09931162C FIMS Hardware Guide
09931162C FIMS Hardware Guide
09931162C FIMS Hardware Guide
FIMS
FLOW INJECTION MERCURY SYSTEM
Hardware Guide
FIMS
Hardware Guide
2 . FIMS Hardware Guide
Release History
Any comments about the documentation for this product should be addressed to:
User Assistance
PerkinElmer
710 Bridgeport Avenue
Shelton, CT 06484-4794
U.S.A.
Notices
The information contained in this document is subject to change without notice.
Except as specifically set forth in its terms and conditions of sale, PerkinElmer makes no
warranty of any kind with regard to this document, including, but not limited to, the
implied warranties of merchantability and fitness for a particular purpose.
PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in
connection with furnishing, performance or use of this material.
Copyright Information
This document contains proprietary information that is protected by copyright.
All rights are reserved. No part of this publication may be reproduced in any form whatsoever or
translated into any language without the prior, written permission of PerkinElmer, Inc.
Trademarks
Registered names, trademarks, etc. used in this document, even when not specifically marked as such,
are protected by law.
Table of Contents
Introduction ...................................................................................... 7
About This Manual ................................................................................... 9
About This Handbook......................................................................... 9
Using this Handbook .......................................................................... 9
Before You Start .................................................................................... 10
Other Useful Handbooks for the FIMS Analysis System ............................. 11
Conventions Used in this Manual ............................................................. 12
Notes, cautions and warnings ........................................................... 12
Translation of Warnings .......................................................................... 15
Maintenance .................................................................................... 93
PerkinElmer Service ................................................................................ 95
Checklists for Regular Maintenance Tasks ................................................ 96
General Preventative Maintenance .................................................... 96
Spectrometer Maintenance ...................................................................... 97
Fluid System Maintenance ....................................................................... 98
FIMS-Cell Maintenance ............................................................................ 99
Measuring the Absorbance of the FIMS-Cell Windows ......................... 99
Removing the FIMS-Cell from the Spectrometer ................................. 99
Installing the FIMS-Cell in the Spectrometer .................................... 100
Removing the Windows from the FIMS-Cell ..................................... 100
Fitting the Windows from the FIMS-Cell ........................................... 100
Cleaning the Windows .................................................................... 100
Cleaning the FIMS-Cell ................................................................... 101
Gas/Liquid Separator and Manifold Maintenance ..................................... 102
Cleaning Gas/Liquid Separator and Manifold .................................... 102
Changing the Separator Filter ......................................................... 102
FIAS-Valve Maintenance........................................................................ 103
Cleaning the FIAS-Valve ................................................................. 103
Removing the FIAS-Valve from the Pump Unit ................................. 103
Fitting the FIAS-Valve to the Pump Unit........................................... 103
Dismantling the FIAS-Valve............................................................. 104
Reassembling the FIAS-Valve .......................................................... 105
Carrier Gas System Maintenance ........................................................... 106
Nonreturn Valve ............................................................................. 106
Changing the Mercury Filter .................................................................. 107
Changing the Air Filter .......................................................................... 109
Changing the Source Lamp ................................................................... 110
Changing the Fuse ................................................................................ 112
.5
If you find an error in this handbook or have any comments or suggestions, please tell us so
that we can correct the mistake or otherwise improve the handbook. Our address is on the
inside of the front cover.
This handbook contains detailed descriptions of procedures. Many sections start with a
summary of the procedures described in that section. Once you are thoroughly familiar with
the instrument, you may only need to refer to the summaries for the correct order of more
frequent procedures, and detailed instructions for less frequent procedures. Until you are
familiar with the system, read the relevant section completely, from the beginning.
UPPERCASE text, for example ENTER or ALT, refers to keys on the PC keyboard. '+' is used
to show that you have to press two keys at the same time, for example, ALT+F.
All eight digit numbers are PerkinElmer part numbers unless stated otherwise.
NOTE: A note indicates additional, significant information that is provided with some procedures.
Introduction . 13
CAUTION We use the term CAUTION to inform you about situations that could
result in serious damage to the instrument or other equipment. Details
about these circumstances are in a box like this one.
D Caution (Achtung)
Bedeutet, daß die genannte Anleitung genau befolgt werden muß, um
einen Geräteschaden zu vermeiden.
DK Caution (Bemærk)
Dette betyder, at den nævnte vejledning skal overholdes nøje for at
undgå en beskadigelse af apparatet.
E Caution (Advertencia)
Utilizamos el término CAUTION (ADVERTENCIA) para advertir sobre
situaciones que pueden provocar averías graves en este equipo o en
otros. En recuadros éste se proporciona información sobre este tipo de
circunstancias.
F Caution (Attention)
Nous utilisons le terme CAUTION (ATTENTION) pour signaler les
situations susceptibles de provoquer de graves détériorations de
l'instrument ou d'autre matériel. Les détails sur ces circonstances
figurent dans un encadré semblable à celui-ci.
I Caution (Attenzione)
Con il termine CAUTION (ATTENZIONE) vengono segnalate situazioni
che potrebbero arrecare gravi danni allo strumento o ad altra
apparecchiatura. Troverete informazioni su tali circostanze in un
riquadro come questo.
NL Caution (Opgelet)
Betekent dat de genoemde handleiding nauwkeurig moet worden
opgevolgd, om beschadiging van het instrument te voorkomen.
P Caution (Atenção)
Significa que a instrução referida tem de ser respeitada para evitar a
danificação do aparelho.
14 . FIMS Hardware Guide
We use the term WARNING to inform you about situations that could
result in personal injury to yourself or other persons. Details about
these circumstances are in a box like this one.
WARNING
D Warning (Warnung)
Bedeutet, daß es bei Nichtbeachten der genannten Anweisung zu einer
Verletzung des Benutzers kommen kann.
