click Cancel and free up the minimum required disk space. If the disk space is
OK, click Next to accept the default installation directory or click Browse to change the
installation location, then click Next.

Disk space required for


installation

Disk space available


for installation

6. On the Choose Start Menu Folder screen, select a folder for the program shortcut. Select one of
the following:

• click Install to accept the default location


• select another folder from the list, then click Install
• enter a new folder name in the text box, then click Install

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Gemini VII Installing the Software

7. When installation completes, the Gemini VII Installed screen displays. Click Next.

8. The Analyzer Configuration screen is used to configure the system for the each analyzer and
serial number to be installed.

In the Step 1 group box:

If... Then..

installing the analysis select the number of analyzers to be installed.


program during initial
installation

using the analysis program select 0.


for offline data reduction

moving an analyzer from select 0 when using the Moving an Analyzer from One PC to
another computer to this Another PC, page 4-16 option.
one

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Installing the Software Gemini VII

a.) In the Step 2 group box, enter the serial number for each analyzer to be attached to this
computer. The analyzer’s serial number label is located near the power switch.

b.) Click Next.

9. On the Ethernet Ports screen, select one option from the following table:

If... Then...

the configured port is listed Select the port then click Next to proceed to the next step.

the configured port is not Click Specify.


listed
On the Specify Ethernet Port screen, enter the remaining portion of
the IP address in the enabled fields then click Next.

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Gemini VII Installing the Software

10. The Analyzer S/N [n] Installed screen displays. Click Next. A screen displays for each unit
installed.

11. If installing a SmartPrep at this time, on the Configure SmartPrep screen, select the number of
SmartPrep instruments to be installed and the Com Port connected to the first SmartPrep. Click
Next. If not installing the SmartPrep, select None for step 1 and click Next.

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Installing the Software Gemini VII

12. The Product Release Information screen displays containing information about updates and
changes included in the release. Click Next.

13. The Product Registration screen displays. Click the appropriate link to register the product or to
log into your portal or click Next to register later.

14. The Completing the Gemini VII Setup screen displays. Select one of the following:

• Reboot now
• I want to manually reboot later

Select the Create a desktop icon checkbox to have the system install a program shortcut onto the
desktop, then click Finish to close the Setup program.

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Gemini VII Installing the Software

Starting the Setup Program


To start the setup program:

1. Ensure that the analysis program is not operating and the analyzer is idle.

2. Insert the setup CD into the CD-ROM drive. The setup program starts automatically.

If the program does not start automatically, navigate to the CD drive and double-click the
setup.exe file.

3. The Welcome screen displays. Click Next.

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Installing the Software Gemini VII

4. On the Select Task screen, select the task to perform, then click Next. Use the following sections
to complete the selected task.

Installing Software Updates or Reverting to a Previous Version


When performing a software update, existing data files are not overwritten. There are three types of
subsequent installations:

• a later version than the current installation


• the same version as the current installation
• an earlier version than the current installation

The setup program automatically detects which type of installation applies and customizes the selec-
tion accordingly.

1. Insert the setup CD into the CD-ROM drive. The setup program starts automatically.

If the program does not start automatically, navigate to the CD drive and double-click the
setup.exe file.

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Gemini VII Installing the Software

2. The Welcome screen displays. Click Next.

3. On the Select Task screen, select one of the following software options (only the applicable
option displays) and click Next:

• Upgrade software to version [n] from version [n]


• Reinstall software version [n]
• Downgrade software to version [n] from version [n]

If the option Downgrade software to version (previous number) displays, contact your
Micromeritics representative before proceeding. Reverting to a previous version can
damage existing sample files.

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Installing the Software Gemini VII

4. The Gemini VII Installed screen displays. Click Next.

5. The Gemini VII Reinstalled screen displays. Select one of the following:

• Reboot now
• I want to manually reboot later

Select the Create a desktop icon checkbox to have the system install a program shortcut onto the
desktop. Click Finish.

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Gemini VII Installing the Software

Adding an Analyzer
An Ethernet switch is required when connecting multiple analyzers. After connecting the Ethernet
switch, continue with the Software, page 4-14 section.

Ethernet Switch
1. Connect the power cord of the Ethernet switch to an appropriate power outlet.

2. For each analyzer to be added, connect an Ethernet cable from the Ethernet labeled port on the
rear of the analyzer to a numbered port on the Ethernet switch taking care not to use the uplink
port on the switch.

3. Use an Ethernet cable to connect the computer to the Ethernet switch.

4. Ensure the power is turned on to the computer, the Ethernet switch, and each analyzer.

The finished configuration should look similar to the following:

Ethernet switch Be sure cables are not


connected to the uplink
port.

5. Ensure the power is turned on to the computer, the Ethernet switch, and each analyzer.

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Installing the Software Gemini VII

Software
1. Start the setup program. The Welcome screen displays. Click Next.

2. On the Select Task screen, select Add an analyzer. Click Next.

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Gemini VII Installing the Software

3. On the Add Analyzer screen, enter the serial number of the analyzer being added. Click Next.

4. The Analyzer S/N [n] Installed screen indicates a successful install. Click Next.

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Installing the Software Gemini VII

5. The Analyzer Added screen displays. Click Finish.

Moving an Analyzer from One PC to Another PC


This section provides instructions on moving a configured analyzer (along with its status, calibration,
and log file) from one computer (Source PC) to a another (Destination PC). This operation does not
move sample or parameter files. Use a file management program such as Explorer or a backup/restore
utility to move these types of files.

1. Ensure the analyzer program is installed on the destination computer. If this is a new install, refer
to Installing the Software, page 4-2 and select ’0’ as the number of analyzers to be installed.

2. Start the setup program on the Source computer. On the Welcome screen, click Next.

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Gemini VII Installing the Software

3. On the Select Task screen, select Move an analyzer from one PC to another PC. Click Next.

4. On the Move Analyzer screen, use the dropdown list to select the source analyzer to be moved.
Click Next.

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Installing the Software Gemini VII

5. On the new Move Analyzer screen, select the new destination for the analyzer to be moved. This
location is where the Analyzer SN [n] Installer.exe file will be located. To accept the default
location, click Next or click Browse to select a new destination, then click Next.

6. The analyzer serial number [n] files are moved to the install program and the Analyzer Installer
Created screen displays. Click Finish.

a.) Remove the CD from the CD-ROM drive and store in a safe location.

b.) Disconnect the Ethernet cable from the Source computer and reconnect it to the configured
Ethernet port on the Destination computer. If moving the analyzer to a computer that already
has an analyzer attached, an Ethernet switch is required.

c.) If the move destination was a local drive, navigate to the drive and copy the Analyzer SN [n]
Installer.exe file to a media device such as a USB stick. Install the file on the destination
computer, then double-click the Analyzer SN [n] Installer.exe file.

If the move destination was a network drive, navigate to the location then double-click the
Analyzer SN [n] Installer.exe file.

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Gemini VII Installing the Software

7. The Welcome screen displays. Click Next.

8. On the Move Analyzer screen, click Next.

9. On the Analyzer Installed screen, click Finish.

Sample and parameter files are not copied and moved with the analyzer. Use a file
management program such as Explorer or a backup/restore utility to move these 
files.

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Installing the Software Gemini VII

Removing an Analyzer
1. Start the setup program. On the Welcome screen, click Next.

2. On the Select Task screen, select Remove an analyzer. Click Next.

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Gemini VII Installing the Software

3. On the Remove Analyzer screen, from the dropdown list, select the unit and serial number of the
analyzer to be removed. Click Next.

This operation removes the selected instrument from the list of attached instruments.
It does not remove calibration and status files associated with the analyzer nor does it
remove sample and parameter data files.

4. The Analyzer Removed screen displays. Click Finish.

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Installing the Software Gemini VII

Changing the Analyzer Setup


This section provides instructions and changing an analyzer’s Ethernet port in case of an Ethernet port
malfunction. Ensure that the new Ethernet port has been configured.

1. Start the setup program. On the Welcome screen, click Next.

2. On the Select Task screen, select Change analyzer setup. Click Next.

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Gemini VII Installing the Software

3. On the Ethernet Ports screen, select one option from the following table:

If... Then...

the configured port is listed Select the port then click Next to proceed to the next step.

the configured port is not Click Specify.


listed
On the Specify Ethernet Port screen, enter the remaining portion of
the IP address in the enabled fields the click Next.

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Installing the Software Gemini VII

4. On the Analyzer Configuration Updated screen, click Finish.

Reinstalling Calibration Files for an Analyzer


Calibration files specific to the analyzer are contained on the original calibration CD only and not on
an update CD.

1. Start the setup program. On the Welcome screen, click Next.

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Gemini VII Installing the Software

2. On the Select Task screen, select Reinstall calibration files for an analyzer. Click Next.

3. On the Reinstall Calibration Files screen, select the unit and serial number from the dropdown
list. Click Next.

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Installing the Software Gemini VII

4. On the Analyzer S/N [n] Installed screen, click Next.

5. On the Analyzer Calibration Reinstalled screen, click Finish.

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Gemini VII Installing the Software

Importing an Analyzer from a Previous Installation on this PC


This section provides instructions on importing an analyzer from a previous installation on the same
PC.

1. Start the setup program. On the Welcome screen, click Next.

2. On the Select Task screen, select Import an analyzer from a previous installation on this PC.
Click Next.

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Installing the Software Gemini VII

3. On the Import Analyzer screen, click the Browse button to locate the installation directory of the
previously installed instrument, then select the serial number of the instrument files to be
imported. Click Next.

4. When the previously installed files have been imported, the Analyzer SN [n] Installed screen
displays. Click Next.

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Gemini VII Installing the Software

5. On the Analyzer Added screen, click Finish.

Adding or Modifying SmartPrep


This section provides instructions on how to configure the software to connect up to four SmartPrep
instruments.

1. Start the setup program. On the Welcome screen, click Next.

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Installing the Software Gemini VII

2. On the Select Task screen, select Add or Modify SmartPrep. Click Next.

3. On the Configure SmartPrep screen, select the number of SmartPrep units to be installed and the
Com Port for the first SmartPrep unit. Click Next.

4-30 239-42828-01 - Dec 2012


Gemini VII Uninstalling the Analysis Program

4. On the Completing the Gemini VII Setup screen, to place a shortcut icon on the desktop, select
the Create a desktop icon checkbox. Click Finish to complete the process.

Uninstalling the Analysis Program


This section provides instructions on uninstalling the analysis program, status files, analyzer setup files
and resulting empty directories. It does not remove data files.

1. Double-click the uninstall.exe file located in the directory where the Gemini VII files are
installed.

2. On the Uninstall Gemini VII screen, click Uninstall.

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Uninstalling the Analysis Program Gemini VII

3. The Uninstallation Complete screen displays. Click Next.

4. The Completing the Gemini VII Uninstall screen displays. Click Finish to close the setup
program.

4-32 239-42828-01 - Dec 2012


Gemini VII Introduction

5. FILE MENU

Introduction
This chapter contains information specific to the File menu options used to manage sample and param-
eter files. This chapter provides details of File menu options, commonly used functions and buttons,
and field descriptions.

Menu bar

Arrow indicates
submenu

Common field and button descriptions are listed in a Common table at the beginning
of their respective chapters. Field and button descriptions not listed in the Common
table are listed in their appropriate heading.

Refer to the Appendix section of this manual for further details on report calculations
(CALCULATIONS, page C-1) and DFT models (DFT MODELS, page F-1).

Common Fields and Buttons - File Menu Options


The following fields and buttons are common to many of the File Menu windows. Field and button
descriptions not listed below are found in their respective sections.

Field or Button Description

Autoscale checkbox When working with report parameters screens, when enabled, allows the X-
and Y-axes to be scaled automatically.

Axis Range When working with report parameters screens, the From / To fields are
enabled when Autoscale options are not selected. Enter the starting and
ending values for the X- and/or Y-axes.

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Common Fields and Buttons - File Menu Options Gemini VII

Field or Button Description (continued)

Browse button Click to search for a file. Select from a file in the Name column and click
Open or double click the file name in the Name column to open (or import)
the file.

Cancel button Cancels any changes made to the screen.

Close button Closes the active window. If changes were made to the file and not yet
saved, a prompt displays providing the option to save the file.

Delete button When working with report parameters screens, click Delete to remove the
selected report. Deleted reports will have to be regenerated if deleted in
error.

Destination  • Preview - sends the file to the screen. Click Print on the report screen to
group box send the file to the printer.

• Print - sends the file to the default printer.

• Copies - select the number of copies to print. This field is only enabled
when Print is selected.

• File - saves the report as a file. Click the Browse icon to the right of the
text field to select the directory where the new file will be stored. Enter
the new file name in the File name text box.

• File Type - select to save the new file with a .TXT, .XLS or .REP file
extension. This field is only enabled when File is selected.

.REP (Report system) - saves the report in a format that can be opened
within the program.
.TXT (ASCII text) - saves the report as a common machine language
file.
.XLS (Spreadsheet file) - saves the report in a format that can be opened
within a spreadsheet program.

Edit button When working with report parameters screens, highlight the item in the
Selected Reports list box and click Edit to modify report details.

File name text box Select the file to print (or open) from the Name column. The file name will
appear in the File name text box. Click Open or double-click the file name
in the Name column to open the file. Multiple files can be selected by
holding down the Ctrl key on the keyboard while selecting multiple files.

5-2 239-42828-01 - Dec 2012


Gemini VII Common Fields and Buttons - File Menu Options

Field or Button Description (continued)

From / To text boxes When working with report parameters screens, enter the From and To range
for autoscaling the X- and/or Y- axes.

Name column A list of files in the selected directory.

OK button Click to save and close the active window.

Open button Click to open the selected file (or double-click the file name in the Name
column to open the file).

Preview button Click to preview predefined reports. Click the tabs across the top of the
window to preview each selected report. Refer to Report Tool Bar, page 7-
14. When an analysis has not been run on a sample, this button is disabled.

Print button Sends the report to the selected destination (screen, printer or file).

Replace button Click to select another file where the values will replace the current file’s
values. The original file will remain unchanged.

Save button (or menu Saves the active file.


option)

Save All menu option Saves all active files.

Save As menu option Saves the active file under a new file name.

Table buttons • Insert - inserts one row above the selected row.
• Delete - deletes the selected row.
• Clear - clears all table entries and displays only one default value.
• Append - inserts one row at the end of the table.

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Open Gemini VII

Open
Opens a sample file, parameter file, or report option.

• Sample Information files - the File name text box contains the next sequential file name generated
by the program. The sample information file extension is .SMP.

• Parameter files - the File name text box contains an asterisk (*) and a default file extension
depending on the type of parameter file selected. Default file extensions are:

*.DEG Degas Conditions


*.ANC Analysis Conditions
*.ADP Adsorptive Properties
*.RPO Report Options

Save
Saves the active window under the current file name.

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Gemini VII Save As

Save As
Saves the active window as another file type or file name.

• Saves a file in the active window under a different file name.

• Saves a subset (parameter) of the sample file in the active window as a standalone parameter file, for
example, select Analysis Conditions from the Save As menu to create a standalone parameter file of
the analysis conditions portion of the active sample file.

Save As (t-Curve or Alpha-S Curve)


t-Curve - saves the relative pressures and corresponding thicknesses as an ASCII text file with a .THK
file extension. These data are derived by dividing the condensed volume of adsorptive by the selected
surface area. The density conversion factor in the adsorptive properties file is used to convert quantity
adsorbed to volume of condensed adsorptive.

Alpha-S - saves the relative pressures and resulting quantities adsorbed as an ASCII text file with a
.ALS file extension. These data are derived by dividing the isotherm by the quantity adsorbed at 0.4
relative pressure.

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Save All Gemini VII

Save All
Saves all active windows under the current file names.

Close
Closes the active window. If changes were made and not yet saved, a prompt displays providing the
option to save the file.

Close All
Closes all active windows. If changes were made and not yet saved, a prompt displays providing the
option to save the file.

Print
Prints the contents of one or more sample or reports options files to either the screen, a printer, or to a
file.

List
Provides the option to create a list of sample or report options file information, for example, file name,
date / time the file was created or last edited, file identification and file status.

Export
Exports isotherm data in a sample information file as a .TXT or .XLS file. When saved to a file, the
data can be imported into other applications. The output file contains elapsed time, absolute pressure,
relative pressure, and specific quantity adsorbed in column format.

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Gemini VII Convert

Convert
Converts the following sample file types to be compatible with the Gemini VII application:

File Type File Name Convention

ASAP 2000 SIcarbon.DAT

ASAP 2000 Micropore SMcarbon.DAT

ASAP 2400 SIcarbon.DAT

ASAP 2405 SKcarbon.DAT

StarDriver carbon.MGD

NOTE: Substitute the word carbon (shown above)


for the actual filename.

Exit
Exits the analysis program.

• If an analysis is in progress, it will continue to completion.

• If changes have been made to a file and not yet saved, a prompt displays providing the option to save
the file.

• If an analysis is in progress, a prompt displays providing the option to exit the program.

– YES saves the changes before exiting the program


– NO exits the file without saving the changes
– CANCEL cancels any changes

239-42828-01 - Dec 2012 5-7


Sample Information Files Gemini VII

Sample Information Files


File > Open > Sample Information (or use the F2 keyboard shortcut)

Each analysis must be linked with a sample information file before the analysis can proceed. A sample
information file can consist of multiple parameter files; however, parameter files can also stand alone.

Parameter files allow repeated use of the file, for example, if the same analysis conditions exist for
multiple analyses, create an Analysis Conditions file containing the recurring conditions. When the
sample file is created, select the Analysis Conditions file for the analysis conditions. Once it becomes
part of the new sample file, edit the new file as needed without affecting the original Analysis Condi-
tions file. Sample Information files can be created or opened in Advanced, Basic, or Restricted
formats.

Specify or change the default format by selecting Options > Option Presentation or
select Basic / Advanced from the dropdown list at the bottom of the window. Refer to
Specifying Sample Defaults, page 3-1 for a description of the Advanced, Basic, and
Restricted formats.

Field or Button Description

Sample text box Enter a sample description.

Operator / Submitter Enter the name of the operator or submitter performing the analysis.
text boxes

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Gemini VII Sample Information Files

Field or Button Description (continued)

Bar Code text box Enter bar code reader information if a bar code reader is connected to the
computer’s USB port. If a bar code reader is not used, this alpha/numeric
field can be used to enter additional information about the sample; such as, a
sample lot number, sample ID, chain of custody, etc.

Mass group box • Enter - when selected, enables the Sample Mass field. Enter a value for
the sample mass.

• Calculate - enables the Empty tube and Sample + tube fields. Enter the
values necessary to calculate the sample mass. Equation used to calculate
sample mass:

Masssample = Masssample+tube – Masstube

• Density - value is used for the Calculated free space method only. Use
0.000 for a blank analysis.

Type of Data group • Automatically collected - select if the type of data will be automatically
box collected while an analysis is running.

• Manually entered - select to manually enter data. If Manually entered


is selected, an Entered Data tab displays at the top of the window.

User Parameters These fields are primarily used for the SPC (Statistical Process Control)
group box reporting to specify sample characteristics or its manufacturing process but
may be used for other data by entering specific analysis conditions or
sample criteria.
These parameters display on the Sample Description window, in Reports >
SPC Report Options, and the Summary Report.
Modify the default field labels (alpha/numeric) in Options > Sample
Defaults.

Comments text box Enter comments about the sample or its analysis conditions. Comments will
appear in the report header.

Add Log Entry Click to enter information to appear in the sample log report. Click the
button button again to enter multiple log entries.

Replace All button Click to select another file where the values will replace all values for the
Sample Information file. The original file will remain unchanged.

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Degas Conditions Files Gemini VII

Field or Button Description (continued)

Close button
Preview button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
Save button

Degas Conditions Files


File > Open > Degas Conditions (or click the Degas Conditions tab when in Advanced format)

The Degas Conditions tab provides details for setting up the Degas Conditions parameter file. This
information will be automatically applied during the degassing procedure if using the SmartPrep
Degasser. Use this option when the SmartPrep Degasser is installed.

Field or Button Description

Description text box Contains the description of the current file.

Conditions table Enter up to five stages of degas conditions. Available columns are:
• Temperature - soaking temperature with flowing gas.

• Temperature Ramp Rate - rate at which the temperature is to change


when advancing to the soak temperature.

• Time - amount of time to soak the sample.

5-10 239-42828-01 - Dec 2012


Gemini VII Analysis Conditions Files

Field or Button Description (continued)

Close button
Preview button
Replace button Refer to the field and button table in Common Fields and Buttons - File
Menu Options, page 5-1.
Save button
Table buttons

Analysis Conditions Files


File > Open > Analysis Conditions (or click the Analysis Conditions tab when in Advanced format
or use the F3 keyboard shortcut)

The Analysis Conditions tab provides details for setting up the sample analysis conditions file.

Use this window to manually enter the pressures or use the Insert Predefined button to insert default
system values.

A pressure table consists of relative pressure points (and possibly calculation assignments) at which
data (isotherms) are to be collected. The relative pressures may span the entire range of 0.00000001 to
0.995 p/po. There must be one adsorption branch followed optionally by one desorption branch.

Several analysis conditions files containing complete pressure tables are included with the analysis
program. To use these files, it is recommended to use the File > Save As option to save the file as a dif-
ferent name and edit the new file.

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Analysis Conditions Files Gemini VII

The pressure table for automatically collected data includes the pressure points for data collection and
(when the Use calculation assignments checkbox is selected) identifies calculations through which
the data are processed.

Field or Button Description

Description text box Refer to Degas Conditions Files, page 5-10.

Replace button Refer to Common Fields and Buttons - File Menu Options, page 5-1.

Absolute pressure Select to specify pressure targets in mmHg, mbar, or kPa rather than
dosing checkbox relative pressure. This option is typically selected when using adsorptives
at analysis conditions above the critical point of the gas; for example, H2
adsorption on carbon at liquid nitrogen temperature.

Use calculation Select to use assigned collected data points. If this option is not selected,
assignments checkbox each report (with the exception of Langmuir and BET) will use a range of
pressures as selected in the report options. The Langmuir and BET reports
interpolate to entered relative pressures on the report options.
The outlier points can be selected so they will not be reported.

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Gemini VII Analysis Conditions Files

Field or Button Description (continued)

Insert Range Click to enter starting pressure, ending pressure, the number of points to
button insert within the specified range and whether to have linear or geometric
progression.

• Linear - select to insert evenly spaced points into the table.

• Geometric from low pressure - select to insert geometrically spaced


points from the low pressure range. For example, to insert 5 points with
a 0.01 starting pressure and a 0.16 ending pressure, the following points
are inserted into the table:

0.01
0.02
0.04
0.08
0.16

• Geometric towards saturation - select to insert geometrically spaced


points from the saturation pressure. For example, to insert 5 points with
a 0.99 starting pressure and a 0.84 ending pressure, the following points
are inserted into the table:

0.99
0.98
0.96
0.92
0.84

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Analysis Conditions Files Gemini VII

Field or Button Description (continued)

Insert Predefined Insert Predefined button - this button is disabled if Absolute pressure
button dosing is selected on the previous window. The predefined pressures are
logical only if nitrogen is used as the adsorptive. These options can be used
to select the system’s default pressures which can then be edited on the
Entered Pressures window.
Click the dropdown arrow to select predefined pressure points for surface
area, t-Plot micropore, and/or BJH adsorption/desorption.

Select Adsorption total pore volume, Desorption total pore volume,


and/or Saturation to include them in the Entered Pressures table.

Preparation button Click to enter analysis preparation details.

• Evacuation rate - enter the evacuation rate at which unrestricted


sample evacuation is to begin.

• Evacuation time - enter the length of time for preliminary evacuation


which takes place prior to the free space measurement or sample
analysis if free space is to be Entered or Calculated.

5-14 239-42828-01 - Dec 2012


Gemini VII Analysis Conditions Files

Field or Button Description (continued)

Free Space button Click to enter the type of free space measurement.

• None - select if free space will not be used.


• Previously measured - select if free space has been previously
measured. Recommended if measuring a series of samples with similar
volumes.
• Measure - select to measure the free space automatically over the
sample prior to data collection.
• Enter - select to enter warm and cold free space manually and enter the
amount in the text box.
• Calculate - select to have the free-space calculated using the value
entered for Volume Correction (entered on the Unit > Unit
Configuration window) and the non-ideality factor (entered on the
Adsorptive Properties window).

po and T button Click to select options for obtaining the saturation pressure (Po) and
analysis bath temperature.

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Analysis Conditions Files Gemini VII

Field or Button Description (continued)

po and T button • Entered - select to manually enter the Po in the text box.
(continued)
• Most recent measured - select to use the most recently measured
saturation pressure.

• Measure Po for each point (models 2390p and 2390t only) - select if
Po is to be measured for each point.

• Bath temperature - calculates Po using the entered bath temperature.

Analysis Method Select the method of analysis.


button

• Equilibrate - select if the analysis method is to be equilibrated and


enter the equilibration time in seconds between successive pressure
readings during equilibration. With this method, the analyzer increases
pressure in steps to the next specified level for data collection. It
maintains this pressure and monitors volumes (or quantities) adsorbed.
When the rate of adsorption (volume adsorbed) falls below 0.1%,
equilibration is assumed to have occurred. The instrument then
introduces the next adsorbate gas dose.

• Scan - applies to adsorption only. Select if the analysis method is to be


scanned and enter the minimum equilibration in minutes. This method
allows the adsorbate gas pressure to be raised continuously at a
constant rate based on the pressures to be achieved and the length of the
analysis.

Cancel button
Close button
OK button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
Save button
Table buttons

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Gemini VII Adsorptive Properties Files

Adsorptive Properties Files


File > Open > Adsorptive Properties (or click the Adsorptive Properties tab when in Advanced for-
mat or use the F4 keyboard shortcut)

The Adsorptive Properties window is used to specify the characteristics of the gases used during an
analysis.

Field or Button Description

Adsorptive text box Enter a description of the adsorptive gas or select the adsorptive using the
Replace button.

Mnemonic text box Enter the mnemonic of the adsorptive gas.

Non-ideality factor  Enter a factor to compensate for the forces of attraction between molecules
text box in a real gas. This value is used for a calculated free space.

Density conversion  Enter the density conversion factor which is determined by obtaining the
factor text box ratio of the gas density (STP) to the liquid volume.

Molecular  Enter the molecular cross-sectional area.


cross-sectional area
text box

Close button
Preview button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
Replace button
Save button

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Report Options Files Gemini VII

Report Options Files


File > Open > Report Options [file]

Use to specify report options for collected (from an analysis) or manually entered data. They also help
in customizing report details such as axis scale, axis range, column headings, and components of thick-
ness curve equations. Refer to REPORTS MENU, page 7-1.

Customized report options files can be created then loaded into the original converted sample file
allowing the quick and easy generation of reports.

To include the parameter files in the dropdown list on the Basic and Restricted Sample
Information windows, save the file to the directory specified in Options > Parameter Files
Directory. Refer to UNIT MENU, page 6-1.

Field or Button Description

Description text box Refer to Degas Conditions Files, page 5-10.

Show report title Select and enter a report title to appear on the report header.
checkbox and text box

Show graphic  Select to show a graphic on the report header. Click the Browse button to
checkbox and text box locate the graphic in either .BMP or .EMF format.
• Height / Width - enter the height and width of the selected graphic.
These values determine the graphic appearance on the generated report.

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Gemini VII Report Options Files

Field or Button Description (continued)

Apply thermal Select to correct the temperature-induced pressure difference between the
transpiration manifold and the chilled sample tube. This option is most significant for
correction checkbox pressures less than approximately 1.0 mmHg. Do not use filler rods in the
sample tube when applying correction for thermal transpiration.
Always use thermal transpiration when performing micropore analyses.
Refer to CALCULATIONS, page C-1 for additional information on
thermal transpiration.

Inside diameter of Enabled when Apply thermal transpiration correction is selected. Enter
sample tube text box the inside diameter of the sample tube used in the analysis.

Selected Reports  Select the checkbox to the left of the report names to include in the report.
list box
Calculated pore width (w), pore radius (R) or pore diameter (D) for BJH
reports. Select Options > Units to specify default calculations.

Overlays button Refer to Multiple Sample Overlays, page 3-35.

Browse button
Close button
Edit button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
Preview button
Replace button
Save button

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Report Options Files Gemini VII

Summary Report
The Summary Report provides a condensed listing of selected data results. In the Selected Reports
list box, highlight Summary, then click Edit. Select the data types to include in the Summary report.

In the Pore Volume column, if Adsorption total or Desorption total is selected, the P/Po field is
enabled. Enter the relative pressure used to calculate the total pore volume.

If Use calculation assignments is not selected on the Collected Data window, the isotherm is interpo-
lated to the value in the P/Po fields and the point is used for the total pore volume calculation.
Otherwise, the point selected with calculation assignment is used. Pass/Fail criteria can be specified
for up to four parameters.

Field or Button Description

Select All /  Selects (or deselects) all choices.


Deselect All buttons
Used to enable the first Pass/Fail item. Until the Summary Report is
selected, S A Single-point BET will be displayed by default. When a
checkbox is selected, click the Pass/Fail button and select criteria options
for pass/fail options.
• S A: Single-point BET checkbox - select to enable the Pass/Fail [n]
button in the Item [n] group box.

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Gemini VII Report Options Files

Field or Button Description (continued)

Select All /  • Pass/Fail [n] button - select the S A: Single-point BET checkbox to
Deselect All buttons enable this button. Click the Pass/Fail [n] button to display the Pass/
(continued) Fail Options window for selection of pass/fail criteria.

Item [n] group boxes • Upper/Lower options and text boxes - specify upper and lower limits
for the selected parameter. A range can be left open by not selecting the
limit. In the text box to the right of Upper / Lower, enter a message
line of operator instructions to be displayed if a failure is encountered.

Cancel button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button

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Report Options Files Gemini VII

Isotherm Report Options


The Isotherm report indicates adsorption (up to saturation pressure) and desorption (down from satu-
ration pressure) of a gas by a solid held at constant temperature. In the Selected Reports list box,
highlight Isotherm, then click Edit.

Field or Button Description

Select Reports  Select the checkbox to the left of each applicable report to include the
group box option on the final report.

Options buttons Click to display related linear plot options. All plot windows contain
identical fields.

• Plot curve / Plot points - select to plot curves and/or points


• Overlay Samples - select to overlay sample files.

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Gemini VII Report Options Files

Field or Button Description (continued)

Options buttons • Autoscale X-axis - linear X-axes begin at zero. Logarithmic X-axes
(continued) begin at an appropriate value. The X-axis field shows the relative or
absolute pressure.

• Autoscale Y-axis - Y-axes begin at zero. The Y-axis field shows the
quantity of gas adsorbed.

Tabular Options  Select the options to include on the report.


group box
• Weight % - enter the weight percentage when plotting pressure
composition.

• Elapsed time - time elapsed during the analysis.

• Time between points - time elapsed between points during the


analysis.

Plot Options  Select the type of isotherm to plot (adsorption or desorption).


group box

Quantity Adsorbed  Select how to report the quantity adsorbed.


group box
• Per gram (cm3/g)
• Per BET Surface Area (cm3/m2)
• Per other Surface Area (cm3/m2)

Weight group box Enabled when the Pressure Composition plot checkbox is selected on the
Isotherm Report Options window.
• Adsorbate Molecular Weight - this plot is useful for plotting pressure
as a function of Weight % adsorbed (i.e. H2 adsorbed on carbon).

Cancel button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button

239-42828-01 - Dec 2012 5-23


Report Options Files Gemini VII

BET/Langmuir Surface Area Report Options


The Langmuir and BET Surface Area windows are identical unless otherwise specified. In the
Selected Reports list box, highlight BET (or Langmuir), then click Edit.

• The BET calculation obtains the sample surface area value by determining the monolayer volume
of adsorbed gas from the isotherm data.

• The Langmuir calculation determines the surface area of a sample by relating the surface area to
the volume of gas adsorbed as a monolayer.

Field or Button Description

BET (or Langmuir) fit Enter values in the From / To fields to indicate the fit pressure range.
pressure range text
boxes

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Gemini VII Report Options Files

Field or Button Description (continued)

Pressures button Click to enter a range of pressure points or to modify table values for
pressure points.

If Use calculation assignments is not selected on the Analysis


Conditions window, the isotherm is interpolated to these pressure points.
The interpolated values are used in the BET (or Langmuir) calculations.
If Use calculation assignments is selected, collected data are used.
• Use pressure range option- select and enter the pressure range to be
used in the text boxes if not using the Interpolate pressures table.

• Interpolate pressures option- select to indicate if the system should


use the table or entered data.

• Insert Predefined button - click to insert a predefined (default) set of


points into the report. This button does not display for the Langmuir
report. Interpolate pressures checkbox must be selected to enable this
button.

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Report Options Files Gemini VII

Field or Button Description (continued)

BET (or Langmuir) Select to generate a traditional BET (Langmuir) surface area plot used to
Transform plot determine monolayer volume and BET C constant.
• X-axis - linear X-axes begin at zero. The X-axis field shows the
relative pressure for BET and show absolute pressure for Langmuir.

• Y-axis - Y-axes begin at zero. The Y-axis field shows BET (Langmuir)
transformation.

BET (or Langmuir) Select to use the BET (Langmuir) monolayer volume and constant to
Isotherm plot produce an isotherm.
Uses the BET (Langmuir) monolayer volume and constant to produce an
isotherm.
• X-axis - linear X-axes begin at zero. The X-axis field shows the
relative pressure for BET and show absolute pressure for Langmuir.

• Y-axis - Y-axes begin at zero. The Y-axis field shows the quantity of
gas adsorbed.

Tabular Report Select to have a report of the pressure points generated.


checkbox

Overlay Samples Select to overlay sample files.


checkbox

Cancel button
Close button
From / To text boxes
OK button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
Preview button
Save button
Table buttons

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Gemini VII Report Options Files

Freundlich Report Options


The Freundlich Isotherm is an empirical isotherm used to model low-pressure adsorption data. It can
also be applied to model some micropore isotherms. In the Selected Reports list box, highlight
Freundlich, then click Edit.

Field or Button Description

Specify monolayer Select and enter the monolayer capacity of the sample.
capacity checkbox

Absolute pressure Enter a pressure range when calculation assignments are not used.
range text boxes

Tabular Report
checkbox
Refer to BET/Langmuir Surface Area Report Options, page 5-24.
Overlay Samples
checkbox

Transform plot Plots the log(P) vs log(Q) in a straight line.


checkbox
• X-axis - The X-axis field shows the absolute pressure.
• Y-axis - The Y-axis field shows the quantity of gas adsorbed.

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Report Options Files Gemini VII

Field or Button Description (continued)

Freundlich Isotherm Plots the absolute pressure vs quantity adsorbed. Shows best fit line.
plot checkbox
• X-axis - linear X-axes begin at zero. The X-axis field shows the
absolute pressure.

• Y-axis - Y-axes begin at zero. The Y-axis field shows the quantity of
gas adsorbed.

Cancel button
From / To text boxes Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button

Temkin Isotherm Report Options


The Temkin isotherm is used to model adsorption data where the heat of adsorption drops linearly with
increasing coverage. In the Selected Reports list box, highlight Temkin, then click Edit.

Field or Button Description

Specify monolayer  Refer to Freundlich Report Options, page 5-27.


capacity checkbox

Specify differential  Select and enter the differential heat of adsorption at zero surface
heat of adsorption coverage. This allows inclusion of all Temkin constants.
checkbox

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Gemini VII Report Options Files

Field or Button Description (continued)

Absolute pressure  Enter a pressure range when calculation assignments are not used.
range text boxes

Transform plot Plots a linear form of the Temkin isotherm.


checkbox
• X-axis - the X-axis field shows the logarithm of pressure (ln).
• Y-axis - the Y-axis field shows the quantity of gas adsorbed.

Temkin Isotherm plot Overlays the Temkin isotherm with the analysis data.
checkbox
• X-axis - linear X-axes begin at zero. The X-axis field shows the
absolute pressure.

• Y-axis - Y-axes begin at zero. The Y-axis field shows the quantity of
gas adsorbed.

Tabular Report
checkbox
Refer to BET/Langmuir Surface Area Report Options, page 5-24.
Overlay Samples
checkbox

Cancel button
From / To text boxes Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button

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Report Options Files Gemini VII

t-Plot Report Options


The t-Plot calculation allows quantitative analysis of the area and total volume ascribed to micropores.
Matrix area (the area external to micropores) is directly determined and often proves to be a valuable
way of characterizing complex mixed materials. In the Selected Reports list box, highlight t-Plot,
then click Edit.

Field or Button Description

Thickness Curve  Select the thickness curve. Click Edit to modify the values in the equation
group box for the selected curve. The Frenkel-Halsey-Hill thickness curve can be
applied using the Halsey option.
Reference option - select Reference and click the Edit button to define a
t-curve by entering the relative pressure and thickness values. One
predefined curve is shipped with the analysis program and is found in the
Reference directory.

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Gemini VII Report Options Files

Field or Button Description (continued)

Thickness Curve 
group box (continued)

To import values from an existing thickness curve (.THK file), click Open
and select the file containing the values. The table to be imported must be
saved as ASCII text with a .THK extension. It must have a two-column
format with the relative pressures in the first column and the thickness
values in the second column. Columns must be separated by a space or a
tab.
Kruk-Jaroniec-Sayari / Halsey / Harkins and Jura / Broekhoff-de
Boer / Carbon Black STSA - select the thickness curve option and click
the Edit button. Modify the equation for the selected curve as needed.

Surface Area  Select the surface area value used for thickness calculations. BET is the
group box most commonly used option.

Fitted thickness range Enter the minimum and maximum thicknesses to include in the thickness
text boxes curve. The values entered for the thicknesses can be expressed in
angstroms or nanometers. Select Options > Units to specify default units.
Refer to UNIT MENU, page 6-1.

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Report Options Files Gemini VII

Field or Button Description (continued)

Pressure Range button Click to enter minimum and maximum relative pressures.
If Use calculation assignments is not selected on the Analysis
Conditions window, all of the non-outlier points of the collected data
within the specified range are used for calculating the data for this report.
If Use calculation assignments is selected, collected data points assigned
to this report type are used.

Surface area  Enter the value to correct for surface areas that are not smooth. This brings
correction factor  the values for BET surface area and micropore surface area into
text box accordance. For most samples, the default value of 1.000 is adequate.

t-Plot checkbox Select to have a graphical representation of data generated.


• X-axis - the X-axis field shows the statistical thickness of the adsorbed
film.

• Y-axis - the Y-axis field shows the quantity of gas adsorbed.

Tabular Report
checkbox
Refer to BET/Langmuir Surface Area Report Options, page 5-24.
Overlay Samples
checkbox

Cancel button
From / To text boxes Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button
Table buttons

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Gemini VII Report Options Files

Alpha-S Method
The Alpha-S plot converts the standard adsorption isotherm into a dimensionless isotherm using the
quantity adsorbed at a relative pressure of 0.4. In the Selected Reports list box, highlight Alpha-S
Method, then click Edit.

One predefined curve is shipped with the analysis program and is located in the Reference directory.
Use the table to enter relative pressure and the alpha-s values.

Field or Button Description

Open button To import values from an existing thickness curve (.ALS ASCII file), click
Open, and select the file containing the values.
The table to be imported must be saved as ASCII text with a .ALS
extension. It must have a two-column format with the relative pressures in
the first column and the alpha-s values in the second column. Columns
must be separated by a space or a tab.

Relative pressure  Enter the pressure range when calculation assignments are not used.
range text boxes

Fitted Alpha-S range Enter minimum and maximum relative pressures to determine the fit.
text boxes

Ref. surface area  Enter the surface area from the reference curve. This value is used to
text box calculate the sample surface area.

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Report Options Files Gemini VII

Field or Button Description (continued)

Alpha-S plot  Select to plot data in graph format.


checkbox
• X-axis - the X-axis field shows the relative pressure.
• Y-axis - the Y-axis field shows the quantity of gas adsorbed.

Tabular Report
checkbox
Refer to BET/Langmuir Surface Area Report Options, page 5-24.
Overlay Samples
checkbox

Browse button
Cancel button
From / To buttons Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button
Save As button
Table buttons

f-Ratio Method
The f-Ratio report uses the measured isotherm and normalizes it using a reference isotherm. In the
Selected Reports list box, highlight f-Ratio Method, then click Edit.

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Gemini VII Report Options Files

Field or Button Description

Reference isotherm Click Browse to select a sample file to use as a reference for the isotherm.
Select a file containing an isotherm measured from a non-porous sample of
the same material as the current sample. When the referenced file is
selected, the file name appears to the left of the Browse button.

f-Plot checkbox Select to generate a normalized isotherm.


• X-axis - the X-axis field is dimensionless in units of alpha-s ratio.
• Y-axis - the Y-axis field shows the quantity of gas adsorbed.

Relative pressure Enter a pressure range when calculations assignments are not used.
range text boxes

Tabular Report
checkbox
Refer to BET/Langmuir Surface Area Report Options, page 5-24.
Overlay Samples
checkbox

Browse button
Cancel button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
From / To text boxes
OK button

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Report Options Files Gemini VII

BJH Adsorption/Desorption Report Options


The BJH calculation determines the mesopore volume/area distribution which accounts for both the
change in adsorbate layer thickness and the liquid condensed in pore cores. Reports can be generated
from both adsorption and desorption data.

