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Operating Manual
Thermo Scientific is a registered trademark of Thermo Fisher Scientific Inc. in the United States.
Microsoft and Windows are registered trademarks of Microsoft Corporation in the United States and
other countries.
The following are registered trademarks in the United States and possibly other countries: CETAC is
a trademark of Teledyne Instruments, Inc. Kalrez is a registered trademark of E.I. du Pont de
Nemours & Co. QR Code is a registered trademark of DENSO WAVE INCORPORATED in Japan
and other countries. Teflon is a registered trademark of E. I. du Pont de Nemours & Co. Tygon is a
registered trademark of Saint-Gobain Performance Plastics Company. Viton is a registered trademark
of DuPont Performance Elastomers LLC.
All other trademarks are the property of Thermo Fisher Scientific Inc. and its subsidiaries.
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Fisher Scientific Inc.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) i
Contents
ii iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Contents
Chapter 6 Operation.................................................................................6-1
Operation of AA Systems ............................................... 6-2
Spectrometer Status Indicators .................................... 6-2
Hollow Cathode Lamps .............................................. 6-3
Alignment and Operation of the iSQ Module................ 6-4
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) iii
Contents
iv iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Contents
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) v
Contents
vi iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
1
Using this Manual
Contents
• The spectrometer
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 1-1
Using this Manual
Typographical Conventions
Typographical Conventions
This section describes typographical conventions that have been
established for Thermo Fisher Scientific manuals.
Signal Word
Make sure that you follow the precautionary statements presented in
this manual. The special notices appear different from the main flow of
text:
NOTICE Points out possible material damage, data loss, impaired data quality
and other important information in connection with the instrument.
Viewpoint Orientation
The expressions left and right used in this manual always refer to the
viewpoint of a person that is facing the front side of the instrument.
Data Input
Throughout this manual, the following conventions indicate data input
and output via the computer:
• For brevity, expressions such as “choose File > Directories” are used
rather than “pull down the File menu and choose Directories.”
• Any button that you click on the screen is represented in bold face
letters. For example, “click Close”.
1-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Using this Manual
Typographical Conventions
Topic Headings
The following headings are used to show the organization of topics
within a chapter:
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 1-3
Using this Manual
Reference Documentation
Reference Documentation
This iCE 3000 Series AA Spectrometers Operating Manual represents the
Original Operating Instructions. In addition to this manual, Thermo
Fisher Scientific provides other documents for the iCE 3000 Series
spectrometers that are not part of the Original Operating Instructions.
• Methods Manual
1-4 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Using this Manual
Contacting Us
Contacting Us
There are several ways to contact Thermo Fisher Scientific. You can use
your smartphone to scan a QR Code, which opens your email
application or browser.
2. For the first login, you have to create an account. Follow the
instructions given on screen. Accept the invitation within six
days and log in with your created Microsoft™ password.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 1-5
Using this Manual
Contacting Us
1-6 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
2
Scope of Delivery
This chapter lists the standard components of your iCE 3000 Series
system and optional components.
Contents
• Printed manuals
- iCE 3000 Series Operating Manual
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 2-1
Scope of Delivery
Optional System Components
2-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
3
System Description
Contents
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-1
System Description
Description of AA Systems
Description of AA Systems
The fully functional AA system with complete multi-element capability
is controlled by a Data Station running SOLAAR software under
Microsoft™ Windows™. Flame absorption/emission systems can be
extended to graphite furnace or vapor absorption modes by ordering the
appropriate accessory atomizer.
3-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
System Description
Description of AA Systems
Optical System
All systems (except the iCE 3400 spectrometer) are fitted with Stockdale
double beam optics giving maximum signal-to-noise ratio during the
signal measurement. All mirrors are silica coated, and the optics are
sealed to prevent dust ingress. The self-calibrating Echelle
monochromator and prism post-monochromator provide automatic
wavelength and bandpass setup.
Flame System
All AA flames are supported by the universal finned 50 mm titanium
burner with chamfered slot design giving high solids handling, excellent
flame stability and low carbon build-up. The burner height is
automatically adjustable, and controls are provided to adjust the burner
rotation and transverse position. An optional 100 mm burner for
air/acetylene flames is also available. Automatic flame ignition is
provided by a high tension electric spark.
A flame sensor responding to all flame types ensures safe gas handling if
the flame goes out. All active gas lines are fitted with flame arrestors and
blow back valves, with MFC controlled line pressures to provide
automatic safe shutdown if the line pressure falls below the safe limits.
The gas control system shuts down safely if the power fails. The totally
enclosed, draft proof “kitchen” area is fitted with a safety door
containing a heat and UV absorbing window.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-3
System Description
Description of AA Systems
Electronics
Spectrometer electronics are based on the Motorola 68340
microprocessor, with the system firmware residing in Flash PROM.
Firmware can be downloaded to the Flash PROM from an external PC
without removing any covers. Interfacing to the Data Station is via USB.
Accessories including autosamplers, furnace and VP100 interface to the
spectrometer is via RS-232C at 9600 baud.
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System Description
Description of AA Systems
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-5
System Description
Description of AA Systems
3-6 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
System Description
Spectrometer System
Spectrometer System
Thermo Fisher Scientific does not guarantee that the instrument will
work, nor that the published specification will be met when using
third party lamps that are 37 mm in diameter.
Certain older types of HCL are fitted with four base pins. Do not use
these lamps with your iCE 3000 Series spectrometer. They may cause
severe damage to the instrument
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-7
System Description
Spectrometer System
1 2
4 3
3-8 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
System Description
iSQ Module
iSQ Module
The iSQ Module allows Intelligent Spectrometer Qualification (iSQ)
tests to be run by the SOLAAR software, to confirm that your
spectrometer is operating correctly. The module provides a set of
certified traceable neutral density and polaroid filters in a motorized
filter mount that are used to automatically measure the performance of
your spectrometer.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-9
System Description
Flame System
Flame System
The spectrometer uses a flame or a furnace to provide atoms that are
analyzed to indicate the concentration of an element in an unknown
sample. A flame uses acetylene as the fuel, and either air or nitrous oxide
is required as oxidant for the flame. A nitrous oxide flame also requires
air to allow the system to stabilize before a nitrous oxide flame is used.
Gas Connections
Three gas inlet connections are provided on the spectrometer.
• Air
• Acetylene
• Nitrous Oxide
Burners
Two types of burners are available for iCE 3000 Series spectrometers:
3-10 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
System Description
Flame System
Air Compressor
The air compressor is an accessory that provides a flow of clean, dry,
compressed air for use as the oxidant for air supported flames. See
Figure 3-4.
1 2 3
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-11
System Description
Flame System
3-12 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
System Description
Flame System
Spray Chamber
NOTICE Do not remove the Teflon sleeve from the stem of the spray chamber.
The drain tube connection of the spray chamber has also been modified
to incorporate an O-ring seal. This prevents leaks that can occur with
certain low viscosity solvents such as white spirit.
Drain Tube
O-Rings
The Solvent Resistant Flame Kit includes a set of O-rings made of the
perfluoroelastomer Kalrez™, which are resistant to certain solvents that
cause the standard Viton™ O-rings to swell and degrade. Three of the
standard Viton O-rings are replaced with Kalrez O-rings. These are
located at the spray chamber neck, the spray chamber drain, and the
nebulizer-to-spray chamber seal.
Auxiliary Oxidant
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-13
System Description
Flame System
The Variable Flow Auxiliary Oxidant Kit (see also “Variable Flow
Auxiliary Oxidant Accessory” on page 3-12) is an optional accessory
that provides facilities for adjusting the flow rate of the additional
oxidant, so permitting a wider range of less common solvents to be used.
Flame Atomizer
Unless the solvent that you are planning to use is freely miscible with
water, remove any aqueous solutions from the spray chamber before
introducing the solvent. Then re-fill the spray chamber with clean
solvent. These procedures are described in “Maintenance of the Flame
System” on page 7-9.
Therefore, remove any solvent from the spray chamber drain when you
have finished your analysis. If you intend to use the solvent again when
you use the instrument the next time, you can leave the spray chamber
drain dry. If you intend to use aqueous samples the next time, re-fill the
spray chamber drain with clean water.
Other Accessories
If you use an autosampler fitted with a wash facility, ensure that you fill
the wash reservoir with clean solvent.
If you use the ID100 Autodilutor, ensure that you use clean solvent as
the diluent.
Check the various parts for wear and damage at regular intervals.
Replace any damaged parts immediately.
3-14 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
System Description
Furnace
Furnace
The GFS35Z Zeeman graphite furnace system can be used on iCE 3400
and 3500 spectrometers to provide graphite furnace analyses with
Zeeman background correction capability.
Services
Inert Gas
Inert gas protects the hot cuvette from atmospheric oxygen and flushes
sample vapors from the cuvette interior. Argon is recommended whereas
nitrogen can be used with some loss of performance for some elements.
NOTICE Connect the inert gas supply to the inlet port labeled ARGON 2 at
the rear of the furnace power supply unit. Regulate the inert gas supply
to 1.03±0.14 bar (15±2 psi).
Alternate Gas
An alternate type of gas can be passed through the cuvette to modify the
sample behavior.
NOTICE Connect the alternate gas supply to the inlet port labeled AIR 1 at the
rear of the furnace power supply unit. Regulate the alternate gas
supply to 1.03±0.14 bar (15±2 psi).
Fume Extraction
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-15
System Description
Furnace
Cooling Water
NOTICE Do not allow the pressure to exceed 6.9 bar (100 psi).
CAUTION Toxic Fluids. Risk of intoxication. Fungicides and biocides are toxic.
Follow laboratory safety rules and manufacturers’ instructions for
handling. Refer also to the Material Safety Data Sheets (MSDSs).
Connect the cooling water inlet and outlet hoses to the water inlet and
outlet connections on the furnace power supply unit. See Figure 3-5.
3-16 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
System Description
Furnace
Recirculation Chillers
GFS Autosampler
The GFS autosampler, Figure 3-6, is designed for use with the
GFS33/35 and GFS35Z graphite furnace systems. It provides fully
automated sample injection facilities. It also provides facilities for
automated matrix modification, and standard and sample solution
preparation.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-17
System Description
Furnace
1 2 3 4
14
13 5
12
11
10
9 8 7 6
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System Description
VP100 Continuous Flow Vapor System
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-19
System Description
VP100 Continuous Flow Vapor System
1 2
5 4 3
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4
Safety
Contents
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-1
Safety
Safety Symbols and Signal Words in this Manual
CAUTION Points out a hazardous situation that can lead to minor or medium
injury if not avoided.
WARNING Points out a hazardous situation that can lead to severe injury or death
if not avoided.
DANGER Points out a hazardous situation that will lead to severe injury or death
if not avoided.
4-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Safety
Safety Symbols on the Instrument
CAUTION Hot Surface. Risk of Burn. See This label is attached to the furnace.
Hot surfaces. manual for instructions.
Risk of burn.
See manual for safety
instructions.
Also refer to “Furnace Safety” on
page 4-24.
WARNING Read and fully understand This label is attached inside the flame
Read and fully understand
operator‘s manual before
operator’s manual before you use compartment. The label is attached
using this machine.
Failure to follow operating
instructions could result in
this machine. Failure to follow at the bottom left hand side.
death or serious injury.
operating instructions could result in
death or serious injury.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-3
Safety
Safety Symbols on the Instrument
WARNING
Heavy Object. Can cause back This label is attached near the rating
Heavy object.
Can cause back injury
injury during transportation. See plate to the rear side of the
during transportation.
See manual for
manual for instructions. instrument.
instructions.
4-4 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Safety
Safety Symbols on the Instrument
Rating Plate
To identify the instrument correctly when you contact Thermo Fisher
Scientific, always have the information from the rating plate available.
The rating plate is attached to the rear side of the spectrometer. It
contains the serial number, which is important in any type of
communication with Thermo Fisher Scientific.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-5
Safety
Intended Use
Intended Use
The iCE 3000 Series instrument is a bench top instrument that is
designed for atomic absorption analyses of liquid samples.
4-6 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Safety
Intended Use
Qualified Personnel
• Electrical Connections
The electrical installation must be carried out by qualified and
skilled personnel (electrician) according to the applicable
regulations (for example, cable cross-sections, fuses, earth
grounding connection).
• Installation
Only employees of Thermo Fisher Scientific or personnel who act
on behalf of Thermo Fisher Scientific are allowed to install the
iCE 3000 Series atomic absorption spectrometer.
• General Operation
The iCE 3000 Series atomic absorption spectrometer is designed
to be operated by qualified laboratory personnel. Before they start,
all users must be instructed about the hazards presented by the
instrument and the chemicals applied. The users must be advised
to read the relevant Material Safety Data Sheets (MSDSs).