DK Warning (Advarsel)
Betyder, at brugeren kan blive kvæstet, hvis anvisningen ikke
overholdes.
E Warning (Peligro)
Utilizamos el término WARNING (PELIGRO) para informarle sobre
situaciones que pueden provocar daños personales a usted o a otras
personas. En los recuadros como éste se proporciona información
sobre este tipo de circunstancias.
F Warning (Danger)
Nous utilisons la formule WARNING (DANGER) pour avertir des
situations pouvant occasionner des dommages corporels à l'utilisateur
ou à d'autres personnes. Les détails sur ces circonstances sont
données dans un encadré semblable à celui-ci.
I Warning (Pericolo)
Con il termine WARNING (PERICOLO) vengono segnalate situazioni
che potrebbero provocare incidenti alle persone. Troverete
informazioni su tali circostanze in un riquadro come questo.
NL Warning (Waarschuwing)
Betekent dat, wanneer de genoemde aanwijzing niet in acht wordt
genomen, dit kan leiden tot verwondingen van de gebruiker.
P Warning (Aviso)
Significa que a não observância da instrução referida poderá causar
um ferimento ao usuário.
Introduction . 15
Translation of W arnings
16 . FIMS Hardware Guide
Introduction . 17
18 . FIMS Hardware Guide
Introduction . 19
20 . FIMS Hardware Guide
Introduction . 21
22 . FIMS Hardware Guide
Introduction . 23
24 . FIMS Hardware Guide
Introduction . 25
26 . FIMS Hardware Guide
Introduction . 27
28 . FIMS Hardware Guide
Introduction . 29
30 . FIMS Hardware Guide
Safety P ractices
Safety Practices . 33
Overview
This chapter describes the general safety practices and precautions that must be observed
when operating the FIMS.
This advice is intended to supplement, not supersede, the normal safety codes in the user's
country. It is also a supplement to the PerkinElmer standard Safety and Health Policy. The
information provided does not cover every safety procedure that should be practiced.
Ultimately, maintenance of a safe laboratory environment is the responsibility of the analyst
and the analyst's organization.
Please consult all manuals supplied with the FIMS and accessories before you start working
with the instrument. Carefully read the safety information in this chapter and in the other
manuals supplied. When setting up the instrument or performing analyses or maintenance
procedures, strictly follow the instructions provided.
WARNING
WARNING
• Be sure that the voltage of the FIMS corresponds to the voltage used in your
laboratory. There is a 110/220 voltage selector switch behind the instrument. Ensure
proper voltage selection is set before the power cord is installed.
• Never remove the side panels of the FIMS without shutting down the instrument and
disconnecting the instrument power cord from line power.
• Before the instrument is installed, the area around, under and behind the instrument’s
planned location is to be cleared of any dirt and dust to prevent their entry into the
instrument’s interior which could cause a negative effect on performance.
36 FIMS Hardware Guide
WARNING
Si l'équipement est utilisé d'une manière non spécifiée ici, la
protection fournie par l'équipement peut être altérée.
AVERTISSEMENT
The FIMS has been designed and tested in accordance with PerkinElmer specifications and in
accordance with industry safety requirements.
The FIMS is only for indoor use under the following conditions:
• Indoor use
• The location must be free of smoke, dust, corrosive fumes, direct sunlight and excessive
vibration.
• Temperature: +5 to +40 °C (40 °F to 104 °F)
• Relative humidity: 20% to 80%, without condensation
• Altitude: in the range -400 m to 2,000 m (1,312 feet to 6,562 feet)
Storage conditions:
• Ambient temperature: –20°C to +60°C (–4°F to +140°F)
• Relative humidity: 20% to 80%, without condensation
• Altitude: in the range -400 m to 12,000 m (1,312 feet to 39,370 feet)
If possible, avoid any adjustment, maintenance and repair of the opened, operating
instrument. If any adjustment, maintenance and repair of the opened instrument is
necessary, this must be done by a skilled person, trained by PerkinElmer, and who is aware
of the hazard involved..
Whenever it is likely that the FIMS is unsafe, make it inoperative. The FIMS may be unsafe if
it:
• shows visible damage
• fails to perform the intended measurement
• has been subjected to prolonged storage in unfavorable conditions
• has been subjected to severe transport stresses.
38 FIMS Hardware Guide
Electrical Safety
The instrument has been designed to protect the operator from potential electrical hazards.
This section describes some recommended electrical safety practices.
The instrument must be correctly connected to a suitable electrical supply. The supply must
have a correctly installed protective conductor (earth ground) and must be installed or
checked by a qualified electrician before connecting the instrument.
To ensure satisfactory and safe operation of the instrument, it is essential that the
green/yellow lead of the line power cord is connected to true electrical earth (ground).
Safety Practices . 39
If any part of the instrument is not installed by a PerkinElmer service representative, ensure
that the line power plug is wired correctly:
International USA
• Connect the instrument to a correctly installed line power outlet that has a protective
conductor connection (earth ground).
• Do not operate the instrument with any covers or internal parts removed.
• Disconnect the instrument from all voltage sources before opening it for any
adjustment, replacement, maintenance, or repair. If afterwards, the opened instrument
must be operated for further adjustment, maintenance, or repair, this must only be
done by a PerkinElmer Service engineer.
• Whenever it is possible that the instrument is no longer electrically safe for use, make
the instrument inoperative and secure it against any unauthorized or unintentional
operation. The electrical safety of the instrument is likely to be impaired if, for example,
the instrument shows visible damage; has been subjected to prolonged storage under
unfavorable conditions; or has been subjected to severe stress during transportation.
• Use only fuses with the required current rating and of the specified type for
replacement. Do not use makeshift fuses or short circuit the fuse holders.
• Whenever it is likely that the instrument is no longer electrically safe for use, make the
instrument inoperative and secure it against any unauthorized or unintentional
operation.