The fields for both report options are identical unless otherwise specified. In the Selected Reports list
box, highlight BJH Adsorption (or BJH Desorption), then click Edit.

Does not display on the


Desorption window.

An incomplete pore distribution may be generated if a thickness curve selection is not


a good match for the sample being analyzed.

Field or Button Description

Thickness Curve  Refer to t-Plot Report Options, page 5-30.


group box

BJH Correction  Select the type of correction to apply to calculations. The selected type
group box displays in the report header.
• Standard - uses original BJH models.
• Kruk-Jaroniec-Sayari - good for reference thickness curves.
• Faas - good for statistical thickness curves.

Minimum / Maximum Enter the minimum and maximum diameter (radius or width) of pores to
BJH width text boxes include in the BJH reports.

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Gemini VII Report Options Files

Field or Button Description (continued)

Fraction of pores  During adsorption calculations, the analysis program assumes that all
open at both ends text pores are closed at one end. Occasionally, a percentage of pores may be
box open at both ends causing disagreement in the adsorption and desorption
data or in the values for total volume and total BJH pore volume. Enter the
fraction of pores open at both ends to compensate for this error.
This field is not available for the BJH Desorption Report Options
window.

Adsorptive button Displays the BJH Adsorptive Options window. The recommended
adsorptives and their values are shown. Up to eight adsorptive / adsorbate
property factor combinations may be specified.

Smooth differentials Select the checkbox to smooth all differential calculations thus eliminating
checkbox variations in the differential computation caused by noise in the input data.

Cumulative Reports • Larger - select to report the total volume found in pores larger than the
options current pore size.

• Smaller - select to report the total volume found in pores smaller than
the current pore size.

Selected Reports  Refer to Report Options Files, page 5-18.


list box

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Report Options Files Gemini VII

Field or Button Description (continued)

Pressure Range button Click to enter minimum and maximum relative pressures.
If Use calculation assignments is not selected on the Analysis
Conditions window, all of the non-outlier points of the collected data
within the specified range are used for calculating the data for this report.
If Use calculation assignments is selected, collected data points assigned
to this report type are used.

Cancel button
Edit button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button

Tabular Report Options


Highlight BJH Tabular Report in the Selected Reports list box and click Edit to specify the method
of data reduction.

Field or Button Description

Fixed pore size table Select to specify exact pore sizes for volume or area data.
Click the Table button to modify the fixed pore size table. Reference
Table and Columns below for information on the use of these buttons.

Collected points Select to include all relative pressure points collected. Reference the
Columns button referenced below.

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Gemini VII Report Options Files

Field or Button Description (continued)

Columns button Click the dropdown arrow and select the data types to include in the report.
These selections indicate the column order and data contents for the report.

Table button The fixed pore size table must contain a minimum of two points. The
points must be strictly decreasing. Enabled only when Fixed pore size
table is selected.

Cancel button
OK button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
Table buttons

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Report Options Files Gemini VII

Plot Options
The fields for all plot options are identical for specifying plotting methods and customizing plots.
Highlight any plot option in the Selected Reports list box and click Edit.

Field or Button Description

Plot curve / Plot  Refer to Isotherm Report Options, page 5-22.


points checkboxes

X-Axis Select to have the X-axis on a logarithmic or linear scale.

Y-Axis • Variable dropdown list- click to select a variable.


• Overlay dropdown list - click to select an option to overlay on the
current report.

Autoscale checkbox
Cancel button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button

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Gemini VII Report Options Files

Dollimore-Heal Adsorption/Desorption Report Options


This report option generates Dollimore-Heal reports from both adsorption and desorption data. In the
Selected Reports list box, highlight Dollimore-Heal Adsorption (or Dollimore-Heal Desorption),
then click Edit.

Dollimore-Heal Adsorption/Desorption fields and buttons are identical to the BJH Adsorption/
Desorption Report Options, page 5-36.

Or Dollimore-Heal
Desorption Report
Options

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Report Options Files Gemini VII

Horvath-Kawazoe Report Options

The Horvath-Kawazoe method plots individual peaks for different pore sizes even if the difference
between one pore size and the next is only one Angstrom (0.10 nm) or less. In the Selected Reports
list box, highlight Horvath-Kawazoe, then click Edit.

Field or Button Description

Pore Geometry  Select the option that best represents the physical geometry of the
group box micropores in the sample material. When Sphere is selected, options in the
Interaction Parameter group box are disabled.

Interaction Parameter  Select to determine which interaction parameter will be used in the report.
group box These options are disabled if Sphere is selected in the Pore Geometry
group box.
• Computed - select to calculate using the parameters on the Horvath-
Kawazoe Physical Properties window (click the Properties button to
display the Physical Properties window). The interaction parameter is
recalculated each time a parameter on the Physical Properties window
is edited.
• Entered - select to calculate using the value entered in the text box.

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Gemini VII Report Options Files

Field or Button Description (continued)

Properties button Click to view or edit the constants describing the physical properties of the
adsorbent and adsorptive.

These options are disabled if Entered is selected in the


Interaction Parameter group box.

Adsorbent group box -


Contains the parameters for the sample. If using Computed for the
interaction parameter, all fields are enabled. If using Entered, only the
values in the Diameter and Diameter at zero energy text fields may be
edited.
• Description dropdown list - click to select the name of the adsorbent
used in the analysis.

• Diameter - enter the diameter of the sample (or adsorbent) atom.

• Diameter at zero energy - enter the diameter of an atom at zero


interaction energy: (2/5)1/6 × diameter.

Adsorptive group box -


Contains the parameters for the adsorptives (provided with the software
and/or user-defined). If using Computed for the interaction parameter, all
fields are enabled. If using Entered, only the values in the Diameter and
Diameter at zero energy text fields may be edited.
• Mnemonic dropdown list - click to select the mnemonic of the
adsorptive gas in use.

• Diameter - enter the diameter of the gas phase (or adsorbent) atom.

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Report Options Files Gemini VII

Field or Button Description (continued)

Properties button • Diameter at zero energy - enter the diameter of an atom at zero
(continued) interaction energy: (2/5)1/6 × diameter.

• Polarizability - enter the polarizability of the adsorbent (or


adsorptive).

• Magnetic susceptibility - enter the magnetic susceptibility of the


adsorbent (or adsorptive).

• Density - enter the density per unit area of the adsorbent (or
adsorptive).

Apply Cheng/Yang  Select to apply the Cheng/Yang correction to the pore size analysis. This
correction checkbox correction substitutes the Langmuir equation of state for Henry’s Law in
the Horvath-Kawazoe derivation.

Smooth differentials
checkbox
Refer to BJH Adsorption/Desorption Report Options, page 5-36.
Pressure Range button

Selected Reports  Refer to Report Options Files, page 5-18.


list box

Cancel button
Edit button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button

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Gemini VII Report Options Files

Tabular Report Options


Highlight H-K Tabular Report in the Selected Reports list box and click Edit. To customize the
order and data contents of reports, click the dropdown arrow for a column, and select the data type for
that column.

Plot Options
Highlight a plot option in the Selected Reports list box and click Edit to customize the plotting
method.

Field or Button Description

Plot curve / Plot  Refer to Isotherm Report Options, page 5-22.


points checkboxes

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Report Options Files Gemini VII

Field or Button Description (continued)

X-Axis / Y-Axis • X-Axis - the X-axis field shows pore radius or diameter in angstroms
or nanometers.

• Y-Axis - the Y-axis field shows the quantity of gas adsorbed.

• Variable dropdown list - click to select a Y-axis variable for the report.

• Overlay dropdown list - click to select an option to overlay on the


current report.

Autoscale checkbox
Cancel button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
Edit button
OK button

DFT Pore Size Report Options


The DFT Pore Size report contains the results of pore size distribution analyses using a non-local DFT
range of micro and mesopore ranges. In the Selected Reports list box, highlight DFT Pore Size, then
click Edit.

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Gemini VII Report Options Files

Field or Button Description

Type dropdown list Click the dropdown arrow to specify either:


• DFT - model based on the density functional theory.

• Classical - model based on the Kelvin equation and thickness


for determining the pore size distribution.

Refer to DFT MODELS, page F-1 for further discussion on


models.

Geometry  Click the dropdown arrow to select the pore shape.


dropdown list

Pressure Range button Refer to BJH Adsorption/Desorption Report Options, page 5-


36.

Models list box Lists the models that meet the criteria specified and which match
the adsorbate and temperature of the sample data. If no models
appear, no models meet the selected criteria. One model must be
selected.

Link to Micromeritics Click to hyperlink to the NLDFT Model Table on the


NLDFT Models button Micromeritics web page.

Regularization  Select the extent of smoothing to apply to the data.


dropdown list and text box
If 0.00000 (user) is selected, enter a number in the text box
giving a relative weight for the smoothing during deconvolution.
Larger values produce more smoothing.

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Report Options Files Gemini VII

Field or Button Description (continued)

Reports to Generate Click the checkbox to select the reports to generate. To edit
list box graph details, highlight the graph option and click Edit. The Log
Goodness of Fit and Goodness of Fit graphs cannot be edited.

• Plot Type group box - select the method for data display.

• Autoscale Options group box - select to autoscale the x-axis


and/or y-axes.

• Overlay dropdown list - select an overlay for the report.

• Axis Range group box - From / To fields are enabled when


Autoscale options are not selected. Enter the starting and
ending values for the X- and/or Y-axes.

– X-axis - the X-axis field shows the pore size.


– Y-axis - the Y-axis field shows the area.

Cancel button Refer to Common Fields and Buttons - File Menu Options,
page 5-1.
From / To text boxes
OK button

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Gemini VII Report Options Files

DFT Surface Energy Report Options


The DFT Surface Energy report contains the results of surface energy distribution analyses. In the
Selected Reports list box, highlight DFT Surface Energy, then click Edit.

DFT Surface Energy Report Options fields and buttons are identical to the DFT Pore Size Report
Options, page 5-46.

Dubinin Report Options


The Dubinin method provides pore volume distributions for microporous materials by making use of
an expression for the adsorption potential. In the Selected Reports list box, highlight Dubinin, then
click Edit.

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Report Options Files Gemini VII

Field or Button Description

Report Type  Select the checkbox to specify report types. If Astakhov is selected, either
group box select the Optimize exponent checkbox or enter an appropriate exponent
value in the text box.

Fitted Radushkevich Enter the minimum and maximum limits on relative pressures included in
(Astakhov) relative  the line fit.
pressure range 
text boxes

Pressure Range button Refer to BJH Adsorption/Desorption Report Options, page 5-36.
Adsorptive button

Selected Reports  Refer to Report Options Files, page 5-18.


list box

Cancel button
Edit button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button

Tabular Report Options


Highlight Dubinin Tabular Report in the Selected Reports list box and click Edit. To customize the
order and data contents of reports, click the dropdown arrow for a column and select the data type for
that column.

Log (po/p )^n - the value for [n] is the optimized exponent if Optimized Astakhov exponent is
selected on the Dubinin Report Options window. If not, then the value for [n] is the entered exponent
value.

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Gemini VII Report Options Files

Transformed Isotherm Plot Options


Highlight Transformed Isotherm in the Selected Reports list box and click Edit.

The transformed Dubinin isotherm is the logarithm of quantity adsorbed as a function of the log of rel-
ative pressure raised to a power. Isotherms for which the Dubinin method is applicable produce
straight lines when transformed in this way.

Field or Button Description

Overlay Samples Refer to BET/Langmuir Surface Area Report Options, page 5-24.
checkbox

Autoscale x-axis / Select an option to have the X- and/or Y-axes scaled automatically. Both
Autoscale y-axis axes begin at 0; the system uses the highest values collected during
checkboxes analysis as the ending points for axis ranges.
To enter beginning and ending values manually, deselect these
checkboxes.
X-axis - shows the quantity of gas adsorbed at standard temperature and
pressure.
Y-axis - shows the log of relative pressure.

Cancel button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button

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Report Options Files Gemini VII

Pore Volume Options


Highlight dV/dw Pore Volume in the Selected Reports list box and click Edit.

This option plots differential pore volume as a function of pore width.

Field or Button Description

Plot curve / Plot  Refer to Isotherm Report Options, page 5-22.


points checkboxes
Overlay Samples
checkbox

Autoscale x-axis / Select an option to have the X- and/or Y-axes scaled automatically. Both
Autoscale y-axis axes begin at 0; the system uses the highest values collected during
checkboxes analysis as the ending points for axis ranges.
To enter beginning and ending values manually, deselect these
checkboxes.

Cancel button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button

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Gemini VII Report Options Files

MP-Method Report Options


The MP method provides pore volume distributions for microporous materials by correlating quantity
adsorbed with the thickness of the adsorbed layer as determined from a user-selected thickness curve.
In the Selected Reports list box, highlight MP-Method, then click the Equation button.

Pore size can be expressed in angstroms or nanometers. Select Options > Units to
specify the unit. Refer to UNIT MENU, page 6-1.

Field or Button Description

Thickness Curve  Refer to t-Plot Report Options, page 5-30.


group box

Selected Reports  Refer to Report Options Files, page 5-18.


list box

Pressure Range button Refer to BJH Adsorption/Desorption Report Options, page 5-36.

Cancel button
Edit button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button

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Report Options Files Gemini VII

Tabular Report Options


Highlight MP Tabular Report in the Selected Reports list box and click Edit. To customize the order
of columns 3 through 6 and data contents of reports, click the dropdown arrow for a column, and select
the data type for that column.

The MP-Method reports hydraulic radius only. If Pore size in diameter is selected from
the Unit Selection window, pore size in radius will be reported.

Plot Options
Highlight a plot option in the Selected Reports list box and click Edit to customize the plotting
method.

Field or Button Description

Plot curve / Plot  Refer to Isotherm Report Options, page 5-22.


points checkboxes

Variable and Overlay Refer to Plot Options, page 5-40.


dropdown lists

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Gemini VII Report Options Files

Field or Button Description (continued)

Autoscale checkboxes
Cancel button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
OK button

Options Report
The Options report provides a subset of the contents report. The Options report cannot be edited. It
provides pertinent information for:

• Degas conditions
• Adsorptive properties
• Analysis conditions
• Free space
• Saturation pressure (Po) and temperature
• Analysis method
• Isotherm collection

Sample Log Report


In the Selected Reports list box, select Sample Log. This report provides the following information:

• Manual control operations performed during analysis.


• Information entered using Add Log Entry on the sample file editor.
• Warnings and/or errors which occurred during analysis.

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Report Options Files Gemini VII

Validation Report
Use this report to have the data examined by the software to determine if the results are within typical
ranges.

If the data selected for validation are determined to be out of range, a warning displays and suggestions
are given for corrective action. This information is also detailed in the report and plotted on the graph
as a unique plot symbol.

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Gemini VII Entered or Collected Data File

Entered or Collected Data File


If Manually Entered is selected on the Advanced view of the Sample information window, an
Entered Data tab displays.

If Automatically Collected is selected, a Collected Data tab displays after the analysis is completed.

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Entered or Collected Data File Gemini VII

Field or Button Description

Pressures group box For manually entered data only, select if the pressures are Relative or
Absolute.

Use calculation Select if calculation data are to be used.


assignments checkbox

pº and T button Refer to Analysis Conditions Files, page 5-11.

Close button
Save button Refer to Common Fields and Buttons - File Menu Options, page 5-1.
Preview button
Table buttons

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Gemini VII Introduction

6. UNIT MENU

Introduction
This chapter contains information specific to the Unit menu options. These options are used to run
analyses on one or more units attached to a controlling computer. This chapter provides details of Unit
menu options, and descriptions of commonly used functions and buttons.

The title bar of the main window displays as Unit [n] - S/N [n] for each attached unit. Each unit has a
status window displayed in different colors.

The Unit menu does not appear on the menu bar if the analysis program is being used
for offline data operations on a computer other than the one controlling the analyzer.

Common field and button descriptions are listed in a Common table at the beginning
of their respective chapters. Field and button descriptions not listed in the Common
table are listed in their appropriate heading.

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Common Fields and Buttons - Unit Menu Options Gemini VII

Common Fields and Buttons - Unit Menu Options


The following fields and buttons are common to many of the Unit menu options. References are made
to these fields and buttons throughout this manual.

Field or Button Description

Browse button Click to search for a file. Select from a file in the Name column and click
Open or double click the file name in the Name column to open (or
import) the file.

Cancel button Discards any changes made to the screen or cancels the current process.

Close button Click to close the active window.

OK button Click to save and close the active window.

Start button Click to start the analysis.

Start Analysis
Unit [n] > Start Analysis

Use to begin an analysis. Select an existing analysis file or create a new one. Then specify analysis
defaults.

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Gemini VII Start Analysis

Port Activity
window

Status
window

Field or Button Description

View dropdown • Operation - displays the current mode of the operation.

• Instrument Log - displays a list of recent analyses, calibrations, and


error or messages. Refer to Show Instrument Log, page 6-15.

• Instrument Schematic - displays a schematic of the analyzer. Refer to


Show Instrument Schematic, page 6-12.

Edit button Click to edit information in the sample information file.

Clear button Click to clear all fields on the window.

Density text field Use to modify the sample mass density.

Mass text field Use to modify the sample mass weight. If the field is disabled, click Edit
then click the Enter option in the Mass group box on the Sample
Description tab.

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Start Analysis Gemini VII

Field or Button Description (continued)

Sample + Tube text Use to modify the weight of the sample plus the sample tube. If the field is
field disabled, click Edit then click the Enter option in the Mass group box on
the Sample Description tab.

Empty Tube text field Use to modify the weight of the empty sample tube. If the field is disabled,
click Edit then click the Enter option in the Mass group box on the
Sample Description tab.

Report After Analysis Click to select a print destination.


button

• Report after analysis checkbox - select to send the report to the


screen, printer, or file in either ASCII, .XLS, or REP format.

• Export after analysis checkbox - select to send the isotherm report to


the screen, printer, or file in either ASCII or .XLS format.

Refer to Destination group box in Common Fields and Buttons - File


Menu Options, page 5-1.

Start / Next button Starts the analysis and displays a graph during analysis. When the first
analysis is complete, the Start button changes to Next.

Browse button Refer to Common Fields and Buttons - Unit Menu Options, page 6-2.
Close button

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Gemini VII QuickStart Analysis

QuickStart Analysis
Unit [n] > QuickStart Analysis

Use to analyze samples of the same type using the same analysis conditions, adsorptive properties, and
report options. The QuickStart Analysis option automatically creates a sample information file for
and assigns the default parameters. Edit the parameters of a file using the Edit button or select another
file using the Browse button.

Additional analyses can be scheduled by clicking Next after the completion of the first series of analy-
ses. The Next button appears after the first set of analyses is complete. The sample cannot be removed
or added until the analysis has completed.

QuickStart Analysis fields and buttons are identical to the Start Analysis, page 6-2.

239-42828-01 - Dec 2012 6-5


Start Po Measurement Gemini VII

Start Po Measurement
Use to measure the saturation pressure.

Not displayed for


Model 2390a

Analyzer Model Description

Model 2390a Measure the Po only in the Sample tube. Ensure a sample tube with no
filler rod is attached to the sample port then click Start to begin the
measurement.

Models 2390p and A Po tube is installed on the Model 2390p and 2390t. Measure the Po in
2390t the Po tube or in the Sample tube. Ensure a sample tube with no filler rod
is attached to the sample port, then click Start to begin the measurement.

The window closes at the end of the measurement. The value obtained is stored and recorded on the
Unit Configuration window as the most recently measured Po and is available for subsequent sample
analyses. The Po option is selected from the Analysis Conditions tab by clicking the Po and T button.

6-6 239-42828-01 - Dec 2012


Gemini VII Blank Analysis

Blank Analysis
Unit [n] > Blank Analysis

Use to obtain sample tube parameters when using a calculated free space. A blank analysis can also be
used for diagnostic purposes.

Blank Analysis fields are identical to the Start Analysis, page 6-2 window with the exception of Den-
sity, Sample + Tube, Mass, and Tube fields.

239-42828-01 - Dec 2012 6-7


Enable Manual Control Gemini VII

Enable Manual Control


Unit [n] > Enable Manual Control

Use to enable the manual control of certain system valves and elevator components. When this option
is enabled, a checkmark appears to the left of the menu item. Enable this option by selecting Enable
Manual Control on the menu.

If the following instrument schematic is not immediately visible, select Unit [n] > Show Instrument
Schematic.

Po tube, valve, and


transducer reading not
displayed for Model 2390a.

Field or Button Description

Open Sample File Click to open the Open Sample Information File window.
button

Start Report button Click to open the Start Report window.

Start Analysis button Click to display the Analysis window.

QuickStart Analysis Click to display the QuickStart Analysis window.


button

SPC Control Chart Click to display the Control Chart window.


button

6-8 239-42828-01 - Dec 2012


Gemini VII Enable Manual Control

Instrument Schematic Components

Component Description

Valve - open. The icon color changes to green when open.

Valve - closed. The icon color changes to yellow when closed.

Servo Valve

Elevator

The following components cannot be controlled manually.

Component Description

Reservoir for the balance tube (left side) and sample tube.

Volume adsorbed transducer (upper) and the differential pressure


transducer. The reading for the Volume Adsorbed transducer is displayed
just above its symbol. The reading for the sample pressure transducer is
displayed just below the analysis servo valve and valve 5-s.

Balance volume adjustment. Can be adjusted only by a Micromeritics


service representative.

Pressure relief valve. Prevents excessive pressure build-up in the event of


abnormal operation.

Represents the balance tube (left side) and the sample tube.

239-42828-01 - Dec 2012 6-9


Enable Manual Control Gemini VII

Component Description (continued)

Saturation pressure (Po) tube. Not displayed for Gemini VII 2390a.

Po tube, valve, and


transducer reading not
displayed on Model
2390a

System Valves
Select Unit [n] > Show Instrument Schematic to display the instrument schematic.

Valves Description

1 Vacuum valve

2 Adsorptive valve

3 Helium valve

4-b Balance reservoir valve

4-s Analysis reservoir valve

5-b Balance port valve

6-10 239-42828-01 - Dec 2012


Gemini VII Enable Manual Control

Valves Description (continued)

5-s Analysis port valve

6 Po port valve (Models 22390a and 2390t)

Instrument Schematic Shortcut Menus


Each manually controlled component has a shortcut menu displaying the operations available for that
particular component such as, Open, Close, Pulse. To access the shortcut menu, hover the mouse cur-
sor over the component and right click.

Shortcut Icon Description

When the cursor changes to this icon, right click to display options for the
selected component:
• For Valves:

Open - opens the selected valve. The valve symbol changes to green. An
alternate method is to either double click the valve or select the valve
and press the keyboard spacebar to turn it off/on.
Open Both - opens valves 4b and 4s or valves 5b and 5s. The valve
symbol changes to green. An alternate method is to either double click
the valve or select the valve and press the keyboard spacebar to turn it
off/on.
Close - closes the selected valve. The valve symbol changes to yellow.
An alternate method is to either double click the valve or select the valve
and press the keyboard spacebar to turn it off/on.
Close Both - closes valves 4b and 4s or valves 5b and 5s. The valve
symbol changes to yellow. An alternate method is to either double click
the valve or select the valve and press the keyboard spacebar to turn it
off/on.
Pulse - select to quickly turn the valve on and off allowing the operation
to proceed in small increments.
• For Balance Servo Valve:

Enable - enables the balance servo valve. Operations for the Sample
servo will also be performed by the Balance servo.
Disable - disables the balance servo valve. Operations for the Sample
servo will also be ignored by the Balance servo.

239-42828-01 - Dec 2012 6-11


Show Instrument Schematic Gemini VII

Shortcut Icon Description (continued)

• For Servo Valve

On/Off - turns the servo valve on or off.


Increase / Decrease - increased pressure by dosing the sample.
Decreases pressure by evacuating the sample.
Enter target - displays the Servo Valve Settings window. The entered
target pressure displays to the left of the sample servo valve icon.

When the cursor changes to this icon, right click to display options for the
elevator:
• Raise - raises the elevator. Select Raise and press the keyboard space
bar to raise/lower the elevator.

• Lower - lowers the elevator. Select Lower and press the keyboard space
bar to raise/lower the elevator.

• Stop - select to stop the elevator from raising or lowering.

Show Instrument Schematic


Unit [n] - Show Instrument Schematic

Use to display an analyzer schematic. To operate the valves and elevator from this window, Manual
Controls must be enabled (Unit [n] > Enable Manual Control).

Po tube, valve, and


transducer reading not
displayed on Model
2390a

6-12 239-42828-01 - Dec 2012


Gemini VII Show Status

Refer to Enable Manual Control, page 6-8 for additional details on this schematic.

Valve State Description

Green indicates an open valve.

Yellow indicates a closed valve.

Show Status
Unit [n] > Show Status

Use to show only the status window of the analyzer.

If multiple instruments are attached to the computer, the status window for each
instrument is displayed in a different color.

The buttons across the bottom of the window are described in Enable Manual Control, page 6-8.

The status window shows the current status for each port. Use this option if:

• there is an automatic operation in progress and the sample file needs to be edited.

• there are multiple units attached to the computer. Select Show Status on each unit menu and have
the status for all units displayed at one time.

239-42828-01 - Dec 2012 6-13


Show Status Gemini VII

Field or Button Description

Analysis status bar • Preliminary - evacuation and free space measurement. Displays green
during progression.

• Analysis - data are collected. Displays blue during progression.

• Termination - the device lowers the elevator and analysis terminates.


Displays grey during progression.

Analysis details Sample Sample file number


Stage Stage of the analysis (as in status bar)
Last Point Last point and number of points requested
P Absolute pressure of last point
P/Po Relative pressure of last point
Q Quantity adsorbed
Po Absolute pressure of last measured or entered saturation
pressure (Po)
Run Time Elapsed time since the start of analysis

Step details Provides details of the current step in the analysis process.

Open Sample File


button
Start Report button
Start Analysis button
Refer to Enable Manual Control, page 6-8.
QuickStart Analysis
button
SPC COntrol Chart
button

6-14 239-42828-01 - Dec 2012


Gemini VII Show Instrument Log

Show Instrument Log


Unit [n] > Show Instrument Log

Use to display a log of recent analyses, calibrations, errors or messages. This information is logged for
a 7-day period for analyses and a 30-day period for messages and calibrations.

Field or Button Description

Analysis /  Select which logs to display.


Calibration / Message
checkboxes

Add Log Entry button Click to manually enter information into the instrument log window, for
example, Changed the port filter. To enable the Add Log Entry button,
enter information into the text box, then click Add Log Entry. The entry
then appears in the information log.

Report button Click to display the Log Report Settings window to specify report output
options.

Analysis status bar Refer to Show Status, page 6-13.


Analysis details
Step details

239-42828-01 - Dec 2012 6-15


Unit Configuration Gemini VII

Unit Configuration
Unit [n] > Unit Configuration

Use to display hardware/software configurations, calibrations and gas selections of the connected
analyzer.

Field or Button Description

Configuration  Displays the IP address used by the analysis program and the serial number
group box of the selected analyzer.

Software Versions Displays the software versions of the MIC BIOS, controller and analysis
group box program.

Last Measured Po Displays the value for the last measured saturation pressure.

Volume Displays the volume correction of the attached analyzer. If a different value
Correction text box is entered in this field, it is stored with sample data at the start of an
analysis. The value in this field is used in a calculated free space.

Change IP button Click to display the Unit IP Setup window. Shows the IP address and
Subnet mask assigned during installation. Do not edit these fields unless
instructed by a Micromeritics service representative.

Restore Factory Deletes all stored analysis data and resets instrument parameters to factory
Defaults button defaults. It does not affect sample and parameter files.

Cancel button Refer to Common Fields and Buttons - Unit Menu Options, page 6-2.
OK button

6-16 239-42828-01 - Dec 2012


Gemini VII Diagnostics

Diagnostics
Unit [n] > Diagnostics

Use to clean and verify gas lines when connecting or changing a gas. Refer to Cleaning and Verifying
the Gas Line, page 9-22. Also used to perform diagnostic tests requested by a service representative.

This option is typically used and/or requested by a service representative. These tests create and save
files to the Gemini VII\Service\USERDIAG directory. The service representative may request an
emailed or faxed copy of the file for diagnostic purposes.

Field or Button Description

Test dropdown list Click to select the diagnostic test to run.

Operator text box Enter an operator name or ID.

Repeat button Click the repeat the previous test. Enabled when the previous test is
complete.

Start / Next button Starts the analysis and displays a graph during analysis. When the first
analysis is complete, the Start button changes to Next.

Report after analysis


button
Refer to Start Analysis, page 6-2.
View dropdown
Close button

239-42828-01 - Dec 2012 6-17


Diagnostics Gemini VII

Field or Button Description

View dropdown Refer to Start Analysis, page 6-2.

Skip button Click to skip an analysis. This button is only visible when an analysis is in
progress. Select the ports containing the analysis to skip.

Suspend / Resume Click to suspend or resume an analysis in progress. Select the ports
buttons containing the analysis to suspend or resume.

Report button Click to view a list of reports to be generated during the test.

Report dropdown list Select a report to generate.

Item [n] dropdown list Click to select the data available for the current window.

Repeat button Click to repeat the last test.

Start button Click to start the test.

Item [n] dropdown list Click to select the data available for the current window.

Cancel button Refer to Common Fields and Buttons - Unit Menu Options, page 6-2.

6-18 239-42828-01 - Dec 2012


Gemini VII Calibration

Refer to Report Tool Bar, page 7-14 for additional information on viewing, customizing, and printing
reports.

Calibration
Unit [n] > Calibration

Use to perform system calibrations. Disabled calibration options can be accessed only with the assis-
tance of a service representative and are not covered in this manual.

239-42828-01 - Dec 2012 6-19


Calibration Gemini VII

Zero Pressure
Unit [n] > Calibration > Zero Pressure

Use to evacuate the manifold and zero out the selected transducers. Refer to Zero Pressure, page 9-30.

Match Transducers
Unit [n] > Calibration > Match Transducers

Use to zero and match the selected transducers to the main manifold transducer. Refer to Match
Transducers, page 9-31.

This option is disabled for the Gemini 2390a.

6-20 239-42828-01 - Dec 2012


Gemini VII Calibration

Reset Pressure Calibration


Unit [n] > Calibration > Reset Pressure Calibration

Use to reset the unit’s pressure scale to factory defaults.

Sample Servo
Unit [n] > Calibration > Sample Servo

Use to calibrate the servo valve to the sample pressure transducer. The sample pressure transducer
should be calibrated before starting this calibration procedure. The servo valve should always be reca-
librated after a pressure calibration has been performed. Refer to Sample Servo, page 9-31.

Balance Servo
Unit [n] > Calibration > Balance Servo

Use to calibrate the balance servo valve. Ensure that empty sample tubes are installed on the sample
and balance ports.

239-42828-01 - Dec 2012 6-21


Calibration Gemini VII

Save to File
Unit [n] > Calibration > Save to File

Use to save the current calibration settings to a backup file which can later be reloaded using Unit [n]
> Calibration > Load from File menu option.

Field or Button Description

File name dropdown list The default file naming convention for calibration files can be used
or the filename can be changed. The default file name is interpreted
as:
0217 - 2011-06-10.CAL

File name extension

Date calibration file was saved


Instrument serial number

6-22 239-42828-01 - Dec 2012


Gemini VII Service Test

Load from File


Unit [n] > Calibration > Load from File

Use to load a previously saved calibration file.

It is recommended that the current calibration settings be saved using Unit [n] > Calibration > Save to
File prior to loading another calibration file. When loading a previously saved calibration file, a
backup of the current file is created and saved as [SN]last.cal. The backup file is overwritten each time
a new one is created.


Changing the calibration may affect the instrument’s performance.

Service Test
Unit [n] > Service Test

Use for service tests performed only with the assistance of a trained Micromeritics service representa-
tive. These tests provide the service representative with troubleshooting tools and readouts.

This option is enabled only when the analysis program is operating in Service Test mode. Refer to
Service Test Mode, page 8-4.

239-42828-01 - Dec 2012 6-23


Service Test Gemini VII

6-24 239-42828-01 - Dec 2012


Gemini VII Introduction

7. REPORTS MENU

Introduction
This chapter contains information specific to the Reports menu options used to customize and run
reports. This chapter provides details of Reports menu options, commonly used functions and buttons,
field-by-field descriptions, and sample reports.

Reports can be generated for data:

• collected on a sample that has completed analysis


• collected on a sample currently being analyzed
• manually entered

239-42828-01 - Dec 2012 7-1


Common Fields and Buttons - Reports Menu Options Gemini VII

Common Fields and Buttons - Reports Menu Options


The following fields and buttons are common to many of the report files. References are made to these
fields and buttons throughout this chapter.

Field or Button Description

Browse button Click to locate another file.

Cancel button Closes the window and cancels any unsaved changes.

Destination  Refer to Common Fields and Buttons - File Menu Options, page 5-1.
group box

File name text box Select the file to print (or open) from the Name column. The file name will
appear in the File name text box. Click Open or double-click the file name
in the Name column to open the file. Multiple files can be selected by
holding down the Ctrl key on the keyboard while selecting multiple files.

From / To text boxes Enter the From and To range for autoscaling the X- and/or Y-axes.

Name column Displays a list of files in the selected directory.

OK button Click to save and close the active window.

Open button Click to open the selected file (or double-click the file name in the Name
column to open the file).

Report button Click to generate the report.

Save button Saves the active file.

Show graphic  Select to show a graphic on the report header. Click the Browse button to
checkbox and text box locate the graphic in either .BMP or .EMF format.
• Height / Width - enter the height and width of the selected graphic.
These values determine the graphic appearance on the generated report.

Start Report
Reports > Start Report > [file] (or use the F8 keyboard shortcut)

Use to generate a report on a sample analysis.

7-2 239-42828-01 - Dec 2012


Gemini VII Close Reports

Close Reports
Reports > Close Reports (or use the F9 keyboard shortcut)

Use to close all open report windows. This option is unavailable if reports are being generated.

Open Report
Reports > Open Report > [file]

Use to open a saved report.

SPC Report Options


Reports > SPC Report Options

Use to generate reports with various SPC (Statistical Process Control) options. All selected variables
must be computed for each sample file used in an SPC report; therefore, it is more efficient to select
only the necessary variables.

The selected items appear as options on the Reports > Regression Report screen as selections in the
dropdown boxes and are used in graph selection in Reports > Control Chart.

239-42828-01 - Dec 2012 7-3


SPC Report Options Gemini VII

If additional report options are required, click the More button.

The selected items also appear as options on the Reports > Control Chart screen. (Click the Graph [n]
button, then click the Statistic dropdown arrow.)

7-4 239-42828-01 - Dec 2012


Gemini VII Regression Report

Regression Report
Reports > Regression Report

Use to generate an SPC (Statistical Process Control) Regression report to determine the interdepen-
dency between two variables. Up to three dependent variables (Y-axis) may be plotted against a single
independent variable (X-axis). The degree of correlation between the variables is also reported.

Field or Button Description

Show report title checkbox Select and enter a report title to appear on the report header.
and text box

Show graphic  Select to show a graphic on the report header. Click the Browse button
checkbox and text box to locate the graphic in either .BMP or .EMF format.
• Height / Width - enter the height and width of the selected graphic.
These values determine the graphic appearance on the generated
report.

X- and Y-Axis  Use to designate the X- and Y-axes variables. The variables in the
Variable  dropdown lists are those selected in the Reports > SPC Report Options
dropdown lists window. Use these options to plot the regression of up to three Y-axis
variables against the X-axis variable.

Axis Range  Enter the beginning and ending values for the X- and Y-axis ranges.
text boxes These fields are disabled if Autoscale is selected.

Autoscale checkboxes When enabled, allows the X- and Y-axes to be scaled automatically.

239-42828-01 - Dec 2012 7-5


Regression Report Gemini VII

Field or Button Description (continued)

Tabular report checkbox Select to generate a tabular report of the included samples. A tabular
report contains the numeric values contributed by each sample.

Recalculate archived  Select to have archived SPC values recalculated ensuring any changes
SPC results checkbox made to the SPC Report Options are included in the new report.
Selecting this option lengthens the time required to generate the report.

Label data checkbox Select to label the points on the plot to correspond with the values in
the sample files.

Samples button Click to select sample files for report generation. Multiple files can be
selected by holding down the Ctrl key on the keyboard while selecting
the files.

• Available Files - contains files located in the directory specified in


the Look In text box.

• Selected Files - files added from the Available Files list box.

• Use all files in this directory - click to select all files in the
Available Files list box. The Add and Remove buttons become
disabled.

• Add / Remove buttons - select a file in the Available Files list box
and click Add to move the file to the Selected Files list box. Or
select a file in the Selected Files list box and click Remove to move
the file back to the Available Files list box. Or double-click the file
name to move the file from one list box to the other.

• Click OK to display the Regression Report window.

7-6 239-42828-01 - Dec 2012


Gemini VII Control Chart

Field or Button Description (continued)

Report button Click to view the report for the items selected.

Save as Default button Click to save selected report options as default report settings.

Browse button
Cancel button Refer to Common Fields and Buttons - Reports Menu Options,
page 7-2.
Destination group box
From / To text boxes
OK button

Control Chart
Reports > Control Chart

Use to generate an SPC (Statistical Process Control) control chart report which plots the changes in a
statistic.

239-42828-01 - Dec 2012 7-7


Control Chart Gemini VII

Field or Button Description

X Axis Order by  Select the order in which X-axis statistics are placed.
group box
• Time - sorts by the time the files were analyzed.

• File name - sorts in alphanumeric order.

• Date - sorts by the date the files were analyzed.

• Minutes - sorts by the minutes elapsed from the first file placed on the
list, which is the earliest-analyzed file.

• Days - sorts by the number of days elapsed from the first file placed on
the list, which is the earliest-analyzed file.

Graph [n] buttons Click to define the Y-axis of each graph.

• Y-Axis group box -

Statistic dropdown list - displays the SPC variables selected at Reports


> SPC Report Options window. The selected variable will be plotted
against time. This selection also becomes the Y-axis label.
Autoscale checkbox - allows the Y-axis to be scaled automatically. To
specify a range, deselect this option and enter a range in the From and
To fields.

7-8 239-42828-01 - Dec 2012


Gemini VII Control Chart

Field or Button Description (continued)

Graph [n] buttons • Center Line group box - displays placement options for the center line
(continued) in the graph. Choose Entered to specify placement of the line.

• Limit Lines group box - displays limiting lines options. Lines can be
placed at some multiple of the standard deviation or at specified
positions (Entered). When Entered is selected, enter the High limit
and Low limit fields with appropriate values.

Show report title


checkbox and text box
Show graphic
checkbox and text box
Tabular report
checkbox Refer to Regression Report, page 7-5.
Samples button
Destination group box
Save as Default button

Browse button
Cancel button Refer to Common Fields and Buttons - Reports Menu Options, page 7-
2.
Report button

239-42828-01 - Dec 2012 7-9


Heat of Adsorption Report Gemini VII

Heat of Adsorption Report


Reports > Heat of Adsorption

Use to select sample files, define quantities and generate a Heat of Adsorption report. The isosteric
heat of adsorption is an important parameter for characterizing the surface heterogeneity and for pro-
viding information about the adsorbent and the adsorption capacity. Multiple adsorption isotherms are
obtained on the same sample using the same adsorptive but at different temperatures to obtain the heat
of adsorption.

Field or Button Description

Table Contains files added by using the Add Samples button. Also provides the
quantity adsorbed.

Add Samples button Click to add a sample file to the table.


1. Click the Add Samples button.

2. Double-click the file in the Name column or select the file name and
click Open.

Remove Sample  Click to remove the selected sample from the list.
button

7-10 239-42828-01 - Dec 2012


Gemini VII Heat of Adsorption Report

Field or Button Description (continued)

Clear Samples  Click to remove all samples from the table.


button

Edit Quantities  Use to specify the range of surface coverage to include in the report.
button

• Insert Range button - click to specify the starting and ending quantities
adsorbed and number of points to insert.

• Insert button - insert a row above the selected row.


• Delete button - deletes the selected row.
• Clear button - clears the entire table of all entries except one.
• Append button - inserts one row at the end of the table.
• Load Table button - click to import values from another file.
• Save Table button - save the current table as a. QNT file.
• Apply button - click to apply all table changes.
• Close button - click to close the table without saving changes.

239-42828-01 - Dec 2012 7-11


Report Features and Shortcuts Gemini VII

Field or Button Description (continued)

Tabular report Refer to Regression Report, page 7-5.


checkbox

Isostere plot Select to generate a graph showing quantities of gas adsorbed versus the
checkbox temperature.

Heat of adsorption  Select to generate the Heat of Adsorption data in a graphical format.
plot checkbox

Open button Click to select and open a Heat of Adsorption file.

Browse button
Cancel button Refer to Common Fields and Buttons - Reports Menu Options, page 7-
2.
OK button
Report button
Save button

Report Features and Shortcuts

Reports
List Box

Generated
Report
Tabs

Header

Data display
(either graphical
or text)

Tool Bar

7-12 239-42828-01 - Dec 2012


Gemini VII Report Features and Shortcuts

Report Header
All reports contain a header displaying file statistics.