• Decommissioning
Only employees of Thermo Fisher Scientific or personnel who act
on behalf of Thermo Fisher Scientific are allowed to
decommission the iCE 3000 Series atomic absorption
spectrometer.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-7
Safety
Electrical Safety
Electrical Safety
WARNING High Voltage. High voltages capable of causing an electric shock are
used in the instrument.
• Never run the system without the housing on. Permanent damage
can occur. When leaving the system, make sure that all protective
covers and doors are properly connected and closed, and that
heated areas are separated and marked to protect unqualified
personnel. Never rig or override any safety switches or safety
functions. Risk of electric shock, burn hazard or damage to your
system can occur.
• Before using any other procedures, users should check with the
manufacturers that the proposed method will not damage the
equipment.
4-8 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Safety
Spectrometer Safety
Spectrometer Safety
CAUTION Risk of Implosion. Hollow cathode lamps are filled with an inert gas
at pressures significantly below normal atmospheric pressure. If the
envelope is scratched or damaged, the lamp could implode. Inspect
lamps regularly, and discard any that have scratches or damage to the
envelope.
CAUTION High Voltage. Hollow cathode lamps are powered by high voltage
power supplies. If the lamp becomes damaged or broken while it is
fitted to the spectrometer, switch off the spectrometer and disconnect
it from the mains supply before attempting to remove the lamp.
CAUTION Risk of Eye Injury. The majority of hollow cathode lamps have the
potential to emit intensive radiation. Category 1 visible radiation
according to EN 12198 might cause retinopathy. Avoid long exposure
of several hours.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-9
Safety
Spectrometer Safety
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Safety
Spectrometer Safety
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-11
Safety
Flame System Safety
CAUTION Burn Hazard. Keep a safety distance to the flame and do not lean over
the chimney to avoid severe burns. When the flame has extinguished,
the surfaces surrounding it are still hot and can cause burns. Let the
system cool to ambient temperature before rebuilding the burner.
4-12 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Safety
Flame System Safety
Flame Safety
CAUTION Risk of Eye Injury. Nitrous oxide supported flames emit intense
radiation which can damage your eyes if viewed directly. Visible and
invisible radiation according to EN 12198 might cause retinopathy.
Category 2. Avoid long exposure of several hours. Wear safety goggles
that include an UV filter and provide protection against brightness.
CAUTION Risk of Flashback. A whistling noise from the flame may be the
precursor of a flashback due to carbon build up. Turn off the flame
immediately.
CAUTION Do not let run dry nitrous oxide supported flames (that is, only
aspirating air) to prevent any damages resulting from overheating (for
example, carbon build up).
Flashback
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-13
Safety
Flame System Safety
CAUTION Only align the burner with an air/acetylene flame. Do not align the
burner with a nitrous oxide/acetylene flame. Do not attempt to adjust
the impact bead with a nitrous oxide supported flame burning.
The normal operating sound level of the spectrometer does not exceed
85 dBA.
NOTICE After a flashback has occurred, do not use the instrument until it has
been certified as safe by a Thermo Fisher Scientific field service
engineer or agent.
❖ To avoid flashbacks
• Keep the burner clean. Monitor any carbon build up. Remove
carbon deposits carefully without damaging the slot and only with
an extinguished flame. Afterwards, allow the burner to warm up
before using the spectrometer again.
• Conduct gas leak tests regularly after moving the system, after
replacing tubings and after maintenance operations. See “Gas Leak
Test” on page 7-16.
• Do not adjust the impact bead with a nitrous oxide supported flame
burning.
• Follow the guidelines for the correct drain system. See “Drain” on
page 4-20. Do not make changes to the drain system with a flame
burning.
4-14 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Safety
Flame System Safety
Perchloric Acid
CAUTION Explosion Hazard. Take the measures described below to reduce the
risk of an explosion or a flashback. Aspiration of solutions of
perchloric acid and metal perchlorates into a nitrous oxide supported
flame can increase the risk of an explosion or a flashback.
Consequently, Thermo Fisher Scientific does not recommend using
perchloric acid in sample preparation for nitrous oxide supported
flame analyses.
If the use of perchloric acid is essential, you minimize the hazards if you:
• Ensure that the burner is kept clean, and do not allow deposits to
accumulate around the slot.
• Thoroughly flush the spray chamber, and empty and refill the drain
trap with clean water at the end of the analysis.
• Ensure that the burner is kept clean, and do not allow deposits to
accumulate around the slot.
• Reduce the metal concentrations as much as possible before
aspirating the solutions.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-15
Safety
Flame System Safety
• Thoroughly flush the spray chamber, and empty and refill the drain
trap with clean water at the end of the analysis.
Organic Solvents
Do not store organic or volatile solvents near the instrument, not even
for a short time.
• Make sure that the solvent you wish to use has suitable
characteristics.
- Avoid halogenated solvents as these may create toxic fumes.
- Avoid solvents with low flash points as they have a potential
explosive risk.
- Avoid solvents with low specific gravity (generally lower than
0.75) as they may breach the seals within the nebulizer and
sample chamber.
- Avoid unsaturated hydrocarbons, such as xylene and toluene, as
these have poor burning characteristics.
• Ensure that any aqueous solution in the drain trap is removed and
replaced with organic solvent before starting the analysis.
• Ensure that the organic solvent is removed from the drain trap and
replaced with clean water as soon as the analysis is finished.
If you use organic samples, the waste bottle must be marked with a
Biohazard symbol. See margin.
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Safety
Flame System Safety
Use gloves that are resistant to organic solvents when handling the waste
bottle.
Gases
Follow the local safety guidelines provided by local standards and
regulation of authorities. Ensure that all gas lines, fittings, etc., are free
from oil or grease contamination. Check regularly for leaks in all gas
lines and fittings.
Fit gas cylinders with appropriate pressure reducing regulators. See “Gas
Connections” on page 5-17 for the respective pressures. A flashback
arrestor must be fitted to pressure regulator outlets.
Acetylene
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-17
Safety
Flame System Safety
The following materials must not be used for parts that will come into
contact with the gas:
Nitrous Oxide
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Safety
Flame System Safety
CAUTION Burn Hazard. Keep a safety distance to the flame and do not lean over
the chimney to avoid severe burns.
Do not adjust the burner or impact bead position with a nitrous oxide
supported flame burning.
Fume Extraction
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-19
Safety
Flame System Safety
Ensure that your laboratory is properly vented and that fresh air for
the exhaust is continuously provided.
CAUTION Burn Hazard. With the flame running (and for some minutes after it
is turned off ), the metal fume extraction chimney might reach elevated
temperatures. Take sensible precautions to avoid touching it.
Drain
The position and routing of the internal spectrometer drain tube and
liquid trap are critical to the safe operation of the flame system. They
must not be modified in any way.
The spray chamber drain contains a ball valve sealing device, which
must not be modified, removed or re-sited.
Turn off the flame before any adjustment works on the drain system.
The drain tubing and waste vessel must be arranged properly prior to
flame ignition in order to guarantee a safe operation.
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Safety
Flame System Safety
The lower end of the drain extension must always be above the level of
the liquid in the drain vessel/waste container! Do not use a glass or
metal drain vessel. The drain extension tube must provide a vertical
free-flowing drain outlet to prevent formation of any additional
U-traps, and must be free of kinks, obstructions and sharp bends.
Once out of the instrument, it must be oriented straight down in a
vertical position.
Empty and clean the waste container regularly. If you have used an
organic solvent, do not let the solvent accumulate in the waste container,
as vapor might cause a fire hazard.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-21
Safety
Flame System Safety
Risk Assessment
2. Ensure that any aqueous solution in the drain trap is removed and
replaced with organic solvent before starting the analysis.
3. Ensure that the organic solvent is removed from the drain trap and
the vicinity of the instrument, as soon as the analysis is finished.
4. Ensure that the drain vessel is resistant to the solvent being used, and
is suitably vented to prevent build-up of vapor inside the vessel.
Empty the drain vessel frequently to minimize the quantity of
solvent in the vicinity of the spectrometer.
6. Ensure that the nebulizer, spray chamber and burner are clean and
leak free.
7. Ensure that the gas supplies are set to the correct operating pressures
(as listed in the Operating Manual), that the pressure regulators are
operating properly and that the gas connections are leak free.
CAUTION Many common laboratory solvents are unsuitable for use with flame
AAS. Halogenated solvents (chloroform, Freons) produce large
quantities of toxic gases when burned. Solvents with low flash points
(ethers, light petroleum spirit) present too great a flammability hazard
to be safely used, and unsaturated aromatic hydrocarbons (toluene,
xylene) do not have suitable burning characteristics.
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Safety
Flame System Safety
Drain Vessel
• The neck of the drain vessel is wide relative to the body of the vessel,
so that waste solvent can enter freely and vapors can disperse easily.
CAUTION Hot Surface. During normal operation, the temperature of the slotted
tube is in excess of 1000 °C. Ensure that the tube and its holder have
cooled for at least 15 minutes before handling them.
Do not use nitrous oxide supported flames with this accessory because
this can impede flame safety and result in a flashback.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-23
Safety
Furnace Safety
Flame Atomizer
CAUTION Fire Hazard. Do not leave solvent in the spray chamber when you do
not use the instrument. Solvent vapor can accumulate in and around
the spectrometer, creating a fire hazard and potentially damaging
plastic and other components.
Furnace Safety
CAUTION Risk of Eye Injury. The intense light emitted by a heated graphite
cuvette can harm your eyes. Although you are protected from direct
glare in normal operation, light escapes from the injection port and
the furnace head windows. Do not operate the furnace at high
temperatures unless it is in the normal operating position in the
sample compartment.
CAUTION Hot Surface. The furnace head is water cooled. All components return
to ambient temperature within about a minute from the end of the
furnace cycle. Nevertheless, ensure that the heating cycle has ended,
and that all components have cooled before handling or opening the
furnace head.
NOTICE If a cuvette fails in use, it may break up into small pieces inside the
furnace head. Remove any debris that could cause a short circuit and
consequent damage to the head. Clean the temperature control system
window and the lens before fitting a new cuvette.
NOTICE The magnet fitted to the GFS35Z Zeeman furnace head produces a
variable magnetic field up to 0.85 Tesla at mains frequency during the
atomization and autozero phases. This can affect other electronic
systems in the vicinity.
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Safety
Furnace Safety
CAUTION Heavy Load. The magnet and head assembly is heavy. Take care if you
have to lift or move the assembly. Ensure that it is securely attached to
the spectrometer before use
CAUTION Danger of Bruises. When tilting the GFS35Z on the tilt mount,
avoid trapping your fingers in the moving mechanism.
Fume Extraction
CAUTION Hazardous Fumes. Hot, potentially toxic and corrosive fumes derived
from the sample are vented above the furnace head and must be
removed by a suitable fume extraction system.
Fire the furnace only when the furnace head is securely attached to the
spectrometer, it is not tilted, and there is suitable extraction.
Gases
CAUTION Toxic Gases. Risk of intoxication. Fungicides and biocides are toxic.
Follow laboratory safety rules and manufacturers’ instructions for
handling. Refer also to the Material Safety Data Sheets (MSDSs).
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-25
Safety
Furnace Safety
• Ensure that any aqueous solution in the wash and waste bottle is
removed and replaced with organic solvent before starting the
analysis.
• Ensure that the organic solvent is removed from the wash and waste
bottle and from the vicinity of the instrument as soon as the analysis
is finished.
• Ensure that the gas supplies are set to the correct operating pressures
as listed in this manual, that the pressure regulators are operating
properly and that the gas connections are leak free.
CAUTION Many common laboratory solvents are unsuitable for use in the
graphite furnace. Halogenated solvents (chloroform, Freons) produce
toxic gases. Solvents with low flash points (ethers, light petroleum
spirit) present too great a flammability hazard to be safely used.
Unsaturated aromatic hydrocarbons (toluene, xylene) are unsuitable.
4-26 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Safety
Vapor Safety
Vapor Safety
The gaseous products of the hydride reaction used in Vapor AAS are
combustible and may be toxic. Ensure tat your fume extraction system is
working correctly before you use the technique. All gas and liquid
connections are secure and leak free.
Reagents
CAUTION Sample solutions and reagents used in Vapor AAS are corrosive and
may be toxic. Ensure that you take all necessary precautions when you
handle these materials.
CAUTION Hot Surface. Flame heated atomization cells can reach temperatures
in excess of 1100° C during use. Do not handle the cell or the cell
holder until they have cooled for at least 15 minutes after the flame has
been extinguished.
NOTICE Do not use a nitrous oxide supported flame to heat the atomization
cell.
