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iCE 3000 Series AA Spectrometers

Operating Manual

BRE0011709 Revision C December 2018


iCE 3000 Series AA Spectrometers
Operating Manual

BRE0011709 Revision C December 2018


Legal Notices
© 2018 Thermo Fisher Scientific Inc. All rights reserved.
Original Operating Instructions
Published by:
Thermo Fisher Scientific (Bremen) GmbH, Hanna-Kunath-Str. 11, 28199 Bremen, Germany
Tel: +49(0)421 5493 0, Fax: +49(0)421 5493 396

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.

Thermo Fisher Scientific does not endorse any manufacturer or products other than its own. Unless
otherwise stated, companies and products listed in this document are given as examples only.

Thermo Fisher Scientific Inc. provides this document to its customers with a product purchase to use
in the product operation. This document is copyright protected and any reproduction of the whole or
any part of this document is strictly prohibited, except with the written authorization of Thermo
Fisher Scientific Inc.

Release History: Revision A released in July 2017.


Revision B released in October 2018.
Revision C released in December 2018.
C
Contents
Chapter 1 Using this Manual .................................................................1-1
About this Manual ......................................................... 1-1
Typographical Conventions ........................................... 1-2
Signal Word................................................................ 1-2
Viewpoint Orientation................................................ 1-2
Data Input .................................................................. 1-2
Topic Headings........................................................... 1-3
Reference Documentation.............................................. 1-4
Contacting Us................................................................ 1-5

Chapter 2 Scope of Delivery ..................................................................2-1


Standard System Components ....................................... 2-1
Optional System Components ....................................... 2-2

Chapter 3 System Description ...............................................................3-1


Description of AA Systems............................................. 3-2
Optical System............................................................ 3-3
Flame System .............................................................. 3-3
Graphite Furnace Systems ........................................... 3-4
Graphite Furnace TeleVision (GFTV) ........................ 3-4
Electronics .................................................................. 3-4
Data Station Control .................................................. 3-5
Data Station Software ................................................. 3-5
Spectrometer System ...................................................... 3-7
Hollow Cathode Lamps .............................................. 3-7
Universal Mount in Right Hand Sample
Compartment ............................................................. 3-7
Universal Mount in Left Hand Sample
Compartment ............................................................. 3-9
iSQ Module ................................................................... 3-9
Flame System ............................................................... 3-10
Gas Connections....................................................... 3-10
Burners ..................................................................... 3-10
Air Compressor ......................................................... 3-11
CETAC ASX-560 and ASX-280 Flame
Autosamplers ............................................................ 3-11
ID100 Autodilutor Accessory.................................... 3-12
Slotted Tube Atom Trap (STAT) ............................. 3-12
Variable Flow Auxiliary Oxidant Accessory ............... 3-12
Solvent Resistant Flame Kit....................................... 3-12
Other Accessories ...................................................... 3-14
Furnace ........................................................................ 3-15

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) i
Contents

GFS35 and GFS35Z Graphite Furnace Systems ....... 3-15


Services ..................................................................... 3-15
GFS33 Graphite Furnace System .............................. 3-17
GFS Autosampler...................................................... 3-17
VP100 Continuous Flow Vapor System....................... 3-19
EC100 Electrically Heated Atomizer......................... 3-20

Chapter 4 Safety....................................................................................... 4-1