UV R adiation
The lamp emits intense UV radiation which can damage your eyes.
Do not gaze into a lighted lamp.
WARNING
Rayonnem ent UV
You should be aware of the health hazard presented by UV radiation. The source lamp
generates UV radiation. Always wear UV-absorbing eye protection when viewing the radiation
from the source lamp. When the spectrometer is on, do not remove any covers unless
specifically instructed to do so in the instruction manual.
Safety Practices . 41
W aste Disposal
Waste vessels may contain acidic or organic solutions and small amount of elements that
were analyzed. If these materials are toxic, you may have to treat the collected effluent as
hazardous waste. Refer to your local safety regulations for proper disposal procedures.
Mercury lamps contain small quantities of the lamp element in a very pure form. When you
dispose of lamps containing toxic elements you must treat them as hazardous waste.
Mercury lamps are maintained under reduced pressure. Handle and dispose correctly to
minimize the implosion risk.
Treat the used mercury filters as hazardous waste and dispose of them according to local
safety regulations.
42 FIMS Hardware Guide
Sodium Tetrahydroborate
Sodium tetrahydroborate solutions are unstable and decompose, releasing hydrogen. They
also release hydrogen when they come into contact with acids.
• Ensure that the work area has an adequate ventilation system to prevent the buildup
of explosive hydrogen/air mixtures.
• When you are using sodium tetrahydroborate as the reductant with the flow-injection
system, hydrogen is formed when it comes into contact with the acidic carrier
solution.
To prevent air entering the system make sure that the tubing connections
are correctly assembled and tight.
At the end of the work session, pump deionized water through the sodium
tetrahydroborate tubing system to remove all traces of the reductant.
Safety Practices . 43
Chem icals
WARNING
AVERTISSEMENT
Use, store and dispose of chemicals that you require for your analyses in accordance with the
manufacturer’s recommendations and local safety regulations.
44 FIMS Hardware Guide
We recommend that gas cylinders should be located outside of the laboratory and the gases
led to the laboratory through approved piping. Use only approved tubing, connectors and
regulators for gas supply lines.
Safety Practices . 45
Tox ic Fum es
Avant que vous puissiez utiliser cet instrument, votre laboratoire doit
AVERTISSEMENT
s'être doté d'un système de ventilation efficace pour les fumées.
Use, store and dispose of chemicals that you require for your analyses in accordance with the
manufacturer’s recommendations and local safety regulations.
A charcoal filter is used to absorb the mercury vapor emitted from the FIMS-cell.
CAUTION
Do not restrict air intake or exhaust.
EM C Com pliance
EM C Directive
This product has been designed and manufactured, having regard to the state of the art, to
ensure that:
a) the electromagnetic disturbance generated does not exceed the level above which
radio and telecommunications equipment or other equipment cannot operate as
intended;
b) it has a level of immunity to the electromagnetic disturbance to be expected in its
intended use which allows it to operate without unacceptable degradation of its
intended use.
Europe
All information concerning EMC standards is in the Declaration of Conformity, and these
standards may change as the European Union adds new requirements.
2) this device must accept any interference received, including interference that may
cause undesired operation.
P ollution Degree
This product will operate safely in environments that contain nonconductive foreign matter
up to Pollution Degree 2 in EN/IEC 61010-1.
Safety Practices . 47
or
A label with a crossed-out wheeled bin symbol and a rectangular bar indicates that the
product is covered by the Waste Electrical and Electronic Equipment (WEEE) Directive and is
not to be disposed of as unsorted municipal waste. Any products marked with this symbol
must be collected separately, according to the regulatory guidelines in your area.
The objectives of this program are to preserve, protect and improve the quality of the
environment, protect human health, and utilize natural resources prudently and rationally.
Specific treatment of WEEE is indispensable in order to avoid the dispersion of pollutants into
the recycled material or waste stream. Such treatment is the most effective means of
protecting the customer’s environment.
Requirements for waste collection reuse, recycling, and recovery programs vary by regulatory
authority at your location. Contact your local responsible body (e.g., your laboratory
manager) or authorized representative for information regarding applicable disposal
regulations. Contact PerkinElmer at the web site listed below for information specific to
PerkinElmer products.
Web address:
http://www.perkinelmer.com/pages/010/onesource/environmental-health-and-
safety/environmental-directives-compliance.xhtml
For Customer Care telephone numbers select “Contact us” on the web page.
Products from other manufacturers may also form a part of your PerkinElmer system. These
other producers are directly responsible for the collection and processing of their own waste
products under the terms of the WEEE Directive. Please contact these producers directly
before discarding any of their products.
Consult the PerkinElmer web site (above) for producer names and web addresses.
48 FIMS Hardware Guide
Decontam ination
Customers wishing to return instrumentation and/or associated materials to
PerkinElmer for repair, maintenance, warranty or trade-in purposes are advised
that all returned goods must be certified as clean and free from contamination.
Certificate form:
http://www.perkinelmer.com/Content/technicalinfo/dts_perkinelmercertificationofdecontaminat
ionform.pdf
If you do not have access to the internet and are located in the U.S., call toll free at 1-800-
762-4000 or (+1) 203-925-4602, 8:30 a.m. - 7 p.m. EST and speak to Customer Support.
In Canada, call toll free 800-561-4646 and speak to Customer Support.
If you are located outside of the United States or Canada, please call your local PerkinElmer
sales office for more information.
W arning Labels
WARNING
Lorsque cette étiquette est apposée sur un instrument, cela signifie que
vous devez vous reporter au manuel.
AVERTISSEMENT
The instrument interface is a set of five potential-free relays that are used for controlling
accessories such as the Amalgam System. The voltages and currents that you apply to these
relays must not exceed the values shown in the table below.
I max V max
DC 1.0 A 42.4 V
AC 0.5 A 30 V
Safety Practices . 51
• Safe Practices in Chemical Laboratories, Royal Society of Chemistry, London, UK, 1989.
