BASIC OPERATION GUIDE FOR QUANTACHROME ASiQ

A. GENERAL

Startup
1. Turn on the power and UPS unit.
2. Go to the ASiQ unit, turn on the “Mains” switch followed by “Electronics” switch at right panel
of ASiQ instrument.

3. Double click on ASiQWin button to initialize the software control. Enter user ID as requested.
4. Go to ASiQ instrument tab (next to Help tab), click “Connect”. Operation tab on top left will
turn green if connection between software and instrument is successful.

Shutdown
1. Unload all samples cells and fit with suitable dowel pins.
2. ASiQ instrument tab > Disconnect > Operation panel will turned red
3. After disconnect the software from instrument, close the software and shutdown the computer.
4. Go to the ASiQ unit, turn OFF the “Mains” and “Electronics” switches at right panel of ASiQ
instrument.
5. Turn OFF the UPS unit and main power.
 BASIC OPERATION GUIDE FOR QUANTACHROME ASiQ

B. PHYSISORPTION

Cell Calibration Procedure

Note: Cell calibration procedure can take long time to be completed. It’s only needed for void volume
measurement using NOVA mode. Cell calibration is not required when use Helium mode.

1. Install coolant level sensor and P0 cell appropriately. Refer images below, Left: 2 stations
setup; Right: 3 stations setup.
2. Place empty cells onto respective stations (with appropriate cell adapter and also filler rod – if
going to use during analysis)
3. Fill the dewar with liquid nitrogen to the lower tip of level indicator.
4. From software, go to ASiQ Instrument tab > Analysis > Select Type > Cell calibration
5. Later, go to ASiQ Instrument tab again > Analysis > Edit Parameters
6. At common tab, input the Absorbate Gas (from dropdown menu), gas port (from dropdown
menu), tick “Auto”, set P0 option to “Station” and tick the station in-used.
7. At station tab, select “Cell Type” and define cell ID for the cell to be calibrated. Click OK.
8. ASiQ Instrument tab > Analysis > Start Analysis

Outgassing Procedure

1. Weigh the empty cell, cell with sample and record in the Physisorption Weighing Sheet.
2. Place cell with sample into heating mantle
3. Install the cell onto ASiQ outgasser (without filler rod) with appropriate o-rings and fittings
4. Secure the heating mantle with the hooks at top
5. Create outgassing profile in ASiQWin software > ASiQ Instrument > Outgasser > Stn 1/Stn 2 >
Edit Program
6. Setup the heating profile suitable for samples, select “Backfill” under Completion State, select
“Fine Powder” under Evacuation Cross Over, and input “390 torr” under Backfill pressure.
7. Then click “Load” to send outgassing profile to instrument to start the outgassing procedure.
8. Enter the weighing details accordingly and click OK.
9. Upon completion, allow mantle to cool below 100 °C before unloading. Status and
temperature could be monitored from left panel of Outgasser (Third panel from top).
10. Cool to room temperature either at ASiQ outgass stations or dessicator before weighing.
 BASIC OPERATION GUIDE FOR QUANTACHROME ASiQ

Sample Measurement

1. Measurement of sample weight after outgassing:

Sample weight = After outgas weight (Cell and Sample) – Cell Weight
2. Assemble sample cell as below (with filler rod as necessary) and install to respective stations
at left chamber with blue door.

3. From the software, select physisoption mode from ASiQ instrument tab > select type >
physisorption
4. Create analysis profile from ASiQ Instrument tab > Analysis > Edit Parameters
5. At common tab, input following settings.
 Absorbate Gas – select nitrogen, gas port (#1 nitrogen) and tick “Auto”
 External equipment – None
 P0 option - “Station”
 Void volume remeasure – enabled
 Evacuation cross over – fine powder
 Select station - tick the station in-used.
6. Go to station tab > Admin tab, allow automatic naming without modification of file name.
7. Then, Analysis tab > input following settings
 Void Volume Mode – Helium measure, helium removal time – 15 min
 Delta V max - untick
 Advance Options – select cell type (size, and filler rod option), include leak test of 1 min
 Speed-up options – tick Maxidose
8. Then, Points tab > input following settings
 Analysis Mode (Right-bottom) > Standard
 Click at adsorption branch > Advanced selections > select 20 points (for full isotherm)
 Click at desorption branch > Advanced selections > select 20 points (for full isotherm)
 Select all points > tick S and M tag at ON column (for BET analysis), tick Tol = 3, tick Equ
= 2 > Apply to selected
9. Then, Data Reduction tab > input following settings
 Open Report after run > demo.bet
 Save Text Report after run > demo.bet
10. After setup for all stations, click Load/Save > Save Preset files and Save Stn 1/2/3> Click OK
11. Finally, go to ASiQ Instrument tab > Analysis > Start Analysis >
12. Input weighing details as requested > Click OK
 BASIC OPERATION GUIDE FOR QUANTACHROME ASiQ

Data Analysis
1. Go to File > Open > select raw files with .qds extension or auto-generated report on-screen
2. Right click on the isotherm curve > Select “Edit Data Tags” > Add or remove the tagging here
for different evaluation techniques > Apply to selected points > Click OK
Note: Add tag by apply tick at ON column, remove tag by apply tick at OFF column