Safety Symbols and Signal Words in this Manual........... 4-2
Observing this Manual................................................ 4-2
Safety Precautions ....................................................... 4-2
Safety Symbols on the Instrument.................................. 4-3
Rating Plate................................................................. 4-5
Intended Use.................................................................. 4-6
Qualified Personnel..................................................... 4-7
Electrical Safety.............................................................. 4-8
Equipment Cleaning and Decontamination................... 4-8
Spectrometer Safety........................................................ 4-9
Hollow Cathode Lamp Hazards.................................. 4-9
Flame System Safety..................................................... 4-12
Flame Safety.............................................................. 4-13
Flashback .................................................................. 4-13
Perchloric Acid.......................................................... 4-15
Silver, Gold and Copper Samples.............................. 4-15
Organic Solvents ....................................................... 4-16
Gases......................................................................... 4-17
Flame Sample Compartment Door ........................... 4-19
Fume Extraction ....................................................... 4-19
Drain ........................................................................ 4-20
Safety Guidelines for Flame Measurements in
Organic Solvents ....................................................... 4-22
Slotted Tube Atom Trap........................................... 4-23
Flame Atomizer......................................................... 4-24
Furnace Safety.............................................................. 4-24
GFS33/35 and GFS35Z Furnace Heads ................... 4-24
GFS35Z Zeeman Furnace Head ............................... 4-24
Fume Extraction ....................................................... 4-25
Gases......................................................................... 4-25
Furnace Measurements in Organic Solvents .............. 4-25
Vapor Safety................................................................. 4-27
Reagents.................................................................... 4-27
Flame Heated Atomization Cell ................................ 4-27
VP 100 Continuous Flow Vapor System................... 4-27
EC100 Electrically Heated Atomizer......................... 4-28
In Case of Emergency .................................................. 4-29
Residual Hazards.......................................................... 4-30
Gases......................................................................... 4-30
Waste........................................................................ 4-30
Personal Protective Equipment ................................. 4-31

ii iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Contents

Chapter 5 Installation ..............................................................................5-1


Laboratory Conditions ................................................... 5-2
Power Supply .............................................................. 5-2
Laboratory Temperature ............................................. 5-3
Humidity .................................................................... 5-3
Fume Extraction ......................................................... 5-3
Installation of the Spectrometer ..................................... 5-6
Installation of a Hollow Cathode Lamp ......................... 5-8
Removal of a Hollow Cathode Lamp .......................... 5-9
Universal Mount in Right Hand Side Compartment ... 5-10
Fitting an Accessory to the Universal Mount............. 5-10
Alignment of a Fitted Accessory ................................ 5-10
Fitting the Left Hand Sample Compartment
Universal Mount.......................................................... 5-12
Alignment of a Fitted Accessory ................................ 5-12
Installation of the iSQ Module..................................... 5-14
Alignment of the iSQ Module................................... 5-16
Flame System ............................................................... 5-17
Gas Supply Inlet Pressures......................................... 5-17
Gas Connections....................................................... 5-17
Installation of Burner ................................................ 5-18
Installation of the Air Compressor ............................ 5-19
Installation of the CETAC ASX-560 and ASX-280
Flame Autosampler ................................................... 5-20
Installation of the ID100 Autodilutor ....................... 5-23
Installation of the Slotted Tube Atom Trap .............. 5-25
Alignment of the STAT Tube ................................... 5-26
Installation of the Solvent Resistant Flame Kit .......... 5-27
Installation of GFS35 and GFS35Z Furnace System .... 5-27
Installation of the GFS33 Graphite Furnace System..... 5-31
Removing and Fitting the GFS33 ............................. 5-31
Alignment of the Furnace Head of the GFS33
System ...................................................................... 5-32
Fitting the Cuvettes................................................... 5-35
Installation of the GFS Autosampler ......................... 5-36
Installation of VP100 Continuous Flow Vapor
System ......................................................................... 5-38
Sample Uptake Capillary Tube ................................. 5-39
Gas Liquid Separator................................................. 5-44
Flame Heated Measurement Cell .............................. 5-45
Electrically Heated Atomization Cell......................... 5-47
Mercury Absorption Cell .......................................... 5-47
Installation of the EC100.......................................... 5-49