• Hazards in the Chemical Laboratory, 5th edition, Luxon, S.G., ed., Royal Society of
Chemistry, London, UK, 1993.
• CRC Handbook of Laboratory Safety, 5th edition, Furr, K., ed., The Chemical Rubber Co.
Press, Florida, USA, 2000.
• Sax's Dangerous Properties of Industrial Materials, 11th edition, Sax, N.I. and Lewis, R.J.,
eds., Wiley, New York, USA, 2004.
• Pohanish, R.P., HazMat Data, 2nd edition, Barnes & Noble, New York, USA, 2004.
FRG, DIN-Sicherheitsblätter,
System Description
54 FIMS Hardware Guide
System Description . 55
I ntroduction
FIMS is an acronym for Flow Injection Mercury System
The FIMS is a compact, software-driven, analysis system for mercury determinations. The
basic system consists of the FIMS spectrometer and a computer. Other instruments are
available as options, such as an autosampler (S10), the Amalgam System, and a printer.
With the FIMS analysis system, sample and reagent consumption is much lower than with
traditional manual sample preparation and delivery. This results in lower costs, less waste -
benefits the environment, and more sample being available for other analyses. Another
important advantage of using FIMS is the speed of analysis (up to 144 samples per hour).
56 . FIMS Hardware Guide
9
1
2 3 4 10 5 6 7
2 RS-232-C Interface
3 System Interface
6 Voltage Selector
8 Fuse Holder
The Optical Unit is in the upper part of the FIMS. It contains the radiation source (Hg lamp),
the FIMS-cell compartment and the photocell detector.
R adiation Source
Detector
FIMS-Cell
The mercury vapor flows into the FIMS-cell where the absorption of the mercury is
measured. The FIMS-cell has an inner diameter of 4 mm and an optical path length of 260
mm. The cell is heated to about 50 °C to prevent the formation of condensation.
FIMS uses peristaltic pumps to transport the various liquids through the system. The speed
of the pumps is under software control: 20-120 rpm or off.
Magazines
Each pump accepts up to four magazines which hold the pump tubing. There are different
magazines for the different sizes of pump tubing. The pressure adjustment lever regulates
the pressure applied to the pump tubing. A list of the magazines that are available is given in
the Parts chapter.
Pump Tubing
A variety of pump tubes with differing diameters is available. The different sizes have
differently colored collars. The pump tubing is available in acid-resistant and solvent resistant
materials.
A list of the sizes and types that are available is given in the Parts chapter.
The FIMS is normally shipped with a 5-port valve. The valve has two positions, Fill and
Inject.
In the Fill position the sample is drawn into the sample loop. The carrier stream flows
continuously to the manifold. In the Inject position the sample loop is switched into the
carrier stream and the sample is transported to the manifold. The sample pump stops while
the valve is in the Inject position.
60 . FIMS Hardware Guide
Sample Loops
The sample loops are made from PTFE tubing and have screw connectors. The sample loops
are available in different lengths with volumes between 50 µL and 1000 µL. A list of the sizes
that are available is given in the Parts chapter.
An inert carrier gas is required for mercury determinations with the FIMS system. The carrier
gas carries the mercury vapor from the manifold to the FIMS-cell in the spectrometer unit.
The requirements for the carrier gas are described in Laboratory Requirements.
The inlet for the carrier gas is on the rear of FIMS (the GAS IN connection). The FIMS has a
gas economy function: when FIMS is not used for more than 10 minutes the gas flow is
automatically turned off.
The gas outlet, flow regulator and flow gauge are on the front panel of the FIMS unit. The
gauge is calibrated for argon. Useable flows are between 40 mL/min and 250 mL/min at a
recommended gas inlet pressure between 320 kPa (46 psi and 3.2 bar) and 400 kPa (58 psi
and 4 bar). The gas flow is off (0 mL/min) when the control knob is turned fully clockwise.
System Description . 61
Nonreturn Valve
The nonreturn valve at the gas outlet prevents liquid from the manifold entering the gas
control system.
Manifold
In the manifold two fluid streams are mixed. This can be to initiate a reaction or to dilute one
of the streams.
The manifold blocks have three channels that are interconnected blocks as shown below. The
inlets of the channels have a 1/4"- 28 UNF internal screw thread. The locks are made of an
inert, translucent plastic. Each block has two additional holes for connector pegs to join
adjacent blocks.
Gas/Liquid Separator
The gas/liquid separator is used in the mercury cold vapor technique to separate the gaseous
product and liquid waste in the mixture that leaves the manifold.
The gas/liquid separator block is joined to a manifold block with a plug connector.
62 . FIMS Hardware Guide
Plug Connector
(B050-7960)
The connection tubing is made from PTFE tubing and have screw connectors. The screw
connectors are color coded to identify the internal diameter of the tubing. A list of the sizes
that are available is given in the Parts chapter.
System Description . 63
A selection of adapters and connectors is available to connect the different types and sizes of
connector and pump tubing. Lists of the adapters and connectors that are available are given
in the Parts chapter.
Technical Data
Principle Single-beam atomic-absorption spectrometer with integral flow injection
sample-delivery system.
Computer Lenovo M83 Computer; Intel Core i5-4670 Processor (3.4GHz, 6M Cache);
1TB 7200RPM HDD; Intel HD Integrated Graphics;
4GB X 2 DIMM 1600MHz; UDIMM DDR3; Optical DVD Recordable; Wireless
WiFi 6235, 2 serial ports and one network port and Win 7 Ultimate 64-bit
Operating system; optional 19” or 24” monitor XVGA, mouse and printer.
Control System
Special application program with graphics user interface, mouse and
keyboard control. Online help function. Hard disk or floppy storage of
measurement data, signals and complete analytical methods
Graphics
High resolution graphics and numerical display of the signals. Calibration
curve display; newest + previous if a reslope or recalibration is done.