CAUTION Do not mix the waste from vapor analysis with waste from other
analyses.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-27
Safety
Vapor Safety
CAUTION Hot Surface. Risk of Burns. The electrically heated atomization cell
can reach temperatures in excess of 1100° C during use. Do not open
the furnace or handle the cell for at least 15 minutes after the power to
the furnace has been switched off.
Open the furnace head using the insulated furnace handles only.
Remove the T-cell with great care, handling only the end of the silica
inlet tube or Tygon™ hydride tubing. The T-cell wide body might still
be hot.
T
4-28 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Safety
In Case of Emergency
In Case of Emergency
The power plug must be accessible easily and at all times to quickly
separate the instrument from the mains in case of emergency.
WARNING Electric Current. Electric shock hazard. Do not use the electronics
service switch to shut down the instrument. The electric components
of the vacuum system will be still connected to the electric power
supply and the pumps will be running.
1. Press the Flame Off push button at the left hand side of the flame
compartment to shut off the flame.
2. Switch off the instrument at the power switch, see Figure 4-2. All
power to the instrument is switched off.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-29
Safety
Residual Hazards
Residual Hazards
Users of the iCE 3000 Series atomic absorption spectrometer must pay
attention to the following residual hazards.
Gases
CAUTION Toxic Gases. Risk of intoxication. Fungicides and biocides are toxic.
Follow laboratory safety rules and manufacturers instructions for
handling. Refer also to the Material Safety Data Sheets.
Waste
4-30 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Safety
Residual Hazards
This manual can only give general suggestions for personal protective
equipment (PPE), which protects the wearer from hazardous substances.
Refer to the Material Safety Data Sheets (MSDSs) of the chemicals
handled in your laboratory for advice on specific hazards or additional
equipment.
Eye Protection
The type of eye protection required depends on the hazard. For most
situations, safety glasses with side shields are adequate. Where there is a
risk of splashing chemicals, goggles are required.
Protective Clothing
When the possibility of chemical contamination exists, protective
clothing that resists physical and chemical hazards should be worn over
street clothes. Lab coats are appropriate for small chemical splashes and
solids contamination, while plastic or rubber aprons are best for
protection from corrosive or irritating liquids.
Gloves
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-31
Safety
Residual Hazards
4-32 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
5
Installation
Contents
To be sure that your laboratory is ready for installation of the system, all
requirements specified in the iCE 3000 Series Pre-Installation
Requirements Guide must be met. This guide also provides
comprehensive information to assist in planning and preparing your lab
site.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-1
Installation
Laboratory Conditions
Laboratory Conditions
Power Supply
Spectrometer
Furnace
The furnace power supply unit will require a single phase mains supply
of 200/210/220/230 or 240 VAC, 7.2 kVA, 50/60 Hz (see red label on
furnace power supply for individual voltage setting). In normal
operation, the furnace power supply may draw surge currents in excess
of the nominal rating. A dedicated supply should be used which may
require the inclusion of delayed action protection devices such as circuit
breakers or motor start fuses.
Others
NOTICE For operation of the furnace, both power supply units must be
connected to line power.
5-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Laboratory Conditions
Laboratory Temperature
The laboratory room temperature must be maintained between 10 and
40 °C (50 and 104 °F). The optimum temperature of operation is
between 18 and 21 °C (65 and 70 °F). For best operating conditions,
the temperature should not vary more than ±2 °C per hour.
Humidity
The relative humidity of the operating environment must be between
20 and 80% m/v for an ambient temperature between 10 and 30 °C and
20 and 60% m/v for an ambient temperature between 30 and 40 °, with
no condensation and non-corrosive atmosphere.
NOTICE Operating an iCE 3000 Series system at very low humidity might
cause accumulation and discharge of static electricity, which can
shorten the life of electronic components. Operating the system at
high humidity might cause condensation, oxidation, and shorten
circuits, and will also block the filters on the cooling fans.
Fume Extraction
Smoke and fumes from the sample decomposition must be extracted
away from the vicinity of the instrument.
• The hood of the extraction system over the flame must have a
circular cross section of at least 250 mm (10 in), the tubing at least
150 mm (6 in).
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-3
Installation
Laboratory Conditions
• The hood and the first meters of the duct become hot, especially
when working with a nitrous oxide flame. Thermo Fisher Scientific
recommends marking the hood over the spectrometer with a hot
surface marking.
• A flow rate of at least 2800 L/min (100 ft3/min) through the duct
over the flame must be ensured.
Additional Considerations
• The minimum flow rate through the ducting over the flame must be
ensured. This is important especially for installations, where
multiple tubes end up into a single fan.
• The hood over the furnace must extract at least 200 L/min.
5-4 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Laboratory Conditions
• Suitable extraction must also be used for the EC100 if used instead
of a flame, and in particular for the Mercury-Cell (toxic fumes) used
with no flame or EC100.
NOTICE The minimum flow rate is a requirement for safe operation of the
flame. There is no value added to the safety of operation or the quality
of the analysis when increasing the flow to values beyond the specified
minimum.
The upper limit of the flow rate may be determined by the point at
which the signal is negatively impacted. In particular, an unnecessarily
high flow rate may cause the flame to flicker and/or to decrease the
stability of the analytical data which will be reflected in higher relative
standard deviations.
WARNING Hot Surface. Risk of burning. Do not touch the hood or the tubing
over the flame of the spectrometer while the flame is on or directly
after extinction of the flame.
Air
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-5
Installation
Installation of the Spectrometer
6 3
5 4
Labeled Components: 1=spectrometer connection panel, 2=lamp compartment, 3=left hand sample compartment,
4=flame off button, 5=ignition ready/flame ignite, 6=gas connection panel
Figure 5-1. iCE 3000 Series spectrometer - front/side view
Table 5-1 shows the dimensions and weights of the iCE 3000 Series
spectrometers.
5-6 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of the Spectrometer
• Installation
For instructions about installing the data station, refer to the iCE
3000 Series AA Spectrometers SOLAAR Software Manual.
You may connect a suitable printer to the data station. Any printer
that is supported by your Data Station operating system may be
used. Printer installation procedures are described in the iCE 3000
Series AA Spectrometers SOLAAR Software Manual.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-7
Installation
Installation of a Hollow Cathode Lamp
4. Confirm from the software Lamp Status display that the power to
the lamp position is off.
5. Open the lamp carousel door. Figure 5-2 shows the lamp
compartment.
7. Install the lamp by pushing it firmly into the socket, so that it is held
in place by the lamp clip.
8. Confirm that the software lamp status displays are updated correctly.
5-8 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of a Hollow Cathode Lamp
3. Use the software commands to rotate the carousel to bring the lamp
to the front.
NOTICE If, and only if, the spectrometer is not turned on, you can carefully
rotate the carousel by hand.
4. Confirm from the software Lamp Status display that the power to
the lamp is off.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-9
Installation
Universal Mount in Right Hand Side Compartment
1. Tilt the graphite furnace forward on the tilt mount or remove the
graphite furnace on its fixed mount.
3. Use the supplied tool to push the spring retainer into the location
plate.
1. Ensure that the right hand sample compartment optical path is clear
of obstruction.
3. Use the system control software to set up the optical system in the
right hand sample compartment.
4. Use the system control software to display the live absorbance signal
from the right hand sample compartment.
7. Use a piece of white card to locate the optical beam in the sample
compartment.
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Installation
Universal Mount in Right Hand Side Compartment
1 2
4 3
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-11
Installation
Fitting the Left Hand Sample Compartment Universal Mount
4. Engage the support brackets with the accessory support bar at the
front of the sample compartment.
5. Tilt the mount towards the rear of the sample compartment, until
the rear adjustment screw rests securely against the rear wall.
1. Ensure that the left hand and right hand sample compartments
optical paths are clear of obstruction.
The right hand sample compartment is used for the reference beam.
4. Use the software to display the live absorbance signal from the left
hand sample compartment.
5. Fit the accessory mount and accessory assembly into the operating
position.
7. Use a piece of white card to locate the optical beam in the sample
compartment.
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Installation
Fitting the Left Hand Sample Compartment Universal Mount
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-13
Installation
Installation of the iSQ Module
1. Fasten the iSQ Module to the support bracket using the two
supplied screws.
3. Connect one end of the 9-way data lead to the data socket on the
iSQ Module.
5. Fit the round plug from the power supply in the power socket on
the iSQ Module.
4 3
5-14 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of the iSQ Module
If the furnace head is fitted on a tilt mount, tilt the furnace head
forward out of the sample compartment.
2. Fit the accessory mount and iSQ Module assembly in the relevant
compartment.
3. Connect the free end of the data lead to a free accessory port on the
spectrometer connection panel.
4. Connect the mains lead to a suitable power outlet.
5. Switch on the spectrometer and then the iSQ Module power supply.
During a normal start, the red LED 3 on the iSQ Module flashes
whereas LEDs 1 and 2 are extinguished.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-15
Installation
Installation of the iSQ Module
NOTICE Ensure that an optical setup has been successfully carried out before
the installation of the iSQ Module.
❖ To align the iSQ Module and carry out the iSQ tests
6. Follow the instructions on screen until you reach the Install and
Align Lamps page.
When the optical setup has been completed successfully, re-fit the
assembly and proceed with the alignment procedure.
10. Continue to follow the wizard instructions to complete the iSQ tests
sequence.
5-16 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Flame System
Flame System
Before setting up the flame system, read and understand the section
“Flame System Safety” on page 4-12.
Before you use the flame system, see “Maintenance of the Flame System”
on page 7-9.
NOTICE The gas pressures on the gas box are maximum pressures.
CAUTION Explosive Gas. Do not use oxygen as a support gas. There is a high
risk for explosion damage to the instrument and users. Only use air as
specified in the iCE 3000 Series Pre-Installation Requirements Guide.
Gas Connections
Before you disconnect any gases from the spectrometer, ensure that the
gas supply is shut off at the source, and that the gas lines are vented.
After connecting the gas supplies to the spectrometer, carry out a gas
leak test as described at “Gas Leak Test” on page 7-16 and rectify any
leaks before using the instrument. Carry out gas leak tests at regular
intervals thereafter.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-17
Installation
Flame System
Air/Acetylene Flame
1. Connect the air supply to the connector marked Air using the clear
hose supplied.
1. Connect the air supply to the connector marked Air using the clear
hose supplied.
Installation of Burner
❖ To install a burner
5-18 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Flame System
3. Fit the burner to the spray chamber stem. Push firmly home.
4. Fit the burner plug to the burner socket located on the lower left
panel of the sample compartment.
❖ To remove a burner
1. Ensure that the flame has been extinguished and that the burner has
cooled sufficiently to be safely handled.
3. Lift the burner from the spray chamber stem using the heat resistant
handle.
CAUTION Do not separate the burner from the plastic base when it is fitted to the
spray chamber.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-19
Installation
Flame System
6. Connect the clear air hose from the outlet of the filter/regulator unit
to the spectrometer air inlet connector.
3. Mount the sample probe assembly, install the sample probe and set
the Z axis travel as described in the user documentation of the
autosampler.
1. Connect the 9-9 way RS-232C interface cable supplied between one
of the accessory connections on the spectrometer and the COM 1
RS-232C socket on the rear of the unit.
5-20 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Flame System
serial port
NOTICE If you decided to use the 0.8 mm ID uptake tube supplied, you find a
short length of 0.5 mm ID tube attached to the free end of the tube.
This is necessary to allow the larger tube to fit securely on to the
nebulizer capillary. Remove the section of 0.5 mm ID tube before
cutting the main tube to length. Then refit it after cutting
1. Assemble the sample racks required. Place them in the sample tray.
All the sample racks must be of the same type.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-21
Installation
Flame System
Figure 5-7 shows the CETAC ASX-560 sample changer in front view.
2
1
4 3
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Installation
Flame System
1 1
2
1 2
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-23
Installation
Flame System
2. Connect a suitable power lead between the power inlet socket and a
power outlet.
4. Nebulizer tubing
6. Diluent tubing
Manual Sampling
CETAC Autosampler
Either fit a spare gray miniature 10/32 connector to the free end of the
CETAC sample probe tube, and fit that to Port A of the autodiluter, or
fit a 10/32 connector to a short piece of 0.8 mm ID PTFE tubing, fit
that to Port A of the autodilutor, then attach the CETAC sample probe
tubing to this with a short piece of the thick walled silicone rubber tube
supplied with the autosampler.
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Installation
Flame System
Connectors
Miniature 10/32 compression fittings are used for the autodilutor fluid
connections.
3. Slide the ferrule on to the tubing until part of the taper has passed
through the ferrule.
4. Grip the tapered end of the tubing and pull it through the ferrule, so
that the full width of the tubing passes through the ferrule.