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

Operation of Flame System............................................ 6-5


Safety .......................................................................... 6-5
Organic Solvents ......................................................... 6-5
Lighting the Flame...................................................... 6-6
Warming up the Burner.............................................. 6-7
Alignment of the Burner ............................................. 6-8
Alignment of the Impact Bead .................................. 6-10
Venting the Gas System ............................................ 6-11
Operation of the Air Compressor .............................. 6-12
Handling the Air Compressor ................................... 6-12
Operation of the Autosampler................................... 6-13
Operation of the ID100 Autodilutor......................... 6-13
Operation of the Slotted Tube Atom Trap................ 6-15
Operation of the Variable Flow Auxiliary Oxidant
Accessory................................................................... 6-16
Operation of the Solvent Resistant Flame Kit............ 6-17
Flame Optimization.................................................. 6-18
Operation of the Graphite Furnace System .................. 6-21
Operating the GFS33 Graphite Furnace System ....... 6-21
Operation of the GFS Autosampler.............................. 6-23
Wash Liquid ............................................................. 6-23
Syringe Purge ............................................................ 6-24
Cleaning Autosampler Cups...................................... 6-25
Alignment of Capillary Tip ....................................... 6-25
Vapor Operation.......................................................... 6-27
Reagents.................................................................... 6-27
Parameter Optimization of the VP100...................... 6-28
Sample Measurement Using the VP100 .................... 6-30
Shutdown of the VP100............................................ 6-32
Operation of the EC100 ........................................... 6-33
Optimization of the EC100 ...................................... 6-34
Troubleshooting of the EC100 ................................. 6-34

Chapter 7 Maintenance.......................................................................... 7-1


Safety Guidelines for Maintenance................................. 7-2
General Advice for Maintenance .................................... 7-2
Inspection- and Servicing Plan ....................................... 7-4
Maintenance of the Spectrometer................................... 7-6
Cleaning the Spectrometer .......................................... 7-6
Deuterium Lamp of the iCE 3300 Spectrometer......... 7-6
Replacement of a Spectrometer Fuse ........................... 7-7
Maintenance of the iSQ Module................................. 7-8
Maintenance of the Flame System.................................. 7-9
Maintenance of the Burner ......................................... 7-9
Maintenance of Spray Chamber ................................ 7-12
Maintenance of Nebulizer ......................................... 7-15
Maintenance of Drain ............................................... 7-15
Maintenance of Gas Supply Hoses ............................ 7-16
Maintenance of the Air Compressor.......................... 7-17

iv iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Contents

Maintenance of the Autosampler............................... 7-17


Maintenance of the ID100 Autodilutor .................... 7-17
Maintenance of the Slotted Tube Atom Trap............ 7-18
Maintenance of the Variable Flow Auxiliary
Oxidant Accessory..................................................... 7-18
Maintenance of the Furnace System............................. 7-19
Maintenance of the GFS35/35Z System ................... 7-19
Maintenance of the GFS33 System ........................... 7-27
Maintenance of the GFS Autosampler ...................... 7-27
Maintenance of the VP100 .......................................... 7-30
Maintenance of Peristaltic Pump............................... 7-31
Maintenance of Gas Liquid Separator ....................... 7-32
Replacement of Fuses ................................................ 7-32
Maintenance of the EC100 ....................................... 7-33
Thermo Fisher Scientific Service .................................. 7-34
Returning Parts ......................................................... 7-34
Services to be Performed by Thermo Fisher
Scientific Service Only .............................................. 7-35

Appendix A Legal Documents ..................................................................A-1

Appendix B Specifications .......................................................................B-1


Spectrometer .................................................................. B-2
iCE 3400/3500 Spectrometer ..................................... B-2
iCE 3300 Series Spectrometer ..................................... B-4
Autosampler................................................................... B-5
ASX-560 Flame Autosampler ...................................... B-5
ASX-280 Flame Autosampler ...................................... B-6
ID100 Autodilutor......................................................... B-7
Furnace Head and Power Supply ................................... B-8
Furnace Control........................................................... B-10
GFS Furnace Autosampler ........................................... B-11
VP100 Continuous Flow Vapor System....................... B-12
EC100 Electrically Heated Atomization Cell ............... B-14
AA Validator Kits......................................................... B-15
Calibration Validation Unit ......................................... B-16
Left Hand Universal Accessory Mount......................... B-16
Right Hand Universal Accessory Mount ...................... B-16
iSQ Module ................................................................. B-17

Appendix C Component Suppliers‘ Documents .................................... C-1


Maintenance of the CETAC ASX-560 and ASX-280
Flame Autosampler ........................................................C-2
Safety Guidelines for Handling the Autosampler.........C-2

Index ........................................................................................ I-1

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

Welcome to the Thermo Scientific™ iCE 3000 Series system!