Storage and recall of transient absorbance signals. Hard copy printout of
screen graphics on an associated printer. In continuous mode, printout of
real time signals on an associated printer.
Flow Injection Five-port flow-injection valve with various sizes of sample loop. Valve
Valve setting (fill or inject) is controlled by the application program.
Carrier Gas Inert carrier gas system with flow gauge and flow regulator. Flow is
System automatically stopped when FIMS has been idle for 10 minutes.
Inlet pressure: 320 kPa (46 psi and 3.2 bar) to 400 kPa (58 psi and 4 bar).
Flows: 40-250 mL/minute, or off
Interfaces
RS-232-C interface.
Instrument interface (for Amalgam System) with five potential free relays:
Imax = 1 A (DC); Umax = 42.4 V (DC)
Imax = 0.5 A (AC); Umax = 30 V (AC).
Environmental
+10 °C to +35 °C
Requirements
20-80% relative humidity, non-condensing.
(operating)
Dimensions Width: 415 mm (16.3 in.) Height: 255 mm (10.0 in.) Depth: 410 mm (16.1
in.)
The central component of the flow injection system is the flow injection valve (FIAS-valve).
The FIAS-valve injects a defined and reproducible sample volume into a carrier or reagent
stream. The pump transports the carrier (and sample) and reagent streams to the manifold.
In the manifold the various reagents mix and possibly react. The outflow from the manifold
usually goes to some form of detection system.
System Description . 67
The mercury must be in an ionic form in the sample solution. When the reducing agent (e.g.
NaBH4) mixes with the sample, the ionic mercury is converted to metallic mercury. An inert
carrier gas (e.g. argon) transports the mercury to the spectrometer. A major advantage of
the technique is the inherent separation of the analyte element from the matrix. Nonspecific
background absorption and matrix interference are almost unknown with this technique.
Some important advantages of using FIMS for mercury determinations are the reduction in
sample and reagent consumption and increase in speed of analysis. With FIMS, up to 144
samples per hour can be analyzed.
R educing Agents
For mercury determination, either sodium tetrahydroborate or tin (II) chloride are suitable
reducing agents. It is important to have separate fluid system components reserved for
sodium tetra-hydroborate and tin(II) chloride applications. If you use a system that has had
tin(II) chloride in it for determinations with sodium tetrahydroborate, there is a severe
reduction in sensitivity .
A special Reductant Change kit is available for this purpose; part number B0508594. This
contains all fluid system parts that come into contact with the reducing agent.
The first channel of pump 2 feeds a stream of carrier fluid (HCl) continuously through the
FIAS-valve to the manifold. With the FIAS-valve in the Fill position, pump 1 fills the sample
loop. In the inject position (shown in the illustration) the contents of the sample loop enter
the carrier stream and are carried to the manifold, which acts as the reaction cell.
68 . FIMS Hardware Guide
The second channel of pump 2 carries the reducing agent NaBH4 or SnCl2 directly to the
manifold. The sample (in the acidic carrier stream) and reductant mix in the manifold and a
spontaneous reaction takes place, reducing the ironic mercury to metallic mercury.
The hydrogen that is released from the reductant, along with the stream of carrier gas
(argon or nitrogen), carry the mercury vapor to the gas/liquid separator where the liquid is
separated from the gaseous components.
Am algam Technique
The automatic Amalgam System can greatly improve the detection limit of your mercury
determinations.
In this system the atomic mercury is carried to a gold-platinum gauze with which it forms an
amalgam. This is done for a defined time for each of a number of aliquots of sample and
results in the gauze becoming enriched with mercury. At the end of the enrichment
procedure the gauze is quickly heated to release the mercury, which is then transported to
the measurement cell.
Using this technique the detection limit for mercury can be improved by more than an order
of magnitude. FIMS functions fully automatically with the Amalgam System.
Further details about the Amalgam System are contained in the Amalgam System Operator's
Manual.
I nstalling the FI M S
Analysis System
Installing the FIMS
Analysis System . 71
• Check that nothing is missing; a list of the equipment delivered is given in the Parts
chapter. If you think that something is missing, inform your nearest PerkinElmer
office.
• We recommend that you read the installation instructions in order to become familiar
with the spectrometer and its requirements before you install it or start using it.
• These instructions are also provided in case you need to alter any of the connections
or move the instrument.
For more details about these requirements see Laboratory Requirements. For the
requirements of the computer and any other accessories, see the handbooks provided with
the relevant instrument.
Sitting Accessories
If the autosampler fits securely on the top of the FIMS, we recommend that you place the
autosampler there. Place accessories such as the Amalgam System very close to the FIMS.
This will minimize the length of the sample transfer tubes between the instruments.
1. While the gas supply is off, set the pressure regulator to zero.
2. Remove the knurled nut from the GAS IN nipple on the rear of FIMS and slide it onto
the free end of the gas supply tube.
3. Push this end of the tube onto the GAS IN nipple on the rear of FIMS.
Push the tube over the bulge on the nipple, then slide the knurled nut up the tube to
the screw fitting of the nipple and tighten it securely.
NOTE: The regulator connectors/fittings do not come installed on the gas tube assembly. See the
following figure for the location of these fittings.
4. Connect the other end of the gas supply tube securely to the outlet of the gas supply
pressure regulator.
Electrical Connections
Electrical Hazard
Danger Électrique
1. Switch off the instrument and accessories and disconnect their line cords from the
line power supply.
3. Set the DIP switches to select the interface and set the relevant parameter values,
see page 75.
5. Connect the mouse and printer to the computer as described in the handbooks
supplied with these instruments.
Use the proper cable to connect the printer to the computer. If you use a different
cable the printer may not function correctly.