If configured, the report header can also contain a graphic and a title.

• Tabular and graphical reports contain sample and instrument statistics such as analysis date / time,
analysis conditions, etc.

• The headers contain notes of sample file changes occurring after analysis.

• Summary report headers contain the same information as tabular and graphical reports with the
exception of notes.

239-42828-01 - Dec 2012 7-13


Report Features and Shortcuts Gemini VII

Report Tool Bar

Each report has a tool bar and selectable tabs across the top of the report header. To view a specific
report, select its tab or select the report in the Reports list box and click Show.

Reports can be customized and manipulated using the tool bar, shortcut menus, the zoom feature, or
axis cross-hairs.

Field or Button Description

Reports list box Contains a list of all generated reports. The same reports display as tabs
across the top of the report header unless the report has been hidden
using the Hide button.

Show button Jumps to the selected report in the Reports list box (or select the report
tab to show the report). If the report tab has been hidden using the Hide
button, click Show to display the report and tab.

Delete button Deletes the selected report. Deleted reports will have to be regenerated if
deleted in error.

Hide button Hides (or temporarily removes) the selected report from the tabbed view.
The report name remains in the Reports list box. To redisplay the tab,
select the report in the Reports list box and click Show.

7-14 239-42828-01 - Dec 2012


Gemini VII Report Features and Shortcuts

Field or Button Description (continued)

Print button Displays a print window for report output.

• Printer group box - 

Name dropdown list and Properties button - select the printer and
click the Properties button to change printout orientation, etc.

• Current button- selects the active report (or selected tab).


• All button - selects all reports in the Reports list box.
• Shown button - selects only the reports not hidden.
• Clear button - clears all selections.
• OK button - prints the selected report to the printer indicated.
• Cancel button - closes the Print window.
• Copies group box - select the number of copies and collate option.

Save button Saves all reports of the active file using the sample file name with a
.REP file extension.

Save As button Saves all selected reports to the indicated file format:
• .REP (Report system) - saves the report in a format that can be
opened within the program.

• .TXT (ASCII text) - saves the report as a common machine language


file.

• .XLS (Spreadsheet file) - saves the report in a format that can be


opened within a spreadsheet program.

239-42828-01 - Dec 2012 7-15


Report Features and Shortcuts Gemini VII

Field or Button Description (continued)

Default Style button Click to specify default report parameters for fonts and curve properties.

• Font group box -

Font Type list box - allows font type and attributes to be edited for
the selected item. Select an item in the list, click Edit, and select
from various font options. Click OK when done.

7-16 239-42828-01 - Dec 2012


Gemini VII Report Features and Shortcuts

Field or Button Description (continued)

Default Style button • Curve group box -


(continued)
Thickness text box - enter a thickness number for the curve.
Histogram Fill dropdown list - select a histogram fill option from
the list.
• Graph border line thickness text box - enter a thickness number for
the graph border.

• Load button - click to load the last saved default settings.

• Save button - click to save the changes as the new default settings.

• Close button - click to close the window and save the changes for the
current report.

Report Shortcut Menus


Shortcut menus are accessed by right-clicking on the report header or the report body displayed on the
screen.

Report Header Shortcuts


Display header shortcuts by right-clicking in the report header.

Option Description

Edit Select to edit the report title and/or graphic to display in the report header.

Copy header as text Select to copy the report header as text. Text is copied to the clipboard and
can then be pasted into other documents.

239-42828-01 - Dec 2012 7-17


Report Features and Shortcuts Gemini VII

Tabular Reports Shortcuts

Display tabular report shortcuts by right-clicking in the body of the tabular report. Column shortcuts
require right-clicking on the column to be modified.

Option Description

Resize column Right-click on the column to be resized. Select Resize Column on the
shortcut menu and enter the new column width in inches.

Rename column Right-click on the column to be renamed. Select Rename Column on the
shortcut menu and enter the new column name.

Move column Right-click on the column to be moved. Select Move Column on the
shortcut menu and select Left or Right for the move.

Align column Right-click on the column to be aligned. Select Align Column on the
shortcut menu and select Left, Right or Center.

Hide column Select a column to hide from the list of columns.

Show column Displays a list of all hidden columns. Select a column to show.

Table data font Right-click in the report data. Select Table data font on the shortcut menu.
Deselect the Use default font to enable font options. Select new font
attributes for the report data. To return to the default fonts, select the Use
default font checkbox.

Table header font Right-click in the report data. Select Table header font on the shortcut
menu. Deselect the Use default font to enable font options. Select new
font attributes for the header. To return to the default fonts, select the Use
default font checkbox.

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Gemini VII Report Features and Shortcuts

Option Description (continued)

Edit title Select to edit the report title and/or title font attributes.

Copy table as text Select to copy the report contents to the clipboard as tab delimited text. It
can then be pasted into another document.

Graph Shortcuts

Display graph report shortcuts by right-clicking in the body of the graph report.

Option Description

Autoscale all axes Returns the report to full view after using the zoom feature.

Reset axis limits to Removes the cross-hair and returns the graph back to the initial setting.
initial setting

Show curve /  Shows a hidden curve or hides a selected curve.


Hide curve

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Report Features and Shortcuts Gemini VII

Option Description (continued)

Edit curve Use to edit selected curve properties.

• Title text box - use to change the title of the selected curve.

• Style dropdown list - use to select another style for the collected data
curve.

• Curve group box - options are disabled if Histogram is selected in the


Style dropdown list. Use to change the interpolation, point style and
pen style for the selected curve.

Color button - click to change the curve color.


Use default thickness checkbox - select to use the default curve
thickness. Deselect the checkbox and enter a new thickness number in
the Thickness text box.
• Histogram group box - enabled only if Histogram is selected in the
Style dropdown list. Use to specify the type of fill, fill color and label
position for the selected curve.

• Label dropdown list - select where the graph point labels will display
(left, right, center, etc.) on the SPC report.

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Gemini VII Report Features and Shortcuts

Option Description (continued)

Graph Label

Edit axis Use to edit axis properties.

• Title group box - use to edit the selected axis label.

Title text box - use to modify the label of the selected axis.
Title font button - use to modify the font for the selected axis label.
Deselect the Use default font to enable font options. Select the font
attributes and click OK.
• Scale group box - use to change the graph display.

Linear / Logarithmic - select the option to scale the graph as linear or


logarithmic.

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Report Features and Shortcuts Gemini VII

Option Description (continued)

Edit axis  Autoscale minimum / maximum - select the Autoscale checkbox to


(continued) enable the option. To manually specify minimum / maximum, deselect
the Autoscale checkbox and enter the new amount in the text box.
Invert scale checkbox - select to invert the scale.
Scale font button - use to modify the font for the scale label. Deselect
the Use default font to enable font options. Select the font attributes
and click OK.
Gridlines Major / Minor dropdown lists - select to change how to
display major / minor gridlines.

Edit legend Select to change the legend location and font. Click Font to modify legend
fonts. Deselect the Use default font to enable font options.

Edit title Select to change the graph title and font. Deselect the Use default font to
enable font options.

Copy Graph Copies the graph to the clipboard. It can then be pasted into other
applications.

Copy Data Copies the report data to the clipboard. It can then be pasted into other
applications as tab-delimited columns of text.

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Gemini VII Report Features and Shortcuts

Other On-Screen Features

Zoom Feature
Use the zoom feature to closer examine graph details. To use this feature:

1. Open the graph.

2. Hold down the left mouse button and drag the cursor across the graphical area to be enlarged. A
box will display in the area to be enlarged.

3. Release the mouse button. The enlarged area fills the graph area. To return to normal view, right-
click in the graph area and select Autoscale all axes or Reset all axes to initial setting on the
shortcut menu.

Axis Cross-Hair

X-axis
position

Y-axis Point of


position Coordination

The cross-hair feature displays axis coordinates. To use this feature:

1. Click the left mouse button on the graph to view the cross-hair coordinates.

2. To remove the cross-hair, right-click in the graph area and select Autoscale all axes or Reset all
axes to initial setting from the shortcut menu.

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Report Examples Gemini VII

Report Examples
This section of the manual contains samples of some of the available reports. Most of the
reports can be customized.

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Gemini VII Report Examples

Isotherm Linear Plot

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Report Examples Gemini VII

BET Surface Area Report

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Gemini VII Report Examples

BET Surface Area Plot

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Report Examples Gemini VII

t-Plot

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Gemini VII Report Examples

BJH Adsorption Cumulative Pore Volume

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Report Examples Gemini VII

BJH Adsorption dV/dlog(w) Pore Volume

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Gemini VII Introduction

8. OPTIONS MENU

Introduction
This chapter contains information specific to the Options menu selections used to configure the system
by setting defaults for sample and parameter files.

This chapter contains information on:

• changing the default presentation format - Restricted, Basic, or Advanced


• specifying default parameters for sample information files and report option files
• specifying how units appear on application windows and reports
• specifying how graph grid lines appear on reports
• specifying the location of the parameter files shown in basic presentation mode.

Option Presentation
Options > Option Presentation

Use to change the default editing format - Restricted, Basic or Advanced. Each format type displays
sample information and options differently. For descriptions of the presentation types, refer to Sample
Defaults, page 8-2. When using Restricted format, a password is required to change to Advanced
format.

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Sample Defaults Gemini VII

Sample Defaults
Options > Sample Defaults

Use to specify default parameters for sample information files and report option files in either
Advanced, Basic, or Restricted format. The Restricted format requires a password when entering or
exiting the Restricted format. It is s typically used in laboratories where analysis conditions must
remain constant, for example, in the pharmaceutical industry. The Advanced format is not available
from the Restricted format.

Refer to Specifying Sample Defaults, page 3-1.

Restricted Format
Restricted format presents the sample information file in the same manner as the Basic format except
that the operator cannot switch to Advanced format. This format is password protected and is typically
used in laboratories where sample parameters must remain constant, for example, in pharmaceutical
laboratories.

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Gemini VII Units

Units
Options > Units

Use to specify how data should appear on the application windows and reports. This menu option is
not available if using Restricted format.

Graph Grid Lines


Options > Graph Grid Lines

Use to select how grid lines appear on reports. This menu option is not available if using Restricted
format.

Field or Button Description

X-Axis / Y-Axis Select major and/or minor lines to display in reports for the logarithmic and
options linear scales. To remove the gridlines, deselect these options.

Grid Line Styles  Select if the major and/or minor grid lines should appear as solid or dotted
options lines.

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Service Test Mode Gemini VII

Service Test Mode


Options > Service Test Mode.

Service Test mode is a password protected option used to perform certain service tests with the assis-
tance of a trained Micromeritics service representative. This password is supplied by your service
representative. After Service Test Mode has been enabled, the service tests are accessible from the Unit
menu (Unit > Service Test).

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Gemini VII Introduction

9. TROUBLESHOOTING AND MAINTENANCE

Introduction
The analyzer has been designed to provide efficient and continuous service; however, certain mainte-
nance procedures should be followed to obtain the best results over the longest period of time. This
chapter includes maintenance and calibration procedures.

Troubleshooting
Most operational problems are caused by:

• Leaks (commonly around the sample tube O-ring at the analysis port)
• Sample weighing errors
• Use of too much analysis bath fluid in the Dewar at the start of an analysis
• Entry of incorrect system volume for analysis
• Impure gas supply

When unexpected analysis results occur, check the above first. Some common operational problems
that are not indicated on the screen and their respective causes and solutions are provided in the fol-
lowing table:6

What Happened Why What To Do

Specified pressure not Sample or balance tube not Reattach sample and balance
reached. properly attached. tubes. Ensure both are securely
attached to ports. Replace O-
rings if defective. Refer to
Replacing Port Filter (Frit)
and O-ring, page 9-6.

Leak in gas line. Perform the Adsorptive and


Helium Line tests to determine if
a leak exists. Refer to
Diagnostics, page 6-17.

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Troubleshooting Gemini VII

What Happened Why What To Do (continued)

Unable to reach a Vacuum pump oil level is low or Inspect the oil to see if it is low
satisfactory vacuum. needs to be changed. or needs changing. Refer to
Inspecting and Changing
Vacuum Pump Oil, page 9-8.

Vacuum pump is leaking. Locate and repair the source of


the leak or replace pump.

Centering ring has become too Check the centering ring at the
flat and unable to hold a vacuum. pump intake port. Replace if
necessary. Refer to Replacing
the Alumina in the Oil Vapor
Trap, page 9-11.

Check the centering ring at the


top of the oil vapor trap. Replace
if necessary. Refer to Replacing
the Alumina in the Oil Vapor
Trap, page 9-11.

Nitrogen or helium drained Leak(s) in the gas line Perform the Adsorptive (or
from tank, or depleted in a connection. Helium) Line test to determine
short period of time. the location of the leak. Refer to
Diagnostics, page 6-17 for
details on these tests.

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Gemini VII Troubleshooting

What Happened Why What To Do (continued)

Unit does not work when Power cord not fully inserted at Insert power plug firmly into
power switch is turned on. one end. power source and analyzer power
connector.

No power at outlet. Plug in lamp or small appliance


to test outlet. If there is no power,
contact electrician.

Plug prongs bent so that contact Gently move power plug at outlet
not made at outlet. while watching power indicator
light. If indicator light comes on,
have electrician replace outlet or
plug.

Power cord damaged. Have electrician check cord


using a test meter. Replace the
cord if defective.

Loose internal connection or Call a Micromeritics Service


broken wire. Representative for repair or
replacement information.

Expected results are not Sample improperly degassed. Verify that the degassing
within range. temperature and degas time were
set properly.

Gas bottle(s) may be almost Replace gas bottle. Refer to


empty, causing gas impurity. Connecting Gases, page 9-18.

Undetermined Do the following:


1. Perform a blank analysis
(see Performing a Leak
Test, page 9-16). Print the
results.

2. Perform a reference material


analysis (see Performing a
Reference Analysis, page
9-28). Print the results.

3. Contact your Micromeritics


service representative.

239-42828-01 - Dec 2012 9-3


Preventive Maintenance Gemini VII

Preventive Maintenance
The following table lists the preventive maintenance procedures to keep the analyzer operating at peak
performance. Instructions for each procedure follow the table. Micromeritics also recommends that
preventive maintenance procedures and calibration be performed by a Micromeritics Service Repre-
sentative every 12 months.

Maintenance Required Frequency

Check and clean Dewar Weekly

Replace port filters and O-rings Every 3 to 6 months

Replace sample tube O-ring As required or every 3 to 6 months

Inspect and change vacuum pump fluid* As required or every 3 to 6 months

Replace alumina in oil vapor traps* As required

Clean the outside of the analyzer As required or every 6 months

Test analyzer for leaks As required or every 12 months

Replace vacuum pump exhaust filter As required or every 12 months

Replace diaphragm in vacuum pump (if an oil-free  Every 12 months


pump is used)**

* Oil-sealed vacuum pumps only.

** For oil-free pumps only: After 12 to 18 months of operation, the diaphragm in the pump will wear
out and the pump becomes completely inoperable. To prevent instrument downtime due to an
inoperable pump, it is recommend that the diaphragm be replaced by a Micromeritics Service Rep-
resentative every 12 months.

Recovering from a Power Failure


The analyzer saves entered and collected data in case of power failure. File parameters and any other
data entered will still be present when power is restored. If an analysis was in progress when the power
failure occurred, it will be canceled when the analyzer restarts. Any data collected during the analysis
will still be present, but the analysis should be started again in order to produce complete results.

9-4 239-42828-01 - Dec 2012


Gemini VII Preventive Maintenance

Lubricating Elevator Drive Assembly


The elevator screw is lubricated before it leaves the factory and should not require lubricating. If the
elevator starts to vibrate or becomes noisy when traveling, contact a Micromeritics Service Represen-
tative for disposition.

Cleaning the Analyzer


The exterior casing of the analyzer may be cleaned using a clean cloth, dampened with isopropyl alco-
hol (IPA), a mild detergent, or a 3% hydrogen peroxide solution. Do not use any type of abrasive
cleaner.

Do not allow liquid to penetrate the casing of the analyzer. Doing so could result in
damage to the unit.

Cleaning the Analysis Dewar


When handling Dewars, be sure to observe the Dewar precautions outlined in 
chapter 3.

Ice and suspended frost particles may accumulate in the bottom of an analysis port Dewar. Particles or
deposits exceeding 1/4-in. (0.64-cm) in depth may jam between the bottom of the sample tubes and the
bottom of the Dewar, causing the Dewar not to raise fully. Accumulations of fine particles impede liq-
uid nitrogen circulation around the bottom of the sample tubes. This causes the sample temperature to
be slightly higher which, in turn, can cause pore volume measurement errors in those samples exhibit-
ing high isotherm slope above 0.97 relative pressure.

Accumulated ice is likely to melt and form a pool of water in the Dewar if all liquid nitrogen evapo-
rates. The water must be removed, otherwise it will solidify when liquid nitrogen is added and could
press on the bottom of the sample tube causing breakage.

To ensure problems do not develop due to ice accumulation, check the Dewar after each use. Clean the
Dewar on a weekly basis.

1. Remove the sample tubes from the analysis ports.

2. Go to Unit [n] > Show Instrument Schematic to display the instrument schematic, then go to
Unit [n] > Enable Manual Control.

3. Right-click on the elevator icon and select Lower to lower the elevator to its lowest position.

4. Remove the Dewar and pour the liquid nitrogen from the Dewar into an appropriate cryogenic
container.

Do not pour liquid nitrogen directly into a sink. Doing so may cause drain pipes to
burst.

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Preventive Maintenance Gemini VII

5. Rinse the Dewar with warm water to melt any ice accumulation which may remain in the Dewar,
then dry thoroughly.

Replacing Port Filter (Frit) and O-ring


A filter (frit) is located in each analysis port. If the filter is contaminated, the contaminant may adsorb
or desorb during analysis, affecting the results. A contaminated filter on the analysis port may be indi-
cated as a leak or a free space reading much lower than normal.

A contaminated filter should be replaced as follows:

1. Select Unit [n] > Show Instrument Schematic, then Unit [n] > Enable Manual Control.

2. Right-click on the valve of the appropriate port and select Close to close the valve.

3. Use a wrench to remove the sample tube fitting from the port. Pry out the filter and O-ring.

O-ring

Filter (frit)

Sample tube fitting

To avoid degassing problems, the filter and O-ring should be clean and should not be
touched with bare hands.

4. Replace the filter and O-ring. Carefully reassemble the sample tube fitting and reinstall on the
sample port. Tighten by hand, then with a wrench to prevent leaks.

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Gemini VII Preventive Maintenance

Replacing the Sample Tube O-ring


It is important to maintain a vacuum-tight seal near the top of the sample tube stem. If an O-ring
becomes worn or cracked, it does not provide a good seal and will need to be replaced.

Before removing (or installing) a sample tube, ensure that the port valve is closed.
Observe the instrument schematic to verify valve status.

1. Holding the sample tube firmly with one hand, loosen the sample tube connector nut by turning
counterclockwise.

Be careful not to let the sample tube connector nut drop onto the bottom of the tube as
it may break the tube.

Be sure to use the proper size frit for the sample port. The instrument will not operate
properly if the incorrect frit size is used.

2. Carefully pull the sample tube down until it is free from the port. It may be necessary to grasp the
sample tube with both hands.

O-ring

Ferrule

Connector nut

3. Remove the O-ring from the top of the sample tube and replace it with a new one.

If the O-ring remains inside the sample port, use a pair of tweezers or needle-nose
pliers to remove it.

4. After the new O-ring is in place, insert the sample tube back into the sample port until it is fully
seated.

5. Slide the sample tube connector nut up the tube (the ferrule and O-ring will move along with the
connector nut). Then, turning clockwise, hand-tighten the connector nut to the sample connector.

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Preventive Maintenance Gemini VII

Inspecting and Changing Vacuum Pump Oil


This procedure is also shown in one of the How-To videos located on the Help menu.

The oil in the vacuum pump should be changed every three months when the efficiency of the vacuum
pump declines (requiring increased time to reach vacuum levels) or if it becomes discolored. The oil is
easily inspected to determine if a change is necessary.

Inspecting the Oil


View the vacuum pump oil through the oil-level window. The oil level should be midway between the
indicators on the oil-level window when the pump is running. Oil in good condition is clean, clear or
light in color and transparent.

Oil-level window

• Change the oil if it has darkened.


• Add oil if it is below the midway level when the pump is running.

Changing or Adding Oil


Always drain the vacuum pump while the pump is warm and disconnected from the
power source.

Use oil supplied by Micromeritics or refer to the vacuum pump manual for other acceptable oils.

1. Unplug the vacuum pump from the power source.

9-8 239-42828-01 - Dec 2012


Gemini VII Preventive Maintenance

2. Loosen the wing nut on the clamp at the top of the oil vapor trap. Swing the clamp open and
remove the trap from the hose.

3. Grasp the handle on top of the vacuum pump and place it on a work table.

If adding oil, skip to step 5.

4. Drain the used oil:

a.) Place a waste container under the drain spout.

b.) Remove the plug from the drain spout and allow the oil to drain into the waste container.

c.) Replace the drain plug.

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Preventive Maintenance Gemini VII

5. Remove the plug from the oil-fill port.

Oil-fill port

6. Slowly add oil to the port until the level is midway between the indicator lines in the oil-level
window when the pump is running.

Midway level

Do not allow oil to rise above the midway position when the pump is running. Doing so
may cause oil to splash into the oil filter and contaminate it.

7. Check the washer or O-ring used at the oil-filling port and replace if necessary.

8. Insert the oil-fill plug and turn clockwise to tighten.

9. Check the alumina in the oil vapor trap. If most of the pellets are no longer white, replace the
alumina before reattaching the vacuum pump.

10. Reconnect the vacuum pump hose.

11. Reconnect the power cord to the power source.

12. Allow the pump to run a few hours (overnight if possible) to eliminate air and moisture from the
fresh fluid and to produce efficient vacuum operations.

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Gemini VII Preventive Maintenance

Replacing the Alumina in the Oil Vapor Trap


The activated alumina in the oil vapor trap becomes saturated during use. The alumina should be
inspected periodically and replaced when most of the alumina pellets are no longer white.

Do not perform the following procedure on used alumina. The resultant oil vapors may
cause a fire or an explosion.

1. Disconnect the vacuum pump from the analyzer and place it on a work table.

2. Loosen the wing nut on the clamp at the top of the oil vapor trap. Swing the clamp open and
remove the trap from the hose.

3. Loosen the wing nut on the clamp at the bottom of the oil vapor trap. Swing the clamp open and
remove the trap.

4. Remove one end fitting from the trap body and dispose of the used alumina in an appropriate
manner.

5. Wash the trap body with a detergent-based soap. Rinse with water, then rinse with isopropyl or
ethyl alcohol. Set the trap aside and allow to dry thoroughly.

Exposure of the trap body to oil vapor may cause small cracks on the inside surface of
the trap body. Under normal circumstances, these cracks will not cause problems or
leaks.

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Preventive Maintenance Gemini VII

Do not perform the following procedure on used alumina. The resultant oil vapors may
cause a fire or an explosion.

6. Prepare fresh alumina as follows:

a.) Preheat the oven to 300 °C.

b.) Pour approximately 180 grams of fresh alumina into a glass or metal container
(approximately 250 mL if a graduated beaker is used). Place the container in the oven.

c.) Bake the alumina for two hours at 300 °C.

d.) Remove the baked alumina from the oven and allow it to cool until luke warm. A desiccator
may be used to speed the cooling process.

7. Use a small spatula to gently pry the O-ring from the end fittings of each end of the trap body.

8. Inspect the O-rings:

• If dusty, clean with a lint-free tissue.


• If damaged, replace with a new O-ring.

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Gemini VII Preventive Maintenance

9. Screw one of the end fittings onto the trap body.

10. Ensure the trap body is dry and the alumina is lukewarm. Pour the alumina pellets into the trap
until level with the top of the trap body.

11. Screw the other end fitting back onto the trap and tighten securely by hand.

12. Lightly tap both ends of the trap body on the work surface to remove remaining dust from the
pellets.

13. Inspect the centering ring before placing it back on the intake port. If it appears to be flattened,
replace it. A flattened centering ring can cause vacuum leaks.

There are two types of centering rings. Use the one with the smaller opening at the intake port.

14. Place the centering ring in place on the intake port.

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Preventive Maintenance Gemini VII

Centering ring

15. Place the trap on the centering ring.

16. Open the clamp and place it around the flange of the intake port and the flange of the trap. Swing
the clamp fastening screw toward the intake port until it fits into the slot in the other half of the
clamp. Tighten the wing nut securely by hand.

17. Reconnect the hose from the analyzer to the oil vapor trap.

a.) Place the clamp around the vacuum pump hose flange and vapor trap.

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Gemini VII Preventive Maintenance

b.) Swing the c-clamp fastening screw around until it fits into the slot on the other half of the
clamp. Tighten the wing nut securely by hand.

18. Plug the pump power cord into the power source.

19. Allow the pump to run a few hours (overnight if possible) to eliminate air and moisture from the
fresh oil and to produce efficient vacuum operations.

Changing the Vacuum Pump Exhaust Filter


The gases used by the analyzer are exhausted by the vacuum pump. An exhaust filter is installed on the
exhaust port of oil-filled pumps. The filter minimizes the release of oil vapor and should be replaced
when it becomes so saturated with oil that it is ineffective.

Exhaust filters are used to minimize the release of oil vapors. The gases are diluted
substantially upon release from the vacuum pump; however, it may be necessary in
some locations to provide a fume hood for protection from hazardous gases and
vapors released into the work area.

1. Turn the power to the unit off by either removing the plug from the power source or by turning the
power switch to the OFF position.

2. Loosen the wing nut of the clamp at the vacuum pump exhaust port. Swing the clamp away from
the exhaust port and remove it.

3. Remove and discard the exhaust filter. Do not remove the centering ring.

4. Make sure the centering ring is in place on the exhaust port.

5. Place the new filter on the centering ring.

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Preventive Maintenance Gemini VII

6. Open the clamp and place it around the exhaust port flange and the exhaust filter flange. Swing
the clamp fastening screw toward the exhaust port until it fits into the slot in the other half of the
clamp. Tighten the wing nut securely by hand.

7. Turn the power to the unit on by replacing the plug back into the power source or by turning the
power switch to the ON position.

Performing a Leak Test


A service representative may request that a leak test be performed to determine if there is a system
leak. The service representative may request a copy of the report generated by this test.

The following information is displayed during the test:

• Prompts on preparing the instrument for the test


• Approximate time period of the test
• Prompts in which an operator response is required

1. To start diagnostic testing, go to Unit [n] > Diagnostics.

2. Click the down arrow in the Test field and select System Leak Test Rev. [rev].

3. Select Report after test and Preview as the destination. Click OK.

4. Click Next. Data will be inserted into the window as they are collected.

5. A popup window indicates the test is complete. Click OK, then click Close.

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Gemini VII Preventive Maintenance

6. The report is generated and displayed on the screen.

7. Verify that all tests have a Passed status by clicking the tabs and looking for the Passed status for
each test run.

8. Click Save As and accept the default name displayed in the File name field.

9. Click Save. Make a note of the directory and filename, then click Close.

10. E-mail the file to the service representative requesting the report.

239-42828-01 - Dec 2012 9-17


Connecting Gases Gemini VII

Connecting Gases

This procedure is also shown in one of the How-To videos located on the Help menu.

Guidelines for Connecting Gases to the Analyzer


Guidelines when installing regulators and gas lines:

• Place gas bottles close to the analyzer. Using gas line extenders on gas bottles located in remote
areas may degrade gas quality and reduce pressure.

• Use a retaining strap (or other appropriate tether) to secure the gas bottle.

• Carefully route the gas lines from the bottle to the analyzer avoiding overlapping or entangling gas
lines.

• Label the gas line at the instrument inlet for proper identification and maintenance.

• Ensure the gas bottle is closed before connecting to the analyzer.

The following instructions describe a typical installation. Some configurations require additional com-
ponents, for example, regulator expansion kits, when one gas source will be used for several operations
or when the gas bottle cannot be located close to the analyzer.

In order to use oxygen, the analyzer must be equipped with an oxygen-compatible


vacuum pump that uses Fomblin® (or a suitable equivalent) pump oil or a dry pump.
Failure to use the proper vacuum system could result in hazardous conditions
including fire and personal injury.

Disconnecting the Depleted Bottle


1. Close the gas bottle shut-off valve then open the regulator shut-off valve.

Gas bottle
shut-off valve

Regulator
shut-off
valve

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Gemini VII Connecting Gases

2. Both gauges should read at or near zero. If not, open the regulator gas shut-off valve to release
gas. It is not necessary to disconnect the gas line from the regulator or the instrument.

3. Use an appropriate wrench to loosen the nut at the regulator/gas bottle connection then remove
the regulator from the bottle.

Regulator gas shut-


off valve

4. Replace the protective cap on the depleted bottle. Disconnect the retaining strap and remove the
bottle from its current location.

Connecting a Replacement Gas Bottle


Move the replacement bottle close to the instrument and tether it into place. It is not necessary to dis-
connect the gas line from the regulator or the instrument.

When connecting hazardous gases, ensure there is proper ventilation and always
follow the safety procedures established for your lab.

A power failure or loss of cryogen can result in dangerous pressures in the sample
tube. The analyzer uses pressure relief valves to vent this pressure into the instrument
cabinet and return the instrument to a safe condition. When using toxic or flammable
gases, additional venting of the cabinet may be required.

1. Use an appropriate cylinder wrench to remove the protective cap from the replacement bottle.

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Connecting Gases Gemini VII

2. Attach the gas regulator to the gas bottle connector. Hand-tighten the nut then use an appropriate
wrench to tighten an additional 3/4 turn.

Overtightening the fitting may cause a leak.

3. Check for leaks at the high-pressure side of the regulator and in the connector.
HIgh-pressure Gauge

Gas bottle
shut-off valve

Regulator
Regulator connector nut
control knob

a.) Turn the regulator control knob fully counterclockwise.

b.) Slowly open the gas bottle shut-off valve then close it.

c.) Observe the pressure on the high-pressure gauge.

• If the pressure is stable, proceed with the next step.


• If the pressure decreases, tighten the regulator connector nut until it becomes stable. 

4. Purge the air from the lines.

Gas bottle
shut-off valve

Regulator
shut-off valve

9-20 239-42828-01 - Dec 2012


Gemini VII Connecting Gases

a.) Turn the regulator clockwise until the low pressure gauge shows a few pounds of pressure.

b.) Turn the regulator shut-off valve counterclockwise to open.

c.) Open the gas bottle shut-off valve to flow gas.

d.) Close the regulator shut-off valve to stop flow.

e.) Close the gas bottle valve.

5. Set the instrument pressure.


Low-pressure gauge

Regulator
Gas bottle
shut-off valve
shut-off valve

Regulator
control knob

a.) Turn the regulator control knob clockwise until the low-pressure gauge reads 15 psig 
(103 kPag).

b.) Open the regulator shut-off valve.

c.) Open the gas bottle shut-off valve and flow gas for 10 to 30 seconds.

d.) Close the gas bottle shut-off valve.

6. If the gas line to the instrument inlet was previously disconnected, reconnect it now.

7. Verify the line for the newly connected gas is clean.

8. If the previously disconnected gas has been reconnected, resume operation.

239-42828-01 - Dec 2012 9-21


Connecting Gases Gemini VII

Cleaning and Verifying the Gas Line


Always clean the gas lines and verify there are no leaks at the connections after a gas bottle is con-
nected. This test examines the gas line from the instrument to the gas bottle, then from the instrument
to the regulator shut-off valve. A report is generated at the completion of the test verifying that it has
passed or failed. Causes and corrective action for a failure are provided.

Before beginning, confirm that the state for valves and the low-pressure gauge are as follows:
Low-pressure gauge
14 - 15 psig

Gas bottle shut-off valve 


CLOSED

Regulator control knob


OPEN
Regulator shut-off valve
OPEN

1. To start diagnostic testing, go to Unit [n] > Diagnostics.

2. Click the down arrow to the right of the Test field and select Clean and Verify Analysis Gas
Line Rev [n]. This procedure uses the analysis gas as an example. Select Clean and Verify
Helium Gas Line Rev [n] if the helium bottle is being verified.

3. Click Report after analysis and select Preview as the destination. Click OK.

4. Click Start. From the View dropdown list, select either Operation, Instrument Log, or
Instrument Schematic. Refer to Start Analysis, page 6-2.

5. A series of prompts display on the screen requiring operator response. The length of time a test
will run is also indicated on the screen.

9-22 239-42828-01 - Dec 2012


Gemini VII Connecting Gases

6. A popup window indicates the test is complete. Click OK. The report displays on the screen.

On the report, the Leak Rate field on the Instrument to Regulator Shut-off Valve -1 report
should read Passed. A Passed reading indicates the gas line from the instrument to the regulator is
clean and leak-free.

If the Leak Rate field indicates Failed, a leak is indicated between this connection. Check the
connections from the instrument to the gas regulator valve. Tighten as necessary, then run the test
again.

7. Click the Instrument to Gas Bottle Shut-off Valve - 2 tab to display its report.

239-42828-01 - Dec 2012 9-23


Connecting Gases Gemini VII

On the report, the Leak Rate field should read Passed. A Passed reading indicates the gas line
from the instrument to the regulator is clean and leak-free.

If the Leak Rate field indicates Failed, a leak is indicated between this connection. Check the
connections from the regulator shut-off valve to the gas bottle shut-off valve. Tighten as necessary,
then run the test again.

8. Click the Gas Pressure Test - 3 tab to display its report.

9-24 239-42828-01 - Dec 2012


Gemini VII Connecting Gases

On the report, the Minimum field should read Passed. A Passed reading indicates all valves are in
the proper state for operation.

If the Minimum field indicates Failed, one or more valves is not in the proper position. Set the
valves as shown below and ensure the appropriate pressure is displayed on the low-pressure gauge.

Low-pressure gauge
14 - 15 psig

Gas bottle shut-off valve 


OPEN

Regulator control knob


OPEN
Regulator shut-off valve
OPEN

If running the test again, close the gas bottle valve before starting the test.

9. Click Close to close the test report. Click Close again to close the test.

239-42828-01 - Dec 2012 9-25


Performing a Blank Analysis for Diagnostic Purposes Gemini VII

Performing a Blank Analysis for Diagnostic Purposes


A blank analysis is a means of pinpointing operational problems in the analyzer. Leaks, as well as elec-
tronic problems, will result in an unsatisfactory blank analysis. This test should be performed prior to
detailed troubleshooting. The data produced during the blank analysis can be very helpful in identify-
ing the cause of a problem and should be performed before contacting your Micromeritics Service
Representative.

Helium is required for performing a blank analysis since a measured free space is required. If helium is
unavailable, contact a Micromeritics Service Representative for an alternative method of performing
this procedure.

1. Install empty, straight-wall sample tubes (free of cracks or chips) of the same size in the sample
and balance ports. Ensure the O-rings are present and in good condition.

2. Place the Dewar support on the elevator, then place a Dewar of water at ambient temperature on
the Dewar support.

A Dewar support is not necessary for the larger Dewar used with the Gemini VII 2390t. Place the
Dewar directly on the elevator.

9-26 239-42828-01 - Dec 2012


Gemini VII Performing a Blank Analysis for Diagnostic Purposes

3. Select Unit [n] > Blank Analysis.

4. Click Browse to select an existing file or to create a new one. Click Open.

5. Click Edit to make and save modifications or replace all parameters in the open file using the
Replace All button to select another file. Click Save and Close when done.

6. Click Report after analysis to automatically generate reports to the specified destination when
the analysis is complete. On the Report Settings window, select the report destination. Click OK.

7. Click Start to start the analysis. A window displays data as they are collected. A short delay is
encountered before the port status changes from the Idle state at the bottom of the screen. Review
the analysis results to see if they are within the tolerances shown in the following table. If these
results are not achieved, call a Micromeritics Service Representative.

P/Po Tolerance in cm3

0.1 ±0.008
0.2 ±0.010
0.3 ±0.012
0.4 ±0.014
0.5 ±0.016
0.6 ±0.018
0.7 ±0.020
0.8 ±0.022
0.9 ±0.024

239-42828-01 - Dec 2012 9-27


Performing a Reference Analysis Gemini VII

Performing a Reference Analysis


A reference analysis is used to verify that the instrument is operating properly and producing optimum
results. Use the Carbon reference material provided in the accessories kit to perform this analysis. The
results should match those shown on the label of the reference material bottle within the tolerance
level.

1. Select File > Open > Sample Information and create the new sample file, for example,
CARBON1.SMP.

2. Click the Replace All button and select a reference analysis file, for example: Carbon.smp.

3. Click Open. Information from the reference analysis file populates fields in the new file.

4. Click Save, then click Close.

9-28 239-42828-01 - Dec 2012


Gemini VII Performing a Reference Analysis

Analyzing Reference Material


1. Select Unit [n] > Start Analysis.

2. On the Analysis screen, click Browse to select the test file created in the previous steps. Click
Open.

3. Click Edit to make and save modifications or replace all parameters in the open file using the
Replace All button to select another file. Click Save and Close when done.

4. Click Report after analysis to automatically generate reports to the specified destination when
the analysis is complete. On the Report Settings window, select the report destination. Click OK.

5. Click the Start button. Graphs are displayed as the analyses are performed.

When the analyses are complete, compare the BET Surface Area shown on the Summary Report
with the BET Surface Area shown on the reference material bottle. The values should match
within the tolerance level shown on the bottle.

If the BET Surface Area values do not match, refer to the following causes and actions.

Cause Action

The sample was not degassed properly. Degas the sample again.

The gas lines are not clean. Perform the procedure for cleaning and verifying
gas lines, then try again.

239-42828-01 - Dec 2012 9-29


Calibrating the System Gemini VII

Cause Action (continued)

The measured free space is too high. This Use helium that is 99.999% pure, then try again.
indicates the helium is not pure enough.

If the BET Surface Areas match, click Close.

Calibrating the System


A calibration file was created specifically for your analyzer and included with your accessories. Refer
to Reinstalling Calibration Files for an Analyzer, page 4-24. It is not necessary to recalibrate the
system unless you suspect it is out of calibration. Certain calibrations are not allowed unless performed
under the direction of a Micromeritics service representative. Those calibrations are greyed out on the
Calibration menu.

To review calibration details of the analyzer, go to Unit [n] > Unit Configuration.

The following calibrations can be performed without the assistance of a service representative:

• Zero pressure
• Match transducers
• Servo valve

Zero Pressure
Use this option to evacuate the system and zero the transducers.

1. Install a blank sample tube on each applicable port.

2. Go to Unit [n] > Calibration > Zero Pressure.

3. Ensure that all transducers are selected, then click Start. The window closes when the operation is
complete.

9-30 239-42828-01 - Dec 2012


Gemini VII Calibrating the System

Match Transducers
Use this option to zero and match the selected transducers to the main manifold transducer.

A sample or Po tube must be installed on each selected port before clicking Start.

Sample Servo
Ensure the pressure transducer has been calibrated before performing this procedure.
Go to Unit [n] > Unit Configuration and view the calibration information. Contact your
service representative if calibration dates are not listed.

Use to calibrate the servo valve to the sample pressure transducer.

1. Select Unit [n] > Calibration > Sample Servo.

2. Click Start. The window closes when the calibration is complete.

239-42828-01 - Dec 2012 9-31


Calibrating the System Gemini VII

Balance Servo
Use this option to calibrate the balance servo valve.

Ensure that empty tubes are installed on the sample and balance ports before
performing this procedure.

Ensure that empty tubes are installed on the sample and balance ports.

1. Select Unit [n] > Calibration > Balance Servo.

2. Click Start. The window closes when the calibration is complete.

9-32 239-42828-01 - Dec 2012


Gemini VII

10. ORDERING INFORMATION

The Gemini components and accessories can be ordered using one of the following methods:

• Call our Customer Service Department at (770) 662-3636


• Email orders to orders@micromeritics.com
• Contact your local sales representative

When ordering, please use the following information to place an order:

Part Number Item and Description

Analyzer Optional Equipment

060-00023-00 FlowPrep 060, degasses up to six samples at up to 400 ºC with flowing gas
(requires gas regulator).