5. Trim the tapered end from the tubing, leaving 0.5-1 mm of the
tubing visible at the end of the ferrule.
6. Bring the nut up to the ferrule and fit the assembly into the port.
2. Orientate the burner with the burner handle to the right, and the
ignition electrode to the left.
3. Unclip the strap clip, to allow the securing clips to spread open.
4. Gently push the STAT holder assembly on to the burner until the
securing clips click into the locating holes on the burner.
5. Clip the Strap clip together again to hold the assembly in place.
1. Orientate the STAT tube so that the longer slot is at the bottom.
2. Clip the STAT tube into the STAT holder. See Figure 5-10 and
Figure 5-11.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-25
Installation
Flame System
1. With the burner and the STAT holder fitted to the spectrometer, fit
a STAT tube to the holder.
5. Use a piece of white card at the right hand side of the sample
compartment to locate the light beam.
5-26 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of GFS35 and GFS35Z Furnace System
6. Adjust the burner position until the light beam passes along the axis
of the STAT tube.
The GFS35 furnace can be supplied with either a fixed head mount or
with a tilting head mount.
The tilting head mount allows the furnace head to be tilted forward for
maintenance and cleaning, and to allow other accessories to be fitted.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-27
Installation
Installation of GFS35 and GFS35Z Furnace System
1
2
9
3
7
7
1. Remove the head securing screw and the two valance screws above
the furnace conduit. See Figure 5-12.
2. Carefully lift the head and the mount, together with the conduit
and the valance. Place the assembly safely on the bench in front of
the spectrometer.
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Installation
Installation of GFS35 and GFS35Z Furnace System
Electrical Connections
1. Connect the 9 pin serial port on the furnace power supply unit to
the Accessory port on the spectrometer connection panel, using a
standard RS-232C cable.
The furnace head will have been aligned with the spectrometer optical
system when it was installed. Both types of mounting arrangements have
been designed so that the alignment is not lost when the furnace head is
moved. Furnace head alignment should, therefore, seldom be required.
1. If the tilt mount is fitted, tilt the head out of the sample
compartment. It is helpful to remove the furnace head windows,
although this is not essential.
NOTICE Ensure that you do not select any form of background correction.
5. Set up the system software to display the live absorbance signal from
the right hand sample compartment. Confirm that the display
shows zero. Use the auto-zero command if necessary.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-29
Installation
Installation of GFS35 and GFS35Z Furnace System
1 3
5
7
If you have removed the furnace head windows, you should be able
to position the furnace head so that it does not absorb any radiation,
that is the displayed absorbance remains at zero.
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Installation
Installation of the GFS33 Graphite Furnace System
2. Loosen the securing screw to release the assembly from the rear wall
of the sample compartment.
3. Raise the whole assembly until it is free of the accessory support bar.
4. Move the assembly towards you and to the left until it is clear of the
spectrometer. Park it between the spectrometer and furnace power
supply.
4. Move the GFS33 assembly towards you and to the right. Lift it
slightly so that you can position it on the accessory support bar.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-31
Installation
Installation of the GFS33 Graphite Furnace System
6. Confirm that the display shows zero. Use the auto-zero command if
necessary.
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Installation
Installation of the GFS33 Graphite Furnace System
You need the long 8 mm ball-ended hex key supplied with your
furnace system to adjust the vertical position controls. Insert the tip
of the tool in the access port, and push it gently downwards until it
engages with the head of the adjuster screw.
If you have removed the furnace head windows, you should be able
to position the furnace head so that it does not absorb any radiation,
that is the displayed absorbance remains at zero.
1. Ensure that the graphite furnace is correctly aligned before you align
the capillary tip.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-33
Installation
Installation of the GFS33 Graphite Furnace System
NOTICE Do not move the arm horizontally by hand. This may damage the
mechanism
4. Adjust the position of the tip until it enters the cuvette cleanly,
without touching the sides of the injection hole:
5. Use a dentists mirror or the GFTV image to view the capillary tip
inside the cuvette.
7. Use the height adjustment control to set the depth of the capillary
tip so that the tip is approximately 1 mm clear of the bottom of the
cuvette. See Figure 5-15.
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Installation
Installation of the GFS33 Graphite Furnace System
The GFS33, GFS35 and GFS35Z furnace heads accept all types of
cuvettes supplied by Thermo Fisher Scientific for use in these heads. Do
not use cuvettes from any other source, nor those not specifically
designed for these furnace heads.
❖ To fit a cuvette
NOTICE If the cuvette has failed in use, there may be soot and debris inside the
furnace head. Remove any debris, and clean the interior of the head as
described at “Maintenance of the Furnace System” on page 7-19
before fitting the new cuvette
3. Take the new cuvette, and side orientate it so that the injection hole
is pointing upwards.
4. Position the cuvette fully in the furnace head. Carefully close the
clamping lever.
6. Zero the cuvette life counter. Ensure that you set the correct cuvette
type on the Furnace Parameters page of the system software before
attempting to use the cuvette.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-35
Installation
Installation of the GFS33 Graphite Furnace System
2. Lift the GFS autosampler. Insert the supporting arms into the holes
on the right of the sample compartment.
3. Push the autosampler body home until the arms secure into place.
1. Ensure that both the wash and the waste containers are fitted to the
autosampler.
2. Grasp the body of the autosampler firmly. Pull it towards you until
the supporting arms come free from the spectrometer.
Gas Connection
2. Fit the quick release connector on the free end of the tube to the
autosampler gas port on the furnace power supply connection panel.
Electrical Connection
The autosampler power and control signals are generated by the furnace
power supply unit.
2. Fit the free end of the cable to the autosampler socket on the furnace
power supply connection panel.
Drain Assembly
The GFS autosampler is fitted with a waste container to collect the used
wash liquid. The waste container can be replaced by a permanent
connection to a suitable drain, if required.
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Installation
Installation of the GFS33 Graphite Furnace System
2. Locate the waste tube that discharges into the waste container.
NOTICE The liquid must be able to run freely down the drain tube, which
must not contain kinks or liquid traps.
Carousel Cover
The carousel cover protects your sample solution from airborne dust
and prevents contamination. It also reduces evaporation of the sample
solutions. In some ambient conditions, condensation can form on the
lower surface of the cover, which can contaminate the samples.
You can fit small feet to the carousel cover to reduce the condensation
on the under surface, although this increases the sample evaporation
rate. Thermo Fisher Scientific recommends fitting these feet to avoid
problems with condensation.
feet
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-37
Installation
Installation of VP100 Continuous Flow Vapor System
• Power supply: connect the unit to a suitable mains supply via the
main cable supplied.
• Gas supply: using the black nylon tubing supplied, connect a supply
of argon or nitrogen, regulated to a pressure of 0.34 bar (5 psi), to
the gas inlet at the rear of the unit. See Figure 5-17.
CAUTION Do not mix the waste from vapor analysis with waste from other
analyses.
• Main Unit: support the main unit to one side or in front of the
spectrometer, adjacent to the sample compartment that you will be
using. Ensure that you can access the main power switch on the
right hand side of the unit.
Best results will be obtained when the distance between the gas
liquid separator and the measurement cell is kept as short as
possible.
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Installation
Installation of VP100 Continuous Flow Vapor System
1 2 3
4
7 6 5
NOTICE Reagents are contained in the reagent containers supported on the rear
of the unit. If it is necessary to move the unit, ensure that the reagent
containers are empty, or that they are removed to prevent spillages,
before you move the unit.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-39
Installation
Installation of VP100 Continuous Flow Vapor System
1. Locate the thick-walled silicone tubing supplied, and cut off a piece
15-20 mm long. See Figure 5-18.
1 2
2. Grip the sample uptake tube firmly and push it into one end of the
silicone tubing, until 10 mm is inside the silicone tubing.
Use a small piece of abrasive paper to grasp the sample uptake tube
more firmly.
3. Push the free end of the silicone tubing over the green push-on
connector on the VP100 front panel.
Pump Tubing
The VP100 is fitted with a four channel peristaltic pump. The channels
are identified by the color-coded connectors on the pump tube
connection panel of the unit. See Table 5-6 and Figure 5-19.
5-40 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of VP100 Continuous Flow Vapor System
• The black (drain) channel must be fitted with pump tubing with
black/white bridges. That is, a single piece of pump tubing has a
black bridge fitted at one end, and white bridge fitted at the other
end. This tubing has an ID of 3.17 mm and an OD of 4.85 mm.
• The green (sample) channel must be fitted with pump tubing with
two green bridges. This tubing has an ID of 1.85 mm and an OD
of 3.53 mm.
• The blue (acid reagent) channel must be fitted with pump tubing
with yellow/orange bridges. This tubing has an ID of 0.5 mm and
an OD of 2.33 mm.
1
2 3
7
10
9 8
The internal diameters of the pump tubing with the black bridges and
the pump tubing with the yellow/orange bridges are too small to allow
the pump tubing to be attached directly to the connectors on the VP100
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-41
Installation
Installation of VP100 Continuous Flow Vapor System
A disposable pipette tip is ideal for this, but any other object with a
tapering point can be used.
2. Take the pump tubing and insert 3-5 mm inside the expanded
Tygon tubing.
Lubricate the tubes with a drop of water, if necessary. You can use a
small piece of abrasive paper to grasp the tube securely.
1. Fit the pump tubes from the rear of the connection panel towards
the front, in the following order:
5-42 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of VP100 Continuous Flow Vapor System
4. Take the pump tubing and feed it around the pump rollers.
5. Stretch the pump tubing slightly and fit the bridges under the bridge
retaining pillars.
6. Push the ends of the tubing over the appropriate push on connectors
on the VP100 connection panel.
10. Adjust the pressure screw to release the pressure on the tubing.
3. Place the reagent uptake tubes and the sample uptake tube in a
container of clean water.
4. Ensure that the drain tube discharges to a suitable low level drain or
drain vessel.
5. Ensure that the clamp arms are correctly positioned and that the
plunger arm pressure screws have been fully released.
6. Use the system software to set up a Vapor method using the VP100.
10. Tighten the pressure screws in each plunger arm in turn until each
channel starts to pump.
NOTICE Do not overtighten the pressure screw. This would shorten the life of
the pump tubing and may damage the pump mechanism.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-43
Installation
Installation of VP100 Continuous Flow Vapor System
The flow rate in the drain channel is significantly greater than the total
flow rate of the three other channels. In normal operation, bubbles are
present from the evolved reactant gases in the pumped fluid in the drain
channel.
The flow rates in the acid and reductant channels are low so that it takes
a short time before the fluid reaches the pump. Do not set the final
pressure on the tube until the fluid has filled the pump tubing.
These parts are supplied with the VP100. They must be fitted before the
accessory is used.
1. Unscrew the top cap of the gas liquid separator. See Figure 5-21.
5-44 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of VP100 Continuous Flow Vapor System
Prevent the glass beads from falling into the drain where they may
cause blockage.
4. Carefully re-fit the O-ring seal and the top cap, ensuring that the
position of the membrane is not disturbed.
NOTICE The STAT holder and T-cell holder are the same device. If you have
already fitted a STAT holder to your burner, it also supports the T-cell.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-45
Installation
Installation of VP100 Continuous Flow Vapor System
2. Orientate the burner with the burner handle to the right and the
ignition electrode to the left.
3 2
3. Unclip the strap clip on the T-cell holder. Spread the securing clips
slightly.
4. Gently push the T-cell holder assembly on to the burner until the
securing clips click into the locating holes on the burner. See
Figure 5-23.
5. Re-clip the strap clip together to secure the holder to the burner.
1. Fit the burner, the T-cell holder and the T-cell assembly to the spray
chamber stem.
2. Move the cell holder so that the T-cell is in the Parked position,
away from the burner slot.
5. Move the cell holder so that the T-cell is in the Operating position
over the burner slot.
6. Use a piece of white card at the right hand side of the sample
compartment to locate the light beam.
5-46 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of VP100 Continuous Flow Vapor System
7. Adjust the burner position until the light beam passes along the axis
of the T-cell.
NOTICE It is possible to fit the mercury absorption cell to the standard T-cell
holder. Thermo Fisher Scientific does not recommend this, because it
is then possible to light a flame that destroys the mercury cell.
4. Fit the mercury absorption cell into the cell clips of the cell mount.
See Figure 5-24.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-47
Installation
Installation of VP100 Continuous Flow Vapor System
The T-cell or mercury absorption cell must be connected to the exit port
at the top of the gas liquid separator of the VP100.
1. Cut a suitable length, each for the sample inlet and the exhaust
outlet, of the 8 mm OD Tygon tubing provided.
Use the shortest possible length of tubing for the sample inlet and
sufficiently long tubing for the exhaust outlet. See Figure 5-24.