NOTE: With the serial connection, all the dip switches should be turned off.
Voltage Selector
Baud Switch
Rate [1] [2]
9600 off off
19200 on off
38400 off on
Electrical Hazard
Danger Électrique
To avoid problems of interference caused by earth loops, always connect the FIMS, the
computer and the printer to the same phase of the line power supply. The most convenient
method is to use a multi-socket distributor.
See Laboratory Requirements for details of the line power supply. See the computer and
printer manuals for details of their power requirements.
1. Before you alter or make any new electrical connections, switch off all the
instruments in the system and disconnect their line cords from the line power supply.
Connect the communication cables correctly, see page 75.
Set the DIP switches to select the interface and set the relevant parameter values,
see the previous page.
Set the voltage selector correctly, see page 75.
Make sure that the two fuses in the power input socket on the rear of FIMS are of
the correct type, 6.3 AT, slow- blow, see page 112.
2. Connect the line cords of the FIMS, the computer and the printer to the multi-socket
distributor.
3. Connect the multi-socket distributor to a correctly installed line power supply that
has a protective conductor connection (earth/ground)
NOTE: When you switch on the instruments, follow the correct procedure described in the
handbooks supplied with each instrument installation.
78 . FIMS Hardware Guide
Auto-
sampler
For a description of specific applications, see the booklet Recommended Analytical Conditions
and General Information for Flow Injection Mercury/Hydride Analyses.
Constricted Tubing
The normal pump tubing supplied with the FIAS are not resistant
to organic solvents. Use solvent resistant pump tubing if you are
pumping organic solvents.
Constricted Tubing
Tube-Connector Key
Tighten the screw fittings on the PTFE tubing by hand or with the tube connector key (Part
No. B0501315). Do not use any other tool. Do not over tighten the connector; the connection
will be distorted and may leak.
The pump tubing is placed in the magazine using the middle collar and one of the remaining
collars. The other side of the pump tubing can be used after the first side becomes worn.
When the system is not being used, one of the collars should be removed from the
magazine, or it will wear prematurely.
Since each pump tube has three collars, each tube has two sections that you can use to
tension the tube in the magazine. If the section of tube in the magazine becomes deformed,
but there is no other damage, you can tension the other section of tube in the magazine.
82 . FIMS Hardware Guide
The flow is from the left to right for pump magazines placed above the pump
rotor and right to left for pump magazines placed below the pump rotor.
Installing the FIMS
Analysis System . 83
2. Rotate the pressure adjustment lever until the end of the screw locates in the notch
on the back of the pump magazine.
• Start the pumps and adjust the flows as described in the FIMS Software
Guide.
To increase the flow, rotate the pressure adjustment screw clockwise to
press the magazine against the pump rotor and increase the pressure on
the pump tubing.
To decrease the flow, rotate the pressure adjustment screw counter
clockwise to decrease the pressure on the pump tubing. Adjust the
pressure to obtain a steady flow without bubbles.
Do not over tighten the pressure adjustment screw since this shortens the working life of the
tubing, and may slow or stop the pump.
84 . FIMS Hardware Guide
FI AS–Valve Connections
Part numbers for PTFE tubes, sample loops and other fluid system components are given in
the Parts chapter.
Installing the FIMS
Analysis System . 85
FIMS-Cell Connections
Toxic Gases
WARNING The FIMS uses a charcoal filter which has been attached during
installation, removes the toxic fumes.
Constricted Tubing
Gaz Toxiques
Constricted Tubing
To install (or remove) the FIMS-cell from the cell compartment of FIMS, use the procedure
described on page 99.
When you press the power switch to the ON position, the green light under the switch
illuminates. The instrument is ready for use and the FIMS-cell heating and the source lamp
are switched on.
When you press the power switch to the off position, the green control light under the switch
goes out and O is shown on the upper edge of the switch. All instrument functions are
interrupted.
Installing the FIMS
Analysis System . 89
The booklets: Preparing Your Laboratory for PerkinElmer Atomic Spectroscopy Instruments,
and Preparing Your Laboratory for PerkinElmer Flow Injection Atomic Spectroscopy, available
from PerkinElmer, also contain useful information.
• Indoors
Storage conditions:
You should have sufficient room around the instruments to reach all the connections on the
rear, and reach the gas and electric supply points.
FIMS requires a stable single phase, 115 V or 230 V ± 10%, 50 Hz or 60 Hz ± 1%, line
power supply that has a correctly wired protective conductor terminal (earth/ground). The
instrument uses 450 VA maximum power.
The line power supply must conform with your local safety regulations and be checked by a
qualified electrician before you connect the instrument.
Installing the FIMS
Analysis System . 91
Autosampler
Autosampler
Carrier Gas
The FIMS requires a supply of inert carrier gas. Argon is recommended but purified nitrogen
can be used.
• The gas supply system must conform with your local safety regulations. PerkinElmer
recommends that cylinders or tanks be stored outside the laboratory and the gas piped
to the instrument in approved gas lines.
• The gas supply line must contain a suitable pressure reducing valve and an on/off valve
between the gas supply and the FIMS spectrometer. Either the gas manufacturer or
PerkinElmer can supply suitable two-stage pressure reducing valves.
• You must be able to reach the on/off valve and pressure regulator and see the pressure
gauge while you are working with FIMS.
Maintenance . 93
M aintenance
94 . FIMS Hardware Guide
Maintenance . 95
PerkinElm er Service
You should only perform the maintenance procedures described in this handbook.
For maintenance procedures that are not described in this manual, contact your local Perkin-
Elmer office to arrange for a service engineer to visit.
In particular you must only allow a PerkinElmer service engineer to perform any work on the
electrical components inside the instrument.
Complete analysis system For safety reasons, and to avoid contaminating new
and work area samples, make sure that the instrument and the work area
are kept absolutely clean. This is especially important
when working with toxic substances and when measuring
trace amounts of any elements.