061-00023-00 VacPrep 061, degasses up to six samples at up to 400 ºC; uses flowing gas or
evacuation by vacuum (evacuation requires a vacuum pump and a regulator)

065-00000-00 SmartPrep 065, Windows interface allowing programmable ramp and soak
rates; degasses up to six samples with flowing gas

236-33005-00 PrepSeal Accessory Kit; for degassing and transferring air-sensitive samples
to an analysis port without contamination

Dewar and Accessories

004-61064-00 Dewar, 600 mL; for Models 2390a and 2390p

236-31802-01 Dewar Cover, right side; for 600 mL glass Dewar

236-31802-02 Dewar Cover, left side; for 600 mL glass Dewar

239-31802-00 Dewar Cover; for 2.75 liters Dewar

239-33601-00 Dewar, 2.2 liters, stainless steel; includes cover (Gemini 2390a and 2390p)

239-33602-00 Dewar, 4.0 liters, stainless steel; includes cover (for Gemini 2390t)

300-25861-20 Dewar, 2.75 liters; for Model 2390t

239-42828-01 - Dec 2012 10-1


Gemini VII

Part Number Item and Description (continued)

Gas Bottle Accessories

004-33601-00 Expansion Kit; adds an additional outlet to the gas regulator

004-33602-00 Pressure Relief Kit (recommended for both gas supplies); prevents excessive
gas pressure in the event of regulator failure (not to be used with toxic gases)

004-62230-58 Gas Regulator, CGA 580, 30 psig, 30 psig (He, N2)

290-25846-00 Gas Inlet Line, 1/8 in. x 6 ft long, copper

290-25846-01 Gas Inlet Line, 1/8 in. x 16 ft long, copper

Reference Material

004-16816-00 Reference Material, Alumina, ~ 0.25 m2/g, 15 g

004-16818-00 Reference Material, Glass, SA ~ 5.8 m2/g

004-16821-00 Reference Material, Silica alumina, ~ 215 m2/g, 10 g

004-16833-00 Reference Material, Carbon black, ~ 30.6 m2/g, 10 g

Sample Tubes and Accessories

004-25022-00 O-Ring, Buna-N size 012; for 3/8 in sample tube

004-25619-03 Sample Tube Ferrule, 3/8 in

004-27024-00 Frit, 2m, for sample port

004-27046-00 Frit, 40 m, for sample port

004-32004-00 Stopper, rubber, for 3/8 and 1/2 in sample tubes

004-54611-00 Sample Tube Brush, 8 mm diameter, for straight-wall sample tubes

004-54612-00 Sample Tube Brush, 25 mm diameter, for bulb sample tubes

004-54618-00 Tool, for removing sample port O-ring

004-61065-00 Glass Beads, 3 mm diameter, 90 grams

10-2 239-42828-01 - Dec 2012


Gemini VII

Part Number Item and Description (continued)

236-61702-00 Sample Tube, bulb; 3/8 in. (0.95 cm) OD × 6.1 in. (15.5 cm) long, 3/4 in.
(1.91 cm) OD bulb

236-61703-00 Sample Tube, straight-wall; 3/8 in. (0.95 cm) OD × 6.1 in. (15.5 cm) long

236-61704-00 Filler Rod, 7 mm (1/4 in.) × 146.1 mm (5.75 in.)

236-61705-00 Filler Rod, 7 mm × 101.6 mm (4 in.)

238-61703-00 Sample Tube, straight-wall; 3/8 in (0.95 cm) OD × 8.1 (20.5 cm) in. long (for
Gemini 2390t)

240-14855-00 Sample Tube Rack

240-25853-00 Sample Tube Funnel, polypropylene

280-32800-00 Weighing Support

Software and Manuals

239-20828-00 Gemini VII - current version software

239-42828-01 Gemini VII - operator’s manual

Vacuum Pump and Accessories

004-16003-01 Vacuum Pump Oil, 1 liter

004-16830-00 Activated Alumina, 500 grams; for oil vapor trap

004-25630-00 Centering Ring, NW 16

004-25652-00 O-ring, for oil vapor trap (end fitting)

004-25653-00 Centering Ring, NW 16/10; for vacuum pump intake port

062-00000-11 Vacuum Pump with built-in anti-suckback valve, 100/120 VAC, includes hose
kit

062-00000-23 Vacuum Pump with built-in anti-suckback valve, 220/240 VAC, includes hose
kit

062-00003-00 Vacuum Pump, hybrid (oil free); includes vacuum hose, fittings, and manual.

239-42828-01 - Dec 2012 10-3


Gemini VII

Part Number Item and Description (continued)

062-33002-00 Oil Vapor Trap; includes alumina and instructions

Cables

003-63801-01 Cable, Ethernet straight-thru

Miscellaneous

021-00000-00 Liquid Nitrogen Transfer System, Model 021

10-4 239-42828-01 - Dec 2012


Gemini VII Appendix A

A. FORMS

This appendix contains the following form:

• Sample Data Worksheet

Copy and use this form as needed.

239-42828-01 - Dec 2012 A-1


Sample Data Worksheet

Use this worksheet to record the values necessary to calculate the sample mass.

Sample Tube Identification:_________________________________

Sample Mass (g)

NOTE: Record all values in grams.


Before Degas After Degas After Analysis

A. Mass for empty sample tube set: ____________

B. Sample tube set plus sample mass: ____________ ____________ _____________

C. Sample mass (B - A): ____________ ____________ _____________

Degas Information

Degas apparatus: ____________________________________________


Temperature (ºC): ____________________________________________

Time (hours): ____________________________________________

Actual time started: ____________________________________________

Actual time finished: ____________________________________________

Degas notes: _______________________________________________________________________

_________________________________________________________________________________

_________________________________________________________________________________

_________________________________________________________________________________

_________________________________________________________________________________

_________________________________________________________________________________
Gemini VII Appendix B

B. ERROR MESSAGES

Error messages for the Gemini program are listed numerically. If the Action response instructs you to
contact a service representative, record the error message and make backup copies of any files
involved in the operation.

2400 Series
2430- Error accessing file [file name], error code = [n].
Cause A: Media may be damaged.

Action A: Clean the media drive. If this does not eliminate the problem, attempt
operation using a backup copy of the file.

Cause B: Hard disk may be damaged.

Action B: Contact a Micromeritics service representative if this error message


continues.

Cause C: A software error occurred when the file was accessed.

Action C: Contact a Micromeritics service representative if this error message


continues.

2431- Error writing file [file name], error code = [n].


Cause: Insufficient hard disk space to perform the operation.

Action: Copy files not used regularly from the hard disk to an external media,
delete them from the hard disk and try the operation again

2432- Invalid response from MMI ‘FILE_READ’ request.


Cause: An internal processing and/or hardware error has occurred.

Action: Contact a Micromeritics service representative if this error message


continues.

239-42828-01 - Nov 2013 B-1


Appendix B Gemini VII

2433- New entries have been found in this directory. Refresh the directory
information?
Cause: Several analyzer files (sample information, analysis conditions,
adsorptive properties or report options) have been added to this
directory by some function other than the analyzer program.

Action: Select Yes to update the directory information with data from each
new file. This operation may take a minute.
Select No to locate the file manually. This option may be feasible if a
large number of files have been copied into the directory and the
name of the file is known.

2434- File [file name] — Subset # [n] wrote wrong amount of data.
Cause: An internal processing and/or hardware error has occurred.

Action: Contact your service representative if you continue to receive this


error message.

2436- Path specification [path name] is invalid.


Cause: An invalid path name and/or extension was entered.

Action: Type a valid path name (including the proper extension) and press
Enter.

2437- File/Overlay file [file name] does not exist.


Cause: The entered file specification does not exist.

Action: Enter an existing file specification or select a file name from the list
box.

2439- Could not register file.


2440- Subset not found.
2441- Seek within file failed.
2442- Bad header in subset file.
2443- Subset owner denied access.
2444- Not a valid file format.
2445- Subset wrote the wrong amount of data.
2446- Error reading data.
2447- Error writing data.
Cause: An unexpected error occurred when trying to access a data file.

Action: Contact a Micromeritics service representative if this error message


continues.

B-2 239-42828-01 - Nov 2013


Gemini VII Appendix B

2448- File directory [path name] is invalid. Resetting to the installation directory.
Cause: A working directory specified in the .INI file is invalid or has been
moved or deleted.

Action: The installation directory will be substituted. The next time a file is
opened, use the Directories list to move to the correct directory.

2449- This field does not contain a valid file specification.


Cause: An invalid file name was entered.

Action: See the description of file naming conventions in a Windows manual


and re-enter the name.

2456- Insufficient file handles available. Application cannot continue.


Cause: More than 50 files are open at the same time.

Action: Refer to an operating system manual and set the limit for open files to
50 or greater.

2458- An instrument is performing a critical operation. Wait a few moments before


exiting the application.
Cause: An attempt was made to exit the application while the instrument was
performing a critical operation. This operation must be completed
before the application can be stopped.

Action: Wait a short time and attempt to stop the application again.

2459- An instrument is busy. A delay in restarting this application could result in loss
of new data. Continue with program Exit? [Yes, No]
Cause: An attempt was made to exit the application while an analysis was in
progress. While this is possible, the data collected when the
application is inactive will not be permanently recorded until the
application is re-started. A power failure to the instrument could
cause some data to be lost.

Action: If not concerned with the potential for loss of data should a power
failure occur, click Yes to continue; otherwise click No.

239-42828-01 - Nov 2013 B-3


Appendix B Gemini VII

2460- Fatal Communications error on Unit [n] - S/N: [n].


Cause: There was a fatal error in communication between the application and
the software in the instrument. All displays for that instrument will be
closed.

Action: Ensure that the analyzer is connected to the computer on the


communications port configured in the Setup program. Stop and
restart the analyzer software. Contact a Micromeritics service
representative if this error message continues.

2461- No instruments are in operation. This application will unconditionally


terminate.
Cause: At least one instrument must be active for the application to operate.
The initialization of all of the instruments configured with the Setup
program has failed. The application stops.

Action A: Usually this message is preceded by another message giving the


reason for the instrument’s failure to initialize. Refer to the
instructions for that message.

Action B: Ensure that the instrument is attached to the computer on the


communications port configured with the Setup program. Verify that
the instrument has the power switch in the ON position and that the
light on the front panel is illuminated. If the application continues to
fail in its attempts to initialize the instrument, contact a Micromeritics
service representative if this error message continues.

2477- Unit [n] - S/N: [n] did not properly initialize.


Cause: The software was unable to initialize this instrument. This is usually
caused by one of the conditions listed in the error messages above.

Action: Correct the problem as described above then restart the application.

2480- File [name] cannot be analyzed. It is currently being edited.


Cause: An attempt was made to start an analysis using a file that is open for
editing.

Action: Finish editing the file, save and close it then start the analysis.

2481- Error accessing the sample information file [file name].


Cause: An unexplained error prevented access to this file.

Action: The hard disk drive may be corrupt. Run diagnositics.

B-4 239-42828-01 - Nov 2013


Gemini VII Appendix B

2482- File cannot be opened for writing. It is already in use.


Cause: An attempt was made to open a file currently being used.

Action: Locate the application using the file (in the Micromeritics application,
use the Windows menu item to get a list of all windows, one of which
may contain this file).

2483- An analysis cannot be performed on [file name]. It is open for editing and con-
tains errors.
Cause: An attempt was made to use a sample file containing errors that is
currently open.

Action: Go to the window containing the file, correct the errors and save it.

2484- The edit session for [file name] must be saved before the analysis. Save 
changes and continue with the analysis? [Yes, No]
Cause: An attempt was made to start an analysis using a file that contains
unsaved changes and is open for editing.

Action: Select Yes to save the changes and proceed with the analysis. Select
No to cancel the analysis and continue editing the Sample
Information file.

2486- Could not construct [name] report type. Program will terminate.
2487- Could not start report generator. Error code [n]. Program will 
terminate.
Cause A: Full rights to the application’s folders and files is required.

Action A: Contact a system administrator to have full rights granted.

Cause B: An internal processing and/or hardware error has occurred.

Action B: Contact a Micromeritics service representative if this error message


continues.

2488- File [file name] cannot be opened for editing. It is already in use.

Cause: The specified file is being used in another edit operation.

Action: Check the Windows list to locate the other edit session.

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Appendix B Gemini VII

2489- File [file name] cannot be opened for writing. It is already in use.
Cause: The specified file in a Save As operation is already open for edit.

Action: Select a different file for the Save As operation.

2490- No ‘.INI’ file present. Application will terminate.


Cause: The ASCII file containing initialization information and system
options information used during program startup does not exist.

Action: Run the analyzer setup program, select Change analyzer setup and
create the control file used by the analyzer.

2491- Highlighted fields contain errors. Please correct the errors before closing dia-
log box.
Cause: The highlighted fields contain invalid entries. The dialog box cannot
be closed until all errors are corrected.

Action: Check the entries, correct the errors and close the window.

2492- This field’s entry is invalid.


Cause: The highlighted field contains an invalid entry.

Action: Check the entry and correct the error.

2493- An entry is required for this field.


Cause: This field requires a valid entry to proceed.

Action: Enter or select an appropriate value.

2494- Value is out of the valid range.


2496- Invalid number.
Cause: An invalid number entered in the highlighted field.

Action: Check the entry and enter or select a valid number.

2497- This field contains an invalid character.


Cause: An invalid character was entered in the highlighted field.

Action: Check the entry and enter valid characters.

B-6 239-42828-01 - Nov 2013


Gemini VII Appendix B

2499- Sequence number must contain at least 3 digits.


Cause: An attempt was made to enter a sequence number that did not contain
at least three digits.

Action: Enter a sequence number that contains at least three digits.

2500 Series
2500- All sample file names that can be created using the sequence number pattern
already exist. You may want to modify the next sequence number.
Cause: No more sample information files can be created using the currently
entered file name sequence number.

Action: Select Options > Sample defaults and enter another sequence
number.

2505- Error logger cannot be initialized. Error code [n]. Program will exit.
Cause: An internal processing error has occurred.

Action: Contact a Micromeritics service representative if this error message


continues.

2506- Sample file [file name] has a 'No Analysis' status and cannot be used for this
operation.
Cause: The selected sample file does not have collected data and cannot be
used for operations, for example, reporting.

Action: Enter the name of a file with a status of Complete, Analyzing or


Entered or select a sample file from the list box.

2508- [sample file] Overlay file [name] was not found. It will not be included in the
reports.
Cause: The specified overlay file could not be found.

Action: Ensure the file specified as an overlay exists.

2509- [sample file] Error opening file [name] [error]. Reports cannot be produced.
Cause: An error occurred while the program was opening a file necessary to
the report operation.

Action: Use the name given in the error message to investigate. Contact a
Micromeritics service representative if this error message continues.

239-42828-01 - Nov 2013 B-7


Appendix B Gemini VII

2510- [sample file] Error parsing reports from file [name]. Reports cannot be
produced.
Cause A: One or more data entry fields in the sample file may contain an
invalid character (such as a single quote or double quotes).

Action A: Review the data entry fields (for example, the Sample field) and
remove the invalid character.

Cause B: The system was unable to create the usual temporary files during the
report, possibly due to insufficient disk space.

Action B: Check the space available on the hard disk.

Cause C: An internal processing error occurred.

Action C: Contact a Micromeritics service representative if this error message


continues.

2511- Print job [name] has been cancelled due to insufficient disk space. Delete
unnecessary files and restart the report.
Cause: The disk drive does not have required space for the temporary file.

Action: Delete unnecessary files from the disk. At least five megabytes of free
space is required for normal operation.

2512- Print job [name] cancelled.


Cause: The print job was canceled by the operator.

Action: None required.

2513- Unable to read the calibration file [file name].


Cause: An invalid calibration file was selected or one that cannot be read.

Action: Ensure the media containing the calibration file has no problems.

2514- Unable to write the calibration file [file name].


Cause: An attempt to save calibration data has failed due to possible media
problems.

Action A: Ensure the destination location has no problems.

Action B: Choose an alternate media to save the calibration data.

B-8 239-42828-01 - Nov 2013


Gemini VII Appendix B

2515- Warning: Changing the calibration information will affect the performance of
the instrument. Only qualified service personnel should do this. Do you wish to
proceed?
Cause: The process of performing a calibration operation was started.

Action: Calibration operations should only be done by or under the direction


of qualified service personnel.

2516- Warning: Keeping a backup copy of the calibration data is recommended by


Micromeritics. Would you like to do so now?
Cause: A calibration operation was performed and a backup copy is
recommended.

Action: Perform a calibration Save operation.

2517- Canceling this dialog will reset the calibration state to what it was when this
dialog was first opened. Are you sure you want to cancel?
Cause: The calibration has not been accepted.

Action: If the calibration operation was successful, press Accept.

2520- No data points available for reporting.


Cause: The selected sample file does not have collected data and cannot be
used for reporting.

Action: Select a different sample file.

2522- Invalid controller application file.


Cause: The application’s control file has been corrupted or deleted.

Action: Reinstall the analysis program.

2532- The instrument contains a different software version. Do you want to reset it?
Cause: The application has discovered a different version of software
operating in the analyzer.

Action: If there are no analyzers other than the Gemini connected to the
computer, select Yes and allow the updated software to load.

239-42828-01 - Nov 2013 B-9


Appendix B Gemini VII

2533- Analyzer initialization failed.


Cause: An internal processing and/or hardware error has occurred.

Action: Contact a Micromeritics service representative if this error message


continues.

2585- The following libraries are missing: <library-name>, <library-name>, ....

Cause: This message is triggered on application start up if any of the library


files used by an application, does not exist on disk

Action: Add the library into the Libraries folder.

2599- The selected file has an extension that is not supported by this operation.

Cause: The selected file does not have a supported file extension.

Action: Open the adsorptive properties file. Open the FPI file selector and
select another file with a supported file extension.

4000 Series
4003- Error Converting Pressures.
4004- Error Computing Volume Adsorbed.
Cause: An internal processing and/or hardware error occurred during report
generation.

Action: Contact a Micromeritics service representative if this error message


continues.

4005- Pressures were not smoothed. Not enough pressures below 0.10 P/Po.

Cause: The Smooth pressures below 0.10 P/Po option was selected on the
Report Options window. There must be at least 10 pressures within
this range for smoothing to occur.

Action: Deselect this option to disable this message.

4006- Report Type Not Found.


4007- Error Processing Report.
Cause: An internal processing and/or hardware error occurred during report
generation.

Action: Contact a Micromeritics service representative if this error message


continues.

B-10 239-42828-01 - Nov 2013


Gemini VII Appendix B

4008- Report requested on sample file with no data points.


Cause: The selected file contains no collected data.

Action: Select another file which contains collective data and restart the
report.

4014- File [name] is not a valid file for conversion.


Cause: The file selected for conversion is not a valid file.

Action: Select only files that have been created by the proper program.

4023- The file [file name] cannot be prepared for analysis. It is open for editing and
contains errors.
Cause: An attempt was made to start an analysis using a file that contains
errors and is open for editing.

Action: Finish editing this file, save and close it, then start the analysis.

4026- Cannot calculate Dubinin-Astkahov: bad least squares data.


Cause: Less than two selected data points are within the fitted pressure range.

Action: Edit the calculation assignments on the Collected Data window or


change the fitted pressure range on the Dubinin report options
window.

4027- Fewer than two sample files have data suitable for heat of adsorption reports.
Cause: Less than two of the selected sample files for heat of adsorption
reports contain appropriate data.

Action: Edit the Quantity Adsorbed table or select other sample files.

4028- Dubinin calculations cannot be performed because the affinity coefficient of


the analysis gas is zero.
Cause: Dubinin values could not be calculated because the affinity
coefficient of the analysis gas is zero.

Action: Access the Dubinin Report Adsorptive options in the sample file and
enter an appropriate value for the analysis gas.

239-42828-01 - Nov 2013 B-11


Appendix B Gemini VII

4029- At least two fitted data points are needed for Alpha-S calculations.
Cause: Fewer than two data points fall within the selected Alpha-S range.

Action: Edit the calculation assignments or the fitted Alpha-S range or use a
different reference curve.

4030- Preparations failed in primary data.


Cause: Appropriate data were not available to generate the report.

Action: This message was preceded by a different error message. Refer to the
cause/action of the preceding message.

4031- Not enough points with a relative pressure in the range [n,n]
Cause: Fewer than two data points selected for the Dubinin report fall within
the selected relative pressure range.

Action: Edit the calculation assignments or the fitted relative pressure range.

4033- Not enough points to generate Dubinin Tabular Report.


Cause: There are fewer than two valid data points available for the Dubinin
tabular reports.

Action: Examine the calculation assignments in the Collected Data window


of the sample file. At least two micropore pressures must be selected
for inclusion in the Dubinin report.

4034- Fewer than 2 points available for Dubinin calculations.


Cause: There are fewer than two valid data points available for Dubinin
reports in one of the sample files selected for overlaying.

Action: Examine the calculation assignments in the Collected Data window


of the sample file. At least two micropore pressures must be selected
for inclusion in the Dubinin report.

4035- Cannot calculate optimized Astakhov exponent: Not enough points with a rel-
ative pressure in the range [(pressure), (pressure)].
Cause: There are fewer than two valid data points in the relative pressure
range specified. Astakhov reports will not be produced.

Action: Examine the calculation assignments in the Collected Data window


for the sample file. At two pressures in the given range must be
selected for inclusion in the Dubinin report.

B-12 239-42828-01 - Nov 2013


Gemini VII Appendix B

4036- Fewer than 2 points available for Horvath-Kawazoe calculations.


Cause: At least two data points must be selected for inclusion in the Horvath-
Kawazoe analysis on the Collected Data window. No report will be
produced.

Action: From the Collected Data window, select the data points to be
analyzed.

4037- Computations failed while processing the primary data set. No reports will be
produced.
Cause: The preparation of data for reporting could not be successfully
completed. No Horvath-Kawazoe reports will be produced. This
message will always be preceded with another one containing
additional information.

Action: Refer to the number of the error message which preceded this one for
an explanation.

4038- Fewer than 2 points available for the Langmuir Qm computation. Cheng/Yang
correction will not be applied.
Cause: The Cheng/Yang correction to the Horvath-Kawazoe equation
requires the value of the monolayer volume as calculated from the
Langmuir equation. The isotherm must include at least two points
above 0.02 relative pressure for the Langmuir equation to be applied.

Action: The analysis will be performed without the Cheng/Yang correction.


Deselect Apply Cheng/Yang correction on the Horvath-Kawazoe
Report Options window to prevent this message from appearing on
future reports.

239-42828-01 - Nov 2013 B-13


Appendix B Gemini VII

4039- The isotherm does not meet the constraints of the Cheng/Yang assumption.
Cheng/Yang correction will not be applied.
Cause: The Cheng/Yang correction to the Horvath-Kawazoe equation
requires the value of the monolayer volume as calculated from the
Langmuir equation. The isotherm does not correlate to the Langmuir
assumption with a coefficient of 0.98 or more. The correction is not
applicable to this isotherm or to the range of the data points selected.

Action A: The analysis will be performed without the Cheng/Yang correction.


Deselect Apply Cheng/Yang correction on the Horvath-Kawazoe
Report Options window to prevent this message from appearing on
future reports.

Action B: Generate the Langmuir report for the same data points selected for the
Horvath-Kawazoe report. If the Langmuir correlation coefficient can
be brought above 0.98 by removing some points at high relative
pressure, remove them and reproduce the Horvath-Kawazoe reports.

4040- The value of Qm computed from the Langmuir equation is too low. The pore
size will not be computed for all data points.
Cause: The Cheng/Yang correction to the Horvath-Kawazoe equation
requires the value of the monolayer volume as calculated from the
Langmuir equation. The computed value is less than the volume
adsorbed at the largest relative pressure included in the analysis. The
correction is not applicable to this isotherm or to the range of the data
points selected.

Action: The analysis will be performed and the Cheng/Yang correction will
be applied to all points with a volume adsorbed less than the value of
Vm. The pore size will not be calculated for data points with an
invalid volume adsorbed. Deselect Apply Cheng/Yang correction on
the Horvath-Kawazoe Report Options window to clear this message.

4041- Cheng/Yang correction is inappropriate for some P/Po.

Cause: The Cheng/Yang correction is usually inappropriate for any P/Po


above the isotherm knee. In some instances, the computed pore sizes
may decrease above the knee. While it is possible to include these
relative pressures (usually above 0.1 P/Po) in the analysis, the
computed pore sizes for these pressures are usually meaningless.

Action: Change the data points selected for the Horvath-Kawazoe report to
include only relative pressures at or below the knee of the isotherm or
change the Horvath-Kawazoe report options so that the Cheng/Yang
correction is not applied.

B-14 239-42828-01 - Nov 2013


Gemini VII Appendix B

4042- 0.0 cannot be a starting or ending pressure for a geometric progression from
low pressure.
Cause: An attempt was made to generate a pressure table from a
geometrically progressing range.

Action: Change the 0.0 entered value.

4043- 1.0 cannot be a starting or ending pressure for a geometric progression toward
saturation.
Cause: An attempt was made to generate a pressure table from a
geometrically progressing range.

Action: Change the 1.0 entered value.

4044- Points in the Langmuir report pressure table lie outside the collected data.
Cause: Calculation assignments are not being used and more than one of the
report pressure table points is above the range of the collected data
and more than one is below.

Action: Change the report pressure table to be more consistent with the
collected data.

4045- Points in the report pressure table lie outside the collected data.
Cause: Calculation assignments are not being used and more than one of the
report pressure table points is above the range of the collected data
and more than one is below.

Action: Change the report pressure table to be more consistent with the
collected data.

4046- [file name] could not be opened for reading.


Cause: A thickness curve file could not be opened.

Action: If the problem persists, restart the computer and optionally perform a
media integrity check (using ScanDisk).

4047- Warning: An error occurred while reading [file name].


Cause: An error happened during a read operation of a thickness curve file.

Action: If the problem persists, restart the computer and optionally perform a
media integrity check (using ScanDisk).

239-42828-01 - Nov 2013 B-15


Appendix B Gemini VII

4048- Warning: An error occurred while restoring the heat of adsorption report editor.
Cause: The state of the heat of adsorption report editor could not be restored.
Default settings will be used.

Action: No action.

4049- The sample [file name] does not have enough data. A minimum of two adsorp-
tion points is required.
Cause: A sample file has been included in the Heat of Adsorption report that
does not have enough data.

Action: Remove the file from the selected file list.

4050- None of the requested quantities adsorbed is within the range of the collected
data of more than one sample file.
Cause: The Heat of Adsorption report failed because the specified quantities
are not within the range of the collected data.

Action: Edit the quantities adsorbed so that they are within the range of the
collected data or select other sample files.

4051- The sample [file name] does not have any data in the range of the requested
quantities adsorbed.
Cause: The sample’s data cannot be interpolated to any of the quantities
adsorbed.

Action: Edit the quantities adsorbed so that they are within the range of the
collected data.

4052- Fewer than two points are selected for this report.
Cause: At least two points are required for the BET calculations.

Action: Edit the calculation assignments for the BET report.

B-16 239-42828-01 - Nov 2013


Gemini VII Appendix B

4053- At least two data points must be selected for t-Plot calculations.
Cause: At least two points are required for the t-Plot calculations.

Action: Edit the calculation assignments for the t-Plot report.

4054- Fewer than two data points are inside the fitted thickness range.
Cause: At least two points must be within the fitted thickness range for the t-
Plot calculations.

Action A: Edit the calculation assignments for the t-Plot report.

Action B: Edit the fitted thickness range in the t-Plot report editor.

4055- A positive BET surface area was not calculated.


Cause: Fewer than two points were assigned to the requested surface area
calculation in the collected data table.

Action A: Assign more points to the surface area calculation.

Action B: Select a different surface area in the t-Plot report editor.

4056- A positive Langmuir surface area was not calculated. Please check your Lang-
muir report.
Cause: Fewer than two points were assigned to the requested surface area
calculation in the collected data table.

Action A: Assign more points to the surface area calculation.

Action B: Select a different surface area in the t-Plot report editor.

4057- At least two data points are needed for Freundlich calculations.
Cause: Less than two data points have been selected for the Freundlich
report; at least two are required.

Action: Select Freundlich points on the Collected Data window. If calculation


assignments are not being used, edit the Freundlich Report options,
Absolute pressure range in the sample file.

239-42828-01 - Nov 2013 B-17


Appendix B Gemini VII

4057- At least two data points are needed for Freundlich calculations.
Cause: Less than two data points have been selected for the Freundlich
report; at least two are required.

Action: Select Freundlich points on the Collected Data window. If calculation


assignments are not being used, edit the Freundlich Report options,
Absolute pressure range in the sample file.

4059- Fewer than 2 points available for MP-Method calculations.


Cause: At least two points are required for the MP-Method calculations.

Action: Edit the calculation assignments for the MP-Method report.

4060- Sample [file name] contains no data points.


Cause: An attempt was made to save a sample without collected data as a t-
curve or alpha-S curve.

Action: Repeat the Save As t-curve or Save As Alpha-S operation after


opening a sample that has collected data.

4061- The t-curve must contain at least 2 points.

Cause: At least two points are required in a thickness curve definition.

Action: Edit the thickness curve.

4062- Error during report preparation.


Cause: An internal processing error has occurred.

Action: Contact a Micromeritics service representative if this error message


continues.

4063- The data requested on this report are not available. No subreports selected.
Cause: There is no information in the sample log to report.

Action: A sample file was selected which no instrument operations has been
used. Select a sample file with a status of Prepared, Preparing,
Analyzing or Complete to obtain a valid sample log report.

B-18 239-42828-01 - Nov 2013


Gemini VII Appendix B

4067- No data points are within the range of pressures in the reference isotherm.
Cause: There are no collected data points within the range of pressures in the
reference isotherm.

Action: Select data points that are in the range of the reference isotherm or
select a more appropriate reference isotherm.

4068- No points were selected for the f-Ratio report.


Cause: The collected data column for the f-Ratio report does not have any
points selected.

Action: Edit the collected data window and select points for the f-Ratio
report.

4070- Unable to load deconvolution model [name].


Cause: For some reason, the list of available models was corrupted,
therefore, the model selected could not be loaded for the
deconvolution.

Action: Exit the program and reinstall the software, then try again.

4071- The selected pressures points do not form a valid set for deconvolution.
Cause: The data points selected for analysis do not contain enough
information to allow a DFT data reduction.

Action A: Edit data points in the table of the Collected Data window or select
another sample file. At least two points with strictly increasing
pressures and volumes adsorbed are required for a DFT Plus data
reduction.

Action B: Edit the pressure range on the DFT report options window.

4072- The range of pressures selected is too small to deconvolute using this model.
Cause: A null result was found using the selected model.

Action: Edit data points in the table of the Collected Data window or select
another sample file. At least two points with strictly increasing
pressures and volumes adsorbed are required for a DFT data
reduction.

239-42828-01 - Nov 2013 B-19


Appendix B Gemini VII

4073- The analysis gas [name] does not match the model gas [name].
Cause: The model assumes a specific gas and the sample file uses a different
one.

Action: Select a model that assumes the same gas.

4074- The analysis temperature [nn] does not match the model temperature [nn].

Cause: The temperature for the selected model did not match the analysis
temperature.

Action: Select a different model.

4075- The models cannot be located in the models folder. Reinstall the software.

Cause: The models could not be located. They may have been inadvertently
deleted or moved.

Action: Reinstall the software.

4077- Cannot get surface area for: [file name].

Cause: The Isotherm report for the named overlay file has Per gram selected
for the Volume Adsorbed and the Isotherm report for the primary file
has a surface area option selected for the Volume Adsorbed.

Action A: Edit the Isotherm report for the named overlay file and select a
surface area option for Volume Adsorbed.

Action B: Click Overlays on the Report options window of the primary file and
remove the named overlay file from the list.

4078- Slope and Y-Intercept cannot be determined from the selected points.
Cause: The Langmuir report cannot be generated from the selected points.

Action: Edit the calculation assignments in the Langmuir column on the


Collected Data window.

4079- Points found with negative pressure values will not appear on the graph.
Cause: Collected data contains negative pressure values.

Action: Negative pressure points are automatically removed from isotherm


graphs. To display negative pressure values appear on the graph:
Open the sample file and click the Collected Data tab. Deselect Use
calculation assignments and then select the points with negative
pressures as Outliers.

B-20 239-42828-01 - Nov 2013


Gemini VII Appendix B

4135- HOA file [filename] does not exist.

Cause: The sample file in the Heat of Adsorption report list does not exist.

Action: Go to Report > Heat of Adsorption. Click Add Samples, then select
the sample file.

4136- HOA [filename] is corrupt.

Cause: The sample file in the Heat of Adsorption report is corrupt.

Action: Go to Report > Heat of Adsorption. Select the correct sample file,
then click Remove Sample. Rerun the Heat of Adsorption report.

4400- The computer does not have the communications port specified for the Smart-
Prep. Cannot initialize.
Cause: The communications port associated with this unit was not valid.

Action: Run the setup program and set up the unit on a valid port.

4401- The communications port specified for the SmartPrep is already in use. Cannot
initialize.
Cause: The communications port associated with this instrument is in use by
some other program in the system.

Action: Close the other program to release the port. Restart the analysis
application.

4402- The communications port specified for the SmartPrep cannot be accessed.
Cannot initialize.
4403- Cannot communicate with SmartPrep Unit [n] - S/N: [nn].
Cause: The communications port associated with this unit was not valid.

Action: Run the setup program and set up the unit on a valid port.

4404- The application version of the SmartPrep Unit [n] - S/N: [nn] is invalid.
Cause: The controller software running on the designated instrument is
invalid.

Action: Use the SmartPrep setup program to download the proper controller
software to the instrument, or if unavailable, contact a Micromeritics
service representative.

239-42828-01 - Nov 2013 B-21


Appendix B Gemini VII

4405- Fatal communications error with SmartPrep Unit [n] - S/N: [nn].
Cause: There was a fatal error in the serial communications between the
application and the SmartPrep Instrument Controller. All displays for
that SmartPrep will be closed.

Action: Ensure that the SmartPrep is properly chained to the computer on the
communications port configured in the Setup program. Stop and re-
start the application. Contact a Micromeritics service representative if
this error message continues.

6000 Series
6000- An error occurred while loading the application control information. Data entry
cannot be performed. [Code number]
Cause: An error occurred accessing the control information disk file required
by this application.

Action: The disk drive may have failed or be corrupt. Run diagnostics on the
disk drive.

6008- The sample has an invalid status and cannot be used for this analysis.
Cause: A sample file with a status other than No Analysis or Prepared was
selected.

Action: Select a sample file with a status of No Analysis or Prepared.

6023- Desorption points in this sample file cannot be processed by this instrument.
Continue with adsorption points?

Cause: The selected sample file in this analysis has desorption points
selected in the pressure table. The analyzer (Gemini 2390a or 2390p)
cannot report desorption data.

Action A: Click Yes to continue with the analysis and report adsorption data
only.
Click No to choose a different file, or to edit the current file.

Action B: If using a Gemini 2390t, select Start Analysis for that unit.

6024- Some selected reports are invalid for this instrument.

Cause: The requested report cannot be generated with the Gemini 2390a.

Action: Edit the report selections on the Report Options window.

B-22 239-42828-01 - Nov 2013


Gemini VII Appendix B

6025- Serial write queue full.

Cause: There was a fatal error in communication between the analyzer and
the software. All displays for that instrument will be closed.

Action: Ensure the Ethernet cable is securely connected. Exit the application
and then restart it. Contact a Micromeritics service representative if
this error message continues.

6026- Measure Po for each point is not supported by this model. Choose another
sample file for analysis or change the Po option in the analysis conditions.

Cause: Measure Po for each point was selected as the saturation method.
This option is only available for the Gemini 2390p or 2390t.

Action: Edit the Po options in the analysis conditions and select Entered or
Most recent measured as the saturation pressure method.

6027- Analysis: Po dosing failure.

Cause: The Dewar does not contain enough cryogen to take an accurate
reading in the Po tube.

Action: Refill the Dewar with cryogen and restart the analysis.

6028- This instrument does not provide measured Po analyses.


Cause: An attempt was made to start an analysis on the Gemini 2390a using
a sample file in which Measure Po for each point was selected as the
saturation method. This feature is available only for the Gemini
2390p and 2390t.

Action A: Cancel the analysis, open the sample file, and choose Entered or
Most recent measured for the Po value. Restart the analysis.

Action B: Select a different file and continue with the analysis.

Action C: If a Gemini 2390p or 2390t is attached, select Start Analysis for that
unit.

6029- Instrument is not completely calibrated.


Cause: The instrument in use is missing calibrations.

Action: Select Unit > Calibration > Load from File and select a file
containing calibration data. Contact a Micromeritics service
representative if this error message continues.

239-42828-01 - Nov 2013 B-23


Appendix B Gemini VII

6030- A sample must be selected to proceed.


Cause: Select a sample file prior to starting a blank analysis or a QuickStart
analysis.

Action: Select a sample file and proceed with the analysis.

6031- Cannot read the analysis conditions parameter file


6032- Cannot read the adsorptive properties parameter file.
6033- Cannot read the report options parameter file.

Cause: The file is corrupt.

Action: Recreate the file or select a different file.

6035- The instrument [S/N nn] is not calibrated.

Cause: Upon initialization, the analyzer was unable to locate the calibration
file.

Action: Select Unit > Calibration > Load from File and select a file
containing calibration data. Contact a Micromeritics service
representative if this error message continues.

6036- Pressure is out of range.

Cause: There is a problem with the analyzer’s calibration.

Action: Select Unit > Calibration > Load from File and select a file
containing calibration data. Contact a Micromeritics service
representative if this error message continues.

6037- Sample pressure underrange.

Cause: A test of the sample pressure transducer showed a low reading. The
current operation will continue.

Action: Contact a Micromeritics service representative if this error message


continues.

6038- Sample pressure overrange.

Cause A: Adsorbate gas pressure is too high. The current operation will
continue.

Action A: Verify that the gas inlet pressure regulator setting does not exceed 15
to 18 psi (103.4 to 124.1 kPa). Contact a Micromeritics service
representative if this error message continues.

B-24 239-42828-01 - Nov 2013


Gemini VII Appendix B

Cause B: An error occurred in the pressure measurement electronics.

Action B: Contact a Micromeritics service representative if this error message


continues.

6039- Po pressure underrange.

Cause: A test of the Po pressure transducer showed a low reading. The


current operation will continue.

Action: Contact a Micromeritics service representative if this error message


continues.

6040- Po pressure overrange.

Cause A: The gas pressure in the Po tube is too high. The current operation will
continue.

Action A: Verify that the gas inlet pressure regulator setting does not exceed 15
to 18 psi (103.4 to 124.1 kPa). Contact a Micromeritics service
representative if this error message continues.

Cause B: An error occurred in the pressure measurement electronics.

Action B: Contact a Micromeritics service representative if this error message


continues.

6041- Quantity adsorbed underrange.

Cause: A test of the quantity adsorbed pressure transducer showed a low


reading. The current operation will continue.

Action: Contact a Micromeritics service representative if this error message


continues.

6042- Quantity adsorbed overrange.

Cause A: The rate of adsorption by the sample exceeded the response capacity
of the analyzer, preventing normal refilling of the gas reservoirs.

Action A: Repeat the analysis using a smaller amount of sample.

Cause B: An error occurred in the pressure measurement electronics.

Action B: Contact a Micromeritics service representative if this error message


continues.

239-42828-01 - Nov 2013 B-25


Appendix B Gemini VII

6043- Evacuation timeout.

Cause: The analyzer failed to reach a suitable vacuum level within the
specified evacuation time.

Action A: Remove and reattach the sample and balance tubes, ensuring that both
are securely in the port.

Action B: Verify that the vacuum pump is operating properly.

Action C: If actions A and B don’t correct the problem, degas the sample again
and repeat the analysis.

Action D: Contact a Micromeritics service representative if this error message


continues.

6044- Dosing timeout.

Cause A: The adsorbate gas supply was depleted by the analyzer during
analysis or termination.

Action A: Verify that the inlet valve on the gas bottle is open and that the gas
pressure regulator setting is between 15 and 18 psig (103.4 and 124.1
kPa). Check the adsorbate gas bottle to see if it is empty; replace if
necessary.

Cause B: Sample has adsorbed the maximum amount of gas available.

Action B: If additional data points are required, repeat the analysis with a
smaller amount of sample (to avoid exceeding 100 cm3 STP total
volume adsorbed).

6045- Elevator timeout.

Cause: The elevator was unable to reach the raised or lowered position.

Action: Check for obstructions. Contact a Micromeritics service


representative if this error message continues.

6048- Po fill timeout.

Cause: The adsorbate gas supply was depleted during and analysis or a Po
measurement.

Action: Verify that the inlet valve on the gas bottle is open and that the gas
pressure regulator setting is between 15 and 18 psig (103.4 and 124.1
kPa). Check the adsorbate gas bottle to see if it is empty; replace if
necessary.

B-26 239-42828-01 - Nov 2013


Gemini VII Appendix B

6049- Operator cancelled operation.

Cause: Cancel was clicked while an analysis or a Po measurement was in


progress.

Action: Restart the operation.

6050- Valve failure.

Cause: An error in the valve control electronics has occurred.

Action: Contact a Micromeritics service representative if this error message


continues.

6051- Power failure.

Cause: A power failure occurred during an automatic operation. The


operation was cancelled.

Action: Restart the operation.

6052- Zero calibration failed.


6053- Scale calibration failed.
6054- Transducer match failed
6055- Dosing servo calibration failed.
6056- Balance servo calibration failed
6057 Quantity adsorbed calibration failed.

Cause A: Calibration was out of the tolerance range.

Action A: Verify the preparatory steps for the calibration were performed
properly. For example, the sample tube may not have been empty.
If all preparatory steps were followed and no other message was
displayed, contact a Micromeritics service representative.

Cause B: One of the steps in the calibration failed. An additional error message
is displayed.

Action B: Refer to the Cause/Action for the error message that displayed with
this one.