If you are using the left hand (Flame) sample compartment, feed the
tubing through the aperture in the sample compartment door, so
that you can perform your measurements with the door closed.
CAUTION Hazardous Chemical. Mercury vapors are highly toxic. Make sure
that you have appropriate extraction in place.
2. Connect the tubing between the top cap connection on the gas
liquid separator and the inlet of the T-cell or mercury absorption
cell.
Loosely plug the other arm of the mercury absorption cell with a
small piece of cotton wool to prevent the ingress of dust. This
increases the sensitivity, but also increases the washout time.
5-48 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of VP100 Continuous Flow Vapor System
3. Connect the sample tubing to one of the open ports (as inlet) of the
mercury absorption cell. This tubing leads to the exit port at the top
of the gas liquid separator. See Figure 5-24.
4. Connect the exhaust tubing to the other port (as outlet). Attach it
appropriately to the exhaust system. See Figure 5-24.
NOTICE The sample and exhaust tubing must not interfere with the light path.
4. Perform an autozero.
2. Confirm that the voltage selector on the rear panel matches your
mains voltage.
1. Fit the furnace head, Figure 5-25, to the appropriate mount using
the two securing screws on the base of the furnace.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-49
Installation
Installation of VP100 Continuous Flow Vapor System
Ensure that the power cable is fed through the hole in the left hand
universal mount to emerge from the front of the instrument.
1 2
3
6
4
2. Locate the pink sensor lead. Connect it to the pink sensor plug on
the furnace head.
4. Connect the power cable from the furnace head to the head socket
on the back of the power supply:
c. To disconnect the plug from the socket, pull the metal locking
piece towards the cable to release the lock.
5. Fit the sensor lead to the sensor socket on the back of the power
supply.
6. Loosen the furnace head closure knobs, and open the furnace head.
5-50 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of VP100 Continuous Flow Vapor System
10. Connect the T-cell to the gas liquid separator outlet connector of the
VP100.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-51
Installation
Installation of VP100 Continuous Flow Vapor System
5-52 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
6
Operation
This chapter outlines the basic system operations and checks before
operation.
Contents
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-1
Operation
Operation of AA Systems
Operation of AA Systems
NOTICE When the system starts without error, a pattern moves across the LEDs
for a second, and stops with the Standby LED flashing rapidly (about
five times a second) and all other LEDs off. Any other pattern denotes
a failure. See “Spectrometer Status Indicators” on page 7-2
STANDBY
FC1
GFTV
FC2
FC3
HALT
PRINTER
6-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of AA Systems
Lamp Types
Thermo Fisher Scientific does not guarantee that the instrument will
work, nor that the published specification will be met when using third
party lamps that are 37 mm in diameter. 50 mm lamps cannot be fitted
in the carousel.
NOTICE Certain older types of HCL are fitted with four base pins. Do not use
these lamps with your iCE 3000 Series spectrometer. They may cause
severe damage to the instrument.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-3
Operation
Alignment and Operation of the iSQ Module
NOTICE Ensure that an optical setup has been successfully carried out before
the installation of the iSQ Module.
❖ To align the iSQ Module and carry out the iSQ tests
6. Follow the instructions on screen until you reach the Install and
Align Lamps page.
When the optical setup has been completed successfully, re-fit the
assembly and proceed with the alignment procedure.
10. Continue to follow the wizard instructions to complete the iSQ tests
sequence.
6-4 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of Flame System
Safety
Read and understand the flame safety sections in this manual. See
“Flame System Safety” on page 4-12.
Before you use the flame system, see “Maintenance of the Flame
System” on page 7-9.
• Check that the spray chamber drain is clear and that it discharges
freely into a suitable receptacle.
• Perform a gas leak test when the instrument has been moved or
rebuilt. See “Gas Leak Test” on page 7-16.
Organic Solvents
If you are certain that the solvent is safe to be used for Flame Atomic
Absorption measurements, check the following before lighting the
flame:
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-5
Operation
Operation of Flame System
You will normally use the Auxiliary Oxidant feature and adjust the fuel
gas flow rate to obtain the correct flame chemistry for your analysis.
These commands are on the Flame page of the system software. If your
instrument is fitted with a Variable Flow Auxiliary Oxidant Kit, see
“Auxiliary Oxidant” on page 3-13.
When you have completed your analysis, empty the residual organic
solvent from the drain and replace it with clean water. How to empty
the drain safely is explained at “Maintenance of Drain” on page 7-15.
• Do not change the routing of the drain tube within the flame
compartment from its original way.
• The drain valve must always remain in its original direction and
place for normal operation.
NOTICE Do not leave the drain full of organic solvent when you do not use the
instrument. The solvent vapors may cause damage if they accumulate.
• the required fuel and oxidant gases (for example, air and acetylene)
- are connected to the spectrometer,
- have the correct pressure settings.
6-6 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of Flame System
NOTICE The MFC controlled gas box measures the flows during ignition. The
flashing of the button reflects only the door interlock and burner
present sensor.
NOTICE If you cannot ignite a flame after two attempts, it is likely that
there is a problem with the burner, ignition system, or gas
supplies. See “Maintenance of the Flame System” on page 7-9.
Identify and rectify any problems before you try again to light the
flame.
CAUTION Risk of Electric Shock. High voltages are present between the
ignition electrode and the body of the burner during the ignition
sequence. Do not touch either of these components during the
ignition sequence.
3. Use the system software to adjust the fuel flow rate and the oxidant
gas type as required.
NOTICE Allow the burner to warm up properly before you start measurements,
to ensure that your results are stable, and to minimize carbon
deposition when using a nitrous oxide supported acetylene flame.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-7
Operation
Operation of Flame System
1. Set up a suitable analysis with the system software, ensuring that you
select the Air Acetylene Flame Type, with a fuel gas flow rate
between 0.8 and 1.2 L/min.
6. Allow the flame to burn for ten minutes before starting the analysis.
❖ To warm up the burner for use with a nitrous oxide acetylene flame
5. Confirm that the oxidant gas changeover takes place correctly, and
that the nitrous oxide acetylene flame is burning correctly.
6. Let the flame burn for ten minutes before starting the analysis.
6-8 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of Flame System
The stiffness of this operation can be adjusted with the flame off and
the system allowed to cool down. Open the door, remove the burner
head and adjust the 2 thumbscrews at the top of the spray chamber
bracket.
6. Use the Burner Height controls in the system software to adjust the
height of the burner to maximize the test signal.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-9
Operation
Operation of Flame System
5. Aspirate a suitable test solution that gives a signal between 0.1 and
0.8 absorbance units.
6. Use the Impact Bead control to adjust the position of the impact
bead to maximize the signal from the test solution.
6-10 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of Flame System
1
1
3
4
6 2
5
standard impact bead adjuster micro-adjustable impact bead
Labeled Components: 1=oxidant gas inlet, 2=micro-adjuster, 3=nebulizer, 4=handle, 5=guide pin, 6=impact bead
adjuster
Figure 6-3. Impact bead control types
Do not adjust the impact bead with a nitrous oxide supported flame
burning.
NOTICE Do not adjust the impact bead position too far towards the nebulizer
as it might damage either the nebulizer or the surface of the impact
bead.
After about 10 seconds, you hear a click, and the gases are vented
through the burner.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-11
Operation
Operation of Flame System
1. Ensure that the drain plug at the base of the filter/regulator unit is
closed and that the system is leak free.
8. After use, switch off the compressor and vent the gas control system.
NOTICE When the air compressor has been switched off, do not switch it on
again until the line pressure has dropped to below 0.14 bar (2 psi).
Otherwise, you might damage the compressor motor.
6-12 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of Flame System
3. Use the Data Station software facilities to define the type and
number of sample racks, and the number of solutions required.
NOTICE The ID100 autodiluter can be used manually or with any of the flame
autosamplers. It is not compatible with the VP100 Vapor Generation
accessory.
2. Turn on and set up the spectrometer and lamps in the normal way.
Light the flame.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-13
Operation
Operation of Flame System
10. If the measured signal drifts during the measurement, increase the
Nebulizer Delay parameter.
11. Set the Wash Time parameter on the Sampling parameters page to
30 seconds. Set the Wash Frequency to Wash between Samples.
12. If you are analyzing samples that are similar to each other in
concentration, you may find that it is not necessary to wash the
autodilutor between samples.
15. During the analysis, ensure that the liquid level in the diluent
container does not fall below the level of the uptake tube.
16. If you are working manually, carefully follow the prompts displayed.
Particularly, always confirm that the sample uptake tube connected
to Port A of the autodilutor is placed in the correct solution before
acknowledging the prompt.
17. When the analysis has finished, replace the sample and diluent with
clean deionized water. Perform 2-5 wash cycles to ensure that all
sample and diluent is flushed from the dilutor.
6-14 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of Flame System
NOTICE If the outlet of the dilutor is blocked, a small amount of liquid may be
ejected from the leak port. If this happens, stop the dilutor
immediately. Investigate and rectify the cause of the problem before
using the dilutor again.
Particulate material present in the samples can cause serious damage to
the ID100 autodilutor. Ensure that your samples do not contain any
particulate material before using them with the ID100 autodilutor.
CAUTION Hot Surface. During normal operation, the temperature of the slotted
tube is in excess of 1000 °C. Ensure that the tube and its holder have
cooled for at least 15 minutes before handling them.
Do not use nitrous oxide supported flames with this accessory because
this can impede flame safety and result in a flashback.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-15
Operation
Operation of Flame System
3. Normally set the Fuel Flow Rate parameter to its minimum value.
6. Use the Flame Setup command in the system software to set your
chosen flame parameters.
8. Slowly open the needle valve until the yellow color disappears from
the flame.
9. Stop aspirating the sample. Confirm that the flame remains stable.
If the flame lifts off the burner, adjust the needle valve to slightly
decrease the auxiliary oxidant flow rate and/or increase the fuel flow
rate to the flame.
11. Make fine adjustments to the auxiliary oxidant flow rate, the fuel gas
flow rate, the burner height and the impact bead position, to obtain
the best signal from your sample.
6-16 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of Flame System
Flame Atomizer
NOTICE Unless the solvent that you are planning to use is freely miscible with
water, remove any aqueous solutions from the spray chamber before
introducing the solvent. Then re-fill the spray chamber with clean
solvent. These procedures are described in “Maintenance of the Flame
System” on page 7-9.
Remove any solvent from the spray chamber drain when you have
finished your analysis. If you intend to use the solvent again when you
use the instrument the next time, you can leave the spray chamber
drain dry. If you intend to use aqueous samples the next time, re-fill
the spray chamber drain with clean water.
CAUTION Fire Hazard. Do not leave solvent in the spray chamber when you do
not use the instrument. Solvent vapor can accumulate in and around
the spectrometer, creating a fire hazard and potentially damaging
plastic and other components.
Always ensure that the burner head has been properly warmed up before
you start any measurements. This gives you the most stable and accurate
results. It also minimizes carbon deposition on and around the burner
slot if you use a nitrous oxide supported flame.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-17
Operation
Operation of Flame System
3. Set the flame type to Air Acetylene, with a Fuel Flow Rate of
1.2 L/min.
c. When the flame has stabilized, reduce the Fuel Flow Rate to
3.8 L/min.
This should result in a lean flame, with a small red zone no more
than 1-2 mm high.
CAUTION Risk of Explosion. If the red zone at the base of flame disappears
entirely, immediately extinguish the flame and check the nitrous
oxide supply pressure. It should not be higher than 40 psi
(2.7 bar).
Flame Optimization
6-18 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of Flame System
If you reach the minimum fuel flow rate (0.8 L/min) before the
flame becomes clear, reduce the uptake of the solvent by changing to
a narrower bore and/or longer length of nebulizer uptake tubing.
3. When you have established the conditions that give you a clean
flame, stop aspirating the solvent. Confirm that the flame does not
lift off the burner.
Slowly and carefully open the auxiliary oxidant flow control needle
valve until the flame becomes clear.
If you open the needle valve too far, the flame may lift off the burner
head and may go out. If this happens, close the valve, re-light the
flame, and open the valve a lesser amount.
You can also adjust the fuel flow rate and the nebulizer uptake rate as
described at “To measure the nebulizer uptake rate” on page 7-15 to
obtain a clean flame while aspirating your solvent, that is also stable
when solvent is not aspirated.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-19
Operation
Operation of Flame System
When the burner has been properly warmed (see “Warming up the
Burner when Using an Organic Solvent” on page 6-17), aspirate the
clean solvent into the flame.
If the bright white color of free carbon appears in the flame, reduce the
fuel flow rate and/or reduce the sample uptake rate as described at “To
measure the nebulizer uptake rate” on page 7-15 to obtain a clean flame.