Mercury Filter PerkinElmer guarantees that the filter will safely adsorb all
the mercury leaving the FIMS-cell for a period of 6 months
or up to a total mercury load of 5.5 mg, whichever occurs
sooner.
Instrument outer surfaces Exterior surfaces may be cleaned with a soft cloth,
dampened with a mild detergent and water solution. Do
not use abrasive cleaners or solvents.
FIMS-cell, inner surface Clean the inner surface of the cell only if there is a
decrease in sensitivity which is not attributable to other
factors, such as unsuitable analytical parameters or
instrument settings, or incorrectly prepared or
contaminated solutions.
Complete fluid system When you have finished an analysis, rinse the fluid system. See
the FIMS Software Guide (Part No. 09931164) for the correct
procedure to use.
Organic Solutions
Pump rollers Wipe the rollers with a dry lint free cloth.
All tubes On a daily basis, make sure that all tubing is clean and free of
kinks. Replace any tubing that may be damaged, worn, or
contaminated.
Waste bottle Empty the waste bottle regularly; never allow it to overflow or
allow the liquid to reach the end of the drain tubing.
Solutions that are left over at the end of the day must be
combined in a waste container that is in a fume hood.
FIAS-valve The FIAS valve is easily clogged. You can remove the FIAS-valve
to clean it or replace parts; see page 103.
Maintenance . 99
FI M S-Cell M aintenance
M easuring the Absorbance of the FI M S-Cell W indow s
1. Switch on the FIMS analysis system as described in the FIMS Software Guide (Part
No. 09931164).
4. Remove the FIMS-cell from the cell compartment of FIMS; see page 99.
If the absorbance is greater than 0.75, remove the windows from the FIMS-cell and clean
them.
2. Carefully disconnect the exhaust tube and sample transfer tube from the FIMS-cell.
3. Grip the two nipples on the cell window assemblies and pull the cell out of the cell
compartment.
100 . FIMS Hardware Guide
2. Carefully insert the tip of a small screwdriver in the notch of the window assembly and
remove the outer O-ring.
2. Push and simultaneously twist the cell window assemblies onto the ends of the FIMS-cell.
NOTE: Install the cell in the spectrometer and measure the absorption of the windows; see page 99.
If the absorbance is still too great, either clean the windows more thoroughly, or install new
windows. See the Parts chapter for part numbers.
Take care not to scratch or touch the surface of the quartz windows. You
CAUTION
must replace scratched windows. The more you rub the surface of the
windows, the more chance there is of scratching them. Wearing gloves
are recommended.
Keep cleaning solutions and water away from other parts of the instrument.
1. Remove the FIMS-cell from the cell compartment of the spectrometer; see page 99.
3. Wash the windows with mild laboratory-grade detergent, and rinse with plentiful of
deionized water and allow them to dry.
4. Clean the windows with a soft, lint-free cloth moistened with a spectroscopic-grade
alcohol or absolute alcohol.
Do not use too m uch alcohol since this m ay produce drying m arks.
Maintenance . 101
NOTE: Install the cell in the spectrometer and measure the absorption of the windows; see page 99.
If the absorbance is still too great, either clean the windows more thoroughly, or install new
windows. See the Parts chapter for part numbers.
When you have finished an analysis, rinse the fluid system. See the FIMS Software Guide
(Part No. 09931164) for the correct procedure to use.
Hydrochloric Acid
Acide Chlorhydrique
• If necessary, use a nylon filament and compressed air to unblock the fluid channels
of the blocks.
• Rinse the manifold and separator blocks with 1:1 hydrochloric acid (v/v, one part
concentrated hydrochloric acid diluted with one part water -about six molar).
• Rinse the manifold and separator components thoroughly with deionized water.
FI AS-Valve M aintenance
Cleaning the FI AS-Valve
Norm al Procedure
• When you have finished an analysis, rinse the fluid system. See the FIMS Software Guide
(Part No. 09931164) for the correct procedure to use.
If the procedure described above is not sufficient to clean the valve, you can dismantle the
valve and clean the component parts as described below.
2. Remove the valve from the pump unit, see page 103.
4. Clean the individual parts of the valve with deionized water. Pump deionized water
through each channel of the valve components. If necessary, use a nylon filament and
compressed air to unblock the channels of the valve. A squirt bottle can be used to direct
water into a valve opening with a short piece of pump tubing connected to a fitting.
3. Using a 3 mm hexagonal key unscrew the two screws that secure the valve to the pump
unit.
2. Tighten the two screws that hold the FIAS-valve onto the pump unit.
104 . FIMS Hardware Guide
1. Remove the FIAS-valve from the pump unit as described on page 103.
2. Place the dismantling tool on the rear of the FIAS-valve. Make sure that the lug on the
dismantling tool engages the notch in the spindle.
3. Hold the valve and dismantling tool securely and, with a 7 mm wrench, unscrew and
remove the securing bolt.
• Use deionized water or use a soft lint free cloth moistened with ethanol, or isopropanol
(IPA).
Maintenance . 105
• If necessary, use a nylon filament and compressed air to unblock the channels in the
valve.
NOTE: The valve rotor and the valve body are matched components. If either is damaged you must
replace both with a matched pair of components.
2. Reassemble the valve components as shown below. Make sure that the groove in the
valve rotor locates correctly over the pin on the valve body.
3. Screw the securing bolt into the spindle, first by hand, then use the 7 mm wrench. Do
not over tighten the securing bolt.
4. Pump deionized water through the channels of the valve to make sure that the channels
are open.
Periodically check the nonreturn valve. If the rubber sleeve shows signs of deterioration,
replace it.
Maintenance . 107
1. Connect the silicone exhaust tube (Part No. B0046948) to the left-hand nipple on the
FIMS-cell.