239-42828-01 - Nov 2013 B-27


Appendix B Gemini VII

B-28 239-42828-01 - Nov 2013


Gemini VII Appendix C

C. CALCULATIONS

This appendix contains the calculations used in the analysis program.

Saturation Pressure
Saturation pressure (Po) is selected on the Po and Temperature Options dialog. It may be entered or
measured in the Po tube or on port 3.

• If entered, Po = user-entered value


• If measured, Po = equilibrated pressure reading after saturating Po tube or the sample tube

Relative Pressure Calculations


If Po was measured at intervals in the Po tube and several data points were collected in the interval:

• For points taken before the previous Po measurement,

 Po 2 – Po 1    t I – to 1 
Po I = Po 1 + ----------------------------------------------------------
 to 2 – to 1 

• For points taken after the previous Po, use the previous Po:

PoI = Po1

If Po was entered, use the entered Po:

PoI = PoE

Calculate relative pressure for the Ith data point:

P1
P rel = --------
1 Po I

where

PoI = saturation pressure for the Ith data point (mmHg)


Po1 = most previous measured saturation pressure before Ith data point (mmHg)
Po2 = first measured saturation pressure after the Ith data point (mmHg)
PoC = calculated Po
PoE = entered saturation pressure (mmHg)
tI = time when the Ith data point was taken (minutes)
to1 = time when Po1 was measured (minutes)
to2 = time when Po2 was measured (minutes)

239-42828-01 - Dec 2012 C-1


Appendix C Gemini VII

PrelI = relative pressure for the Ith data point (mmHg)


PI = absolute pressure for the Ith data point, taken at equilibrium (mmHg)

Quantity Adsorbed Calculations

Free Space

Measured
Measured free-space volumes are calculated using the following equations:

V MAN P1
V FW = --------------  ------ – 1  T STD
T MAN P2

P2
V FC = V FW  ------
 P 3

V FC – V FW
V BATH = --------------------------
T BATH
1 – ---------------
T AMB

where:

P1 = system manifold pressure before dosing helium onto sample (mmHg)


P2 = system manifold pressure after dosing helium onto sample (mmHg)
P3 = sample pressure after raising Dewar and equilibrating with helium (mmHg)
TSTD = standard temperature (273.15 K)
TAMB = approximate room temperature (298 K)
TMAN = system manifold temperature before dosing helium onto sample (K)
VMAN = manifold volume (cm3)
VFC = volume of free space, cold (cm3 at standard temperature)
VFW = volume of free space, warm (cm3 at standard temperature)
VBATH = portion of cold free space at analysis bath temperature: used in non-ideality
correction (cm3 at standard temperature)
TBATH = analysis bath temperature (K)

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Gemini VII Appendix C

Calculated
The calculated free space is determined by subtracting the gas capacity of the volume occupied by the
sample from the measured free space of the empty tube.

T STD
V FW = V WB + V – VS  -------------
T AMB

T STD
V FC = V CB + V – V S  ----------------
T BATH

where

VFW = calculated warm free space


VFC = calculated cold free space
VWB = warm free space of the empty tube
VCB = cold free space of the empty tube
ΔV = VP - VPB
VP = volume of the port used for analysis
VPB = volume of the port used for the blank analysis
VS = sample mass/density

239-42828-01 - Dec 2012 C-3


Appendix C Gemini VII

Equilibration
Equilibration is reached when the pressure change per equilibration time interval (first derivative) is
less than 0.01% of the average pressure during the interval. Both the first derivative and average pres-
sure are calculated using the Savitzky-Golay1 convolution method for polynomial functions. The
equations below are those used to compute weighted average and first derivative, respectively, for the
6th point of an 11-point window.

– 36  P 11 + P 1  + 9  P 10 + P 2  + 44  P 9 + P 3  + 69  P 8 + P 4  + 84  P 7 + P 5  + 89  P 6 
P AVG = -------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
429

5  P 11 – P 1  + 4  P 10 – P 2  + 3  P 9 – P 3  + 2  P 8 – P 4  +  P 7 – P 5 
P CHG = ----------------------------------------------------------------------------------------------------------------------------------------------------------------
110

P CHG
P PCPI = 100% --------------
P AVG

where the numerical constants are from the Savitzky-Golay convolution arrays, and

PAVG = average pressure (mmHg)


PCHG = change in pressure (mmHg)
PPCPI = percent change per interval
PI = Ith pressure reading taken at equilibrium intervals (mmHg)

If a non-zero value that is too small is entered for the maximum equilibration time, the
points are collected before equilibration is reached.

If PAVG is greater than 0.995 times the current Po, equilibration will not take place until
the Minimum equilibration delay for P/Po 0.995 has expired, in addition to the standard
equilibration criteria.

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Gemini VII Appendix C

Thermal Transpiration Correction


During data reduction, thermal transpiration correction is applied to the data if the user selected Ther-
mal transpiration correction from the Report Options dialog. Starting with the first collected
pressure, the following calculations are performed until the pressure ratio (PC/P) is greater than or
equal to 0.99.

2
P  SD  MD 3
Y = ------------------------------------  10
2.33  T

1+GY
 = -----------------------
1+HY

1
F = ------------------------------------------------------
2
  Y  +   Y + 

 T ABT 0.5 
PC =  1 – F –  F  ------------    P
 T RM 

where:

P = equilibrated collected pressure measured by gauge at temp TRM (mmHg)


SD = inside diameter of sample tube (mm), from the Report Options dialog
MD = thermal transpiration hard sphere diameter of gas (Å), from the Adsorptive
Properties dialog
T = average temperature [TABT + TRM] / 2 (K)
 = Weber’s coefficient, 0.033
 = Weber’s coefficient, 0.245
G = Weber’s coefficient, 2.5
H = Weber’s coefficient, 2
TABT = analysis bath temperature (K), from the Po and Temperature Options dialog
TRM = room temperature (298 K)
PC = corrected equilibrated pressure at temperature TABT (mmHg)
F,Y, = intermediate values for subsequent calculations

239-42828-01 - Dec 2012 C-5


Appendix C Gemini VII

BET Surface Area


For each point designated for surface area calculations, the BET2 transformation is calculated as
follows:

P rel
B 1 = ------------------------------------------------
1
-
 1.0 – P rel   N ads
1 1

where BI is in units of g/cm3 STP.

A least-squares fit is performed on the (PrelI ,BI) designated pairs where PrelI is the independent vari-
able and BI is the dependent variable. The following are calculated:

a.) Slope (S g/cm3 STP)

b.) Y-intercept (YINT g/cm3 STP)

c.) Error of the slope (SERR g/cm3 STP)

d.) Error of the y-intercept (YIERR g/cm3 STP)

e.) Correlation coefficient (Cc)

Using the results of the above calculations, the following can be calculated:

BET Surface Area (m2/g):

23
CSA   6.023  10 
SABET = ------------------------------------------------------------------------------------------------------------------------
3 18 2 2
 22414 cm STP    10 nm /m    S + Y INT 

where

CSA = analysis gas molecular cross-sectional area (nm2), user-entered on the Adsorp-
tive Properties dialog
BET C value:

S + Y INT
C = --------------------
Y INT

Volume of the Monolayer (cm3/g STP):

1 1
V M = --------------------- = --------------------
C  Y INT S + Y INT

Error of the BET Surface Area (m2/g):


2 2 0.5
SA BET   S ERR + YI ERR 
BET ERR = ----------------------------------------------------------------------------
Y INT + S

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Gemini VII Appendix C

Langmuir Surface Area


For each point designated for surface area calculations, the Langmuir3 transformation is calculated as
follows:

P rel
L I = ------------I
N ads
I

where LI is in units of g/cm3 STP

A least-squares fit is performed on the (PrelI, LI) designated pairs where PrelI is the independent vari-
able and LI is the dependent variable. The following are calculated:

a.) Slope (S g/cm3 STP)

b.) Y-intercept (YINT g/cm3 STP)

c.) Error of the slope (SERR g/cm3 STP)

d.) Error of the y-intercept (YIERR g/cm3 STP)

e.) Correlation coefficient

Using the results of the above calculations, the following can be calculated:

Langmuir Surface Area (m2/g):

23
CSA   6.023  10 
SA LAN = -------------------------------------------------------------------------------------------------
3 18 2 2
-
 22414 cm STP    10 nm /m   S

where

CSA = analysis gas molecular cross-sectional area (nm2), user-entered on the Adsorp-
tive Properties dialog

Volume of the Monolayer (cm3/g STP):

1
V M = ---
S

Langmuir b Value:

b =  Y INT   V M 

Error of the Langmuir Surface Area (m2/g):

SA LAN  S ERR
LAN ERR = -----------------------------------
S

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Appendix C Gemini VII

t-Plot
For each point designated for t-Plot4 calculations, the following calculations are done:

Thickness for the Ith point (Å):

HP2 HP3
t I = HP1  --------------------- (Halsey5)
ln  P rel 
I

or

HJP1 HJP3
t I = -------------------------------------------- (Harkins and Jura6)
HJP2 – log  P rel 
I

or

2
t I = STSA1  P rel  + STSA2  P rel  + STSA3
1 1

where:

tI = thickness for Ith point


HP1 = Halsey parameter #1
HP2 = Halsey parameter #2
HP3 = Halsey parameter #3
HJP1 = Harkins and Jura parameter #1
HJP2 = Harkins and Jura parameter #2
HJP3 = Harkins and Jura parameter #3
STSA1 = statistical thickness surface area parameter #1
STSA2 = statistical thickness surface area parameter #2
STSA3 = statistical thickness surface area parameter #3
PrelI = relative pressure for the Ith point (mmHg)

A least-squares analysis fit is performed on the (tI, NadsI) data pairs where tI is the independent variable
and NadsI is the dependent variable. Only the values of tI between tMIN and tMAX, the minimum and
maximum thickness, are used. The following are calculated:

a.) Slope (S cm3/g-Å STP)

b.) Y-intercept (YINT cm3/g STP)

c.) Error of the slope (SERR cm3/g-Å STP)

d.) Error of the Y-intercept (YIERR cm3/g STP)

e.) Correlation coefficient

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Gemini VII Appendix C

Using the results of the above calculations, the following can be calculated:

External Surface Area (m2/g):

3 10 3 3
 S cm /g – A STP    10 A/m    D cm liquid/cm STP -
SA EXT = ---------------------------------------------------------------------------------------------------------------------------------------------------------
6 3 3
F   10 cm /m 

where

F = surface area correction factor, user-entered on the t-Plot Report Options dialog
D = density conversion factor, user-entered on the Adsorptive Properties dialog

Micropore Surface Area (m2/g):

SA P = SA TOT + SA EXT

where SATOT is the BET surface area if the user enabled the BET report exclusively, or Langmuir sur-
face area if the user enabled the Langmuir report exclusively. If neither report has been selected, SATOT
is the BET surface area value calculated using a set of default parameters.

Micropore Volume (cm3 liquid/g):

3 3 3
V P =  Y INT cm /g STP    D cm liquid/cm STP 

239-42828-01 - Dec 2012 C-9


Appendix C Gemini VII

BJH Pore Volume and Area Distribution


For adsorption data, the relative pressure and quantity adsorbed data point pairs collected during an
analysis must be arranged in reverse order from which the points were collected during analysis. All
calculations are performed based on a desorption model, regardless of whether adsorption or desorp-
tion data are being used.

The data used in these calculations must be in order of strictly decreasing numerical value. Points
which do not meet this criterion are omitted. The remaining data set is composed of relative pressure
(Pr), quantity adsorbed (Va) pairs from (Pr1, Va1) to (PrN, VaN) where (PrN = 0, VaN = 0) is assumed as
a final point. Each data pair represents an interval boundary (or de-sorption step boundary) for inter-
vals i=1 to i=N-1 where N = total number of (Pr, Va) pairs.

Generally, the desorption branch of an isotherm is used to relate the amount of adsorbate lost in a
desorption step to the average size of pores emptied in the step. A pore loses its condensed liquid
adsorbate, known as the core of the pore, at a particular relative pressure related to the core radius by
the Kelvin7 equation. After the core has evaporated, a layer of adsorbate remains on the wall of the
pore. The thickness of this layer is calculated for a particular relative pressure from the thickness equa-
tion. This layer becomes thinner with successive decreases in pressure, so that the measured quantity
of gas desorbed in a step is composed of a quantity equivalent to the liquid cores evaporated in that
step plus the quantity desorbed from the pore walls of pores whose cores have been evaporated in that
and previous steps. Barrett, Joyner, and Halenda8 developed the method (known as the BJH method)
which incorporates these ideas. The algorithm used is an implementation of the BJH method.

Explanation of Terms
A pore filled with condensed liquid nitrogen has three zones:

a.) The core - evaporates all at once when the critical pressure for that radius is reached; the
relationship between the core radius and the critical pressure is defined by the Kelvin
equation.

b.) The adsorbed layer - composed of adsorbed gas that is stripped off a bit at a time with each
pressure step; the relationship between the thickness of the layer and the relative pressure is
defined by the thickness equation.

C-10 239-42828-01 - Dec 2012


Gemini VII Appendix C

c.) The walls of the cylindrical pore - the diameter of the empty pore is required to determine
the pore volume and pore area. End area is neglected.

Pore

Wall

Insignificant
compared to
core length

Calculations
The volumes adsorbed (Va) are converted to the liquid equivalent volumes (V1, cm3/g):

VII =  Va I   D 

where D is the Density Conversion Factor from the Adsorptive Properties dialog.

The relative pressure (Pr1) is assumed to be close to unity so that substantially all the pores in the sam-
ple are filled.

The corresponding Kelvin core radius is calculated. Only pores smaller than this size will be included:

–A
RcI = -----------------------------------------
 1 + F   ln  Pr I  

where

A = adsorbate property factor (the BJH Adsorptive Options dialog)


F = fraction of pores open at both ends (from the BJH Adsorption Report Options
dialog or the BJH Desorption Report Options dialog); assumed to be zero for
desorption

This radius will be adjusted for the thickness of the adsorbed layer during subsequent calculation steps.

239-42828-01 - Dec 2012 C-11


Appendix C Gemini VII

The thickness of the remaining adsorbed layer at this relative pressure is calculated:

HP2 HP3
Tw1 = HP1 -------------------
ln  Pr 1 

where

HP1, HP2, and HP3 are Halsey Parameters 1, 2, and 3 (respectively) from the Halsey Thickness Equa-
tion dialog.

These calculations illustrate the use of the Halsey thickness equation. If the Harkins/Jura equation was
selected, substitute the following wherever the thickness equation appears:

HJ1 HJ3
Tw 1 = --------------------------------------
HJ2 – log  Pr 1 

where

HJ1, HJ2, and HJ3 are Harkins-Jura Parameters 1, 2, and 3 (respectively) from the Harkins-Jura Thick-
ness Equation dialog.

The following calculations (a-c) are made for each relative pressure interval based on the increment of
volume desorbed during that interval. The variable I refers to the interval number, that is I=1 for the
first interval from Pr1 to Pr2, and so on. J refers to each previous interval during which new pores were
found. K refers to the total number of intervals in which new pores have been found. K is also the num-
ber of lines reported on the BJH table for collected data.

a.) The thickness of the adsorbed layer at the end of the interval is calculated as follows:

HP2 HP3
Tw I + 1 = HP1 -------------------------
ln  Pr I + 1 

(For the last pressure interval from the lowest PrI to zero relative pressure, TwI+1 = 0.)

For the first pressure interval, there are no previously opened pores so the volume desorbed
from walls of previously opened pores is zero (Vd1 = 0), and the remainder of Step (a) is
skipped.

The change in thickness of the wall layer due to desorption from previously opened pores is
calculated:

Tw = Tw 1 – Tw I + 1

The annular cross-sectional area of the wall layer desorbed is calculated for all previously
opened pores:

2 2 – 16 2 2
CSA J =    Rc j + Tw  – Rc j   10 cm /A 

C-12 239-42828-01 - Dec 2012


Gemini VII Appendix C

The total volume of gas desorbed from walls of previously opened pores is calculated:

Vd I =   LpJ   CSAaJ  for all previously opened pores

where LPJ = length of previously opened pores as calculated in Step b(2).

b.) The physical processes occurring for this pressure interval are determined as follows:

(1.) If VdI is greater than the current increment of volume desorbed (VlI - VlI+1), 
desorption from walls only is occurring. Total surface of walls exposed thus far (cm2/
g) is calculated as follows:

–8
SA W =    LPJ   Davg   10 J
cm/A  for all previously opened pores

where

DavgJ = weighted average pore diameter calculated below in Step b(2).

A new layer thickness (Tw) that will not overcompensate for the actual volume
desorbed in this interval is calculated:
8
 V1 I – V1 I + 1   10 A/cm 
Tw = -----------------------------------------------------------------
SAw I

Since no cores are evaporated in this pressure interval, no new pores are revealed.
Thus no ending Kelvin radius and average pore diameter are calculated for this inter-
val. Note that this means the report may have fewer tabulated intervals on the
collected data report than experimental pressure intervals.

(2.) If VdI is less than the volume increment desorbed during this interval  Vl 1 – Vl l + 1  , the
remaining volume is due to new pores with core evaporation taking place in this inter-
val. K, the number of intervals with new pores exposed, is increased by 1. (For the
interval from the lowest Pr1 to zero relative pressure, no new pore volume is calculated
and the rest of Step b is skipped.)

The volume desorbed from newly opened pores in this interval is calculated as
follows:

Vc I =  VI I – VI I + 1  – Vd I

The Kelvin radius for the end of the interval is calculated as follows:

–A
RcK + 1 = -------------------------------------------------
 1 + F   ln  Pr I + 1  

All new pores opened in this interval are represented by one pore having a length-

239-42828-01 - Dec 2012 C-13


Appendix C Gemini VII

weighted average pore diameter and a corresponding length sufficient to account for
the required volume of adsorbate. The weighted average pore diameter is calculated as
follows:

 2   Rc K + Rc K + 1   Rc K   Rc K + 1 
D avg = -----------------------------------------------------------------------------------
2 2
-
K
Rc K + Rc K + 1

DavgK is the diameter of a pore which would have a surface area that is the average of
the areas for pores radius RcK and RcK+1, if its length was the mean of the lengths at
those radii.

The relative pressure corresponding to DavgK is calculated as follows:

–1 – 2A
------------------------------------
-
P avg = ln
K  1 + F   D avg 
K

The thickness of the adsorbed layer at this pressure is calculated as follows:

HP2 HP3
Tw avg = HP1 ------------------------
K ln  P avg 
K

The decrease in thickness of the wall layer by desorption from the walls of new pores
during the lower portion of the pressure interval is calculated as follows:

Td = Tw avg – TW I + 1
K

The cross-sectional area of the newly opened pores is calculated as follows:

Davg K 2
– 16 2 2
CSAc K = ----------------- + Td  10 cm /A 
2

The length of the newly opened pores is calculated as follows:

Vc I
LP K = -----------------
CSAc K

c.) Pore diameters and radii are adjusted for the change in thickness of the adsorbed wall layer
during this interval. If new pores were opened during this interval, the average diameter is
adjusted by the change in layer thickness during the second portion of the desorption interval
as follows:

D avg = D avg + 2  Td 


Knew Kold

The layer thickness change during the whole interval is added to diameters of previously
opened pores as follows:

D avg = D avg + 2   Tw 
Jnew Jold

C-14 239-42828-01 - Dec 2012


Gemini VII Appendix C

(not including DavgK)

The layer thickness change desorbed during this interval also is added to the radii corre-
sponding to the ends of the pressure intervals as follows:

RcJnew = Rc Jold + Tw

for all except RcK+1.

Steps a to c are repeated for each pressure interval.

After the above calculations have been performed, the diameters corresponding to the ends of
the intervals are calculated as follows:

Dp J = 2  Rc J 

for all RcJ including RcK+1.

The remaining calculations are based on DP(I), Davg(I), and LP(I). These calculations are only
done for Davg(I) values that fall between the Minimum BJH diameter and the Maximum BJH
diameter specified by the operator on the BJH Adsorption Report Options dialog or the BJH
Desorption Report Options dialog.

(1.) Incremental Pore Volume (VpI, cm3/g):

D avg 2 16 2 2
Vp I =   Lp I  -------------I 10 cm /A
2

(2.) Cumulative Pore Volume (VpCUM(1), cm3/g):

VP CUM
1
=  VpJ for  J  1 

(3.) Incremental Surface Area (SAI, m2/g):

–2 – 10
SA I =   LP I   10 m/cm   D avg   10 m/A 
I

(4.) Cumulative Surface Area (SACUM(I), m2/g):

SA CUM
10
=  SAJ for J  1

(5.) dV/dD pore volume (dV/dDI, cm3/g-A):

VP I
dV/dD I = --------------------------------
Dp I – Dp I + 1

239-42828-01 - Dec 2012 C-15


Appendix C Gemini VII

(6.) dV/dlog(D) pore volume (dV/dlog(D)I, cm3g):

Dp I
dDv/d log  D  I = VP I / log  ----------------
Dp I + 1

(7.) dA/dD pore area (dA/dDI, m2/g-A):

SA I
dA/dD I = --------------------------------
Dp I – Dp I + 1

(8.) dA/dlog(D) pore area [dA/dlog(D)I, m2/g]:

Dp I
dA/d log  D  I = SA I / log  ----------------
Dp I + 1

For fixed pore size tables (if selected), the following calculations are performed:

(1.) Average Fixed Pore Size (DFavgJ, A):

Dp F + Dp F
DF avg = -----------------------------------
J J+1
-
J 2

calculated for all intervals in the fixed pore size table.

For the intervals with between the Minimum BJH diameter and the Maximum BJH
diameter.

(2.) Cumulative Pore volume (VpFCUMI, cm3/g):

VpFCUM = INTERP  DpF I + 1 


I

where INTERP(x) is the value interpolated from the function X = DpJ+1 and Y =
VPCUMJ, using an AKIMA semi-spline interpolation.

(3.) Incremental Pore Volume (VpFI, cm3/g):

VpFI = VpF CUM – VpF CUM


I I–1

where VpFCUM0 = 0.

(4.) Cumulative Surface Area (SAFCUMI, m2/g):

SAFCUM = INTERP  DpF I + 1 


I

where INTERP(x) is the value interpolated from the function X = DpJ+1 and Y =

C-16 239-42828-01 - Dec 2012


Gemini VII Appendix C

SACUMJ.

(5.) Incremental Surface Area (SAFI, m2/g):

SAFI = SAF CUM – SAF CUM


I I–1

where SAFCUM0 = 0.

(6.) dV/dD pore volume (dV/dDpFI, cm3/g-A)):

dV/dDpF I = INTERP  DpF I + 1 

where INTERP(x) is the value interpolated from the function X = DavgJ and Y = dV/
dDJ.

(7.) dV/dlog(D) pore volume [dV/dlog(DpF)I, cm3/g]:

dV/d log  D pF I  = INTERP  DpF I + 1 

where INTERP(x) is the value interpolated from the function X = DavgJ and Y = dV/
dlog(D)J.

(8.) dA/dD pore area (dA/dDpFI, m2/g-A):

dA/dDpF I = INTERP  DpF I + 1 

where INTERP(x) is the value interpolated from the function X = DavgJ and Y = dA/
dDJ.

(9.) dA/dlog(D) pore area [dA/dlog(DpFI), m2/g]:

dA/d log  D pF I  = INTERP  DpF I + 1 

where INTERP(x) is the value interpolated from the function X = DavgJ and Y = dA/
dlog(D)J.

239-42828-01 - Dec 2012 C-17


Appendix C Gemini VII

Compendium of Variables
Va = volume adsorbed expressed as a volume (cm3/g STP)
Vl = liquid equivalent volume of volume adsorbed (cm3/g)
D = density conversion factor from the Adsorptive Properties dialog cm3/cm3 STP)
Pr = relative pressure
Dp = pore (or core) diameter (A)
Rc = Kelvin radius (A) of core
A = adsorbate property factor; from the BJH Adsorptive Options dialog
F = fraction of pores open at both ends; from the BJH Adsorption Report Options
dialog or the BJH Desorption Report Options dialog
Tw = thickness of adsorbed layer desorbed during interval (A)
Tw = thickness of remaining adsorbed wall (A)

HP1, HP2, and HP3 are Halsey Parameters from the Halsey Thickness Equation dialog.

HJ1, HJ2, and HJ3 are Harkins and Jura Parameters from the Harkins/Jura Thickness Equation dialog.

STSA1, STSA2, and STSA3 are STSA parameters from the STSA Thickness Equation dialog.

Vd = volume of gas desorbed from walls of previously opened pores (cm3/g)


Davg = average pore diameter (A)
CSAa = annular cross-sectional area of the desorbed layer (cm2)
CSAc = cross-sectional area of opening of newly opened pores (cm2)
SAw = total surface area of walls exposed (cm2/g)
Td = thickness of layer desorbed from walls of newly opened pores (A)
Vc = volume desorbed from cores of newly opened pores (cm3/g)
Lp = length of pore (cm/g)

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Gemini VII Appendix C

Horvath-Kawazoe
A relative pressure lower limit is determined such that L-d0 never equals zero. All pressure points less
than this limit are discarded. For each collected relative pressure point, values of L are chosen in an
iterative manner, and the relative pressure (P/Po) determined by solving one of the following
equations:

• Slit Pore Geometry (original Horvath-Kawazoe)


• Cylinder Pore Geometry (Saito/Foley)
• Sphere Pore Geometry (Cheng/Yang)

Slit Pore Geometry (original HK)


When you use the original Horvath-Kawazoe9 method, the following equation is solved for each value
of P. The value of L is determined when the solved-for relative pressure is within 0.1% of the collected
absolute pressure.

32 4 4 4 10 4 10
K- IP  10 JA /J cm
P- = ------    
ln ------  ---------------------------------------------------
4
 ------------------------------3- – ------------------------------9- – ---------------
3
- + ----------------
9
Po RT    L – 2  d0  3   L – d0  9   L – d0  3  d0 9  d0

where

K = Avogadro’s number (6.023 x 1023)


R = gas constant (8.31441 x 107 ergs/mole K)
T = analysis bath temperature (K), from an entered or calculated
value on the Po and Temperature Options dialog
Z +Z
 = gas solid nuclear separation at zero interaction energy (Å), -----------------
S A
-
2

where:

ZS = sample equilibrium diameter at zero interaction energy (Å) from the Horvath-
Kawazoe Physical Properties dialog
ZA = zero interaction energy diameter from the Horvath-Kawazoe Physical 
Properties dialog

DA + DS  A 
d0 = -------------------------------
2

239-42828-01 - Dec 2012 C-19


Appendix C Gemini VII

where:

DA = molecular diameter (Å) from the Horvath-Kawazoe Physical Properties


dialog
DS = diameter of sample atom (Å) from the Horvath-Kawazoe Physical dialog

L = pore width (nucleus to nucleus) (Å)


P = equilibrium pressure (mmHg)
Po = saturation pressure (mmHg)
IP = interaction parameter (10-43 ergs-cm4) from the Horvath-Kawazoe Report
Options dialog

Cylinder Pore Geometry (Saito/Foley)


When you use the Saito-Foley10 method, the following equation is solved for each value of P. The
value of L is determined when the solved-for relative pressure is within 0.1% of the collected absolute
pressure.

32 4 4 d 0 2k  21 d 0 10 d0 4 
3 K IP  10 JA /J cm 1 -
ln  ------- = --- -------  --------------------------------------------------- 1 – -----   ------  k  ----- –  k  ----- 
P
 Po 4 RT d
4
  -----------
k + 1 rp   32  rp  rp

0 k=0

where

K = Avogadro’s number (6.023 x 1023)


R = gas constant (8.31441 x 107 ergs/mole K)
T = analysis bath temperature (K), from an entered or calculated
value on the Po and Temperature Options dialog
L = pore width (nucleus to nucleus) (Å)
P = equilibrium pressure (mmHg)
Po = saturation pressure (mmHg)
IP = interaction parameter (10-43 ergs-cm4) from the Horvath-Kawazoe Report
Options dialog
DA + DS  A 
d0 = -----------------------------
2
where:

DA = molecular diameter (Å) from the Horvath-Kawazoe Physical Properties


dialog

DS = diameter of sample atom (Å) from the Horvath-Kawazoe Physical dialog

– 4.5 – k- 2
k =  -------------------  k – 1 , 0 = 1.0
 k 

2
k =  –-------------------
1.5 – k-
 , = 1.0
 k  k–1 0

rp = radius of the cylindrical pore, L---


2

C-20 239-42828-01 - Dec 2012


Gemini VII Appendix C

Sphere Pore Geometry (Cheng/Yang)


When you use the Cheng/Yang11 method, the following equation is solved for each value of P. The
value of L is determined when the solved-for relative pressure is within 0.1% of the collected absolute
pressure.

* * 3 32 4 4
6  N 1  12 + N 2  22 L  10 J A /J cm
ln  ------- = ---------------------------------------------------------------------------------------------------------
P -
Po 3
RT  L – d  0

d0 6 1 1 d 0 12 1 1
–  -----  ------ T 1 + --- T 2 +  -----  ------ T 3 + ------ T 4
L 12 8 L 90 80

where

R = gas constant (8.31441 x 107 ergs/mole K)


T = analysis bath temperature (K), from an entered or calculated value on the Po
and Temperature Options dialog
DA + DS  A 
d0 = -----------------------------
2

where:

DA = molecular diameter (Å) from the Horvath-Kawazoe Physical Properties


dialog
DS = diameter of sample atom (Å) from the Horvath-Kawazoe Physical dialog

L = pore width (nucleus to nucleus) (Å)


P = equilibrium pressure (mmHg)
Po = saturation pressure (mmHg)
N1 = 4 L2 NS, where NS = number of sample atoms/cm2 at monolayer
N2 = 4 (L - d0)2 NA, where Ns = number of gas molecules/cm2
2
AS 6  MC    
e*12 = -,
------------ where AS = ----------------------------------------------
S A
-
4d S
6  
-----S- + ------A
S A
2
AA 3  MC    
*22 = --------------
- , where A A = ----------------------------------------------
A A
-
4D A
6 2

1 - -------------------
1
T1 = ------------------
3
– 3
1 – S 1 + S

1 1
T2 = -------------------
2
– ------------------2-
1 + S 1 – S

239-42828-01 - Dec 2012 C-21


Appendix C Gemini VII

1 - -------------------
1
T3 = ------------------
9
– 9
1 – S 1 + S
1 1
T4 = -------------------
8
– ------------------8-
1 + S 1 – S

L – d0
where S = --------------
L

Cheng/Yang Correction
This factor corrects for the nonlinearity of the isotherm. It adds an additional term to the equations for
the different geometrics:

1 1
ln  ------- = G  L  – 1 – --- ln  ------------
P
Po  1–

where

G(L) = one of the Horvath-Kawazoe equations given above


 = degree of void filling;  is estimated by first computing the monolayer capacity
(Vm) with the Langmuir equation over the range of data points from relative
pressure 0.02 to 0.2 or the maximum relative pressure included in the Horvath-
Kawazoe analysis.  is computed as the quantity adsorbed over Vm.

C-22 239-42828-01 - Dec 2012


Gemini VII Appendix C

Interaction Parameter
The interaction parameter (IP) results from the following calculations:

The Kirkwood-Muller dispersion coefficients -


2
6  MC   S   A
A S = -----------------------------------------------
S A
------ + ------
S A

2
3  MC   A   A
A A = -----------------------------------------------
2

where

MC2 = kinetic energy of electron (0.8183 x 10-6 erg)


S = polarizability of sample atoms (cm3)
A = polarizability of gas molecule (cm3)
S = diamagnetic susceptibility of sample atom (cm3)
A = diamagnetic susceptibility of gas molecule (cm3)

IP =  N A  A A  +  N S  A S 

where:

NA = number of gas molecules/cm2 at monolayer from the Horvath-Kawazoe Physi-


cal Properties dialog
NS = number of sample atoms/cm2 from the Horvath-Kawazoe Physical Properties
dialog 

Refer to Interaction Parameter Components later in this Appendix for recommended values.

239-42828-01 - Dec 2012 C-23


Appendix C Gemini VII

Additional Calculations
Based on the previous calculations, the following can be calculated:

Adjusted Pore Width (Å):


(Shell to Shell)

AL I = L I – DS

Cumulative Pore Volume (cm3/g):

V CUM = V I  D
I

where

D = density conversion factor (cm3 liquid/cm3 STP) on the Adsorptive Properties


dialog

dV/dD Pore Volume (cm3/g-Å):

dV- V CUM – V CUM


-------- = ------------------------------------------
I I–1
-
dD I AL I – AL I – 1

Median Pore Width (Å):

V CUM
V HALF = ----------------N-
2

log  D G  – log  D L 
D MED = 10 log  D L  +  log  V HALF  – log  V L    -----------------------------------------------
log  V G  – log  V L 

where

VCUMN = total cumulative pore volume (VCUMI) for points designated for Horvath-
Kawazoe calculations
VHALF = 50% of total cumulative pore volume
VL = cumulative pore volume (VCUMI) for first point less than VHALF
VG = cumulative pore volume (VCUMI) for first point greater than VHALF
DL = pore width (LI) that corresponds to VL
DG = pore width (LI) that corresponds to VG

C-24 239-42828-01 - Dec 2012


Gemini VII Appendix C

Interaction Parameter Components


Table C-1. Interaction Parameters

Interaction
Gas Bath Sample Type Parameter
Temperature Calculated
(K) Value*

Argon 87.3 Carbon (Ross/Olivier value) 2.61


Carbon (Horvath/Kawazoe value) 5.89
Zeolite 3.19

Carbon 298.15 Carbon (Ross/Olivier value) 4.20


Dioxide
Carbon (Horvath/Kawazoe value) 9.20
Zeolite 5.08

273.15 Carbon (Ross/Olivier value) 4.34


Carbon (Horvath/Kawazoe value) 9.35
Zeolite 5.22

194.65 Carbon (Ross/Olivier value) 4.72


Carbon (Horvath/Kawazoe value) 9.72
Zeolite 5.60

Nitrogen 77.15 Carbon (Ross/Olivier value) 2.84


Carbon (Horvath/Kawazoe value) 6.53
Zeolite 3.49

* The interaction parameter is entered in the Horvath-Kawazoe Report Options dialog in the
following field:
Interaction parameter: (calculated value) x 10-43 ergs-cm4

239-42828-01 - Dec 2012 C-25


Appendix C Gemini VII

The following values were used to calculate the values in Table C-1.

Carbon-Graphite Zeolite
DS= 3.40 DS= 3.04

NS= 3.845 x 1015 NS= 3.75 x 1015

S= 1.05 x 10-29 (Ross/Olivier) S= 1.94 x 10-29

13.5 x 10-29 (Horvath/Kawazoe, implicit) S = 0.85 x 10-24

S= 1.02 x 10-24

Nitrogen Argon
DA= 3.00 DA= 2.95

A= 6.71 x 1014 A= 7.608 x 1014

A= 3.6 x 10-29 A= 3.22 x 10-29

A= 1.76 x 10-24 A= 1.63 x 10-24

Carbon Dioxide
DA= 3.23

NA= 4.567 x 1014 (25 ºC)

5.45 x 1014 (0 ºC)

7.697 x 1014 (-78 ºC)

A= 5.0 x 10-29

A= 2.7 x 10-24

DA values are from van der Waal’s constant.


NA values are from liquid densities.
 and  values are derived from data found in Ross and Olivier12.

The physical parameters referenced in Saito/Foley are as follows:

Aluminophosphate Aluminosilicate
DS= 2.60 DS= 2.76

NS= 1.48 x 1015 Ns= 1.31 x 1015

S= 1.3 x 10-29 S= 1.3 x 10-29

S= 2.5 x 10-24 S = 2.5 x 10-24

C-26 239-42828-01 - Dec 2012


Gemini VII Appendix C

Dubinin-Radushkevich
The Dubinin-Radushkevich13 equation is as follows:

2 2
BT
log  V  = log  Vo  – ---------------  log Po
-------
 P

where:

V = volume adsorbed at equilibrium pressure (cm3/g STP)


Vo = the micropore capacity (cm3/g STP)
Po = saturation vapor pressure of gas at temperature T (mmHg)
P = equilibrium pressure (mmHg)
B = a constant
 = the affinity coefficient of analysis gas relative to Po gas
(for this application  is taken to be 1)
T = analysis bath temperature (K), from the Po and Temperature Options dialog

For each point designated for Dubinin-Radushkevich calculations, the following calculations are done:

LV = log (V)

2
LP = log  -------
Po
P

The intercept, log(Vo) can be found by performing a least-squares fit on the (LP,LV) designated pairs
where LP is the independent variable and LV is the dependent variable. Assuming the adsorption of
gas is restricted to a monolayer, Vo is the monolayer capacity. Based on this assumption, the following
are calculated:

a.) Slope (S cm3/g STP)

b.) Y-intercept (YI cm3/g STP)

c.) Error of the slope (SERR cm3/g STP)

d.) Error of the y-intercept (YIERR cm3/g STP)

e.) Correlation coefficient

Using the results of the above calculations, the following can be calculated:

Monolayer Capacity (cm3/g STP):

Vo = 10YI

239-42828-01 - Dec 2012 C-27


Appendix C Gemini VII

Error of Monolayer Capacity (cm3/g STP):

VoERR = Vo x (10YIERR - 1.0)

Micropore surface area (m2/g):

23
  Vo   6.023  10 
SDP = ----------------------------------------------------------------------
3 18 2 2
22414 cm   10 nm /m 

where

 = molecular cross sectional area of gas (nm2) from the Adsorptive Properties
dialog

C-28 239-42828-01 - Dec 2012


Gemini VII Appendix C

Dubinin-Astakhov
The Dubinin-Astakhov equation is a follows:

RT N N
log  V  = log  Vo  – ---------  log Po
-------
E 0 P

where

V = volume adsorbed at equilibrium pressure (cm3/g STP)


Vo = the micropore capacity (cm3/g STP)
Po = saturation vapor pressure of gas at temperature T (mmHg)
P = equilibrium pressure (mmHg)
T = analysis bath temperature (K)
R = the gas constant (0.0083144 kJ/mol)
E0 = characteristic energy (kJ/mole)
N = Astakhov exponent, may be optimized or user entered from the Dubinin
Report Options dialog
 = the affinity coefficient of the analysis gas relative to the Po gas, from the
Dubinin Adsorptive Options dialog 

For each point designated for Dubinin-Astakhov calculations, the following calculations are done:

LV = log(V)

N
LP = log Po
-------
P

A least-squares fit is performed on the (LP,LV) designated pairs where LP is the independent variable
and LV is the dependent variable. If the user selected Yes for the Optimize Astakhov Exponent
prompt, a systematic search for the optimum value of N is conducted by recalculating the linear regres-
sion and selecting the value of N that gives the smallest standard error of the y-intercept. The exponent
N is optimized to within 10-4. If the optimum value for N is not found in this range, an exponent of 2 is
used. The following are calculated:

a.) Slope (S cm3/g STP)

b.) Y-intercept (YI cm3/g STP)

c.) Error of the slope (SERR cm3/g STP)

d.) Error of the y-intercept (YIERR cm3/g STP)

e.) Optimized Astakhov exponent (N)

f.) Correlation coefficient

239-42828-01 - Dec 2012 C-29


Appendix C Gemini VII

Using the results of the above calculations, the following can be calculated:

Monolayer Capacity (cm3/g STP):

V0 = 10YI

Micropore Volume (cm3/g):

WI = (VI x D)

where

D = density conversion factor (cm3 liquid/cm3 STP) from the Adsorptive proper-
ties dialog 

Limiting Micropore Volume (cm3/g):

W0 = (V0 x D)

where

D = density conversion factor (cm3 liquid/cm3 STP) from the Adsorptive Proper-
ties dialog 

Error of Limiting Micropore Volume (cm3/g):

W0ERR = W0 x (10YIERR - 1.0)

Characteristic Energy (KJ/mole):

2.303  R  T
E = --------------------------------------
1/N
-
  2.303  S 


Modal Equivalent Pore Diameter (Å):

3 3 3 1/3
 3N 1/N 10 nm /A 
D MODE = 2   ----------------  ----------------------------- 
 3N + 1   Eo 

where

 = affinity coefficient of the analysis gas relative to the Po gas from the Dubinin
Adsorptive Options dialog

C-30 239-42828-01 - Dec 2012


Gemini VII Appendix C

Maximum Differential Pore Volume (cm3/g-Å):

This value is also known as frequency of the mode12

1/3
3N + 1 1/3N   E0 3N + 1
 exp  – ---------------- 
dV -
------------------ Max = 0.5   3N + 1   W o  ----------------  ----------------------------
-
dD mode 3N 3 3 3  3N 
10 nm /A

Mean Equivalent Pore Width (Å):


3 3 3 1/3
10 nm /A -
----------------------------
  E0
D MEAN = 2  -----------------------------------------
3N + 1
  ----------------
 3N 

Micropore surface area (m2/g):

E0 1/3
3N + 1
SDA = 1000  2.0  W 0  ------    ----------------
k  3N 

 is calculated by a polynomial approximation over the domain 0  x  1 as follows:

(x+1) = 1+b1x + b2x2 + b3x3 + b4x4 + b5x5 + b6x6 + b7x7 + b8x8 + (x) | (x) |  3 x 10-7

where

b1 = -0.57719 1652
b2 = 0.98820 5891
b3 = -0.89705 6937
b4 = 0.91820 6857
b5 = -0.75670 4078
b6 = 0.48219 9394
b7 = -0.19352 7818
b8 = 0.03586 8343

and where

3N + 1
x + 1 =  ----------------
3N

239-42828-01 - Dec 2012 C-31


Appendix C Gemini VII

Equivalent Pore Diameter (Å):


N 1/3N
 10 3 nm 3 /A 3
–  -----------------------------
   E0 
D i = 2  -----------------------------------------
ln  W i  – ln  W 0 

dV/dD Pore Volume (cm3/g-Å):

3 3 3 N D i –  3N + 1   10 3 nm 3 /A 3 
N
D i –3N
10 nm /A
  -----  exp –  -----------------------------    -----
dV-
-------- = 0.5  W 0  3N  -----------------------------
dD i   E0  2    E0   2

C-32 239-42828-01 - Dec 2012


Gemini VII Appendix C

MP-Method
For each point designated for MP-method14 calculations, the following calculations are done:

Thickness for the Ith point (Å):

HP2 HP3
t I = HP1  --------------------- (Halsey5)
ln  P rel 
I

or

HJP1 HJP3
t I = -------------------------------------------- (Harkins and Jura6)
HJP2 – log  P rel 
I

where:

tI = thickness for Ith point


HP1 = Halsey parameter #1
HP2 = Halsey parameter #2
HP3 = Halsey parameter #3
HJP1 = Harkins and Jura parameter #1
HJP2 = Harkins and Jura parameter #2
HJP3 = Harkins and Jura parameter #3
PrelI = relative pressure for the Ith point (mmHg)

With the (tI,VI) data pairs, the Akima semi-spline interpolation method is used to interpolate quantity
adsorbed values based on thickness values that are evenly spaced 0.2 Angstrom apart starting at the
first outlier point. Outliers are defined as those points have the maximum instantaneous slope within an
iteratively shrinking subset of all points. The remaining pore surface area calculation result is the slope
of the line defined by two consecutive interpolated points. The slopes of each pair of consecutive
points from the origin to the last point must be monotonically decreasing and non-negative. With the
interpolated points set the following can be calculated:

Average pore hydraulic radius (Å):

tI + tI – 1
R I = --------------------
2

239-42828-01 - Dec 2012 C-33


Appendix C Gemini VII

Remaining pore surface area for the Ith point (m2/g):


–6 3 3
 V I – V I – 1    D  10 m /cm 
S I = ----------------------------------------------------------------------------------
– 10
-
 t I – t I – 1   10 m/A

where

D = density conversion factor (cm3 liquid/cm3 STP) on the Adsorptive Properties


dialog

Incremental pore surface area occluded for the Ith point (m2/g):

S INC = S I – 1 – S I
I

Cumulative pore surface area occluded for the Ith point (m2/g):

S CUM = S INC + S INC +  + S INC


I I I–1 1

dA/dR pore surface area for the Ith point (m2/g-Å):

dA S INC
-------- = -------------------
I

dR I tI – tI – 1

Incremental pore volume occluded for the Ith point (cm3/g):

4 2 2 –8
V INC =  S INC  10 cm /m    R I  10 cm/Å 
I I

Cumulative pore volume occluded for the Ith point (cm3/g):

V CUM = V INC + V INC +  + V INC


I I I–1 1

dV/dR pore volume for the Ith point (cm3/g-Å):

dV V INC
-------- = -------------------
I

dR I tI – tI – 1

C-34 239-42828-01 - Dec 2012


Gemini VII Appendix C

Freundlich Isotherm
The Freundlich isotherm has the form:

Q 1/m
------- = CP
Qm

where

Q = quantity of gas adsorbed


Qm = quantity of gas in a monolayer
C = temperature-dependent constant
m = temperature-dependent constant

The pressure is absolute; typically, m > 1. In terms of quantity adsorbed,

1/m
Q = Q m CP

Taking the log of both sides yields:

1
log Q = log Q m C + ---- log P
m

Temkin Isotherm
The Temkin isotherm has the form,

Q RT
------- = --------- ln  A 0 P 
Qm q0 

where

Q = quantity of gas adsorbed


Qm = quantity of gas in a monolayer
q0 = the differential heat of adsorption at zero surface coverage
A = a0 exp {-q0/RT}, where 0 and a0 are adjustable constants

In terms of quantity adsorbed,

RTQ S
Q = -------------- ln A 0 + ln  -------
P
q0   Po

Thus, the plot of the natural log of absolute pressure vs. quantity adsorbed yields a straight line with
slope RTQm/q0 and intercept (ln A) RTQm/q0.