After you have obtained settings that give you a clean flame while
aspirating clean solvent, perform the final optimization to obtain the
best signals from your samples. You can use the wizards and automatic
flame optimization tools provided in the SOLAAR Data Station
software, or the normal manual procedures, to perform the final
optimization of fuel gas flow and burner height while monitoring the
absorbance signal from your sample.
NOTICE Do not attempt any optimizations that require to open the sample
compartment door while a nitrous oxide flame is burning.
The transverse and rotational burner positions can both be set while
measuring an element that can be atomized in an air supported flame.
They will then also be in the correct positions for measurements in a
nitrous oxide supported flame.
The impact bead has been designed to provide the optimum aerosol
particle size when used with aqueous solvents. When working with
organic solvents, where the density, viscosity and volatility are quite
different from water, the effect of the impact bead cannot be predicted.
6-20 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of the Graphite Furnace System
Investigate the effect of the impact bead position on the signal from
your sample. You may well find that the optimum signal is obtained
with the impact bead moved out of the aerosol path altogether.
NOTICE Do not perform any adjustments of the impact bead with a nitrous
oxide supported flame!
CAUTION Risk of Eye Injury. The intense light emitted by a heated graphite
cuvette can harm your eyes. Although you are protected from direct
glare in normal operation, light escapes from the injection port and
the furnace head windows. Do not operate the furnace at high
temperatures unless it is in the normal operating position in the
sample compartment.
CAUTION Hot Surface. The furnace head is water cooled. All components return
to ambient temperature within about a minute from the end of the
furnace cycle. Nevertheless, ensure that the heating cycle has ended,
and that all components have cooled before handling or opening the
furnace head.
NOTICE If a cuvette fails in use, it may break up into small pieces inside the
furnace head. Remove any debris that could cause a short circuit and
consequent damage to the head. Clean the temperature control system
window and the lens before fitting a new cuvette.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-21
Operation
Operation of the Graphite Furnace System
Graphite Cuvettes
NOTICE • Do not use cuvettes from any other source, nor those not
specifically designed for this furnace head.
❖ To fit a cuvette
3 4
2 5
Furnace window
1
RHS electrode
If the cuvette has failed in use, soot and debris may be inside the
furnace head. Remove any debris and clean the interior of the head
as described at “Maintenance of the GFS33 System” on page 7-27
before fitting the new cuvette.
3. Take the new cuvette and orientate it so that the injection hole is
pointing upwards.
6-22 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of the GFS Autosampler
7. Zero the cuvette life counter. Ensure that you set the correct cuvette
type on the Furnace Parameters page of the system software before
you use the cuvette.
Wash Liquid
A small quantity of the wash liquid is pumped through the internal
plumbing of the unit into the wash reservoir after each injection.
Choose the composition of the wash liquid to efficiently remove traces
of the sample solutions from the capillary. Dilute nitric acid
(approximately 0.1% v/v) is suitable for many aqueous sample types.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-23
Operation
Operation of the GFS Autosampler
Syringe Purge
A command is provided in the system software to purge the syringe to
remove bubbles and contamination before use. Use this command when
the wash reservoir is refilled. See Figure 6-5.
3
1
2 4
6 5
Sample Cups
Three types of sample cups are available for use with the GFS
autosampler:
Reagent cups are provided for use in the six larger reagent positions on
the autosampler carousel. They are Polypropylene cups and hold
approximately 25 mL.
Cup reducing rings are available which allow a normal sample cup to be
used in a reagent position.
6-24 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of the GFS Autosampler
1. Ensure that the graphite furnace is correctly aligned before you align
the capillary tip.
3. Use the Align Probe command in the system software to move the
autosampler arm over the cuvette.
NOTICE Do not move the arm horizontally by hand. This may damage the
mechanism.
4. Adjust the position of the tip until it enters the cuvette cleanly,
without touching the sides of the injection hole.
5. Use a dentists mirror or the GFTV image to view the capillary tip
inside the cuvette.
7. Use the height adjustment control C to set the depth of the capillary
tip so that the tip is approximately 1 mm clear of the bottom of the
cuvette.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-25
Operation
Operation of the GFS Autosampler
10. Check the alignment by selecting the Align Probe command in the
SOLAAR software.
11. You may need to make fine adjustments to the position of the
capillary tip. Repeat if necessary.
6-26 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Vapor Operation
Vapor Operation
Reagents
The optimum composition of the reagents used depends upon the
element being measured and the composition of the sample. The
reagents described below are suitable for the analysis of simple aqueous
solutions.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-27
Operation
Vapor Operation
• Pump speed
Default values for these parameters are provided. If required, you can
edit them in the system software, on the Vapor page of the method.
For each hydride group element, there is an optimum carrier gas flow
rate that gives the maximum sensitivity for that element. For mercury,
the analytical sensitivity increases as the carrier gas flow rate decreases.
Low carrier gas flow rates require longer measurement delays. Higher
carrier gas flow rates allow the use of reagents of shorter measurement
delays, at the expense of some analytical sensitivity, and can be used if
you want to complete the analysis as quickly as possible. Typical default
values are in the range 100-200 mL/min. It is unlikely that flow rates
higher than 300 mL/min are useful.
6-28 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Vapor Operation
• A blank solution
2. Fill the VP100 reagent bottles. Place the reagent uptake tubes into
the correct containers. Place the sample uptake tube into a container
of clean water.
The Vapour Status window updates to show the actual pump speed
and carrier gas flow rate.
9. Wait until the reagents have filled the gas liquid separator mixing
zone.
After 30-60 seconds, the absorbance signal should rise and stabilize.
11. Use the commands on the VP100 submenu to adjust the carrier gas
flow rate and the pump speed to obtain the optimum signal for your
analysis.
As you change the carrier gas flow rate and the pump speed, the
Vapour Status display is updated. The parameter values in the
method are also automatically updated to reflect your changes.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-29
Operation
Vapor Operation
12. When you have obtained the optimum signal for your analysis, place
the uptake tube in the blank solution.
You can use the Running Signal display facility of the Spectrometer
Status window to help you with this. Refer to the Online Help
provided with the Data Station software to learn how to access and
use the Running Signal display.
If you are using an autosampler, you may need to add a few seconds
to the measurement delay that you have measured, to allow for the
longer length of the uptake tube used with the autosampler.
The time period that you have measured is the measurement delay
time that you should set in the Measurement Delay parameter
field on the Vapor page of the method.
Sample Preparation
6-30 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Vapor Operation
3. Prepare the reagents required and place them in the reagent bottles.
9. If you are using a flame heated cell, move the T-cell into the
Operating position and ignite the flame.
If you are using the electrically heated cell, turn on the EC100 and
wait until the furnace temperature has stabilized.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-31
Operation
Vapor Operation
12. Start the VP100. Let it run until the reagents reach the gas liquid
separator and are pumped away through the drain channel.
NOTICE The VP100 does not monitor the amount of reagents in the
reagent bottles, nor detect if the reagents are being pumped into
the gas liquid separator. Especially when working with an
autosampler, periodically check that the reagent bottles have not
been emptied.
While the analysis is running, you can use the Pause button to halt
analysis, if, for example, it is necessary to re-fill the reagent bottles.
You can then use the VP100 Run and Stop commands to ensure
that the reagents have reached the gas liquid separator before using
the Continue button to complete the analysis.
2. Place the reagent and sample uptake tubes in clean water. Run the
VP100 until all the samples and reagents have been flushed from the
tubes, and clean water is being discharged from the drain.
3. Remove the uptake tubes from the water, but allow the VP100 to
run for another few minutes to remove the liquid from the tubes.
4. Stop the VP100. Flip open the plunger arm pressure screws to
release the pressure on the pump tubes.
Wipe up any liquid that might have been spilled on or around the
VP100.
6. Turn off the inert gas supply to the VP100. Turn off the power to
the accessory.
6-32 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Vapor Operation
7. When all the parts have cooled to room temperature, remove the
T-cell and EC100 furnace, if necessary.
If you are using flame heating, the T-cell holder can be left attached
to the burner in the Parked position, where it allows the burner to
be used normally.
CAUTION Hot Surface. Risk of Burns. The electrically heated atomization cell
can reach temperatures in excess of 1100° C during use. Do not open
the furnace or handle the cell for at least 15 minutes after the power to
the furnace has been switched off.
Open the furnace head using the insulated furnace handles only.
Remove the T-cell with great care, handling only the end of the silica
inlet tube or Tygon™ hydride tubing. The T-cell wide body might still
be hot.
2. Turn on the main power switch on the front panel of the power
supply.
3. On the lower (green) display, set the required temperature using the
Up and Down arrow buttons.
4. Ensure that the vapor system carrier gas is flowing through the
atomization cell.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-33
Operation
Vapor Operation
When the red and the green temperature displays are the same, the
furnace head is ready to use.
• Power cable is connected between the furnace head and the back of
the furnace power supply/control box.
6-34 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Vapor Operation
• Power/controller unit has been switched on. See the Mains and Heat
On/Off switches.
• Power trip on the rear panel of the power supply is in the Operating
position.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-35
Operation
Vapor Operation
6-36 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
7
Maintenance
Contents
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-1
Maintenance
Safety Guidelines for Maintenance
Never try to repair or replace any component of the system that is not
described in this manual without the assistance of your Thermo Fisher
Scientific field service engineer.
Only use fuses of the type and current rating specified. Replace fuses
only with same type and rating. Do not use repaired fuses and do not
short-circuit the fuse holder.
7-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
General Advice for Maintenance
- Proceed methodically
- Always wear clean, talc-free, and lint-free gloves when handling
components of the instrument. See “Personal Protective
Equipment” on page 4-31 for a specification for the required
gloves.
- Always place the components on a clean, lint-free surface.
- Do not overtighten a screw or use excessive force.
- Dirty tools can contaminate your system. Keep the tools clean
and use them exclusively for maintenance and service work at
the atomic absorption spectrometer.
- Do not insert a test probe (for example, an oscilloscope probe)
into the sockets of Molex connectors on PCBs.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-3
Maintenance
Inspection- and Servicing Plan
7-4 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Inspection- and Servicing Plan
NOTICE Do not let any liquids come into the inside of the instrument. Leaking
liquids might get into contact with electronic components and cause a
short circuit.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-5
Maintenance
Maintenance of the Spectrometer
To ensure that the instrument operates safely and reliably, carry out
routine maintenance periodically.
NOTICE The covers of the iCE 3000 Series atomic absorption spectrometer are
made of ABS plastic material, which is damaged by strong solvents
and concentrated acids.
• Remove stains and marks on the covers using a soft cloth moistened
with dilute detergent solution.
If the deuterium lamp has reached the end of its useful life, contact a
Thermo Fisher Scientific field service engineer. On the iCE 3000 Series
spectrometer, the deuterium lamp must be replaced by a Thermo Fisher
Scientific field service engineer.
7-6 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Spectrometer
1 2
NOTICE Replace fuses only with same type and rating: 2 × 2.5 AF H 250 V
IEC60127-2, Littelfuse 216 02.5, or equivalent type.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-7
Maintenance
Maintenance of the Spectrometer
❖ To replace a fuse
2. Locate the combined power inlet connector and the fuse holder on
the Power Supply unit.
NOTICE If the new fuse fails immediately, a serious fault in the power supply
exists. Isolate the instrument until it can be rectified by a Thermo
Fisher Scientific field service engineer.
7-8 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Flame System
Turn off all gas supplies and disconnect the spectrometer and
accessories from the mains before you carry out any maintenance
procedures.
CAUTION Hot Surface. Risk of burns. Do not clean the burner while a flame is
burning. Ensure that the burner has cooled before you handle it.
If the burner does not ignite, do not try to obtain a flame by using
whatsoever kind of tools! Instead, check all connections and gas
pressures for correctness (see error messages on the display).
If the burner still does not ignite, align the ignition electrode as
described at “To align the ignition electrode”. See also Figure 7-4.
Turn off all gas supplies and disconnect the spectrometer and
accessories from the mains before you carry out any maintenance
procedures.
1. Clean and polish the top surfaces using a mild abrasive soap cleaner.
2. Clean the burner slot with the burner cleaning tool supplied. Do
not use any abrasive material inside the slot.
3. Wash the burner with detergent solution and rinse with deionized
water. Dry the burner carefully before using it again.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-9
Maintenance
Maintenance of the Flame System
1. While holding the base firmly, twist the burner body anti-clockwise
to release it from the burner retention clip and securing lugs. See
Figure 7-3.
2. Lift the burner head away from the burner base to separate the two
parts.
1
2
6
5
4
NOTICE Do not put the plastic burner base and ignition electrode assembly
into the ultrasonic bath.
2. Orientate the burner head so that the ignition well is on the left
hand side to the rear.