108 . FIMS Hardware Guide
2. With instruments that have the filter holder on the rear panel, cut the silicone tube so
that it reaches the filter holder.
Push one end of the mercury filter onto the silicone tube.
3. Push the mercury filter into the filter holder on the rear panel of the instrument. If there
is no filter holder, let the filter lie on the bench.
Note: Make sure that the silicone tube is not kinked or restricted and that the outlet of the filter is
not blocked.
Maintenance . 109
3. If the old filter is dirty, remove it and insert a new filter (Part No. B0502706).
Electrical Hazard
UV Radiation
The lamp emits intense UV radiation which can damage your eyes.
Do not gaze into a lighted lamp.
Danger Électrique
Le rayonnem ent UV
Change the source lamp if the lamp fails or the intensity falls to an unacceptable level.
1. Switch off the instrument and disconnect the line cord from the line power supply.
2. Using a 2.5 mm hexagonal key remove the two screws securing the lamp cover and
pull off the cover.
3. Hook the Hg lamp removal tool (Part No. B8300243) under the lamp and carefully
pull the lamp out of the socket.
4. Hold the new lamp with a lint free cloth and carefully push it into the lamp socket
until it locks into place.
5. Replace the lamp cover and secure it with the two screws.
Maintenance . 111
112 . FIMS Hardware Guide
Electrical Hazard
Danger Électrique
The fuses are located in the fuse holder of the line power socket (receptacle) at the rear of
the instrument.
1. Switch off the instrument and disconnect the line power cord from the electrical
supply.
2. Remove the line power plug from the socket on the rear of the instrument.
3. Squeeze the two lugs at each side of the fuse holder and gently pull the fuse holder
out of the socket.
4. Remove both fuses and check them. If they have blown, discard them.
The instrument needs two, 6.3 AT, slow blow fuses (Part No. B0155576 for a pack of
10 fuses).
6. Align the lug at the top of the fuse holder with the slot in the socket. Push the fuse
holder into the socket until the lugs snap into place.
NOTE: If the new fuses blow, and the cause cannot be readily determined, then a service call is
needed.
Maintenance . 113
114 . FIMS Hardware Guide
. 115
P arts
116 . FIMS Hardware Guide
Parts . 117
Supplies, replacement parts, and accessories can be ordered directly from PerkinElmer, using
the part numbers quoted in the guides provided with the instrument.
See our website:
http://perkinelmer.com
To place an order for supplies and many replacement parts, request a free catalog, or ask for
information:
If you are located within the U.S., call toll free 1-800-762-4002, 8 a.m. to 8 p.m. EST. Your
order will be shipped promptly, usually within 24 hours.
If you are located outside of the U.S., call your local PerkinElmer sales or service office.
FI AS-Valve P arts
Manifold
B050-7957
Base Plate
B314-0661
122 . FIMS Hardware Guide
Pump Tubes
If you require solvent resistant pump tubing, see the current PerkinElmer price lists.
Sample Loops
Size (µL) Part number
50 B0506714
100 B0506715
200 B0194048
500 B0194049
1000 B0501000
Reaction Loops
Size /Type Part number
300 mm, 0.5 mm i.d B0506712
600 mm, 0.5 mm i.d B0506713
3-D – Reactor, Knotted PTFE Tube B0501595
126 . FIMS Hardware Guide
Parts . 127
I ndex
reducing agent ............................................ 67
Flow Injection Valve ............................................ 59
A Flow System ........................................................ 59
About This Manual ................................................. 9 Fluid System Components ................................... 79
Adaptors and Connectors...................................... 63 Fuse
Air Filter changing ........................................................ 112
changing ........................................................ 109
Amalgam G
technique.......................................................... 68
Gas/Liquid separator ............................................ 61
Gas/Liquid Separator
C cleaning ......................................................... 102
Carrier Gas ......................................................... 60
Carrier Gas System L
maintenance ................................................... 106
Chemical Warnings .............................................. 43 Labels
Cleaning the Instrument........................................ 48 Warning Signs ................................................. 49
Connections Laboratory Requirements
carrier gas ........................................................ 73 environmental conditions ................................ 89
electrical .......................................................... 74 summary .......................................................... 89
FIMS cell ......................................................... 86 Locating
line power ........................................................ 77 accessories....................................................... 72
Conventions computer ......................................................... 72
Notes, cautions and warnings .......................... 12 instrument ....................................................... 72
text ................................................................... 12 printer .............................................................. 72
Customer Precautions ........................................... 36
M
D Maintenance Checklists ....................................... 96
Detector ................................................................ 58 Manifold............................................................... 61
cleaning ......................................................... 102
Mercury Filter
E changing ........................................................ 107
Electrical Safety.................................................... 38
EMC Compliance ................................................. 46 N
Nonreturn Valve................................................. 61
F
FCC Rules ............................................................ 46 O
FIAS Valve
cleaning.......................................................... 103 Optical.................................................................. 58
dismantling .................................................... 104
fitting ............................................................. 103
reassembling .................................................. 105
P
removing ........................................................ 103 Parts
FIMS carrier gas system .......................................... 119
-100 equipment ...................................................... 117
rear panel .................................................... 57 FIAS-valve .................................................... 120
-400 pump tubes .................................................... 122
control ......................................................... 56 spectrometer .................................................. 119
front panel ................................................... 56 Pollution Degree .................................................. 46
spectrometer Precautions.......................................................... 34
FIMS Cell Pump Tubing........................................................ 81
cleaning.......................................................... 101
FIMS-cell
checklist: .......................................................... 97 R
window Radiation Source
checklist ...................................................... 97 References ............................................................ 68
FIMS-Cell............................................................. 58 Replacement Parts .............................................. 119
Flow Injection
mercury cold trap ............................................. 66
128 . FIMS Hardware Guide
Internet: http://www.perkinelmer.com
email: info@perkinelmer.com