239-42828-01 - Dec 2012 C-35


Appendix C Gemini VII

DFT (Density Functional Theory)


The adsorption isotherm is known to convey a great deal of information about the energetic heteroge-
neity and geometric topology of the sample under study. The data of physical adsorption have been
used for many years as the basis for methods to characterize the surface area and porosity of adsor-
bents. Real solid surfaces rarely approach ideal uniformity of structure. It is accepted that in general,
the surface of even a nonporous material presents areas of greater or lesser attraction for adsorbed
molecules.

This energetic heterogeneity greatly affects the shape of the adsorption isotherm with the result that
simple theories such as the Langmuir and BET formulas can, at best, give only approximate estimates
of surface area. Porous solids virtually are never characterized by a single pore dimension, but instead
exhibit a more or less wide distribution of sizes. The observed adsorption isotherm for a typical mate-
rial is therefore the convolution of an adsorption process with the distribution of one or more
properties which affect that process. This was first stated mathematically by Ross and Olivier12 for the
case of surface energy distribution and has become known as the integral equation of adsorption.

The Integral Equation of Adsorption


In a general form for a single component adsorptive, the integral equation of adsorption can be written
as

Qp =  da db dcq  p a b c  f  a b c  (1)

where

Q(p) = the total quantity adsorbed per unit weight at pressure p,


a,b,c,... = a set of distributed properties,
ƒ(a,b,c,...) = the distribution function of the properties, and
q(p,a,b,c,...) = the kernel function describing the adsorption isotherm on unit surface of
material with fixed properties a,b,c,...

Equation (1), a Fredholm integral of the first kind, is a member of a class of problems known as ill-
posed, in that there are an infinite number of functional combinations inside the integral that will pro-
vide solutions. Even when the kernel function is known, experimental error in the data can make
solving for even a single distribution function a difficult task. Solving for multiple distribution func-
tions requires more data than provided by a single adsorption isotherm.

C-36 239-42828-01 - Dec 2012


Gemini VII Appendix C

Application to Surface Energy Distribution


Under certain conditions, an energetically heterogeneous surface may be characterized by a distribu-
tion of adsorptive energies. The conditions are that the sample is not microporous, i.e., that adsorption
is taking place on essentially a free surface with no pore filling processes at least to about 0.2 relative
pressure. Secondly, that each energetically distinct patch contributes independently to the total adsorp-
tion isotherm in proportion to the fraction of the total surface that it represents. This condition is
satisfied if the patches are relatively large compared to an adsorptive molecule, or if the energy gradi-
ent along the surface is not steep. In mathematical terms, this concept is expressed by the integral
equation of adsorption in the following form.

Qp  =  d q  p   f    (2)

where

Q(p) = the experimental quantity adsorbed per gram at pressure p,


q(p,ε) = the quantity adsorbed per unit area at the same pressure, p, on an ideal free
surface of energy e, and
ƒ(ε) = the total area of surface of energy e in the sample.

The exact form of the energy-dependent term depends on the form of the model isotherms expressed in
the kernel function and is provided in the model description.

Application to Pore Size Distribution


Similarly, a sample of porous material may be characterized by its distribution of pore sizes. It is
assumed in this case that each pore acts independently. Each pore size present then contributes to the
total adsorption isotherm in proportion to the fraction of the total area of the sample that it represents.
Mathematically, this relation is expressed by

Qp =  dH q  p H  f  H  (3)

where

Q(p) = the experimental quantity adsorbed at pressure p,


q(p,H) = the quantity adsorbed per unit area at the same pressure, p, in an ideal pore of
size H, and
f(H) = the total area of pores of size H in the sample.

Numerical values for the kernel functions in the form of model isotherms can be derived from modern
statistical mechanics such as density functional theory or molecular simulations, or can be calculated
from one of various classical theories based on the Kelvin equation. Several types are found in the
models library.

239-42828-01 - Dec 2012 C-37


Appendix C Gemini VII

Performing the Deconvolution


The integrations in equations (2) and (3) are carried out over all surface energies or pore sizes in the
model. The functions q(p,ε) and q(p,H), which we call the kernel functions, are contained in numeric
form as model isotherms. Because, in general, there is no analytic solution for equation (1), the prob-
lem is best solved in a discrete form; the integral equation for any distributed property Z becomes a
summation:

Qp =  q  p Z i  f  Z i  (4)
i

Given a set of model isotherms, q(p,Z), from a model chosen from the models library and an experi-
mental isotherm, Q(p), contained in a sample information file, the software determines the set of
positive values f(Z) that most nearly, in a least squares sense, solves equation (4). The distributed prop-
erty, surface energy or pore size, is then displayed on the Report Options window as a selection of
tables or graphs.

Regularization
DFT allows a selectable regularization (also referred to as smoothing) constraint to be applied during
the deconvolution process to avoid over-fitting in the case of noisy data or ill-fitting models. The
method used is based on co-minimization of the second derivative of the distribution. The relative
weight given to this term is determined by the value of the regularization parameter, which is set on the
DFT Pore Size or Surface Energy dialog and also is shown in the header of reports. The value of the
regularization parameter varies from zero (for no second derivative constraint) to ten (indicating a
weight equal to minimizing the residuals), or even larger. When the distribution and residuals obtained
change little with the value of the regularization parameter, it indicates that the chosen model provides
a good representation of the data. Conversely, a large sensitivity to the regularization parameter might
indicate inadequate data or a poor choice of model to represent the data.

C-38 239-42828-01 - Dec 2012


Gemini VII Appendix C

SPC Report Variables

Regression Chart Variables


The line of best fit for the Regression Chart is calculated by the usual Least Squares method. (Refer to
BASIC Scientific Subroutines Vol II, by F.R. Ruckdeschel, Copyright 1981 BYTE Publications/
McGraw Hill, p. 16.) If there is only a single point or all N points have the same x-value, there can be
no line of best fit in the standard form.

 xi
XAve = ---------
N

 yi
YAve = ---------
N

  x i – XAve   y i – YAve 
Slope = --------------------------------------------------------------
2
-
  x i – XAve 

The coefficient of Correlation for this line is also calculated in the usual way. (Refer to Mathematical
Handbook for Scientists and Engineers, by Granino A. Korn and Theresa M. Korn, Copyright 1961,
1968 McGraw Hill, Sec. 18.4.)

2
  x i – XAve 
x = -------------------------------------
N

2
  y i – YAve 
y = ------------------------------------
N

  x i – XAve   y i – YAve 
Cov  x y  = ---------------------------------------------------------------
N

Cov  x y 
Correlation Coefficient = -----------------------
x y

239-42828-01 - Dec 2012 C-39


Appendix C Gemini VII

Control Chart Variables

 yi
Mean = ---------
N

2
  y – Mean  -
StdDev = -----------------------------------
N–1

StdDev
CoefVar = -------------------
Mean

PlusNSig = Mean + n  StdDev

MinusNSig = Mean – n  StdDev

Summary Report
The following calculations and the results of previous calculations (as noted) are used to generate the
summary report:

a.) Single-point Surface Area (m2/g)

23
 Va   1 – Pr    CSA   6.023  10 
S 1PT = -------------------------------------------------------------------------------------------------
3 18 2 2
22414 cm STP  10 nm /m

where

Pr = pressure closest to 0.3 of the relative pressure points designated for surface
area calculations.
Va = volume corresponding to Pr

b.) Multipoint Surface Area

See BET Surface Area Calculations

c.) Langmuir Surface Area

See Langmuir Surface Area Calculations

d.) t-Plot Micropore Surface Area

See t-Plot calculations

e.) t-Plot External Surface Area

See t-Plot calculations

f.) BJH Cumulative Adsorption

C-40 239-42828-01 - Dec 2012


Gemini VII Appendix C

g.) BJH Cumulative Desorption

h.) Adsorption Total Pore Volume

i.) Desorption Total Pore Volume

j.) t-Plot Micropore Pore Volume

See t-Plot calculations

k.) Dubinin-Radushkevich Micropore Surface Area

See Dubinin-Radushkevich calculations

l.) Dubinin-Radushkevich Monolayer Capacity

See Dubinin-Radushkevich calculations

m.) Dubinin-Astakhov Micropore Surface Area

See Dubinin-Astakhov calculations

n.) Dubinin-Astakhov Micropore Volume

See Dubinin-Astakhov calculations

o.) MP-Method Cumulative Surface Area of Pores

MPSTOT = SCUMI, (see MP-method Calculations) for the last collected data point used in the
MP-method Calculations, and the range of hydraulic pore radii over which the cumulative
surface area was computed.

p.) MP-Method Cumulative Pore Volume of Pores

MPVTOT = VCUMI, (see MP-method calculations) for the last collected data point used in the
MP-method calculations, and the range of hydraulic pore radii over which the cumulative
pore volume was computed.

q.) Average Pore Hydraulic Radius (A)

MPV TOT –6 3 10
MPDAVER = ----------------------  10 m /cm  10 Å/m
MPS TOT

239-42828-01 - Dec 2012 C-41


Appendix C Gemini VII

References
1. Savitzky, A. and Golay, M.J.E., Anal. Chem. 36, 1627 (1964).

2. Brunauer, S.; Emmett, P.H.; and Teller, E., J. Am. Chem. Soc. 60, 309 (1938).

3. Langmuir, I., J. Am. Chem. Soc. 38, 2267 (1916); J. Am. Chem. Soc. 40, 1361 (1918); Phys. Rev 8,
149 (1916).

4. deBoer, J. H., et al, J. Catalysis 3, 32, 38, 44, 268 (1964); J. Catalysis 4, 319, 643, 649 (1965);
Cranston, R. and Inkley, F., Adv. Catalysis 9, 143 (1957).

5. Halsey, G., J. Chem. Phys. 16, 931-937 (1948).

6. Harkins, W.D. and Jura, G., J. Chem. Phys. 11, 431 (1943).

7. Kelvin, J. (published under the name of Sir William Thomson), Phil. Mag. 42, 448-452 (1871).

8. Barrett, E.P.; Joyner, L.S.; and Halenda, P.P., J. Am. Chem. Soc. 73, 373-380 (1951).

9. Horvath, G. and Kawazoe, K., J. Chem. Eng. Japan 16(6), 470 (1983).

10. Saito, A. and Foley, H. C., AlChE Journal 37(3), 429 (1991).

11. Cheng, Linda S. and Yang, Ralph T., Chemical Engineering Science 49(16), 2599-2609 (1994).

12. Ross and Olivier, J.P., “On Physical Adsorption,” J. Wiley and Sons, New York (1964).

13. Dubinin, M., Carbon 21, 359 (1983); Dubinin, M., Progress in Surface and Membrane Science 9,
1, Academic Press, New York (1975); Dubinin, M. and Astakhov, V., Adv. Chem. Ser. 102, 69
(1971); Lamond, T. and Marsh, H., Carbon 1, 281, 293 (1964); Medek, J., Fuel 56, 131 (1977);
Polanyi, M., Trans. Faraday Soc. 28, 316 (1932); Radushkevich, L., Zh. fiz. Kemi. 33, 2202
(1949); Stoeckli, H., et al, Carbon 27, 125 (1989).

14. Mikhail, R., Brunauer, S. and Bodor, E., J. Colloid and Interface Sci. 24, 45 (1968).

C-42 239-42828-01 - Dec 2012


Gemini VII Appendix D

D. ETHERNET CONFIGURATION

This section contains instructions for configuring an Ethernet port in either Microsoft® Windows 7 or
Windows Vista. The instructions do not apply to any other operating system.

Windows 7 Professional is recommended for the best user experience.

Configuring the Ethernet Port


The computer and analyzer communicate by means of an Ethernet connection. This appendix contains
instructions for ensuring that the Ethernet connection operates properly.

The windows in this section are Microsoft operating system windows, which may
be subject to change. The windows are included for reference purposes only.

Methods to access to these windows may vary. Refer to the Windows help system
for assistance, if necessary.

Windows 7
1. Select the Windows icon from the Status bar at the bottom of the screen, then select Control
Panel.

2. Click Network and Internet.

239-42828-01 - Dec 2012 D-1


Appendix D Gemini VII

3. Click Network and Sharing Center.

4. Click the Local Area Connection for your analyzer.

D-2 239-42828-01 - Dec 2012


Gemini VII Appendix D

5. Click Properties.

6. Highlight Internet Protocol Version 4 then click Properties.

239-42828-01 - Dec 2012 D-3


Appendix D Gemini VII

7. Click Use the following IP address then enter the following in the IP address field: 
192 168 77 100.

8. The following numbers should display in the Subnet mask field: 255.255.255.0. If not, enter
them. Leave all other fields blank.

9. Click OK then click Close until all windows are closed.

D-4 239-42828-01 - Dec 2012


Gemini VII Appendix D

Windows Vista
Windows 7 Professional is recommended for the best user experience.

1. Select the Windows icon from the Status bar at the bottom of the screen, then select Control
Panel.

2. Double-click Network and Sharing Center.

Click here

3. Click Manage network connection from the Tasks list on the left side of the window then click
Local Area Connection for your analyzer.

239-42828-01 - Dec 2012 D-5


Appendix D Gemini VII

4. Click Properties.

5. Highlight Internet Protocol Version 4 then click Properties.

6. Click Use the following IP address and enter the following in the IP address field:
192 168 77 100.

7. The following numbers should display in the Subnet mask field: 255.255.255.0. If not, enter
them. Leave all other fields blank.

8. Click OK then click Close until all windows are closed.

D-6 239-42828-01 - Dec 2012


Gemini VII Appendix E

E. ANALYZING SAMPLES WITH TOTAL SURFACE AREA OF


1.0M2 OR LESS

Introduction
The unique balanced measurement method used in the Gemini permits small amounts of surface area
to be measured with nitrogen gas that otherwise would be measurable only with krypton. Low surface
area samples often displace many times more nitrogen than they adsorb, especially if composed of
low-density materials of large particle size. The standard, built-in, helium free-space difference mea-
surement and mathematical compensation routine typically removes the effects of more than 99% of
this sample displacement, but the small amount remaining uncompensated can still be significant.

A technique for adding a compensating volume with negligible surface area into the balance tube has
been developed. It can reduce the size of the initial imbalance to low levels and allow precise measure-
ment of adsorbed gas.

This technique can be performed by the following methods:

• Using glass beads in the balance tube


• Using filler rods in the sample and balance tubes

Some users find that a combination of the two methods — using glass beads and filler rods — pro-
duces even better results. This, however, will depend on the type of sample you are analyzing.

Filler rods and glass beads are included in your accessories kit. Either straight-wall or bulb sample
tubes may be used.

Using Glass Beads


This method typically produces the best results.

1. Place an appropriate quantity of sample in a clean sample tube.

2. Load a second sample tube of the same size with glass beads that have a total volume
approximately the same as the sample volume.

a.) Determine the volume (v) of the sample in cm3:

w
v = ----

where

w = mass of sample (g)

 = density of sample (g/cm3); if density is unknown, refer to your laboratory


handbook

239-42828-01 - Dec 2012 E-1


Appendix E Gemini VII

b.) Determine the number (n) of glass beads needed to equal the sample volume:

v
n = ------------------------3-
0.014 cm

where

0.014 cm3 = approximate volume of one bead

3. Outgas the sample in the sample tube at an appropriate temperature for an appropriate amount of
time.

4. Install the sample tube (containing the outgassed sample) onto the analysis port and the sample
tube (containing the glass beads) onto the balance port.

5. Specify a one-point measurement (P/Po = 0.05 to 0.1) so that the initial free-space measurement
can quickly be determined; then perform the measurement.

6. Using the measured free space absolute value and the following relationship, determine the mass
of glass beads to remove from (or add to) the balance tube to reduce the free-space imbalance:

3 3
free space cm  2.515 g/cm -
---------------------------------------------------------------------------- = mass of glass beads  g 
3.53

where

2.515 g/cm3 = density of glass beads

3.53 = thermal correction (no units)

Note that the volume of one glass bead is approximately 0.014 cm3. Therefore, if the
measured free space is less than 0.02 cm3, it is unnecessary to correct the free space.

7. Use a beaker of warm water to bring the balance tube to room temperature before removing it
from the balance port of the Gemini to remove (or add) glass beads. This prevents condensation
of moisture from the laboratory atmosphere onto the cold glass beads.

8. Remove the balance tube:

• If the measured free space is negative (–), add the calculated mass of glass beads into the
balance tube.

• If the measured free space is positive (+), remove the calculated mass of glass beads from the
balance tube.

E-2 239-42828-01 - Dec 2012


Gemini VII Appendix E

9. Reinstall the balance tube onto the balance port of the Gemini analyzer.

For subsequent samples of the same material, you may simply use the same mass of
sample that was used for the initial sample so that the original bead quantity may be
left undisturbed on the balance port.

10. Prepare your analysis Dewar and place it on the elevator.

11. Close the sample compartment door and start your analysis.

Using Filler Rods


Filler rods of two different sizes are included in the accessory kit. Insert them as described below.

1. Clean your sample tube, balance tube, and filler rods; label your sample and balance tubes.

2. Hold the balance tube horizontally, and carefully slide the longer filler rod into the tube.
Filler Rod Sample Balance Tube

Do not hold the rod vertically and drop the rod into the tube; this may break the tube.

3. Prepare your sample and place it into the sample tube; insert the shorter filler rod into the sample
tube.

If you are using bulbous sample tubes, use the same size filler rod as used in the balance tube.

239-42828-01 - Dec 2012 E-3


Appendix E Gemini VII

4. Ensure that the filler rods are equidistant from the top of each tube. If they are not, add or remove
sample until they are the same distance from the top of the tube.

Packing of some powders may restrict gas access to the powder and cause slower
equilibration and/or lower results.

5. Attach the sample tube to the analysis port and the balance tube to the balance port.

6. Prepare your analysis Dewar and place it on the elevator.

7. Close the sample compartment door and start your analysis.

Be sure to select Measure for the free-space measurement.

Using Glass Beads and Filler Rods


This method may further improve results, depending on the sample material you are analyzing.

1. After determining and loading the amount of glass beads to use, insert a filler rod into the balance
tube.

2. Insert a filler rod into the sample tube. Ensure that the filler rods are equidistant from the top of
each tube. If they are not, add or remove sample until they are the same distance from the top of
the tube.

If you are using bulbous sample tubes, use the same size filler rod as used in the balance tube.

3. Attach the sample tube to the analysis port and the balance tube to the balance port.

4. Prepare your analysis Dewar and place it on the elevator.

5. Close the sample compartment door and start your analysis.

E-4 239-42828-01 - Dec 2012


Gemini VII Appendix F

F. DFT MODELS

Theories are developed by scientists in an attempt to explain a class of observed behavior. In the exper-
imental physical sciences, theories are often expressed in terms of a model that can be visualized and
described mathematically. Early models of physical adsorption were quite simple, both conceptually
and mathematically, for very practical reasons — hand computations were required. Today we can
explore complex models that describe adsorption systems on the atomic scale of size and sub-picosec-
ond time frame. This is not because scientists are smarter, but because of available tools. The DFT
models are created by classical approaches to adsorption as well as models based on modern statistical
thermodynamics.

Models Based on Statistical Thermodynamics


Included in this group are methods that model the adsorption system in terms of forces acting between
individual molecules.

Theoretical Background
Traditional adsorption theories attempt to describe experimental adsorption isotherms with an isotherm
equation containing a small number of parameters. At a minimum, these parameters include the extent
of the surface, such as the monolayer capacity (Qm), and the molar intensity of the gas-surface interac-
tion, such as the Langmuir “K” constant or the BET “C” constant. In some equations, additional
parameters take into account the lateral interaction of adsorbed molecules with each other. Other theo-
ries, such as the Dubinin-Astakhov approach, also include parameters for the effect of adsorbent
porosity.

Instead of this classical kinetic or phenomenological approach, we can use a molecular-based statisti-
cal thermodynamic theory that allows us to relate the adsorption isotherm to the microscopic
properties of the system: the fluid-fluid and fluid-solid interaction energy parameters, the pore size, the
pore geometry, and the temperature.

The following example is given so that you may understand how such a theory is constructed.

A clean sample of a solid material containing slit-shaped pores of a single width is placed in an evacu-
ated space. It is kept at a fixed temperature as a known quantity of pure argon gas is admitted into the
space surrounding the sample. The pressure within the space is recorded over time. In this situation,
the pressure falls rapidly from its initial value and gradually approaches a steady reading, called the
equilibrium pressure. The amount adsorbed corresponds to the quantity of gas effectively removed
from the gas phase by the solid surface. A graph that plots amount adsorbed versus equilibrium pres-
sure is called an adsorption isotherm.

Under such conditions, the argon atoms that randomly enter the pore space feel the presence of the
solid surface as the action of an external attractive force (the dispersion forces or Van der Waal’s
forces) and spend more time near the surface. As a result, the space near the surface acquires a greater
average density of argon atoms than regions farther removed.

239-42828-01 - Dec 2012 F-1


Appendix F Gemini VII

If the equilibrium distribution of the gas atoms near the surface could be described as a function of
pressure and the molecular properties of the components of the system, then a model could be con-
structed for the adsorption isotherm for the system. Modern physical chemistry provides several ways
to calculate this distribution. All these methods are based on the fundamental thermodynamic law that
such a system adopts a configuration of minimum free energy at equilibrium. Also needed is a descrip-
tion of the pairwise interaction energy between atoms, U(s), commonly given by a Lennard-Jones
potential:

 12  6
U  s  = 4  --- –  ---
s s

where

ε= a characteristic energy of the adsorptive,


= the diameter of the adsorptive molecule, and
s= the separation distance.

Molecular Simulation Methods


Two simulation techniques are commonly used to determine the distribution of gas molecules in a sys-
tem in equilibrium: the molecular dynamics method and the Monte Carlo method. Both of these are
used as reference methods because their results are considered exact.

Molecular Dynamics Method


In the molecular dynamics method, the position and velocity of individual gas particles are calculated
over time at very short intervals. This method takes into account both the forces acting between the gas
particles themselves and those acting between the gas particles and the atoms of the simulated surface.
As the simulated particles collide with each other and with the surface, the average concentration of
particles in the space near the surface is calculated; this calculation yields the amount of gas adsorbed.

This method can be thought of as a way to determine the chronological record of the movement of
each particle in the system using time steps of 10-14 seconds. Although the mathematics are simple,
the number of calculations required for a system of even a few hundred particles is astronomical and
challenges even the fastest computers.

Monte Carlo Method


In the Monte Carlo method, determination of the system equilibrium distribution begins with an
assumption (which may be only approximate) about the initial configuration of particles in the system.
The system is “equilibrated” through a process of randomly selecting one particle and conditionally
moving it a random distance in a random direction.

If the move results in a configuration of lower total energy, then the move is completed and another
particle is randomly selected to be moved.

F-2 239-42828-01 - Dec 2012


Gemini VII Appendix F

If the move results in a configuration of higher energy, a probability for that event is calculated, and a
random number between zero and one is generated. If the generated number is smaller than the proba-
bility of the event, then the move is accepted; otherwise, another particle is selected and the process is
repeated. This process continues until the average total energy of the system no longer decreases; at
this point, average configuration data are accumulated to yield the mean density distribution of parti-
cles in the system.

Monte Carlo simulations require considerably less computation time than molecular dynamic simula-
tions and can yield the same results; however, neither method provides a really practical way to
calculate complete isotherms.

Density Functional Formulation


Density functional theory offers a practical alternative to both molecular dynamic and Monte Carlo
simulations. When compared to reference methods based on molecular simulation, this theory pro-
vides an accurate method of describing inhomogeneous systems yet requires fewer calculations.
Because the density functional theory provides accuracy and a reduced number of calculations, it is the
basis embodied in the DFT models.

The system being modeled consists of a single pore represented by two parallel walls separated by a
distance H. The pore is open and immersed in a single component fluid (adsorptive) at a fixed temper-
ature and pressure. Under such conditions, the fluid responds to the walls and reaches an equilibrium
distribution. In this condition (by the definition of equilibrium), the chemical potential at every point
equals the chemical potential of the bulk fluid. The bulk fluid is a homogenous system of constant den-
sity; its chemical potential1 is determined by the pressure of the system using well-known equations.
The fluid near the walls is not of constant density; its chemical potential is composed of several posi-
tion-dependent contributions that must total at every point to the same value as the chemical potential
of the bulk fluid.

As noted previously, at equilibrium, the whole system has a minimum (Helmholtz) free energy, known
thermodynamically as the grand potential energy (GPE). Density functional theory describes the ther-
modynamic grand potential as a functional of the single-particle density distribution; therefore,
calculating the density profile that minimizes the GPE yields the equilibrium density profile. The cal-
culation method requires the solution of a system of complex integral equations that are implicit
functions of the density vector. Since analytic solutions are not possible, the problem must be solved
using iterative numerical methods. Although calculation using these methods still requires supercom-
puting speed, the calculation of many isotherm pressure points for a wide range of pore sizes is a
feasible task. The complete details of the theory and the mathematics can be found in the papers listed
under References at the end of this appendix.

The following graphs and accompanying text illustrate the results of using density functional theory to
predict the behavior of a model system.

Figure D-1 shows the density profile for argon at a carbon surface as calculated by density functional
theory for a temperature of 87.3 K and a relative pressure of about 0.5.

1.Chemical potential may be thought of as the energy change felt by a probe particle when it is inserted into the
system from a reference point outside the system. It can also be defined as the partial derivative of the grand
potential energy with respect to density (or concentration).

239-42828-01 - Dec 2012 F-3


Appendix F Gemini VII

Figure D-1. Density Profile for Argon on Carbon at 87.3 K and a Relative Pressure of 0.5

This figure represents a cross-section of the region near the surface. Note the layerwise distribution of
adsorbate; the first monolayer is sharply defined and a third layer can be distinguished. The area under
the profile curve represents the amount adsorbed per unit area at this pressure. The positions of the
maxima are separated by a distance determined by the size of the adsorptive atom.

Given the density profile, the amount adsorbed at the stated pressure can be easily calculated as the
integral over the profile. Repeating this calculation over a range of pressures yields the adsorption iso-
therm for the model. If the value of H is very large, the isotherm obtained corresponds to that of an
external, or free, surface. If H is smaller, a range of pressures is reached where two minima exist for
the grand potential, showing the presence of two metastable phases having different density distribu-
tions but the same chemical potential. The phase with the lower GPE is the stable one. As the pressure
is increased, a point is reached where the other phase becomes the stable one. This phase transition
reflects condensation of adsorbate in the pore; the pressure at which it occurs is called the critical pore-
filling pressure. This pressure is analogous to the condensation pressure predicted by the Kelvin equa-
tion in the classical model of pore filling.

Figure D-2 shows how the profiles change with pressure for a model pore with H = 40 Å. The insets
show the density profiles for the corresponding points of the isotherm.

F-4 239-42828-01 - Dec 2012


Gemini VII Appendix F

Figure D-2. Model Isotherm for Argon at 87.3 K in a 40 Å Slit in a Carbon Substrate

The profiles show the density distribution from one wall to the center of the slit; the other half of the
distribution is a mirror image of the profile shown.

As the pressure is first increased from zero, almost all the adsorbed atoms occupy a position close to
the surface.

• Inset a shows the profile corresponding to point a on the isotherm where the surface is about half
covered.

• At point b, the first layer is so full that it is more favorable for atoms to start a new layer.

• At point c, a third layer is forming. Point c, for this size slit, is the critical pore-filling pressure. In
inset c, the profile shows the density decreasing to near zero (actually the bulk gas density) at 4 or 5
molecular diameters from the surface.

• Inset d shows the profile converging on a density similar to that of bulk liquid argon in the center of
the pore, indicating a phase transition.

Note that the adsorption isotherms for pores larger than the one shown in Figure D-2 is identical up to
point c. The lower branch of the isotherm simply continues to a higher pressure for larger pores. This
trend is illustrated in Figure D-3, where isotherms for some larger size pores are shown. It is clear that
pore size is uniquely characterized by a corresponding critical pore-filling pressure. At large pore
sizes, density functional theory produces results for the critical filling pressures that are in good agree-
ment with those produced by the Kelvin equation.

239-42828-01 - Dec 2012 F-5


Appendix F Gemini VII

Figure D-3. Model Isotherms for Some Larger Pore Widths Argon on Carbon at 87.3 K

Figure D-4 shows model isotherms for pores in the micropore size range. Note the logarithmic scale
for pressure.

Figure D-4. Model Isotherms in the Micropore Size Range of Pore Width
Argon on Carbon at 87.3 K

F-6 239-42828-01 - Dec 2012


Gemini VII Appendix F

Pores of 4 Å width, barely larger than the argon atom (3.38 Å), fill at pressures below 1 millitorr. Pores
below 15 Å fill before a monolayer is completed on the surface of the larger pores. In the micropore
size range, the pore volume fills more gradually with pressure and the total shape of the isotherm is
important in characterizing the pore size.

Models Included

Non-Local Density Functional Theory with Density-Independent Weights


N2 - DFT Model
AR - DFT Model

Geometry: Slit
Substrate: Carbon (graphite)
Category: Porosity
Method: Nitrogen at 77 K; Argon at 87 K

Using the methods of non-local density functional theory, two sets of isotherms have been calculated
to serve as kernel functions for the characterization of porous solids from adsorption data. The model
isotherms are stored in binary format files. These models assume a slit-like pore geometry. The pore
size range from 4.0 to 4000 Å is covered in 91 classes in a geometric progression. The class intervals
are rounded to the nearest 0.02 molecular diameters. A model for the free or external surface is
included to account for unfilled pores. Each of the 92 model isotherms has been calculated at 181 pres-
sure points from near 1x10-6 to near 1.00 relative pressure.

These models are identical to those supplied with the original DOS version of DFT software. Some
slight difference from the DOS results may be noted when they are applied to the same data due to
improvements in the deconvolution algorithm and better regularization of the current software.

Non-Local Density Functional Theory with Density-Dependent Weights


N2 - Modified Density Functional

Geometry: Free surface


Substrate: Surface energy
Method: Nitrogen at 77 K

Using the modified Tarazona prescription described by Olivier (refer to References, numbers 3 and 4),
model isotherms were calculated for a wide range of adsorptive energies to a relative pressure of 0.6.
The model makes no provision for pore filling in the micropore region. If the sample solid contains
small mesopores, the isotherm data should be truncated (using the Select Data Points window) to a
suitably low relative pressure to avoid trying to fit this region; mesopore filling reports as a large area
of low energy in the calculated distribution of adsorptive potential.

The surface energy is reported in terms of the effective Lennard-Jones interaction parameter, ie., for
the adsorptive/adsorbent pair divided by Boltzmann’s constant. The units are therefore Kelvin.

239-42828-01 - Dec 2012 F-7


Appendix F Gemini VII

N2 - Cylindrical Pores - Oxide Surface


AR - Cylindrical Pores - Oxide Surface

Geometry Cylinder
Substrate Oxide
Category: Porosity
Method: Nitrogen at 77 K; Argon at 87 K

Model isotherms were calculated using a combination of statistical mechanical calculations and exper-
imental observations for macroporous silicas and MCM-41 mesoporous silicas as well as zeolites. The
pore-filling pressures were determined as a function of the pore size from adsorption isotherms on
MCM-41 materials characterized by X-ray and other techniques. The variation of the pore fluid den-
sity with pressure and pore size has been accounted for by density functional theory calculations. The
N2 model reports pore sizes ranging from 3.8 to 387 Å and the AR model from 3.8 to over 500 Å.

Reference: M. Jaroniec, M. Kruk, J.P. Olivier, and S. Koch, “A New Method for the
Accurate Pore Size Analysis of MCM-41 and Other Silica-Based
Mesoporous Materials,” Proceedings of COPS-V, Heidelberg, Germany
(1999).

N2 – Cylindrical Pores – Pillared Clay Surface (Montmorillionite)

Geometry Cylinder
Substrate Crystalline Silicate
Category: Porosity
Method: Nitrogen at 77 K

Model isotherms were calculated using a combination of statistical thermodynamic Non-Local Density
Functional Theory (NLDFT) calculations and experimental isotherms for reference samples of mont-
morillionite. The construction method for the hybrid models was analogous to that described in the
first reference below (Jaroniec et al,1999). The additional references add additional theoretical details
as well as examples of the application of the model to pillared clay catalysts. This model reports pore
widths from 3.8 to 387 Å.

F-8 239-42828-01 - Dec 2012


Gemini VII Appendix F

References: Mietec Jaroniec, Michal Kruk, James P. Olivier and Stefan Koch, “A
New Method for the Characterization of Mesoporous Silicas,”
Proceedings of COPS-V, 1999, Studies in Surface Science, Vol 128,
Characterization of porous Solids V , Unger, et al, Eds, Elsevier,
Amsterdam, 2000.
James P. Olivier and Mario L. Occelli, “Surface Area and Microporosity
of a Pillared Interlayered Clay (PILC) from a Hybrid Density Functional
Theory (DFT) Method,” The Journal of Physical Chemistry B; 2001,
105(3), 623-629.
M. L. Occelli, J. P. Olivier, J. A. Perdigon-Melon, and A. Auroux,
“Surface Area, Pore Volume Distribution, and Acidity in Mesoporous
Expanded Clay Catalysts from Hybrid Density Functional Theory (DFT)
and Adsorption Microcalorimetry Methods,” Langmuir 2002, 18, 9816-
9823.9b.
James P. Olivier, “The Importance of Surface Heterogeneity in
Developing Characterization Methods.” 6th International Symposium on
the Characterization of Porous Solids, Studies in Surface Science and
Catalysis 144, Elsevier, 2002.
James P. Olivier and Mario L. Occelli, “Surface Area and Microporosity
of Pillared Rectorite Catalysts from a Hybrid Density Functional Theory
Method,” Microporous and Mesoporous Materials 2003, 57, 291-296.

C02 - DFT Model

Geometry Slit
Substrate Carbon
Category: Porosity
Method: Carbon dioxide at 273 K

Model isotherms were calculated using the non-local prescription of Tarazona, employing molecular
parameters derived from the known bulk properties of carbon dioxide.

AR - Modified Density Functional Model

Geometry Free Surface


Substrate Any
Category: Surface energy
Method: Argon at 87 K

This model was produced in the same manner as the N2 Modified Density Functional model listed ear-
lier, except applicable to argon adsorbed at 87.3 K.

N2 - Tarazona NLDFT, Esf = 30.0K

Geometry Cylinder

239-42828-01 - Dec 2012 F-9


Appendix F Gemini VII

Substrate Oxide
Category: Porosity
Method: Nitrogen at 77 K

Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting
functions and a cylindrical pore geometry. The wall potential used is k = 30 K, typical for a silica or
alumina surface.

This model file is particularly useful for sizing zeolites or zeolite containing materials that have sub-
stantial micropore volume. The reported pore size range is 3.8 to 387 Å.

Reference: P. Tarazona, Phys. Rev. A 31: 2672 (1985).


Idem, Phys. Rev. A 32: 3148 (1985).
P. Tarazona, U. M. B. Marconi, and R. Evans, Mol. Phys. 60: 573 (1987).

N2 - Carbon Slit Pores by NLDFT


Ar - Carbon Slit Pores by NLDFT

Geometry Slit
Substrate Carbon
Category: Porosity
Method: Nitrogen at 77 K; Argon at 87 K

Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting
functions and a slit-like pore geometry. These models are slightly different from N2-DFT and Ar-DFT
models that were calculated using NLDFT with density independent weighting functions.

The reported pore size range is from 3.5 to 1000 Å.

Reference: P. Tarazona, Phys. Rev. A 31: 2672 (1985).


Idem, Phys. Rev. A 32: 3148 (1985).
P. Tarazona, U. M. B. Marconi, and R. Evans, Mol. Phys. 60: 573 (1987).

N2 - Carbon Finite Pores, As=6, 2D-NLDFT


Ar - Carbon Finite Pores, As=6, 2D-NLDFT

Geometry Finite Slit


Substrate Carbon
Category: Porosity
Method: Nitrogen at 77 K; Argon at 87 K

F-10 239-42828-01 - Dec 2012


Gemini VII Appendix F

Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting
functions assuming 2D model of finite slit pores having a diameter-to-width aspect ratio of 6.

This model is particularly useful for microporous carbon materials. The reported pore size range is
from 3.5 to 250 Å.

Reference: Jacek Jagiello and James P. Olivier. “A simple two-dimensional NLDFT


model of gas adsorption in finite carbon pores. Application to pore
structure analysis.,” The Journal of Physical Chemistry C,
113(45):19382-19385, 2009.