Contents

• About this Manual on page 1-1

• Typographical Conventions on page 1-2

• Reference Documentation on page 1-4

• Contacting Us on page 1-5

About this Manual


This iCE 3000 Series AA Spectrometers Operating Manual contains
precautionary statements that can prevent personal injury, instrument
damage, and loss of data if properly followed. It also describes the modes
of operation and principle hardware components of your
iCE 3000 Series instrument. In addition, this manual provides
step-by-step instructions for cleaning and maintaining your instrument.

This manual is intended for all personnel that need a thorough


understanding of the instrument (to perform maintenance or
troubleshooting, for example). Read this manual carefully before using
the instrument and keep it for future reference.

This manual covers the following topics:

• The safety hazards involved in working with the spectrometer and


its accessories, as well as the means by which such hazards can be
minimized.

• The spectrometer

• The flame atomization system

• The flame accessories

• The furnace atomization system

• The furnace accessories

• The vapor generation accessories

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.

Tip Highlights helpful information that can make a task easier.

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:

• Messages displayed on the screen are represented by capitalizing the


initial letter of each word and by italicizing each word.

• Input that you enter by keyboard is identified by quotation marks:


single quotes for single characters, double quotes for strings.

• For brevity, expressions such as “choose File > Directories” are used
rather than “pull down the File menu and choose Directories.”

• Any command enclosed in angle brackets < > represents a single


keystroke. For example, “press <F1>” means press the key labeled
F1.

• Any command that requires pressing two or more keys


simultaneously is shown with a plus sign connecting the keys. For
example, “press <Shift> + <F1>” means press and hold the <Shift>
key and then press the <F1> key.

• 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:

Chapter 1 Chapter Name

Second Level Topics

Third Level Topics

Fourth Level Topics

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.

• iCE 3000 Series Pre-Installation Requirements Guide

• iCE 3000 Series AA Spectrometers SOLAAR Software Manual

• iCE 3000 Series AA Spectrometers SOLAARsecurity Software Manual

• Methods Manual

A printed version of this iCE 3000 Series AA Spectrometers Operating


Manual is shipped with the instrument. The iCE 3000 Series
Pre-Installation Requirements Guide is send out to you prior to
installation. The other manuals are supplied on the CD shipped with
the instrument.

Refer also to the user documentation provided by the manufacturers of


third party components and the Material Safety Data Sheets (MSDSs).

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.

Contact Link / Remarks QR Code


Brochures and Ordering www.thermofisher.com/aas
Information

Service Contact www.unitylabservices.com

Technical Documentation ❖ To get user manuals for your product


SharePoint
1. With the serial number (S/N) of your instrument, request
access on our customer SharePoint as a customer at
www.thermoscientific.com/Technicaldocumentation

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.

3. Download current revisions of user manuals and other


customer-oriented documents for your product. Translations
into other languages may be available there as well.
Customer Feedback ❖ To suggest changes to this manual

You are encouraged to report errors or omissions in the text or


index. Send an email message to the Technical Editor at
documentation.bremen@thermofisher.com.

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

• Standard System Components on page 2-1

• Optional System Components on page 2-2

Standard System Components


The iCE 3000 Series standard system comprises the following
components:

• iCE 3000 Series AA spectrometer

• Data system computer with monitor

• Installation Kit including


- Equipment for connecting the above components (hoses, cables)
- Computer equipment
- Tools for installation and maintenance
- Spare parts

• Printed manuals
- iCE 3000 Series Operating Manual

In addition to these printed manuals, other documents for the


iCE 3000 Series atomic absorption spectrometers are available. See
“Reference Documentation” on page 1-4 for a list.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 2-1
Scope of Delivery
Optional System Components

Optional System Components


For reference, the following list contains components that are frequently
shipped with the standard iCE 3000 Series system. They are not part of
the standard system and may therefore not be present in your
laboratory:

• Thermo Scientific™ GFS33 Graphite Furnace and autosampler for


iCE™ 3300 AA spectrometer

• Thermo Scientific GFS35 or GR35Z Graphite Furnace and


autosampler for iCE 3500 AA spectrometer

• Thermo Scientific SOLAAR Validator Package

• Thermo Scientific SOLAARSecurity Software

• Thermo Scientific ID100 Auto Dilutor

• Thermo Scientific VP100 Continuous Flow Vapor System (includes


T-cell and mercury cell)

• Thermo Scientific EC100 Electrically Heated Atomization Cell

• Thermo Scientific Slotted Tube Atom Trap

• Air compressor KNF N035 (Series N 035 A_.18 pumps, diaphragm


vacuum pumps and compressors, KNF Neuberger, Inc.)

• CETAC™ ASX-560 autosampler (requires dedicated RS-232 on


Data Station)

• CETAC ASX-280 autosampler (requires dedicated RS-232 on Data


Station)

• Thermo Scientific NESLAB ThermoFlex™ recirculating chiller

2-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
3
System Description

This chapter provides an overview of the functional elements of the


iCE 3000 Series atomic absorption spectrometer.

Contents

• Description of AA Systems on page 3-2

• Spectrometer System on page 3-7

• iSQ Module on page 3-9

• Flame System on page 3-10

• Furnace on page 3-15

• VP100 Continuous Flow Vapor System on page 3-19

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.

Figure 3-1. iCE 3000 Series system

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.

Quadline background correction is fitted as standard to all instruments.


Both the Zeeman and the high energy Quadline background correction
system correct for up to 2 A of background with < 2% error. All
iCE 3000 Series spectrometers provide a 6 position data-coded,
auto-aligning lamp carousel, with six independent power supplies
modulated at 200/240 Hz.

Automatic analyses with up to 16 element methods are possible, and


separate methods can be sequentially run in each sample compartment
as a dual analysis. The wide range PMT covers the wavelength range
from 180 nm to 900 nm. GFTV comes with all furnace systems
(iCE 3300 GF, iCE 3400, iCE 3500).

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.

Flame systems are controlled by a fully automatic gas control system


using programmable array state logic and binary flow switching
technology for reliability. Oxidant gas changeover, and fuel and oxidant
flow rates are software controlled and interlocked to prevent operation
with incorrect burners and gas flows.

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.

The inert fluoroplastic spray chamber contains an adjustable impact


bead, flow spoiler and low memory hydrophilic disc front end, with
built-in over pressure relief and automatic empty drain protection. The

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-3
System Description
Description of AA Systems

standard spray chamber configuration is suitable for all flame and


sample types. The standard inert nebulizer has a Pt/Ir capillary and
PTFE venturi, and is factory optimized.

Graphite Furnace Systems


Graphite furnaces are fitted in the right hand sample compartment of
the iCE 3400/3500 Series spectrometers and the left hand sample
compartment of the iCE 3300 spectrometer. The iCE 3500
spectrometer accepts either the GFS35 or the GFS35Z furnace systems
whereas the iCE 3400 spectrometer only accept the GFS35Z furnace.
The iCE 3300 spectrometer only accepts the GFS33.

The GFS35Z Zeeman Furnace is mounted on a pre-aligned tilt mount


which can be tilted forward out of the sample compartment to allow
access to the furnace for maintenance purposes, and to allow other
accessories to be fitted into the sample compartment.

The GFS35 furnace is fitted with a pre-aligned fixed mount as standard,


but can be optionally fitted with the tilt mount if required.

The GFS furnace autosampler is mounted in front of the right hand


sample compartment with a simple self-locating ‘push in’ mount on the
iCE 3400/3500 spectrometers. The GFS furnace autosampler is
integrated into the GFS33 and does not require separate mounting.

Graphite Furnace TeleVision (GFTV)


• GFTV is a standard feature on the iCE 3400/3500 spectrometers
and the furnace only iCE 3300 spectrometer (3300 GF).
• GFTV is optional on the flame only iCE 3300 (iCE 3300 FL)
spectrometer.