7-10 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Flame System
3. Rotate the burner head about 45° anti-clockwise and push it firmly
into the base.
4. Rotate the burner head clockwise in the base so that the securing
lugs engage, and the burner retention clip snaps into place.
2. Gently bend the electrode until the tip touches the top corner of the
chamfer on the setting jig. See Figure 7-4.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-11
Maintenance
Maintenance of the Flame System
2 3
1
19
standard impact bead adjustment
18
17
16
5
15
14 1
6
13 12 11 10 9 8 7
Labeled Components: 1=o-ring, 2=burner stem, 3=baffle and spider assembly, 4=thumbscrew, 5=nebulizer retaining
clip, 6=sample uptake, 7=impact bead micro-adjuster, 8=nebulizer, 9=oxidant inlet, 10=front cap, 11=alumina disc,
12=o-ring and PTFE seal, 13=impact bead, 14=fuel gas inlet, 15=drain, 16=over-pressure disc, 17=burner mount clamp
screw, 18=bayonet mount, 19=clamp ring
Figure 7-5. Components of spray chamber and nebulizer
7-12 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Flame System
1. Use the system software commands to raise the burner until the
burner height is less than 10 mm.
6. Release the burner mount clamp screw by at least three full turns.
Rotate the spray chamber downwards around the axis of the bayonet
mount to release it and the clamp ring/mounting bracket from the
bayonet mount. Remove the assembly.
7. Unscrew the four thumbscrews and remove the spray chamber front
cap.
8. Unscrew the three rear clamp screws. Remove the clamp ring or
clamp ring/mounting bracket and the over-pressure disc.
9. Push the baffle assembly out of the spray chamber body towards the
front.
10. Undo the fuel gas coupling on the spray chamber body. Remove the
gauze disc assembly.
NOTICE Do not dismantle the cap assembly while the spray chamber is still
in the flame compartment.
1. Slacken the impact bead clamp adjusting screw. Withdraw the bead
from the alumina disc side of the cap.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-13
Maintenance
Maintenance of the Flame System
1. Fit the O-ring to the nebulizer body. Re-fit the nebulizer to the cap.
Replace the clip. Tighten the screw.
2. Lightly lubricate the impact bead stem with silicone grease. Pass it
through the alumina disc and fit one O-ring over the stem.
NOTICE Do not contaminate the bead or the alumina disc with grease.
1. Fit the alumina disc to the cap, passing the impact bead stem
through the hole in the cap.
2. Fit the second O-ring to the stem. Slide the bead adjustment
assembly on to the stem. Secure it to the cap.
4. Position the impact bead so that the bead is centrally located in the
nebulizer nose cone, and is as close as possible to the nose cone.
2. Push the baffle assembly into the front of the spray chamber body,
with the baffle to the rear, and a short baffle blade at the bottom.
Push the assembly tightly into the spray chamber body taper.
3. Re-assemble and re-fit the gauze disc assembly and the fuel inlet
coupling.
4. Re-fit the disc and clamp ring using a new over-pressure disc.
7-14 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Flame System
Maintenance of Nebulizer
Figure 7-5 schematically shows the parts of the spray chamber and the
nebulizer.
NOTICE Do not use any other tool or wire to clean the nebulizer.
4. Aspirate the water from the measuring cylinder. Note the volume
aspirated in 1 minute.
Maintenance of Drain
Periodically check the external drain tube. Replace it if it is cracked or
damaged.
2. Leave it to soak. When the blockage has dissolved, empty the drain
and refill it with clean water.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-15
Maintenance
Maintenance of the Flame System
1. Turn off the fuel and nitrous oxide gas supplies at source, but leave
the air supply turned on.
5. Vent the gas system by pressing Flame Off for at least 30 seconds.
This causes the contents of the drain to be blown out to waste.
6. Refill the drain by pouring clean water or solvent into the top of the
spray chamber stem until it flows freely from the drain.
Run a gas leak test at least once every six months, and when the
instrument is moved. Ensure that no leaks are present. See “Gas Leak
Test” on page 7-16.
The gas leak test wizard can be started from the OQ Test software:
The result of the gas leak test is not stored in the results database
when the wizard is started manually.
7-16 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Flame System
The result of the gas leak test is stored in the database with the
results of the other tests in the sequence when the wizard is started
automatically.
NOTICE When you start the gas leak test (by going on to the second page in the
gas leak test wizard), it automatically disables error checking in the
spectrometer so that you can carry out a gas leak test. When it finishes,
it automatically enables error checking in the spectrometer for normal
use.
1. Inspect the filter trap regularly and drain out any liquid collected.
2. Rinse filter bowl with paraffin if necessary. Do not use any other
solvent.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-17
Maintenance
Maintenance of the Flame System
CAUTION Hot Surface. During normal operation, the temperature of the slotted
tube is in excess of 1000 °C. Ensure that the tube and its holder have
cooled for at least 15 minutes before handling them.
Perform the following maintenance routines for the Slotted Tube Atom
trap (STAT).
1. Remove the STAT tube from the holder after using it. The holder
can remain on the burner, where it will not interfere with normal
operation.
NOTICE If the flame is extinguished with the STAT tube in the Operating
position, it becomes coated with soot. This will burn off when the
tube is next used, or remove it by wiping the tube with a dry cloth.
7-18 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Furnace System
CAUTION Risk of Eye Injury. The intense light emitted by a heated graphite
cuvette can harm your eyes. Although you are protected from direct
glare in normal operation, light escapes from the injection port and
the furnace head windows. Do not operate the furnace at high
temperatures unless it is in the normal operating position in the
sample compartment.
CAUTION Hot Surface. The furnace head is water cooled. All components return
to ambient temperature within about a minute from the end of the
furnace cycle. Nevertheless, ensure that the heating cycle has ended,
and that all components have cooled before handling or opening the
furnace head.
NOTICE If a cuvette fails in use, it may break up into small pieces inside the
furnace head. Remove any debris that could cause a short circuit and
consequent damage to the head. Clean the temperature control system
window and the lens before fitting a new cuvette.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-19
Maintenance
Maintenance of the Furnace System
Figure 7-7 and Figure 7-8 show the furnace head of the GFS35 and of
the GFS35Z, respectively, both in interior view.
2
4
1 3
7
5
5
2
4
3
1
8 7
7-20 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Furnace System
If the furnace head windows become dirty, they reduce the optical
energy passing through the cuvette and so increase the baseline noise.
1. If the furnace head is fitted on the tilt mount, tilt the head forward,
out of the spectrometer sample compartment.
If the furnace head is mounted on the fixed mount, remove the head
from the sample compartment. Place the head in a secure, accessible
position in front of the spectrometer.
2. Take the furnace window removal tool supplied. See Figure 7-9.
a. Push the tool firmly into the gap between the window holder
and the furnace body.
b. Use the tool to lever the window holder from its mounting.
3. Remove any debris or deposits from the window holder gas ways.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-21
Maintenance
Maintenance of the Furnace System
If a cuvette has failed in use, it is likely that soot and debris have been
deposited on the temperature control window. Clean the window before
you fit a new cuvette.
3. Unscrew the window holder from the rear of the center block.
NOTICE Take care that the window does not fall out.
3. Pull the center block gently to the right to free it from the locating
spigots.
5. Gently pull the hoses and connections out from the furnace body
until you obtain good access to the rear of the center block.
7-22 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Furnace System
When you feed the hoses and connections back into the furnace
body, ensure that none are trapped or kinked, or otherwise
damaged.
3. Tilt the head back into its normal position in the sample
compartment. Remove the magnet securing bolt with the spanner
provided.
4. Carefully tilt the head forward. The front magnet pole piece opens.
5. Lift the rear magnet pole piece and secure it with the catch provided.
7. Gently pull the hoses and connections out from the furnace body
until you obtain good access to the rear of the center block.
When you feed the hoses and connections back into the furnace
body, ensure that none are trapped or kinked, or otherwise
damaged.
When you re-fit the magnet securing bolt, do not overtighten it.
Finger tight plus half a turn is sufficient.
After typically six months of use, the cuvette contact cones may become
worn, causing poor contact with the cuvette and unreproducible cuvette
temperatures.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-23
Maintenance
Maintenance of the Furnace System
1. If the furnace head is on the tilt mount, tilt it forwards out of the
sample compartment.
If the furnace head is on the fixed mount, remove the head. Position
the head securely in front of the spectrometer.
2. Remove the sample injection port sleeve and both furnace head
window holders.
7. Assemble the cone replacement tool and insert it into one of the
electrodes. See Figure 7-10 or Figure 7-11.
8. Ensure that the body of the tool is locked into position against the
dowel stop, to prevent rotation.
9. Gently tighten the screw with the hex wrench provided, until the
cone is drawn out of the electrode.
7-24 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Furnace System
1 2
removal 3
4
8 8 5
6
4
7
3 2 insertion
removal 2
3
4
5
5
4
3
2
insertion
1
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-25
Maintenance
Maintenance of the Furnace System
3. Fit, then gently tighten the screw until the cone is fully home.
Do not overtighten the screw. This might damage the cone.
7. Re-fit the window holders and the sample injection port sleeve.
8. Fit a new cuvette. Replace the furnace head in its normal position in
the spectrometer sample compartment.
9. Check the optical alignment of the head before using it again. See
“Optical Alignment of the Furnace Head” on page 5-29.
Leak Testing
Leaks might occur in the gas handling system and in the water cooling
system. Inspect your furnace system regularly for leaks in both these
areas.
1. Set the inert gas supply pressure to 1.03 bar (15 psi).
2. Close the cylinder valve to isolate the gas lines and the equipment.
Ensure that you wipe off the soap solution at the end of the test, so
that it does not cause corrosion of the fittings.
7-26 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Furnace System
Internal Leaks
If you suspect a gas or water leak inside the furnace power supply,
conduit or furnace head, turn off all services to the equipment. Do not
use it again until the leak has been located and rectified by a trained
Thermo Fisher Scientific field service engineer.
Replacement of Fuses
The furnace power supply contains some internal fuses. These must
only be replaced by a trained Thermo Fisher Scientific field service
engineer.
Syringe
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-27
Maintenance
Maintenance of the Furnace System
3. Remove the syringe from its mount by carefully pulling the syringe
handling strap.
NOTICE Do not let any of the capillary tubing getting trapped between the
syringe or connector bodies and the autosampler.
You can replace the capillary tube between the syringe and capillary tip
if it should become blocked or damaged, although this is unlikely to
happen in normal use.
2. Pull the exposed capillary tubing gently from the arm and remove
the PTFE cone.
3. Remove the syringe.
5. Gently pull the old capillary tubing out from the autosampler.
6. Feed the new capillary tubing into the autosampler until the end
emerges from the autosampler arm.
7. With a sharp scalpel blade, trim the free end of the tubing to an
acute angle and feed it through a new PTFE cone.
8. Pull the tubing through the cone. Trim it flush with the flat face of
the cone.
NOTICE Do not cause damage to the flat sealing face of the cone.
9. Push the cone back into the arm. Re-fit the capillary tip.
7-28 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Furnace System
10. Attach the new capillary tubing to the syringe. Re-fit the syringe.
11. Thoroughly purge the system before use to remove any bubbles and
contaminations.
NOTICE Do not move the arm horizontally. This might cause damage to
the arm drive mechanism.
2. Carefully unscrew the locking cap. Remove the old capillary tip.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-29
Maintenance
Maintenance of the VP100
NOTICE Do not use any form of solvent-based cleaner, as it may damage the
plastic front cover.
• Remove all reagents from the instrument when not being used.
• Flush all liquid paths with clean water at the end of the analysis.
7-30 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the VP100
2. Examine the part of the tube that is in contact with the pump
rollers.
NOTICE The tubing in the acid channel gradually becomes opaque. This does
not affect normal operation and is not an indication that the tubing
requires replacement.
After you have replaced the pump tubing, or if you suspect that there is
a blockage, check the flow rates of the reductant, acid and sample
channels.
❖ To check the flow rates in the acid, reductant and sample channels
2. Start the VP100 at a pump speed of 30 rpm. Let it run until the
water has filled the gas liquid separator and is being discharged from
the drain.
4. Stop the VP100. Place the uptake tube of the channel that you want
to test into the measuring cylinder.
5. Start the VP100. Measure the volume of liquid drawn from the
measuring cylinder in 1 minute.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-31
Maintenance
Maintenance of the VP100
1. Remove the top cap and the hydrophobic membrane of the gas
liquid separator.
2. Pour clean water into the body of the gas liquid separator.
2. Inspect the internal volume of the gas liquid separator. Remove any
deposits.