Table 1. Data tag for physisorption data analysis methods

Tag Data Analysis Methods
None HK, SF
None DA
P BJH, DH and Kr87
R DR
M, S BET
L Langmuir
T t-plot, statistical thickness method, MP method
R FHH, NK
V Total pore volume
V, M Average Pore Size
P Kr87 Thin Film Pore Size Method

3. To view BET graph, right click > Graphs > BET > Multipoint BET Plot
4. To view BET data in tables, right click > Tables > BET > Multipoint BET
5. To view full BET report, right click on the isotherm curve > select Report > select demo.BET >
latest report with modified tag will be shown > print to PDF from Report window, by using
PhantomPDF printer
6. To export raw data from tables to excel/ text files, right click at Isotherm curve > Tables >
Isotherm > Isotherm > Isotherm raw data will be displayed > Right click on the data > Export
to .CSV/ Save as text
7. To plot graph in excel > open exported data in excel > copy the desorption points to match
with adsorption at same relative pressure > Insert line graph to plot isotherm in excel sheet

C. STATIC CHEMISORPTION

Cell Calibration Procedure

Cell calibration is not required for chemisorption cell.

Outgassing Procedure
Outgassing procedure for physisorption is similarly applied for chemisorption.

Switching from Physisorption to Chemisorption Mode

1. The RTD coolant level detector, used to control the level of the coolant bath in physisorption
experiments, must be removed.
2. The P0 cell must be removed and its port must be sealed using the ¼” (6.3mm) stainless
steel dowel supplied.
3. Be sure to remove any O rings that may remain in the sample cell station. Use only the O-
rings and ferrules required by the chemisorption cell.
 BASIC OPERATION GUIDE FOR QUANTACHROME ASiQ

4. If the system is equipped with a second analysis station, remove any sample cells from
Station 2 and seal the port with the ¼” (6.3mm) stainless steel dowels supplied.
5. If the furnace is to be used, remove the Blue door that encloses the sample stations by
opening it half way and lifting straight up until it slides free of the hinge pins.
6. Remove Ice Reduction / Draft Exclusion kit and the magnetic cover over the fan vent holes
under the dewar lift drive prior to using the furnace.

Sample Measurement
1. Pack the chemisorption cell with quartz wools and weigh the cell with quartz wools.
2. Weigh the sample into cell with quartz wool and later sandwiched the sample with quartz
wool. Record down the weights into Chemisorption weighing sheets.
3. Assemble sample cell with filler rod and install to respective stations (Station 1 – 12 mm and
ChemiVent station – 6 mm) at left chamber with blue door.
4. From the software, select chemisorption mode from ASiQ instrument tab > select type >
chemisorption
5. Create analysis profile from ASiQ Instrument tab > Analysis > Edit Parameters
6. At Admin tab, allow automatic naming without modification of file name.
7. At Analysis tab, input following settings.
 Analysis Gas – eg. ammonia, select installed gas port for respective gas and tick “Auto”
 Analysis Metal – eg. carbon
 Thermal equilibrium – 5 minutes
8. At Points tab > input following settings
 Click at Combined branch > Advanced selections >
select 10 points
 Click at Combined desorption branch > Advanced
selections > select 10 points
 Click at Weak branch > Advanced selections > select
10 points
 Select all points > tick E tag for extrapolation at P=0,
Tol = 3, tick Equ = 2 > Apply to selected
 Set evacuation time between combined and weak
isotherms > 30 minutes
9. At Treatment tab, setup the sequence of treatments
applicable to samples. For examples,
10. Data Reduction tab > input following settings
 Open Report after run > demo.bet
 Save Text Report after run > demo.bet
11. After completion of settings, click Load/Save > Save Preset
files > Click OK
12. Select “Treatment only run” at bottom left, if intended to
perform treatment without analysis
13. Finally, go to ASiQ Instrument tab > Analysis > Start
Analysis >
14. Input weighing details as requested > Click OK
 BASIC OPERATION GUIDE FOR QUANTACHROME ASiQ

Data Analysis
1. Go to File > Open > select raw files or auto-generated report on-screen
2. Right click on the isotherm curve > Select “Edit Data Tags” > Add or remove the tagging here
for different evaluation techniques > Apply to selected points > Click OK
Note: Add tag by apply tick at ON column, remove tag by apply tick at OFF column

Table 2. Data tag for respective data analysis methods

3. To view graph, right click > Graphs > select technique of interest
4. To view data in tables, right click > Tables > select technique of interest
5. To export raw data from tables to excel/ text files, right click at Isotherm curve > Tables >
Isotherm > Isotherm raw data will be displayed > Right click on the data > Export to .CSV/
Save as text
6. To plot graph in excel > open exported data in excel > copy the desorption points to match
with adsorption at same relative pressure > Insert line graph to plot isotherm in excel sheet
7. Collections of chemisorption isotherms may be combined into a single file using the “Convert
to Full Document” command.

Note: For detailed operation steps on other applications, please refer to operation manual
provided in CD (ASiQWin-05098-5.00 REV A).