N2 - Carbon Finite Pores, As=12, 2D-NLDFT


Ar - Carbon Finite Pores, As=12, 2D-NLDFT

Geometry Finite Slit


Substrate Carbon
Category: Porosity
Method: Nitrogen at 77 K; Argon at 87 K

Model isotherms were calculated using the same methods and assumptions that were used in the model
above except in this model, the aspect ratio is equal to 12.

These two finite pore models may be used as a research tool in conjunction with independent analyti-
cal techniques such as high-resolution transmission electron microscopy (HRTEM) and/or X-ray
diffraction (XRD) to obtain comprehensive information about the structure of studied carbon material.

Reference: See above reference.

N2 - Carbon Cylinder, single-wall nanotube by NLDFT


Ar - Argon Cylinder, single-wall nanotube by NLDFT

Geometry Cylinder
Substrate Carbon
Category: Porosity
Method: Nitrogen at 77 K; Argon at 87 K

Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting
functions and cylindrical pore geometry. The pore wall potential is described by the Lennard-Jones
potential of interaction between a gas molecule and the graphitic surface of an infinitely long cylinder.

239-42828-01 - Dec 2012 F-11


Appendix F Gemini VII

This model is particularly useful for characterizing carbon single-wall nanotubes. The reported pore
size range is from 3.5 to 1000 Å.

Reference: P. Tarazona, Phys. Rev. A 31: 2672 (1985).


Idem, Phys. Rev. A 32: 3148 (1985).
P. Tarazona, U. M. B. Marconi, and R. Evans, Mol. Phys. 60: 573
(1987).

N2 - Carbon Cylinder, multi-wall nanotube by NLDFT


Ar - Argon Cylinder, multi-wall nanotube by NLDFT

Geometry Cylinder
Substrate Carbon
Category: Porosity
Method: Nitrogen at 77 K; Argon at 87 K

Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting
functions and cylindrical pore geometry. The pore wall potential is described by the Lennard-Jones
potential of interaction between a gas molecule and multiple concentric graphitic surfaces of infinitely
long cylinders.

This model is particularly useful for characterizing carbon multi-wall nanotubes. The reported pore
size range is from 3.5 to 1000 Å.

Reference: See above reference.

Ar - Zeolites H-Form by NLDFT

Geometry Cylinder
Substrate Zeolite
Category: Porosity
Method: Argon at 77 K

Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting
functions and cylindrical pore geometry. The pore wall potential is described by the Lennard-Jones
potential of interaction between a gas molecule and the oxide surface of an infinitely long cylinder.

This model is particularly useful for characterizing oxides and H+ and (NH4)+ exchanged zeolites. The
reported pore size range is from 3.5 to 300 Å.

F-12 239-42828-01 - Dec 2012


Gemini VII Appendix F

Ar - Zeolites Me-Form by NLDFT

Geometry Cylinder
Substrate Zeolite
Category: Porosity
Method: Argon at 77 K

Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting
functions and cylindrical pore geometry. The pore wall potential is described by the Lennard-Jones
potential of interaction between a gas molecule and the oxide surface of an infinitely long cylinder.

This model is similar to the model above, but it more appropriate is for characterizing alkali metal
exchanged zeolites. The reported pore size range is from 3.5 to 300 Å.

Models Based on Classical Theories


Both surface energy distribution and pore size distribution may be evaluated using classical
approaches to model kernel functions for use with equation (1) of the DFT Theory in the calculations
appendix. Be aware that the deconvolution method only provides a fitting mechanism; it does not over-
come any inherent shortcomings in the underlying theory.

Surface Energy
The use of classical theories to extract adsorptive potential distribution is mostly of historical interest.
At a minimum, the equation must contain a parameter dependent on adsorption energy and another
dependent on monolayer capacity or surface area. This is sufficient to permit the calculation of the set
of model isotherms that is used to create a library model. The Langmuir equation has been used in the
past, as have the Hill-de Boer equation and the Fowler-Guggenheim equation. All of these suffer from
the fact that they only describe monolayer adsorption, whereas the data may include contributions
from multilayer formation.

Pore Size
It is well established that the pore space of a mesoporous solid fills with condensed adsorbate at pres-
sures somewhat below the prevailing saturated vapor pressure of the adsorptive. When combined with
a correlating function that relates pore size with a critical condensation pressure, this knowledge can be
used to characterize the mesopore size distribution of the adsorbent. The correlating function most
commonly used is the Kelvin equation. Refinements make allowance for the reduction of the physical
pore size by the thickness of the adsorbed film existing at the critical condensation pressure. Still fur-
ther refinements adjust the film thickness for the curvature of the pore wall.

The commonly used practical methods of extracting mesopore distribution from isotherm data using
Kelvin-based theories, such as the BJH method, were for the most part developed decades ago and
were designed for hand computation using relatively few experimental points. In general, these meth-
ods visualize the incremental decomposition of an experimental isotherm, starting at the highest
relative pressure or pore size. At each step, the quantity of adsorptive involved is divided between pore
emptying and film thinning processes and exactly is accounted for. This computational algorithm fre-

239-42828-01 - Dec 2012 F-13


Appendix F Gemini VII

quently leads to inconsistencies when carried to small mesopore sizes. If the thickness curve used is
too steep, it finally will predict a larger increment of adsorptive for a given pressure increment than is
actually observed; since a negative pore volume is non-physical, the algorithm must stop. Conversely,
if the thickness curve used underestimates film thinning, accumulated error results in the calculation of
an overly large volume of (possibly nonexistent) small pores.

The use of equation (1) represents an improvement over the traditional algorithm. Kernel functions
corresponding to various classical Kelvin-based methods have been calculated for differing geometries
and included in the list of models.

Models Included

Kelvin Equation with Halsey Thickness Curve


N2 - Halsey Thickness Curve

Geometry Slit
Substrate Average
Category: Porosity
Method: Nitrogen at 77 K

The kernel function is calculated using the Halsey equation with standard parameters:

– 5.00 1/3
t = 3.54  ----------------------
ln  P/Po 

The nitrogen properties used in the Kelvin equation are:

Surface tension = 8.88 dynes cm-1

Molar density = 0.02887 g cm-3

N2 - Halsey Thickness Curve

Geometry Cylinder
Substrate Average
Category: Porosity
Method: Nitrogen at 77 K

The calculation is the same as above except that cylindrical geometry is assumed.

Reference: G. Halsey, J. Chem. Phys 16, 931 (1948).

F-14 239-42828-01 - Dec 2012


Gemini VII Appendix F

Kelvin Equation with Harkins and Jura Thickness Curve


N2 - Harkins and Jura Thickness Curve

Geometry Slit
Substrate Average
Category: Porosity
Method: Nitrogen at 77 K

The kernel function is calculated using the Harkins and Jura equation with standard parameters:

13.99 1/2
t =  ---------------------------------------------
0.034 – log  P/Po 

The nitrogen properties used in the Kelvin equation are:

Surface tension = 8.88 dynes cm-1

Molar density = 0.02887 g cm-3

N2 - Harkins and Jura Thickness Curve

Geometry Cylinder
Substrate Average
Category: Porosity
Method: Nitrogen at 77 K

The calculation is the same as above except that cylindrical geometry is assumed.

Reference: W. D. Harkins and G. Jura, J.A.C.S. 66, 1366 (1944).


J. H. DeBoer et al., J. Colloid and Interface Sci. 21, 405 (1966).

239-42828-01 - Dec 2012 F-15


Appendix F Gemini VII

Kelvin Equation with Broekhoff-de Boer Thickness Curve


N2 - Broekhoff-de Boer Model

Geometry Slit
Substrate Average
Category: Porosity
Method: Nitrogen at 77 K

The kernel function is calculated using the Broekhoff-de Boer equation with standard parameters:

0 – 16.11 – 0.1137
t
log  p/p  = ---------------
2
- + 0.1682
t

The nitrogen properties used in the Kelvin equation are:

Surface tension = 8.88 dynes cm-1

Molar density = 0.02887 g cm-3

N2 - Broekhoff-de Boer Model

Geometry Cylinder
Substrate Average
Category: Porosity
Method: Nitrogen at 77 K

The calculation is similar to the above except that cylindrical geometry is assumed, and the film thick-
ness depends on pore size (see reference).

Reference: Specifically, equations 20 and 21 in: J.C.P. Broekhoff and J.H. de Boer,
“The Surface Area in Intermediate Pores,” Proceedings of the
International Symposium on Surface Area Determination, D.H. Everett,
R.H. Ottwill, eds., U.K. (1969).

F-16 239-42828-01 - Dec 2012


Gemini VII Appendix F

References
The papers listed below provide additional information on DFT models:

1. “Determination of Pore Size Distribution from Density Functional Theoretic Models of


Adsorption and Condensation within Porous Solids,” J.P. Olivier and W.B. Conklin,
Micromeritics Instrument Corp; presented at the International Symposium on the Effects of
Surface Heterogeneity in Adsorption and Catalysts on Solids, Kazimierz Dolny, Poland (July
1992).

2. “Classification of Adsorption Behavior: Simple Fluids in Pores of Slit-shaped Geometry,” Perla


B. Balbuena and Keith E. Gubbins, Fluid Phase Equilibria, 76, 21-35, Elsevier Science
Publishers, B.V., Amsterdam (1992).

3. “Modeling Physical Adsorption on Porous and Nonporous solids Using Density Functional
Theory,” J.P. Olivier, Journal of Porous Materials, 3, 9-17 (1995).

4. “The Determination of Surface Energetic Heterogeneity Using Model Isotherms Calculated by


Density Functional Theory,” J.P. Olivier; presented at the Fifth International Conference on the
Fundamentals of Adsorption, Pacific Grove, CA (1995).

239-42828-01 - Dec 2012 F-17


Appendix F Gemini VII

F-18 239-42828-01 - Dec 2012


Gemini VII Index

INDEX
A Ar Carbon Finite Pores, As=12, 2D-NLDFT model, F-11
Ar Carbon Finite Pores, As=6, 2D-NLDFT model, F-10
Absolute pressure dosing, 5-12
Ar Carbon Slit Pores by NLDFT model, F-10
Accessories, ordering, 10-1
AR Cylindrical Pores - Oxide Surface model, F-8
Adding an analyzer, 4-13
AR DFT model, F-7
Adsorption isotherm, F-1
AR Modified Density Functional Model, F-9
Adsorption points, 1-5
Argon Cylinder, multi-wall nanotube by NLDFT model,
Adsorptive properties
F-12
command, 5-17
Argon Cylinder, single-wall nanotube by NLDFT model,
create file, 3-14
F-11
Advanced format
Avogadro's number, C-19
sample information file, 3-6
Axis, view coordinates, 7-23
Advanced format, Sample defaults, 3-2
All file status, 2-8
Alpha-S Method, 5-33 B
Alumina
Inspecting and Changing Alumina, video, 2-13 Balance tube, on schematic, 6-9
replacing in oil vapor traps, 9-11 Basic
Analysis format, 3-1
bath, 1-6 sample information file, 3-7
blank, 3-27, 9-26 BET surface area
Dewar, 1-9, 3-22 calculations, C-6
Dewar, checking, 9-5 report, 5-24
gas, 1-5, 1-7 BJH
performing, 3-25 Adsorption/Desorption report, 5-36
preparing for, 3-11 calculations, C-10
QuickStart method, 3-26 plot report options, 5-40
small surface area sample, E-1 pore volume and area distribution, C-10
Analysis conditions tabular report options, 5-38
calculation assignments, 5-12 Blank analysis
command, 5-11 command, 6-7
creating the file, 5-11 performing, 3-27, 9-26
defined, 3-13 Boltzmann’s constant, F-7
Analysis program Broekhoff-de Boer thickness curve, 5-31
installing, 4-2
uninstalling, 4-31
C
using, 2-6
version number, 2-13 Calculations, C-1
Analyzer Calibration
adding, 4-13 command, 6-19
changing Ethernet connection, 4-22 information, 6-16
cleaning, 9-5 load file, 6-23
configurations, 6-16 match transducers, 9-31
description, 1-4 reinstalling calibration file, 4-24
maintaining, 9-4 save to file, 6-22
moving, 4-16 servo valve, 6-21, 9-31, 9-32
physical dimensions, 1-9 zero pressure, 6-20, 9-30
removing, 4-20 Carbon Black STSA thickness curve, 5-31
turning on/off, 2-5 Carbon Cylinder
Analyzing file status, 2-8 multi-wall nanotube by NLDFT model, F-12

239-42828-01 - Dec 2012 Index-1


Index Gemini VII

single-wall nanotube by NLDFT model, F-11 Surface Energy, F-13


Cautions, defined, 1-3 Surface Energy options, 5-49
Chemical potential, F-3 Diagnostics
Cheng/Yang gas line test, 9-22
calculations, C-22 leak test, 9-16
Pore Geometry, C-21 Differential free space, 1-5
Cleaning Differential pressure transducer, 6-9
analyzer, 9-5 Dollimore-Heal Adsorption/Desorption report, 5-41
Dewar, 9-5 Dubinin
Close reports command, 7-3 calculations, C-27
CO2 DFT Model, F-9 report, 5-49
Cold free space, 5-15 tabular report options, 5-50
Collected data, 5-57 transformed isotherm plot options, 5-51
Common fields and buttons Dubinin-Astakhov calculations, C-29
for file menu, 5-1 Dubinin-Radushkevich calculations, C-27
for reports menu, 7-2
for unit menu, 6-2
Complete file status, 2-8 E
Components and connectors Electrical, 1-9
front panel, 2-2 Enable manual control command, 6-8
rear panel, 2-4 Entered data, 5-57
sample compartment, 2-3 Entered file status, 2-8
vacuum pump, 2-4 Equilibration, calculations, C-4
Computer requirements, 1-10 Error messages
Control chart, 7-7 2400 series, B-1
Conventions, used in operator’s manual, 1-3 2500 series, B-7
Convert file, 3-34 4000 series, B-10
Coolant, 1-6 6000 series, B-22
Cryogen, 1-6 Ethernet
configuring port for Vista, D-5
configuring port for Windows 7, D-1
D Evaluating Data, video, 2-12
Data Export
collected, 5-57 file, 3-32
entered, 5-57 sample files, 5-6
points, 1-5
Defaults for sample information files, 8-2
Degas conditions F
command, 5-10 File
defining file, 3-12 default file name extensions, 2-8
Degassing export, 3-32
ordering units, 10-1 list, 3-31
units, 1-6 print, 3-30
Density Functional Theory, F-3 StarDriver, convert, 3-34
Dewar status, 2-8
checking, 9-5 File menu
cleaning, 9-5 Adsorptive properties command, 5-17
How to Prepare a Dewar, video, 2-12 Analysis conditions command, 5-11
installing, 3-22 Close, 5-6
precautions, 3-22 Close All, 5-6
DFT models, F-1 Common fields and buttons, 5-1
See Models Convert, 5-7
DFT report Degas conditions command, 5-10
Pore Size options, 5-46 Exit, 5-7

Index-2 239-42828-01 - Dec 2012


Gemini VII Index

Export, 5-6 for multiple samples, 3-35


Print, 5-6
Report options command, 5-18
Sample information files command, 5-8 H
Save, 5-4 Halsey thickness curve, 5-31
Save All, 5-6 Harkins and Jura thickness curve, 5-31
Save As, 5-5 Heat of Adsorption Report, 7-10
Save As (t-Curve or Alpha S-Curve), 5-5 Helium, 1-7
Filler rod Help menu
cleaning, 3-17 Micromeritics web page, 2-12
inserting, E-3 online manual, 2-12
using for low surface area samples, E-1 Horvath-Kawazoe
Format calculations, C-19
advanced, 3-1 physical properties window, 5-43
basic, 3-1 plot report options, 5-45
restricted, 3-1 report, 5-42
Forms, Sample Data Worksheet, A-1 tabular report options, 5-45
f-Ratio Method, 5-34
Free space
balancing, E-1 I
calculations, C-2 Instrument log, 6-15
cold, 5-15 Instrument schematic
differential, 1-5 components, 6-9
warm, 5-15 enable manual control, 6-8
Freundlich shortcut menu, 6-11
report, 5-27 showing, 6-12
report calculations, C-35 Interaction parameter, C-23
Front Panel, 2-2 IP address
Function keys entering, Windows 7, D-4
See Shortcut keys entering, Windows Vista, D-6
Isotherm, report options, 5-22
G
Gas K
behavior, 1-5 Kernel function, F-14, F-15
Cleaning and Verifying Gas Lines, video, 2-13
connecting, 9-18
Connecting Gases, video, 2-13 L
disconnecting depleted bottle, 9-18 Langmuir surface area
Guidelines for Connecting Gases, video, 2-13 report, 5-24
guidelines for connecting to analyzer, 9-18 report calculations, C-7
hazardous, 9-18 Leak checking, 9-26
line, clean and verify, 9-22 Leak test, performing, 9-16
regulators, 1-7 Lennard-Jones, F-2, F-7
requirements, 1-7, 1-9 Liquid nitrogen
toxic, 9-19 bath, 1-5
Gemini Series, 1-4 cryogen, 1-6
Glass beads, using, E-1 List file statistics, 5-6
Graph Loading a sample, 3-21
copying as metafile, 7-22 Log report settings, 6-15
editing onscreen, 7-19 Low surface area samples, analyzing, E-1
grid lines, 8-3
Graph overlay
for multiple graphs, 3-40

239-42828-01 - Dec 2012 Index-3


Index Gemini VII

M plot report options, 5-54


report, 5-53
Main menu bar, 2-9
report calculations, C-33
Maintenance
tabular report options, 5-54
and troubleshooting, 9-1
system, 9-1
videos, 2-13 N
Manual control
accessing shortcut menu, 6-11 N2 Broekhoff-de Boer model, F-16
enabling, 6-8 N2 Broekhoff-de Boer Model model, F-16
MCM-41 materials, F-8 N2 Carbon Finite Pores, As=12, 2D-NLDFT model,
Menu F-11
bar, 2-10 N2 Carbon Finite Pores, As=6, 2D-NLDFT model, F-10
structure, 2-10 N2 Carbon Slit Pores by NLDFT model, F-10
Minimum BJH diameter (or radius), 5-36 N2 Cylindrical Pores - Oxide Surface model, F-8
Models, F-1 N2 Cylindrical Pores - Pillared Clay Surface model, F-8
Ar Carbon finite pores by NLDFT, As=12, F-11 N2 DFT model, F-7
Ar Carbon finite pores by NLDFT, As=6, F-10 N2 Halsey Thickness Curve model, F-14
Ar Carbon slit pores by NLDFT, F-10 N2 Harkins and Jura Thickness Curve model, F-15
AR Cylindrical Pores - Oxide Surface, F-8 N2 Modified Density Functional model, F-7
AR DFT model, F-7 N2 Tarazona NLDFT, Esf = 30.0K model, F-9
AR Modified Density Functional, F-9 Nitrogen, 1-7
Argon Cylinder, multi-wall nanotube by NLDFT, NLDFT Model Table, 5-47
F-12 No analysis file status, 2-8
Argon Cylinder, single-wall nanotube by NLDFT Non-ideality factor, 5-17
model, F-11 Notes, defined, 1-3
based on classical theories, F-13
based on statistical thermodynamics, F-1
O
Carbon Cylinder, multi-wall nanotube by NLDFT,
F-12 Oil vapor trap, replacing alumina, 9-11
CO2 DFT Model, F-9 Open report command, 7-3
N2 Broekhoff-de Boer Model, F-16 Operation, 1-5
N2 Carbon Cylinder, single-walled nanotube by Operator’s manual, conventions, 1-3
NLDFT model, F-11 Options menu
N2 Carbon finite pores by NLDFT, As=12, F-11 graph grid lines command, 8-3
N2 Carbon finite pores by NLDFT, As=6, F-10 service test mode command, 8-4
N2 Carbon slit pores by NLDFT, F-10 Units, 8-3
N2 Cylindrical Pores - Oxide Surface, F-8 Options presentation, 8-1
N2 Cylindrical Pores - Pillared Clay Surface, F-8 Ordering information, 10-1
N2 DFT model, F-7 O-ring, replacing port, 9-6
N2 Halsey Thickness Curve, F-14
N2 Harkins and Jura Thickness Curve, F-15
N2 Harkins and Jura Thickness Curve model, F-15
P
N2 Modified Density Functional, F-7 Parameter files, defining, 3-11
N2 Tarazona NLDFT, Esf = 30.0K, F-9 Parts, ordering, 10-1
Zeolites H-Form by NLDFT, F-12 Pass/Fail options window, 5-21
Molecular dynamics, F-2 Pore filling pressure, F-4
Molecular simulation methods, F-2 Pore size, F-13
Monolayer capacity, 5-27 Power failure, recovering from, 9-4
Monte Carlo, F-2 Prepared file status, 2-8
Montmorillionite, F-8 Preparing file status, 2-8
Moving an analyzer to another computer, 4-16 Pressure
MP-Method absolute pressure dosing, 5-12
plot options, 5-54 offset, 6-20

Index-4 239-42828-01 - Dec 2012


Gemini VII Index

relative, calculations, C-1 file creating, 3-15


table, 5-11 list file statistics, 5-6
Pressure relief valve, 1-7, 6-9 Report relative pressure table, 5-25
Preventive maintenance schedule, 9-4 Reports menu
Print file contents, 5-6 close reports command, 7-3
control chart command, 7-7
heat of absorption report command, 7-10
Q open report command, 7-3
QuickStart analysis, 3-26, 6-5 regression report command, 7-5
SPC report options command, 7-3
start report command, 7-2
R Restricted format
Rear panel, 2-4 defined, 3-1
Reference Analysis, How to Perform a Reference Option Presentation, 8-1
Analysis, video, 2-12 password, 3-5
Reference material, Analyzing Reference Material, sample information file, 3-7
video, 2-12
Regression report
command, 7-5 S
recalculating SPC values, 7-6 Saito-Foley
selecting X- and Y-Axes variables, 7-5 calculations, C-20
Regularization, 5-47 Pore Geometry, C-20
Regulators Sample
gas, 1-7 Cleaning Sample Tubes, video, 2-12
Guidelines for Choosing Regulators, video, 2-13 compartment, 2-3
Relative pressure range, 1-8 degassing, 3-20
Removing an analyzer, 4-20 Degassing the Sample, video, 2-12
Report How to Prepare Samples, video, 2-12
Alpha-S method, 5-33 log report, 5-55
BET Surface Area, 5-24 weighing, 3-18
BJH Adsorption/Desorption, 5-36 Sample defaults
closing, 7-3 advanced format, 3-2
DFT Surface Energy, 5-49 basic format, 3-4
Dollimore-Heal, 5-41 command, 8-2
Dubinin, 5-50 restricted format, 3-5, 8-2
examples, 7-24 Sample information file, 5-8
f-Ratio Method, 5-34 command, 5-8
generating, 7-2, 8-1 convert, 5-7
graphs, editing onscreen, 7-19 creating in Basic format, 3-7
header, 7-13 defining, 3-6
Isotherm, 5-22 export, 5-6
Langmuir surface area, 5-24 How to Prepare Samples, video, 2-12
Sample log, 5-55 list file statistics, 5-6
shortcut menus for, 7-17 print file contents, 5-6
Statistical Process Control (SPC), 7-3 Sample mass, Determining Sample Mass video, 2-12
Summary, 5-20 Sample ports
tabular, editing, 7-18 location, 2-3
tool bar, 7-14 replacing O-rings, 9-6
t-Plot, 5-30 Sample tube
Validation, 5-56 blank, 9-26
zoom feature, 7-23 cleaning and labeling, 3-17
Report options Cleaning Sample Tubes, video, 2-12
command, 5-18 How to Sample Install Tubes, video, 2-12
file, 5-18 installing, 3-21

239-42828-01 - Dec 2012 Index-5


Index Gemini VII

on schematic, 6-9 entering, Windows 7, D-4


replacing O-ring, 9-7 entering, Windows Vista, D-6
specifications, 1-9 Summary report, 5-20
Saturation pressure calculations, C-40
measuring, 6-6 Surface area correction factor, 5-32
tube, 1-4, 6-10 Surface Energy, F-13
Schematic, 6-8 System valves, 6-10
Service test mode, 8-4
Servo valve, calibrating, 6-21
Setup program T
adding an analyzer, 4-13 Tarazona, F-7
moving an analyzer to another computer, 4-16 Temkin
reinstalling calibration files, 4-24 Isotherm Report Options, 5-28
removing an analyzer from the computer, 4-20 report calculations, C-35
uninstalling software, 4-31 Temperature ramp rate, 5-10
Shortcut keys, 2-6 Text, copy graph data as, 7-22
Shortcut menu Thermal
for graphs, 7-19 diffusion, 1-5
for instrument schematic, 6-11 gradient, coolant bath, 1-5
for tabular reports, 7-18 Thermal transpiration
using the software, 2-6 correction, 5-19
Show instrument correction, calculations, C-5
show log command, 6-15 Thermodynamic law, F-2
show schematic command, 6-12 Thickness curve
show status command, 6-13 Broekhoff-de Boer, 5-31
SmartPrep Carbon Black STSA, 5-31
adding or modifying, 4-29 Halsey, 5-31
menu options, 3-20 Harkins and Jura, 5-31
SmartPrep Degasser, 1-6 Kruk-Jaroniec-Sayari, 5-31
Soak time, 5-10 reference, 5-30
Software Title properties window, 7-22
adding an analyzer, 4-13 Tool bar, reports window, 7-14
adding or modifying SmartPrep, 4-29 t-Plot
changing the analyzer setup configuration, 4-22 calculations, C-8
Ethernet switch, 4-13 report, 5-30
importing an analyzer from a previous installation, Transducer
4-27 differential pressure, 6-9
installing, 4-2 match transducer, 6-20
installing updates, 4-10 on schematic, 6-8
moving an analyzer, 4-16 sample pressure transducer, 6-21
reinstalling calibration files, 4-24 volume adsorbed, 6-9
removing an analyzer, 4-20 Troubleshooting, 9-1
revert to a previous version, 4-10
starting the setup program, 4-9
uninstalling the analysis program, 4-31 U
using, 2-6 Unit configuration, 6-16
Specifications, 1-8 Unit menu
StarDriver files, convert, 3-34 blank analysis, 6-7
Start Analysis command, 6-2 calibration command, 6-19
Start Po measurement command, 6-6 diagnostics, 6-17
Start report, command, 7-2 diagnostics command, 6-17
Status window, 6-13 Krypton analysis, 6-7
STSA thickness curve, 5-31 QuickStart analysis, 6-5
Subnet mask service test command, 6-23

Index-6 239-42828-01 - Dec 2012


Gemini VII Index

show instrument log command, 6-15 X


show instrument schematic command, 6-12
X-axis order by, 7-8
show status command, 6-13
Start Po measurement command, 6-6
unit configuration, 6-16 Z
Units, Options menu, 8-3
Zeolites H-Form by NLDFT model, F-12
Zeolites Me-Form by NLDFT model, F-13
V Zero pressure calibration, 6-20
Zoom feature, 7-23
Vacuum pump
changing or adding oil, 9-8
Changing the Vacuum Pump Exhaust Filter, 2-13
connector, 2-4
defined, 1-6
Inspecting and Changing Vacuum Pump Oil, video,
2-13
inspecting oil level, 9-8
replacing alumina in oil vapor trap, 9-11
replacing exhaust filter, 9-15
specifications, 1-8
Validation report, 5-56
Valves, system, 6-10
Van der Waal force, F-1
Video
Analyzing Reference Material, 2-12
Changing the Vacuum Pump Exhaust Filter, 2-13
Cleaning and Verifying Gas Lines, 2-13
Cleaning Sample Tubes, 2-12
Connecting Gases, 2-13
Degassing the Sample, 2-12
Determining Sample Mass, 2-12
Evaluating data, 2-12
Guidelines for Choosing Regulators, 2-13
Guidelines for Connecting Gases, 2-13
How to Install Sample Tubes, 2-12
How to Perform a Reference Analysis, 2-12
How to Prepare a Dewar, 2-12
Inspecting and Changing Alumina, 2-13
Inspecting and Changing Vacuum Pump Oil, 2-13
Maintenance, 2-13
Replacing Analysis Port Frit and O-ring, 2-13
Volume adsorbed transducer, 6-9

W
Wall potential, F-10
Warnings, defined, 1-3
Weighing sample, 3-18
Window menu
arrange icons, 2-11
tile and cascade, 2-11

239-42828-01 - Dec 2012 Index-7


Gemini VII Smart VacPrep Operator Manual

G. Smart VacPrep Operator Manual

Dec 2013 G-1


SMART VACPREP
INTELLIGENT VACUUM SAMPLE PREPARATION SYSTEM

OPERATOR MANUAL
Smart VacPrep Operator Manual

Nov 2013
Micromeritics is a registered trademark of Micromeritics Instrument Corporation.
Microsoft, Windows, and Windows 7 are registered trademarks of Microsoft Corporation.
Smart VacPrep is a registered trademark of Micromeritics Instrument Corporation.

_____________________________________________________________________________________

© Micromeritics Instrument Corporation 2013. All rights reserved. Printed in the U.S.A.

The software described in this manual is furnished under a license agreement and may be used or
copied only in accordance with the terms of the agreement.
Warranty

WARRANTY
MICROMERITICS INSTRUMENT CORPORATION warrants for one year from the date of shipment
each instrument it manufactures to be free from defects in material and workmanship impairing its
usefulness under normal use and service conditions except as noted herein.

Our liability under this warranty is limited to repair, servicing and adjustment, free of charge at our
plant, of any instrument or defective parts when returned prepaid to us and which our examination
discloses to have been defective. The purchaser is responsible for all transportation charges involving the
shipment of materials for warranty repairs. Failure of any instrument or product due to operator error,
improper installation, unauthorized repair or alteration, failure of utilities, or environmental
contamination will not constitute a warranty claim. The materials of construction used in
MICROMERITICS instruments and other products were chosen after extensive testing and experience
for their reliability and durability. However, these materials cannot be totally guaranteed against wear
and / or decomposition by chemical action (corrosion) as a result of normal use.

Repair parts are warranted to be free from defects in material and workmanship for 90 days from the
date of shipment.

No instrument or product shall be returned to MICROMERITICS prior to notification of alleged defect


and authorization to return the instrument or product. All repairs or replacements are made subject to
factory inspection of returned parts.

MICROMERITICS shall be released from all obligations under its warranty in the event repairs or
modifications are made by persons other than its own authorized service personnel unless such work is
authorized in writing by MICROMERITICS.

The obligations of this warranty will be limited under the following conditions:

1. Certain products sold by MICROMERITICS are the products of reputable manufacturers, sold
under their respective brand names or trade names. We, therefore, make no express or implied
warranty as to such products. We shall use our best efforts to obtain from the manufacturer, in
accordance with his customary practice, the repair or replacement of such of his products that
may prove defective in workmanship or materials. Service charges made by such manufacturer
are the responsibility of the ultimate purchaser. This states our entire liability in respect to such
products, except as an authorized person of MICROMERITICS may otherwise agree to in writ-
ing.
2. If an instrument or product is found defective during the warranty period, replacement parts may,
at the discretion of MICROMERITICS, be sent to be installed by the purchaser, e.g., printed cir-
cuit boards, check valves, seals, etc.
3. Expendable items, e.g., sample tubes, detector source lamps, indicator lamps, fuses, valve plugs
(rotor) and stems, seals and O-rings, ferrules, etc., are excluded from this warranty except for
manufacturing defects. Such items which perform satisfactorily during the first 45 days after the
date of shipment are assumed to be free of manufacturing defects.

Smart VacPrep Operator Manual i


Warranty

Purchaser agrees to hold MICROMERITICS harmless from any patent infringement action brought
against MICROMERITICS if, at the request of the purchaser, MICROMERITICS modifies a standard
product or manufactures a special product to the purchaser’s specifications.

MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of
any of its products other than the liability stated above. This warranty is in lieu of all other warranties,
express or implied, including but not limited to, the implied warranties of merchantability or fitness for
use.

ii Smart VacPrep Operator Manual


Elements Used in this Manual

ELEMENTS USED IN THIS MANUAL


The following icons and format may be used throughout this manual to identify notes of importance,
warnings, and cautions.

NOTE - Notes contain important information pertinent to the subject mat-


ter.

CAUTION - Cautions contain information to help prevent actions that


may damage the analyzer or components.

WARNING - Warnings contain information to help prevent actions that


may cause personal injury.

For Chemisorption - Indicates the marked item is applicable to chemisorption analyzers only.

For Physisorption - Indicates the marked item is applicable to physisorption analyzers only.

Related Topics

Related Topics provides links to additional information about the subject matter. Related topic links are
located at the end of each topic.

Smart VacPrep Operator Manual iii


Elements Used in this Manual

Field Labels and Screen Titles


Labels and Buttons Description
Buttons (in the applic- Buttons in the application are represented as bold font weight and blue let-
ation) ters. Some examples are: Save, Edit, Replace All, etc.
Buttons (on the equip- Buttons on the equipment are represented as bold font and black letters.
ment) some examples are: Start or Cancel.
Field Labels Field Labels are represented as italicized words. Some examples are:
Sample, Automatically Collected, Analysis Conditions, etc
Keyboard Commands Keyboard commands are represented as bold font weight and black letters.
Some examples are: F2, Alt+F4, etc.
Menu Instructions Menu instructions are represented as bold and italicized words. Some
examples are:

File > New Sample

Reports > Start Report

Unit [n] > Unit Configuration


Screen Tabs Screen Tabs are represented as italicized words. Some examples are:
Sample Description, Degas Conditions, Analysis Conditions, and Report
Options.
Screen Titles Screen Titles are represented as italicized words. Some examples are: Ana-
lysis Adsorptive Properties, Free Space, Sample Tube, etc

iv Smart VacPrep Operator Manual


Contact Us

CONTACT US
Micromeritics Instrument Corporation
4356 Communications Drive

Norcross, GA 30093-2901, U.S.A.

Phone: (770) 662-3636

Fax: (770) 662-3696

www.Micromeritics.com

---------------

U.S. Inquiries
U.S. Sales: (770) 662-3633

ussales@micromeritics.com

---------------

Quotes, Orders, and Customer Satisfaction


Customer Service: (770) 662-3636

orders@micromeritics.com

---------------

U.S. Instrument Service Department


Phone: (770) 662-3666

Smart VacPrep Operator Manual v


Contact Us

vi Smart VacPrep Operator Manual


Table of Contents

Warranty i

Elements Used in this Manual iii

Contact Us v

1 About the Smart VacPrep 1-1


Specifications for the Smart VacPrep 1-3
Set the Voltage for the Smart VacPrep 1-4

2 About the Software 2-1


Add or Remove a Smart VacPrep 2-1
Add a Smart VacPrep unit 2-2
Remove a Smart VacPrep unit 2-2
Smart VacPrep Configuration 2-3

3 Operate the Smart VacPrep 3-1


Backfill the Smart VacPrep Ports 3-1
Evacuate the Smart VacPrep Ports 3-1
QuickStart Degas Conditions 3-2
Load QuickStart Degas Conditions into a Sample File 3-4
Start Smart VacPrep Degas 3-5
Show Smart VacPrep Dashboard 3-7
Show Smart VacPrep Log 3-8
Show Smart VacPrep Schematic 3-9
Smart VacPrep Schematic Shortcut Menus 3 - 10
Show Smart VacPrep Status 3 - 11

4 Smart VacPrep Calibration 4-1


Smart VacPrep Pressure Offset 4-1
Smart VacPrep Servo Valve Calibration 4-2

5 Smart VacPrep Diagnostics 5-1

Smart VacPrep Operator Manual vii


Diagnostic Test Report for Smart VacPrep 5-1
Schedule Smart VacPrep Diagnostic Test 5-1

6 Maintenance and Troubleshooting 6-1


Enable Manual Control for Smart VacPrep 6-1
Replace the Smart VacPrep Fuse 6-2
Sample Tube Installation on the Smart VacPrep 6-2
Oil Based Vacuum Pump 6-3
Inspect and Change Vacuum Pump Oil 6-3
Replace the Alumina in the Oil Vapor Trap 6-7
Replace the Vacuum Pump Exhaust Filter 6 - 11

7 Parts and Accessories for the Smart VacPrep 7-1

8 Error Messages 8-1

Index Index - 1

viii Smart VacPrep Operator Manual


1 About the Smart VacPrep

1 ABOUT THE SMART VACPREP

The Smart VacPrep is an advanced six-port degassing system that utilizes vacuum to degas samples by
heating and evacuation. Each of the ports may be operated independently of one another. Samples may
be added or removed from degas ports without disturbing the treatment of other samples undergoing
preparation. When starting a new sample, ports already degassing samples are automatically suspended
unless they are in the slow evacuation stage. When unrestricted evacuation is attained by the new
samples, the previously suspended samples will automatically resume their evacuation. Degassing will
automatically terminate when each sample has completed all programmed steps.

The Smart VacPrep remembers the previously selected set of degas conditions and allows them to be
reused. However, the option of programming each port with a different set of parameters is available. A
record of the sample preparation time and temperature can be recorded as part of the sample data file.

The degas program may be started or terminated by using the analyzer software on the computer
attached to the analyzer or with push buttons on the front panel of the Smart VacPrep. The push button
control on each port provides the ability to attach the sample tube with heating mantle, and immediately
start degassing a sample.

There are two methods of starting the degas process from the analyzer software:

l Start Degas menu option. Accessed from the Smart VacPrep > Unit [n] > Start Degas menu selec-
tion. Provides the option to use degas conditions from selected sample files or a degas conditions files
for each Smart VacPrep port. When using the Start Degas menu option, the degas process is started
using the Start button on the Start Degas window. This option is more convenient for samples that
have specific degas requirements that should be associated with the sample file when it is created.

Smart VacPrep Operator Manual 1-1


1 About the Smart VacPrep

l QuickStart menu option and Smart VacPrep panel buttons. Accessed from the Smart VacPrep >
Unit [n] > QuickStart Degas Conditions menu selection. Provides the option to enter commonly used
degas conditions for each Smart VacPrep port without the need for a sample information file.
This option provides three ways to load information into QuickStart Degas Conditions:

1. Load degas conditions from an existing degas conditions file


2. Copy conditions from another Smart VacPrep unit and port
3. Enter degas conditions manually
When using the QuickStart menu option, the degas process is started using the Select button and
Start buttons for each port on the Smart VacPrep unit.

Using the Start Degas option does not change the degas conditions set up in QuickStart. QuickStart
degas conditions are remembered for the next push button operation.

Sample tubes are attached to the sample ports. Heating mantles are then installed and secured to the
sample tube with a metal clip. If using straight wall sample tubes, heating mantles with elastic cords
may be purchased separately.The mantle is plugged into the power and thermocouple connectors on the
front panel. The degassing process can then be started either by pressing the Select and Start buttons on
the Smart VacPrep unit or by going to Smart VacPrep > Unit [n] > Degas > Start Degas.

A Check Seal or TransSeal can be used to transfer air-sensitive samples from the Smart VacPrep to the
analyzer's port without atmospheric contamination. To order these parts, reference the Parts and
Accessories section for the analyzer. Instructions for using the Check Seal or TranSeal are included
with the ordered part.

Smart VacPrep Components Table


Component Description
Cancel button Stops the degas process on all ports where the Select indicator is lit.
Ethernet port Located on the left side panel. Use to connect an Ethernet switch.
Power Switch (not shown) Located on the back of the unit, turns the unit on or off.
Select buttons Used to select the ports to be degassed.
Start button Starts the degas process on all ports where the Select indicator is lit.
Status Indicator Three lights indicate the current status of the station. The lights flash
when the valves are open.

Green. Indicates the station is idle and not hot. The setpoint temperature
is below 30 ºC and the actual temperature is below 50 ºC.

Red. Indicates when the setpoint temperature is greater than 30 ºC and


heat is being applied to the station.

Yellow. Indicates the station is in use, but not currently being heated. The
heating mantle may still be above 50 ºC.

1-2 Smart VacPrep Operator Manual


Specifications for the Smart VacPrep

Related Topics

See "QuickStart Degas Conditions" on page 3 - 2

See "Start Smart VacPrep Degas" on page 3 - 5

See "Set the Voltage for the Smart VacPrep" on the next page

SPECIFICATIONS FOR THE SMART VACPREP


The Smart VacPrep degasser has been designed and tested to meet the following specifications:

Specifications for the Smart VacPrep


Specification Description
Backfill Options Automatically backfill or wait for user command
Capacity 6 ports
Degas Method Heat and vacuum
Physical Dimensions Height: 69 cm (27 in.)

Width: 53 cm (20.75 in.)

Depth: 44 cm (17 in.)

Weight: 32 kg (70 lbs)


Evacuation Period Determined by selected elapsed time or achievement of selected low pres-
sure target
Evacuation Rate Selectable evacuation rate from 1.0 to 50.0 mmHg/s
Heating of Samples Heating mantles
Heating Ramp Rate Selectable from 0.1 oC per minute to 10 oC per minute
Soak Time Zero to 999 minutes in one minute increments (Zero = Manual Cancel).
Temperature Accuracy Deviation less than ±10 oC at the sensing thermocouple embedded in the
heating mantle
Temperature Control One ramp during evacuation phase, five additional ramps during sub-
sequent phases
Temperature Range 40 to 450 oC in one degree increments
Vacuum Control Selectable target pressure controls switchover from restricted to unres-
tricted evacuation.