Replacement of Fuses
The VP100 contains two main fuses located in the mains inlet
connector. It is unlikely that these fuses fail in normal operation, but if
they do, you can replace them. The specification of the fuses is detailed
on the label that is adjacent to the mains inlet connector. Ensure that the
replacement fuse matches this specification.
7-32 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the VP100
CAUTION Hot Surface. Risk of Burns. The electrically heated atomization cell
can reach temperatures in excess of 1100° C during use. Do not open
the furnace or handle the cell for at least 15 minutes after the power to
the furnace has been switched off.
Open the furnace head using the insulated furnace handles only.
Remove the T-cell with great care, handling only the end of the silica
inlet tube or Tygon hydride tubing. The T-cell wide body might still
be hot.
3. Do not use the accessory again until the fault has been rectified by a
trained Thermo Fisher Scientific field service engineer.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-33
Maintenance
Thermo Fisher Scientific Service
Returning Parts
To protect our employees, we ask you for some special precautions when
you send parts back to the factory for exchange or repair.
Your signature on the Health and Safety Form confirms that the
returned parts have been decontaminated and that they are free of
hazardous materials. This form is available on page A-5. Instead of
copying or printing this page, request a copy from the Thermo Fisher
Scientific field service engineer.
7-34 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Thermo Fisher Scientific Service
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-35
Maintenance
Thermo Fisher Scientific Service
7-36 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
A
Legal Documents
Contents
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) A-1
Legal Documents
WEEE Compliance
WEEE Compliance
This product is required to comply with the European Union’s Waste
Electrical & Electronic Equipment (WEEE) Directive 2012/19/EU. It
is marked with the following symbol:
RoHS
For information about the Restriction on Hazardous Substances
(RoHS) Directive for the European Union, search for RoHS on the
Thermo Fisher Scientific European language websites.
A-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Legal Documents
Declaration of Conformity
Declaration of Conformity
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) A-3
Legal Documents
Declaration of Conformity
A-4 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Health and Safety Form Legal Documents
Health and Safety Form
This Decontamination Declaration Form must be completed for all materials returned to Thermo Fisher Scientific. It
should be sent to the destination by e-mail, with approval from an authorized person. A signed hardcopy should be
attached to the outside of the package with shipping paperwork and a further copy should be placed inside the
packaging. The receiving Thermo Fisher Scientific office can help with this form and supply a return number, shipping
address and e-mail address. This form can be used to request warranty. Use the text "not used" to indicate a field not
being used. Where a Thermo Scientific part number is not known, add the supplier name (as for the examples below).
Part Number Quantity Material Description Error Description / Reason for Return Return Part Serial No
3. Contamination
Use the check boxes to state any contaminants the material/instrumentation been exposed to. Contaminated materials
must not be shipped to Thermo Fisher Scientific. If any exposure boxes are ticked, select ‘Yes’, if none, select ‘No’.
serious health
toxic flammable corrosive oxidizing
hazard
hazardous to gas under other harmful
explosive
environment pressure substances
biological radioactive
contaminated contaminated
Yes Æ go to section 4
Thermo Scientific
No Æ go to section 5
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) A-5
a)
b)
c)
d)
e)
f)
Components, materials and/or instruments that have been contaminated to a harmful level by whatever substances and/or compounds
as stated in sections 3. and 4. above will not be accepted without written evidence of proper decontamination.
I hereby declare that the instrument has undergone successfully all required decontamination procedures and is safe to handle for
Thermo Fisher Scientific and/or third-party service personnel or suppliers such as Pfeiffer Vacuum, Leybold Vacuum, Edwards Vacuum
products, or others.
I confirm that all information, which is supplied on this form, is accurate, complete and sufficient to judge any contamination level. I
acknowledge and agree that I will be liable for any personal injury or any other damage, which might result from a false, inaccurate or
incomplete statement and that I will indemnify and defend Thermo Fisher Scientific and/or any other concerned third party for and
against any liabilities, claims, losses, and/or damages of all kinds arising out of and/or caused by such false, inaccurate or incomplete
statements.
Thermo Fisher Scientific reserves the right not to process refunds or returns where the declared or observed use or previous
contamination of the product/material has by Thermo Fisher Scientific judgement impacted its integrity.
Return Number Name of authorized person (block letters) Date Signature Company stamp
A-6 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Contents
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-1
Specifications
Spectrometer
Spectrometer
USB port
Data Station See “Data Station Control” on page 3-5.
Optics Self-referencing single beam Zeeman
iCE 3400 configuration system
Optics Double Beam Stockdale optical system
iCE 3500 configuration
B-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Specifications
Spectrometer
total signal up to 3 A
Gas control fuel flow range:
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-3
Specifications
Spectrometer
USB port
Data Station Refer to “Data Station Control” on
page 3-5.
Optics Double Beam Stockdale Optical system
iCE 3300 configuration
Monochromator Ebert configuration with nominal 0.2, 0.5
and 1.0 nm spectral bandwidths
B-4 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Specifications
Autosampler
total signal up to 3 A
Gas control fuel flow range:
Autosampler
USB cable
Necessary additional items none
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-5
Specifications
Autosampler
USB cable
Necessary additional items none
Power 100-240 V at 50 or 60 Hz
Power consumption 50 VA
B-6 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Specifications
ID100 Autodilutor
ID100 Autodilutor
The ID100 autodilutor provides rapid in-line preparation of calibration
standards and intelligent or fixed ratio dilution of samples for flame
measurements. It is based on a high precision multi-piston pump that is
calibrated for life, and does not require any consumable items. It can be
used with manual sampling or with any of the flame autosamplers.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-7
Specifications
Furnace Head and Power Supply
The binary flow controlled internal gas system, with gas stop, offers a
choice of the inert gas or an alternate gas. The fixed external inert gas
flow protects the cuvette and purges the optical temperature sensor.
Table B-6 lists the specifications of the GFS33, GFS35 and GFS35Z
furnace head and power supply.
Table B-6. Specifications of GFS33, GFS35 and GFS35Z furnace head and
power supply
Item Comment
Standard items Standard (GFS33/35) or Zeeman
(GFS35Z) furnace head
power supply
B-8 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Specifications
Furnace Head and Power Supply
Table B-6. Specifications of GFS33, GFS35 and GFS35Z furnace head and
power supply, continued
Item Comment
Gas flow rate 3.5 L/min external flow
power
furnace open
cuvette present
Power 200/220/240 V at 50/60 Hz, 30 A
single phase
GFS35: 50 kg
GFS35Z: 66 kg
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-9
Specifications
Furnace Control
Furnace Control
The furnace is controlled by the SOLAAR Data Station software via the
spectrometer. A full handshaking RS-232C link is provided to the
furnace power supply. Furnace cycles are set up within a rapid fill table
allowing up to 20 phases to be programmed for temperature, time, ramp
rate, gas type and flow as well as special functions such as optical
temperature control, read phase and non linear ramp. Individual
temperature look-up tables for all cuvette types ensure accurate
temperature calibration.
B-10 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Specifications
GFS Furnace Autosampler
The sample is collected and dispensed via an inert PTFE capillary with
rapidly interchangeable tips. Viscous and Normal modes of injection
ensure that samples are handled appropriately, and an enhanced wash
program eliminates contamination.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-11
Specifications
VP100 Continuous Flow Vapor System
reagent cups: 25 mL
Matrix modifiers up to six per method
Resamples 1 to 99 per measurement
Sampling system 100 L syringe (side port)
Sampling volume 1 to 70 L
Reproducibility of injected volume better than 1% (by mass) at
volumes equal to and exceeding
10 L
Accuracy of injected volume ±0.5 L
Inert gas pressure 0.34 bar (5 psi)
Wash and waste container volume 1 L each
Dimensions [mm] 296 W × 380 H × 320 D
Weight approximately 8 kg
The VP100 operates automatically under Data Station control and can
provide full autosampling operation with a suitable autosampler. When
used with the EC100 Electrically Heated Atomization Cell, unattended
operation is possible.
B-12 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Specifications
VP100 Continuous Flow Vapor System
120 mm long
8 mm internal diameter
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-13
Specifications
EC100 Electrically Heated Atomization Cell
The EC100 must be used with the VP100 and is suitable for all hydride
forming elements.
100-120 V, 60 Hz
Power consumption 720 VA
Dimensions [mm] 280 W × 140 H × 290 D
(power supply)
Weight approximately 13 kg
B-14 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Specifications
AA Validator Kits
AA Validator Kits
Available in three separate kits designed for flame, furnace or flame and
furnace installations, the unique AA Validator Kits provide full system
validation for iCE 3000 Series AA systems, including comprehensive
qualification plans. Full SOP and check sheets, together with complete
supplier assessment questionnaires, are supplied in the Validator
Logbook for recording and demonstrating compliance. All necessary
consumables are provided and even method validation guidelines are
included.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-15
Specifications
Calibration Validation Unit
power supply
B-16 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Specifications
iSQ Module
iSQ Module
The iSQ module is mounted on either the right hand or left hand
sample compartment of iCE 3000 Series instruments. It provides
facilities for automatically testing the spectrometer hardware.
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-17
Specifications
iSQ Module
B-18 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
C
Component Suppliers‘ Documents
Contents
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) C-1
Component Suppliers‘ Documents
Maintenance of the CETAC ASX-560 and ASX-280 Flame Autosampler
• Wipe the exterior surfaces with a soft cloth dipped in soapy water to
remove any marks.
C-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
I
Index
Numerics C
21 CFR Part 11 3-6 Calibration Validation Unit (CVU) B-16
3 mm ball-ended hex key 5-13 carousel cover 5-37
cleaning
burner 7-9
furnace system 7-20
A nebulizer 7-15
AA systems 3-2, 6-2 spray chamber 7-12
AA Validator Kits B-15–B-16 cleaning tool 7-11
accessory trolley 5-39 clothing 4-31
acetone carryover 4-14, 4-18 compressor 3-11
acetylides 4-15 condensation 5-3
acid blank reagent 6-27 cone replacement tool 7-24
acid channel 7-31 contaminated parts 7-34
air compressor 3-11 cooling water 3-16
air/acetylene flame 3-13, 5-18 cuvette
alignment contact cones 7-23
burner 6-8 fitting 5-35
capillary tip 6-25 cuvette life counter 5-35
furnace head 5-29, 5-32 cuvette tool 5-35, 6-23
impact bead 6-10
iSQ Module 5-16, 6-4
lamp 3-7
LH Accessory Mount 5-12 D
RH Accessory Mount 5-10 data station
STAT Tube 5-26 control 3-5
T-Cell 5-46 installation 5-7
alignment and operation 5-16, 6-4 printer installation 5-7
alternate gas 3-15 software 3-5
argon 3-15, 5-38 declaration of conformity A-3
ASX-260 Flame Autosampler B-6 decommissioning, the instrument 4-7
ASX-520 Flame Autosampler B-5 deuterium lamp 7-6
atomization temperature 6-33 drain
autosamplers 3-11, C-2 empty and refill 7-16
auxiliary oxidant 3-14 position drain tube 4-20
auxiliary oxidant flow rate 6-16 tube 3-13
vessel 4-23
drain channel 7-31
B
ball valve 4-20
Biohazard symbol 4-16
E
black nylon tubing 5-38 EC100
description B-14
borohydride reductant reagent 6-27
installation of furnace head 5-49
burner 3-3
installation of power supply 5-49
alignment 6-8
usage 3-19
maintenance 7-9
Echelle 3-3
types 3-10
warm-up 6-7, 6-17 electrical connections
autosampler 5-36
burner cleaning tool 7-9
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) I-1
Index: F–M
I-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Index: N–V
R
reagents 6-27
recirculation chiller 3-17
U
reductant channel 7-31 universal accessory mount
left sample compartment 3-9, B-16
returning, parts 7-34
right sample compartment 3-7, B-16
right hand sample compartment 3-7
user maintenance 7-1, 7-4
risk assessment 4-16, 4-22
room temperature 5-3
V
S Variable Flow Auxiliary Oxidant Accessory 3-12
Variable Flow Auxiliary Oxidant Kit 3-14, 6-6, 6-19
safety glasses 4-31
venting, the gas system 6-11
safety information 4-8
VP100
safety precautions 4-2
carrier gas flow rate 6-28
sample channel 7-31
description 5-40, B-12
sample compartment maintenance 7-30
left, universal accessory mount 3-9, B-16 measurement delay time 6-28
right, universal accessory mount 3-7, B-16 optimizing parameters 6-28
sample cups 6-24 pump speed 6-28
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) I-3
Index: W–Z
Z
W Zeeman 3-3
warming up, the burner 6-7 Zeeman background correction 3-15
wash facility 3-14 zero absorbance baseline 7-6
waste solvent draining 4-23
I-4 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Index: Z–Z
Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) I-5