Computer
Windows 7 Professional or higher operating system is recommended for the best user
experience. If the computer is to be connected to a network, a second Ethernet port on the
computer must be used for that purpose.

Smart VacPrep Operator Manual 1-3


1 About the Smart VacPrep

SET THE VOLTAGE FOR THE SMART VACPREP


The Smart VacPrep voltage setting is housed in a compartment adjacent to the power connector on the
back of the unit.

1. Use a flat head screwdriver to gently pry open the cover of the compartment.
2. Firmly press down on the voltage indicator and roll the indicator to display the appropriate voltage
for your environment. Selections are: 100 Vac, 120 Vac, 230 Vac, and 240 Vac.
3. Firmly press the compartment cover shut. Ensure it closes securely. The selected voltage will
appear in the window on the compartment cover.

1-4 Smart VacPrep Operator Manual


2 About the Software

2 ABOUT THE SOFTWARE

If a software update is required for the analyzer to support the Smart VacPrep, the software can be
downloaded from the internet at this location:

www.micromeritics.com/Smart-VacPrep-Software.aspx

The degasser software is installed as a part of the analyzer installation. During installation, an
IP address will be assigned to the unit allowing the unit to connect automatically during startup. Up to
three additional degasser units can be installed.

Menu options for the Smart VacPrep are provided on the Smart VacPrep menu.

Related Topics

See "Add or Remove a Smart VacPrep" below

ADD OR REMOVE A SMART VACPREP

A Smart VacPrep unit must be removed from one application before it can be added to another
application if they are running on the same subnet.

Smart VacPrep Operator Manual 2-1


2 About the Software

ADD A SMART VACPREP UNIT


Smart VacPrep > Add

1. When prompted, enter the serial number of the unit being added. Duplicate serial numbers are not
allowed.
2. Click Add. Initialization begins.

REMOVE A SMART VACPREP UNIT


Smart VacPrep > Remove

1. Select the serial number to remove.


2. Click Remove.

2-2 Smart VacPrep Operator Manual


Smart VacPrep Configuration

SMART VACPREP CONFIGURATION


Smart VacPrep > Unit [n] > Configuration

Displays the Smart VacPrep configuration and software versions.

Smart VacPrep Unit Configuration Fields and Buttons Table


Field or Button Description
Board ID Click to display the board ID.
Change IP Click to display the Unit IP Setup window. The IP address and Subnet
mask assigned during installation display. Do not edit these fields unless
instructed by a Micromeritics service representative.
OK Saves and closes the active window.
Remove 067 Unit Click to remove the selected Smart VacPrep unit.

Smart VacPrep Operator Manual 2-3


2 About the Software

2-4 Smart VacPrep Operator Manual


3 Operate the Smart VacPrep

3 OPERATE THE SMART VACPREP

BACKFILL THE SMART VACPREP PORTS


Smart VacPrep > Unit [n] > Backfill Ports

Use to backfill ports with gas.

1. Enter the backfill pressure in the Backfill pressure field.


2. Select the ports to be backfilled.
3. Click Start to start the process or Cancel to stop the process.

EVACUATE THE SMART VACPREP PORTS


Unit [n] > Smart VacPrep > Evacuate Smart VacPrep Ports

Allows manual evacuation of up to six degas ports.

Smart VacPrep Operator Manual 3-1


3 Operate the Smart VacPrep

Smart VacPrep Evacuate Ports Fields and Buttons


Field or Button Description
Cancel Discards any changes or cancels the current process.
Evacuate Options l Unrestricted evac. pressure. Pressure value at which unrestricted

sample evacuation should begin.


l Vacuum level. Specify the vacuum level to be achieved before evac-
uation begins.
l Evacuation rate. Rate of evacuation.
Evacuate Port[s] Select the ports() to evacuate.
Start Starts the operation.

QUICKSTART DEGAS CONDITIONS


Smart VacPrep > Unit [n] > QuickStart Degas Conditions

The QuickStart Degas Conditions option provides the ability to enter commonly used degas conditions
for each Smart VacPrep port without the need for a sample information file. Degassing can then be
easily started using the front panel buttons on the Smart VacPrep unit.

This option provides three ways to load information into QuickStart Degas Conditions:

1. Load degas conditions from an existing degas conditions file.


2. Copy conditions from another Smart VacPrep unit and port.
3. Enter degas conditions manually.
Degas conditions can be copied into sample files after degassing for record keeping.

When using the QuickStart menu option, the degas process is started using the Select button and Start
buttons for each port on the Smart VacPrep unit.

QuickStart degas conditions are remembered for the next push button operation.

3-2 Smart VacPrep Operator Manual


QuickStart Degas Conditions

1. Go to Smart VacPrep > Unit [n] > QuickStart Degas Conditions.


2. The six ports are represented by row numbers. Ports that are busy are grayed out and disabled.
Click Edit for the port to be configured.
3. Enter degas conditions using one of the following methods:
l To select degas conditions from a Degas Conditions file, click the dropdown arrow to the right

of the Degas Conditions field. If the file is not shown, select Browse , locate the file, then
click Load.
l To copy QuickStart Degas Conditions from another Smart VacPrep unit, select the unit and
port number to the right of the Copy QuickStart Degas Conditions from Smart VacPrep Unit
field..
l To enter degas conditions manually, complete the fields on the window. Reference the Degas
Conditions section of the Operator Manual
4. Click Save. Repeat these steps for each port to be configured. If multiple ports will have the
same degas conditions parameters, click Edit on the port and use the Copy QuickStart Degas
Conditions from Smart VacPrep Unit [n] Port [n field to load the settings from the first port.
5. Repeat these steps for each applicable unit and port.
6. If using a Check Seal, verify that the Check Seal opener is installed in the Smart VacPrep port.
Follow the instructions included with the Check Seal for instructions on inserting the opener.
7. Load the sample into the sample tube. If using a Check Seal or TranSeal, insert it into the sample
tube.
8. Load the sample on the Smart VacPrep sample port.
9. Attach the heating mantle using the metal clip. If a straight wall tube is used, heating mantles with
elastic cords are available. Reference the Parts and Accessories section of the analyzer Operator
Manual.

Smart VacPrep Operator Manual 3-3


3 Operate the Smart VacPrep

10. Install the safety shield.


11. Press the Select button for the port to be degassed. A blue LED is lit.
12. Press the Start button on the Smart VacPrep panel to start the degas process for all ports that
have a blue LED lit.
13. When degassing is complete and the sample has cooled, the sample can be transferred to an ana-
lysis port.

LOAD QUICKSTART DEGAS CONDITIONS INTO A SAMPLE FILE


QuickStart Degas Conditions can be copied into a sample file. Reference the Degas Conditions section
of the analyzer Operator Manual.

Degas Conditions Fields and Buttons Table


Field or Button Description
Close Closes the active window.
Copy QuickStart Degas Use to copy the degas conditions settings from the selected Smart
Conditions from the VacPrep unit and port.
Smart VacPrep Unit
Degas Conditions Use to browse for a .DEG file that contains degas condition parameters
to be used in the analysis.
Heating Phase This option is applicable when degassing with either a Smart VacPrep or
a SmartPrep.

Enter up to five stages of degas conditions.

l Temperature. Degas temperature.


l Temperature Ramp Rate. Rate at which the temperature is to
change.
l Time. Amount of time to heat the sample.

Use to modify the table contents.

l Insert. Inserts one row above the selected row.


l Delete. Deletes the selected row.
l Clear. Clears all table entries and displays only one default value.
l Append. Inserts one row at the end of the table.

3-4 Smart VacPrep Operator Manual


Start Smart VacPrep Degas

Degas Conditions Fields and Buttons Table (continued)


Field or Button Description
Save Saves changes to the active window.
Smart VacPrep Evac- This option is applicable only when degassing with a Smart VacPrep.
uation
l Backfill sample tube. Indicate if the sample tube should be backfilled
automatically or wait for operator response.
l Evacuation Rate. Rate used for evacuation.
l Unrestricted evac. from. Pressure at which the unrestricted evac-
uation is to begin.
l Vacuum level. Pressure for unrestricted evacuation.
l Evacuation time. Length of time for preliminary evacuation before
proceeding with the Heating Phase temperature schedule. The timer
starts when the vacuum level is reached.
l Temperature ramp rate. Rate at which the temperature is to change
when advancing to the target pressure.
l Target temperature. Targeted pressure for evacuation.
l Hold pressure. Pressure at which heating will stop and hold the
sample temperature approximately constant until the pressure falls
below the Hold pressure. This prevents damage to the sample struc-
ture due to 'steaming' and /or elutriation due to excessive escaping gas
velocity.

START SMART VACPREP DEGAS


Smart VacPrep > Unit [n] > Start Degas

This option allows the degassing of up to six samples simultaneously. A sample can be added to any idle
port and a degas operation started. When adding a sample, the degas operation in progress will be
suspended until the sample reaches the target pressure, then degassing on all ports will resume. If other
samples are still in the initial evacuation phase, the new samples will wait until the fast evacuation is
started. Samples can be removed from any of the six ports without disturbing the degas operations
already in process. Starting several samples as a batch allows them to perform the initial evacuation at
the same time.

Smart VacPrep Operator Manual 3-5


3 Operate the Smart VacPrep

Degas conditions remain the same from degas to degas unless the Degas Conditions file is changed or
replaced by the operator. A manual evacuation can be performed on any idle degas port.

The six ports are represented by row numbers. Ports that are busy are grayed out and disabled.

1. Click Browse to search for a sample file or a degas conditions file. Select the file, then click
Open. Do this for each Smart VacPrep port to be used.
2. If using a Check Seal, verify that the Check Seal opener is installed in the Smart VacPrep port.
Follow the instructions included with the Check Seal for instructions on inserting the opener.
3. Load the sample into the sample tube. If using a Check Seal or TranSeal, insert it into the sample
tube.
4. Load the sample on the Smart VacPrep sample port.
5. Attach the heating mantle using the metal clip. If a straight wall tube is used, heating mantles
with elastic cords are available. Refer to the Parts and Accessories section of the analyzer oper-
ator manual.
6. Install the safety shield.
7. Click Start on the Start Degas window to begin the degas process for the selected Smart
VacPrep ports.
8. Click Start to begin the degas process for the selected Smart VacPrep ports.
9. Allow the samples to cool before transferring them to the analysis ports to start the analysis.
Smart VacPrep Start Degas Fields and Buttons Table
Field or Button Description
Browse Searches for a file. Select a file from the Name column or from the
library, then click Open. Alternatively, double click the file name to
open (or import) the file.
Cancel Discards any changes or cancels the current process.
Clear Clears the field.
Sample Displays the path and file name of the selected .SMP file.
Start Starts the degas operation for the selected ports.

3-6 Smart VacPrep Operator Manual


Show Smart VacPrep Dashboard

Degas ports can also be canceled using buttons on the Smart VacPrep
unit. Press Select on the unit to select the port, then press the Cancel but-
ton.

SHOW SMART VACPREP DASHBOARD


Smart VacPrep > Unit [n[ > Show Dashboard

The dashboard displays the following:

l Number of days until roughing pump maintenance is due


l Manifold outgas rate
Data for the dashboard comes from the logged diagnostic data. The dashboard is automatically kept
current as the relevant diagnostic data items are updated. The gauges will be updated even if the
dashboard window is not open.

Red numbers on the dashboard require attention. To reset the dashboard


numbers, right click on the dashboard setting, then click Reset.

Smart VacPrep Dashboard Gauges and Descriptions Table


Field or Button Description
Days until roughing-pump Annual maintenance is recommended. The number of days until the
service is due anniversary of the last pump maintenance is shown. The displayed value
is updated at least once per day and when the maintenance time is reset.
When the displayed value is 30 or less, the value is displayed in red. Red
negative numbers display if maintenance is past due.
Manifold outgas rate Provides the qualitative indication of the outgas rate in the dosing
manifold. LED images constitute a bidirectional bar graph of the outgas
rate.

The gauge is updated after each outgas rate measurement.

Smart VacPrep Operator Manual 3-7


3 Operate the Smart VacPrep

Smart VacPrep Dashboard Gauges and Descriptions Table (continued)


Field or Button Description
l Three green LEDs are lit if outgas rate is below 30% of outgas rate
limit.
l At 30%, the left LED turns off.
l At 60%, the center LED turns off.
l At 90%, three green LED lights turn off and the center yellow LED is
turned on.
l At 110% and above, only the red LED is lit and attention is required.

SHOW SMART VACPREP LOG


Smart VacPrep > Unit [n] > Show Log

Use to display a log of recent analyses, calibrations, or messages.

Analyzer Log Fields and Buttons Table


Field Description
Add Log Entry Use to enter information to appear in the sample log report that cannot be
recorded automatically through the application. Click the button again to
enter multiple log entries.
Analysis / Select the logs to display.
Calibration /
Message
Report Click to display the Instrument Log Report Settings window to specify
report output options.

3-8 Smart VacPrep Operator Manual


Show Smart VacPrep Schematic

Analyzer Log Fields and Buttons Table (continued)


Field Description
l Start Date. Displays a calendar to select the start date for the report.
l Preview. Previews the predefined report on the screen.
l Print. Sends the report to the default printer.
l Copies. Select the number of copies to print. This field is only enabled
when Print is selected.
l File. Select the destination directory. Enter a new file name in the File
name field, or accept the default. Select to save the file as a report sys-
tem (.REP), a spreadsheet (.XLS), a portable document format
(.PDF), or an ASCII text (.TXT) file format.

SHOW SMART VACPREP SCHEMATIC


Unit [n] > Show Instrument Schematic

Use to display an analyzer schematic. To operate the valves and elevator from this window, manual
control must be enabled (Smart VacPrep > Unit [n] > Enable Manual Control).

Smart VacPrep Schematic Components Icon Table


Field or Button Description
Open Valve. Green indicates an open valve.

Closed Valve. Yellow indicates a closed valve.

Servo Valve. Closed.

Servo Valve. Open.

Sample Tube. Cannot be manually controlled.

Smart VacPrep Operator Manual 3-9


3 Operate the Smart VacPrep

Smart VacPrep Schematic Components Table


Schematic Description
Components
1-6 Sample port valves
7, 8, 9 Vacuum and backfill valves
Heating mantle con- Sets the ramp rate and target temperature
trols

SMART VACPREP SCHEMATIC SHORTCUT MENUS


Each manually controlled schematic component has a shortcut menu displaying the operations available
for that particular component. To access the shortcut menu, hover the mouse pointer over the component
and right click.

Smart VacPrep Schematic Shortcuts Table


Schematic Shortcut Icon Available Options:
Valve options l Close - Closes the selected valve.
l Open Opens the selected valve.
l Set - Use to set the servo valve target pressure and to dose or evac-
uate.
Temperature control l Disable. Select to disable the temperature control options for the selec-
options ted port.
l Set. Select to set the following:
o Enable or disable temperature control

o Control sample temperature


o Control furnace temperature

3 - 10 Smart VacPrep Operator Manual


Show Smart VacPrep Status

Smart VacPrep Schematic Shortcuts Table (continued)


Schematic Shortcut Icon Available Options:
o Cool the sample to less than 50 °C
o Set heater power percent

SHOW SMART VACPREP STATUS


Smart VacPrep > Unit [n] > Show Status

The Smart VacPrep Status window allows the monitoring of degas operations for a manual degas
operation.

Smart VacPrep Status Fields and Buttons Table


Field or Button Description
Cancel Cancels the current degas operation.
Check Click to check the outgassing rate of the samples on the selected port.
The following process occurs:

l The current degassing step is suspended.


l The vacuum valves are closed and the vacuum level on the selected
ports is monitored.
l The Status window indicates that the degassing operation is being
checked and displays the outgassing rate as it becomes available.
During the degas check, the Check button changes to Continue. When
Continue is clicked, the valves open and the degassing operation
resumes.

If the outgassing rate indicated that the sample has been freed of
contaminants (minimal pressure increases), click Skip to advance to the
next state of the degassing operation. For example, if degassing is
checked after the setpoint is attained, Skip advances you to the ramping
stage.

Smart VacPrep Operator Manual 3 - 11


3 Operate the Smart VacPrep

Smart VacPrep Status Fields and Buttons Table (continued)


Field or Button Description
Sample The name of the sample file.
Skip Skips the current degas operation.
Status Indicates the current status of the degas.

3 - 12 Smart VacPrep Operator Manual


4 Smart VacPrep Calibration

4 SMART VACPREP CALIBRATION


Smart VacPrep > Unit [n] > Calibration

Various calibration procedures and service tests are included in the operating program. These procedures
and tests are designed to provide a service representative with instrument readouts, as well as to assist in
troubleshooting potential problems.

Related Topics

See "Smart VacPrep Pressure Offset" below

See "Smart VacPrep Servo Valve Calibration" on the next page

SMART VACPREP PRESSURE OFFSET


Smart VacPrep > Unit [n] > Calibration > Pressure Offset

Use to perform system calibration. This option evacuates the system and zeros the pressure transducer.

Disabled calibration options can be accessed only with the assistance of an authorized Micromeritics
service representative.

Click Start to begin the process.

Smart VacPrep Operator Manual 4-1


4 Smart VacPrep Calibration

SMART VACPREP SERVO VALVE CALIBRATION


Smart VacPrep > Unit [n] > Calibration > Servo Valve

Use to calibrate the servo valve to the manifold pressure transducer. The servo valve should always be
recalibrated after a pressure calibration has been performed. The pressure transducer should be
calibrated before starting this calibration procedure.

1. Go to Smart VacPrep > Unit [n] > Calibration > Servo Valve.
2. Click Start. The window closes when the calibration is complete. Click Cancel to stop the cal-
ibration process.
Servo Valve Fields and Buttons Table
Field or Button Description
Cancel Discards any changes or cancels the current process.
Start Starts the operation.

Related Topics

See "Smart VacPrep Calibration" on the previous page

See "Smart VacPrep Pressure Offset" on the previous page

4-2 Smart VacPrep Operator Manual


5 Smart VacPrep Diagnostics

5 SMART VACPREP DIAGNOSTICS

DIAGNOSTIC TEST REPORT FOR SMART VACPREP


Smart VacPrep > Unit [n] > Diagnostics > Diagnostic Test Report

Displays previously run diagnostic tests. Separate directories store tests run once, daily, weekly, and
monthly.

SCHEDULE SMART VACPREP DIAGNOSTIC TEST


Smart VacPrep > Unit [n] > Diagnostics > Schedule Diagnostic Tests

Allows the specification of one-time or periodic running of a sequence of diagnostic tests. A separate list
of tests is saved for each of the possible test frequencies. Tests are categorized and flagged as requiring
intervention or not. If tests requiring intervention are scheduled, the operator has the option of skipping
these tests if the operator does not respond within a specified time after an initial prompt is displayed,
before the test is started. Events are logged in the instrument log for all starting, ending, and skipped
tests.

Smart VacPrep Operator Manual 5-1


5 Smart VacPrep Diagnostics

Schedule Diagnostics Fields and Buttons Table


Field or Button Description
Available Tests drop- Select one or more tests to run unattended. Select the test and click the
down list Insert button for the test to display in the Test Sequence box.
Cancel Discards any changes or cancels the current process.
Intervention Required Check this option if any test requiring operator intervention should be
skipped if the operator does not respond within the specified time.
OK Saves and closes the active window.
Start Test Sequence if Enter a From and To time for an unattended test to begin if the instrument
Instrument is Idle Any is idle at any time during the entered time frame.
Time Between
Test Frequency Select how often the test is to run unattended.
Test Sequence Provides the test file identification and estimated run time. A check mark
in the Intervention Required column indicates that operator intervention is
required. Click Delete to remove the selected test or Clear to clear the
entire table of all entries. To add a test to the test sequence, highlight a
row in the Test Sequence box, select a test from the Available Tests list
and click Insert. The new test will be inserted above the highlighted row.
Select a row and click Delete to remove the test from the sequence.
Select Clear to remove all entries from the Test Sequence box.

5-2 Smart VacPrep Operator Manual


6 Maintenance and Troubleshooting

6 MAINTENANCE AND TROUBLESHOOTING

ENABLE MANUAL CONTROL FOR SMART VACPREP


Smart VacPrep > Unit [n] > Enable Manual Control

Use to enable the manual control of certain system valves and elevator components. When this option is
enabled, a checkmark appears to the left of Unit [n] > Enable Manual Control.

If the schematic is not immediately visible, go to Unit [n] > Show Instrument Schematic.

Smart VacPrep Schematic Components Table


Schematic Description
Components
1-6 Sample port valves
7, 8, 9 Vacuum and backfill valves
Heating mantle con- Sets the ramp rate and target temperature
trols

Smart VacPrep Schematic Components Icon Table


Field or Button Description
Open Valve. Green indicates an open valve.

Closed Valve. Yellow indicates a closed valve.

Servo Valve. Closed.

Smart VacPrep Operator Manual 6-1


6 Maintenance and Troubleshooting

Smart VacPrep Schematic Components Icon Table (continued)


Field or Button Description
Servo Valve. Open.

Sample Tube. Cannot be manually controlled.

REPLACE THE SMART VACPREP FUSE


The Smart VacPrep uses two 5 amp fuses located in a compartment adjacent to the power connector on
the back of the unit.

1. Use a flat head screwdriver to gently pry open the cover of the compartment.
2. Use the flat head screwdriver to gently pry the fuses out of the holder.
3. Insert a new fuse into each holder, then push the holders back into the slot until snug.
4. Press the compartment cover shut. Ensure it closes securely.

SAMPLE TUBE INSTALLATION ON THE SMART VACPREP


1. While holding the degas port plug, turn the connector nut counterclockwise to loosen. Remove
both the plug and the nut.

2. If using a rubber stopper, remove it from the sample tube.If using a Check Seal or TransSeal, do
not remove them from the sample tube. Place the port connector nut, ferrule, and O-ring onto the
sample tube.

6-2 Smart VacPrep Operator Manual


Oil Based Vacuum Pump

3. If using a Check Seal, verify that the Check Seal opener is installed in the sample port.
4. To attach the sample tube set to the degas port, push the sample tube in to a full stop. Secure the
sample tube in place by sliding the connector nut, ferrule, and O-ring up onto the degas port and
turning the connector nut clockwise. Tighten the nut securely by hand.
5. Place a heating mantle over the sample tube bulb and secure the mantle in place with a mantle
clip.

6. Insert the heating mantle thermocouple plug into the thermocouple connector.

7. Insert the heating mantle power plug into the power connector and twist the power plug to lock
securely.
8. After installing the sample tubes, install the safety shield around the sample tubes and heating
mantles to minimize the risk of receiving a burn by touching hot components.

OIL BASED VACUUM PUMP


INSPECT AND CHANGE VACUUM PUMP OIL

The equipment shown in this section may differ slightly from yours.
However, the process is the same unless otherwise noted.

This procedure is also shown in the How-To Tutorials located on the Help
menu.

Smart VacPrep Operator Manual 6-3


6 Maintenance and Troubleshooting

The oil in the vacuum pump should be changed every three months when the efficiency of the vacuum
pump declines (requiring increased time to reach vacuum levels) or if it becomes discolored.

Inspect the Oil


View the vacuum pump oil through the oil-level window. The oil level should be midway between the
indicators on the oil-level window when the pump is running. Oil in good condition is clean, clear or light
in color and transparent. Change the oil if it has darkened.

Change or Add Oil

Drain the oil while the pump is warm and disconnected from the power
source.

Use oil supplied by Micromeritics or refer to the vacuum pump manual for other acceptable oils.

1. Unplug the vacuum pump from the power source.


2. Loosen the wing nut on the clamp at the top of the oil vapor trap. Swing the clamp open and
remove the trap from the hose.

6-4 Smart VacPrep Operator Manual


Inspect and Change Vacuum Pump Oil

3. Grasp the handle on top of the vacuum pump and place the pump on a work surface.
4. Place a waste container under the drain spout.

5. Remove the drain plug and drain the oil into the waste container.
6. Replace the drain plug.
7. Remove the drain plug from the oil-fill port on top of the pump.

8. Slowly add oil to the port until the level is midway between the indicator lines in the oil-level win-
dow when the pump is running.

Smart VacPrep Operator Manual 6-5


6 Maintenance and Troubleshooting

Do not allow oil to rise above the midway position when the pump is run-
ning. Doing so may cause oil to splash into the oil filter causing con-
tamination.

7. Check the washer or O-ring used at the oil-filling port and replace if necessary.
8. Insert the oil-fill plug and turn clockwise to tighten.
9. Check the alumina in the oil vapor trap. If most of the pellets are no longer white,
replace the alumina before reattaching the vacuum pump. See "Replace the Alu-
mina in the Oil Vapor Trap" on the facing page.
10. Reconnect the vacuum pump hose.
11. Reconnect the power cord to the power source.
12. Turn the vacuum pump on and recheck the oil level.
13. Allow the pump to run a few hours (overnight if possible) to eliminate air and mois-
ture from the fresh fluid and to produce efficient vacuum operations.

Related Topics

See "Replace the Alumina in the Oil Vapor Trap" on the facing page

See "Replace the Vacuum Pump Exhaust Filter" on page 6 - 11

6-6 Smart VacPrep Operator Manual


Replace the Alumina in the Oil Vapor Trap

REPLACE THE ALUMINA IN THE OIL VAPOR TRAP

The equipment shown in this section may differ slightly from yours.
However, the process is the same unless otherwise noted.

The activated alumina in the oil vapor trap becomes saturated during use. The alumina should be
inspected periodically and replaced when most of the alumina pellets are no longer white.

Do not perform the following procedure on used alumina. The resultant


oil vapors may cause a fire.

1. Disconnect the vacuum pump from the analyzer and place it on a work table.
2. Loosen the wing nut on the clamp at the top of the oil vapor trap. Swing the clamp open and
remove the trap from the hose.

3. Loosen the wing nut on the clamp at the bottom of the oil vapor trap. Open the clamp and remove
the trap.

Smart VacPrep Operator Manual 6-7


6 Maintenance and Troubleshooting

4. Remove one end fitting from the trap body and dispose of the used alumina in an appropriate
manner.

5. Wash the trap body with a detergent-based soap. Rinse with water, then rinse with isopropyl or
ethyl alcohol. Set the trap aside and allow to dry thoroughly.

Exposure of the trap body to oil vapor may cause small cracks on the
inside surface of the trap body. Under normal circumstances, these
cracks will not cause problems or leaks.

Prepare fresh alumina


1. Preheat the oven to 300 °C.
2. Pour approximately 180 grams of fresh alumina into a glass or metal container (approximately 250
mL if a graduated beaker is used). Place the container in the oven.
3. Bake the alumina for two hours at 300 °C.
4. Remove the baked alumina from the oven and allow to cool until luke warm. A desiccator may be
used to speed the cooling process.
5. Use a small spatula to gently pry the O-ring from the end fittings of each end of the trap body.

6-8 Smart VacPrep Operator Manual


Replace the Alumina in the Oil Vapor Trap

6. Inspect the O-rings. If dusty, clean with a lint-free tissue. If damaged, replace with a new O-ring.
7. Screw one of the end fittings onto the trap body.
8. Ensure the trap body is dry and the alumina is lukewarm. Pour the alumina pellets into the trap
until level with the top of the trap body.
9. Screw the other end fitting back onto the trap and tighten securely by hand.
10. Lightly tap both ends of the trap body on the work surface to remove remaining dust from the pel-
lets.

11. Inspect the centering ring before replacing it onto the intake port. If it appears to be flattened,
replace it. A flattened centering ring can cause vacuum leaks. There are two types of centering

Smart VacPrep Operator Manual 6-9


6 Maintenance and Troubleshooting

rings. Use the one with the smaller opening at the intake port.
12. Place the centering ring on the intake port.
13. Place the trap on the centering ring.

14. Open the clamp and place it around the flange of the intake port and the flange of the trap. Swing
the clamp fastening screw toward the intake port until it fits into the slot in the other half of the
clamp. Tighten the wing nut securely by hand.

15. Reconnect the hose from the analyzer to the oil vapor trap.
a. Place the clamp around the vacuum pump hose flange and vapor trap.

6 - 10 Smart VacPrep Operator Manual


Replace the Vacuum Pump Exhaust Filter

16. Plug the pump power cord into the power source. Allow the pump to run a few hours (overnight if
possible) to eliminate air and moisture from the fresh oil and to produce efficient vacuum
operations.

Related Topics

See "Inspect and Change Vacuum Pump Oil" on page 6 - 3

See "Replace the Vacuum Pump Exhaust Filter" below

REPLACE THE VACUUM PUMP EXHAUST FILTER

The equipment shown in this section may differ slightly from yours.
However, the process is the same unless otherwise noted.

The gases used by the analyzer are exhausted by the oil-filled vacuum pump. The filter minimizes the
release of oil vapor and should be replaced when it becomes so saturated with oil that it is ineffective.

Exhaust filters are used to minimize the release of oil vapors. The gases
are diluted substantially upon release from the vacuum pump; however,
it may be necessary in some locations to provide a fume hood for pro-
tection from hazardous gases and vapors released into the work area.

1. Turn off the power to the pump and disconnect the pump from the power source.
2. Loosen the clamp wing nut at the vacuum pump exhaust port. Swing the clamp away from the
exhaust port and remove it.

Smart VacPrep Operator Manual 6 - 11


6 Maintenance and Troubleshooting

3. Remove and discard the exhaust filter. Ensure the centering ring remains in place on the exhaust
port.
4. Place the new filter on the centering ring.
5. Open the clamp and place it around the exhaust port flange and the exhaust filter flange. Swing
the clamp fastening screw toward the exhaust port until it fits into the slot in the other half of the
clamp. Tighten the wing nut securely by hand.
6. Turn on the power to the pump.

Related Topics

See "Inspect and Change Vacuum Pump Oil" on page 6 - 3

See "Replace the Alumina in the Oil Vapor Trap" on page 6 - 7

6 - 12 Smart VacPrep Operator Manual


7 Parts and Accessories for the Smart VacPrep

7 PARTS AND ACCESSORIES FOR THE SMART VACPREP


Part Number Item and Description
Cables
003-63801-01 Cable, Ethernet straight-thru; for connecting instrument to control module
(computer)
Gas Cylinder Accessories
004-25549-00 Reducer, 1/8 in tube × 1/4 in tube
004-33601-00 Expansion kit; adds an additional outlet to the gas regulator
004-33602-00 Pressure relief kit; prevents excessive gas pressure in the event of
regulator failure (not to be used with toxic gases)
004-62230-58 Gas regulator, CGA 580 fitting, 30 psig (He, N2, Kr, Ar)
230-02001-00 Gas inlet line, 1/8 in. × 6 ft., copper
Heating Mantle and Accessories
003-26044-00 Smart VacPrep heating mantle 24V, 120W
067-14701-00 Heating Mantle Shield, (1) replacement shield
067-33002-00 Heating Mantle Shield Option, includes (2) shields, each shield covers (3)
heating mantles
230-25808-00 Smart VacPrep heating mantle clip
Operating Supplies
004-25466-00 O-RING, -010 70 DURO BUNA-N; for use with sample port dust frit
004-27041-00 Sample port dust frit, 20 microns
067-33601-00 Operating supplies, sample tube o-rings (1/2 in. and 12 mm), sample port
dust frit , o-rings for sample port dust frit (6-month supply)
067-33602-00 Extended operating supplies, sample tube o-rings (1/2 in. and 12 mm),
sample port dust frit , o-rings for sample port dust frit (12 month supply)
Sample Tubes and Accessories
004-25013-02 O-ring, -013 70 DURO VITON; for use with 12 mm sample tubes
(brown)
004-25022-00 O-ring, -012 70 DURO BUNA-N; for use with 3/8 in sample tubes
004-25044-00 O-ring, -013 70 DURO BUNA-N; for use with 1/2 in sample tubes
(black)
004-25466-00 O-ring, -010 70 DURO BUNA-N; for use with 1/4 in sample tubes
004-25647-01 O-ring, -904, VITON; for use with 9 mm sample tubes (brown)
067-25840-00 Sample tube ferrule, 12 mm (red)
067-25840-01 Sample tube ferrule, 9 mm (red)
067-33603-00 Option kit, 1/4 in. ferrules and O-rings (6 ferrules and 12 O-rings)
067-33604-00 Option kit, 3/8 in. ferrules and O-rings (6 ferrules and 12 O-rings)

Smart VacPrep Operator Manual 7-1


7 Parts and Accessories for the Smart VacPrep

Part Number Item and Description


067-33605-00 Option kit, 9 mm ferrules and O-rings (6 ferrules and 12 O-rings)
260-25843-00 Sample tube ferrule, 1/2 in
300-25824-00 Sample tube nut
300-25825-00 Sample tube ferrule, 1/4 in
300-25826-00 Sample tube ferrule, 3/8 in
Smart VacPrep Systems
067-00000-00 Smart VacPrep (no vacuum pump)
067-00000-11 Smart VacPrep with 110/120V oil-sealed vacuum pump system
067-00000-22 Smart VacPrep with 220/240V oil-sealed vacuum pump system
067-00001-00 Smart VacPrep with hybrid turbo vacuum pump system
Vacuum Pump and Accessories
004-16003-01 Oil, vacuum pump, 1 Liter
004-16830-00 Activated alumina, 500 grams; for oil vapor trap
004-25491-02 Centering ring, NW 40, BUNA-N, AL; for use with hybrid turbo vacuum
pump
004-25509-00 Clamp, NW 10/16
004-25626-08 Flex tube, 3/4-in. OD x 48-in. long, NW-16, NW-40
004-25630-00 Centering ring, NW 16
004-25652-00 O-ring, size 217, for oil vapor trap
004-25860-00 Fitting, elbow, NW-16; for connecting to the vacuum inlet
004-27040-00 Filter, for vacuum pump exhaust
004-62023-01 Service kit, for vacuum pump P/N 062-00004-00 (for Edwards and
VacuuBrand)
062-00000-11 Vacuum pump with built-in anti-suckback valve, 100/120 VAC, includes
hose kit
062-00000-23 Vacuum pump with built-in anti-suckback valve, 220/240 VAC, includes
hose kit
062-00004-00 Hybrid turbo vacuum pump assembly
062-33002-00 Activated alumina oil vapor trap, for one oil-based vacuum pump
260-25896-00 Adapter, KF-16 to 7/16 hose

7-2 Smart VacPrep Operator Manual


8 Error Messages

8 ERROR MESSAGES
Program error messages are listed numerically. If the Action response indicates to contact a
Micromeritics service representative, record the error message, then make backup copies of any files
involved in the operation.

4407 Error searching for installed Smart VacPreps. The registry could not be read..
Cause: The application was not installed properly.
Action: Reinstall the application. If the problem persists, contact your Micromeritics service rep-
resentative.

4408 The %s in %s already has Smart VacPrep S/N %d. The Smart VacPrep
must be removed from the %s before it can be added.
Cause: The Smart VacPrep was already installed for another application / unit.
Action: Remove the Smart VacPrep from the installed unit before adding it to the preferred unit.

4409 A free IP address on the same subnet as %s could not be found."


Cause: All IP addresses on the network for the Ethernet card specified during installation are in
use by other Micromeritics applications on this computer.
Action: Uninstall unused Micromeritics applications.
Action: Configure a different Ethernet card for use by the application using the application
installer.

4410 The .INI file could not be updated with configuration for Smart
VacPrep S/N %s."
Cause: The application .INI file is opened by another application and could not be updated.
Action: Close all open applications and add the Smart VacPrep again using the Smart VacPrep
menu.

4411 Error dosing.


Cause: The backfill timed out.
Action: Ensure there is gas available and the pressure regulator is set to the appropriate pressure.
Also ensure that the gas supply regulator shut-off valve is open.

Smart VacPrep Operator Manual 8-1


8 Error Messages

4412 Error calibrating the servo.


Cause: Calibration results are out of range.
Action: Follow standard calibration procedures and try again. If the problem persists, contact
your Micromeritics service representative.

4413 Error overheating on port [0]. Current = [TEMPC0] [TEMPC-U], Target


= [TEMPC0] [TEMPC-U], Limit = [TEMPC0] [TEMPC-U].
Cause: The temperature of the indicated mantle exceeded the maximum allowed value.
Action: Ensure the power and thermocouple connectors for the mantle are properly installed. If
they are, the mantle may be defective; contact your Micromeritics service rep-
resentative.

4414 Error thermocouple unplugged on port [0]. Target = [TEMPC0]


[TEMPC-U]."
Cause: The thermocouple is unplugged or has malfunctioned.
Action: Ensure the thermocouple is plugged in. If the problem persists, contact your Micro-
meritics service representative.

4420 Communications error.


Cause: The application failed to connect to the Smart VacPrep.
Action: Ensure the unit is powered and properly connected to the network specified during install-
ation. Check the power cable, power switch, and Ethernet cable, then reconnect to the
Smart VacPrep either through the Smart VacPrep menu for this instrument or by restart-
ing the application. If the problem persists, contact your Micromeritics service rep-
resentative.

4421 Smart VacPrep S/N %s is busy and could not be removed.


Cause: The Smart VacPrep cannot be removed because it is currently performing an operation.
Action: Wait until the Smart VacPrep completes the current operation and try again.

8-2 Smart VacPrep Operator Manual


8 Error Messages

4422 The file %s does not exist.


Cause: The selected file does not exist on the disk drive.
Action: Select an existing file. Ensure that the file has been created before use.

4423 The sample %s is already selected on port %d.


Cause: The selected sample file is already selected for use on a different port.
Action: Select another sample file for this port.

4424 The file %s on port %d could not be opened. Check if the sample file is
already in use for editing or analysis.
Cause: The selected sample file is already open by this or another application.
Cause: The selected sample file is damaged.
Action: Select another sample file.

4425 The sample %s on port %d has an invalid status and cannot be used
for degassing.
Cause: The status of the file is not consistent with the current operation.
Action: Select a sample file that has not been used for an analysis. Only sample files with a
status of No Analysis or Prepared may be selected.

4426 Port %d is currently in use. Operation cannot be started.


Cause: The current operation cannot be completed because the port is already in use.
Action: Wait for port to terminate operation or perform the desired operation on an unused port.

Smart VacPrep Operator Manual 8-3


8 Error Messages

8-4 Smart VacPrep Operator Manual


Index

INDEX F
Fuses
B replace on the Smart VacPrep 6 - 2

Backfill port, Smart VacPrep 3 - 1


H
C Heating phase table, degas conditions 3 - 4

Calibration
Smart VacPrep 4 - 1 M
Smart VacPrep, pressure offset 4 - 1
Smart VacPrep, servo valve 4 - 2 Mainteane
Configuration fuse replacement on the Smart VacPrep 6 -
Smart VacPrep 2 - 3 2
Contact Us v Maintenance
install sample tube, Ssmart VacPrep 6 - 2
Manual control
D Smart VacPrep 6 - 1

Dashboard
Smart VacPrep 3 - 7 P
Smart VacPrep, manifold outgas rate 3 - 7
Smart VacPrep, roughing pump 3 - 7 Parts and accessories
Degas Smart VacPrep 7 - 1
using the Smart VacPrep 3 - 5 Pressure offset
Degas conditions Smart VacPrep 4 - 1
heating phase 3 - 4 Pump
soak time 3 - 4 Edwards 6 - 3
temperature ramp rate 3 - 4 inspect and change oil 6 - 3
Diagnostics
Smart VacPrep 5 - 1
Smart VacPrep, schedule tests 5 - 1 S
Smart VacPrep, test report 5 - 1
Sample tube
install, Smart VacPrep 6 - 2
E Schematic
shortcut menus 3 - 10
Edwards vacuum pump SmartVacPrep 3 - 9
inspect and change oil 6 - 3 Servo valve
oil vapor trap 6 - 7 SmartVacPrep, calibrate 4 - 2
replace alumina 6 - 7 Shortcuts
replace exhaust filter 6 - 11 schematic 3 - 10
Elements used in this manual iii Smart VacPrep
Error messages 8 - 1 about 1 - 1
Evacuate ports, Smart VacPrep 3 - 1

Smart VacPrep Operator Manual Index - 1


Index

backfill ports 3 - 1
calibrate servo valve 4 - 2
calibrate, pressure offset 4 - 1
calibration 4 - 1
configuration 2 - 3
diagnostic test report 5 - 1
Diagnostics 5 - 1
evacuate ports 3 - 1
install additional unit 2 - 1
install sample tube 6 - 2
Parts and accessories 7 - 1
QuickStart degas conditions 3 - 2
remove a unit 2 - 1
schedule diagnostic tests 5 - 1
schematic 3 - 9
show dashboard 3 - 7
show status 3 - 11
software
about 2 - 1
specifications 1 - 3
start degas 3 - 5
troubleshooting and maintenance 6 - 1
use 3 - 1
Soak time, degas conditions 3 - 4
Specifications
Smart VacPrep 1 - 3
System valves 3 - 10, 6 - 1

T
Temperature ramp rate 3 - 4
Troubleshooting and maintenance
Smart VacPrep 6 - 1
Smart VacPrep, enable manual control 6 - 1

V
Voltage
set for the Smart VacPrep 1 - 4

W
WARRANTY i

Index - 2 Smart VacPrep Operator Manual

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