The GFTV accessory provides high definition images of events inside


the graphite furnace cuvette, allowing monitoring of the sample
injection, dry and ash phases of the furnace program. A CMOS camera
mounted in the instrument produces live video for display on the Data
Stations screen.

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.

3-4 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
System Description
Description of AA Systems

Data Station Control


The spectrometer system and accessories are controlled via a Data
Station running the SOLAAR AA software package under the Microsoft
Windows XP Professional, Vista Ultimate, Windows 7 Professional, or
Windows 10 Professional operating systems. The Data Station is a
personal computer with the following minimum configuration:

• 800 MHz Pentium processor or equivalent


• 512 MB RAM
• CD ROM drive
• Fixed disk drive with at least 1 GB free space
• 19 in SVGA color monitor
• USB port
• Parallel port
• Windows XP Professional SP2, Vista Ultimate, Windows 7
Professional, or Windows 10 Professional

Data Station Software


The SOLAAR Data Station software controls all iCE 3000 Series
spectrometers. The software is aware of the type of spectrometer that it
is controlling. It only provides relevant parameters and options for each
instrument type and configuration. The Data Station software supports
all the facilities provided by all the AA Series accessories.

The software features a range of wizard-based procedures, and a tabbed


methods dialog to make setting up even complex analyses fast and easy.
All raw data, results and parameters are stored in a single database for
easy retrieval. True Windows multi-tasking is available, so that
SOLAAR can be iconized while running an analysis, allowing
concurrent use of other applications. Methods can be created, edited
and saved, and earlier results can be reviewed, edited and printed, while
an analysis is underway.

The SOLAAR software enables full 16 element methods to be


performed automatically. The flexible and comprehensive tabbed
methods dialog box guides the user through setting up complex,
multi-element analyses. Data coded HCLs are fully supported, and
facilities are provided to record lamp usage.

Up to ten calibration standards and a blank can be used, with segmented


curve, linear or quadratic least squares fit calibration algorithms.
Normal, standard addition and standard curve calibration methods are
supported, with full graphical display and print out of the calibration

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-5
System Description
Description of AA Systems

curve. Full alphanumeric sample details including sample mass and


dilution correction can be entered for each sample, or imported via text
files.

Comprehensive furnace signal graphics are provided, and automated


ash-atomize plots produce graphical data for furnace program
optimization, and even suggest optimum values. For flame systems, fully
automatic fuel gas flow and burner height optimization with graphical
presentation are provided.

Extensive online, context sensitive Help facilities are available. Carefully


structured books allow easy browsing and searching as well as direct
access to any Help topic. Troubleshooting and diagnostics sections
describe simple experiments to first locate the problem and then to
rectify it. A full Cookbook with default parameters for all elements,
common interferences, and the methods to overcome them is included.

The SOLAAR software provides comprehensive printer support


through the Windows operating system. Report formatting enables
customization of the sample details, results, summaries, methods,
system parameters and graphical displays that are to be included in the
report. All reports, as well as individual results, are time- and
date-stamped. Flexible and comprehensive results database filters select
and display the required data, which can be exported to other
applications for further processing. Fully reversible results editing is
available and is automatically audit trailed. Password protection and the
audit trail maintain the validity of the data for accreditation purposes.

Integrated Auto QC software provides comprehensive quality control


protocols automation with checking, testing and re-analysis options,
SPC graphical results display, report generation and data filing.
QC blanks, QC checks, QC duplicates and two forms of QC spikes are
included, each with user definable test criteria and failure actions. Full
QC reporting, including pass/fail results and time and date stamps is
provided on the Results display, and hard copy reporting of all
QC protocols, parameters, results and actions is available. QC data is
linked to the results to which it applies, and can be exported with the
results.

The SOLAAR software is available in the following languages: English,


US English, French, German, Russian, Spanish, Japanese, Chinese and
Polish.

An additional software package, SOLAARSecurity, is available, which


adds to the SOLAAR Data Station software the tools, functions and
facilities required to comply with the Food and Drug Administration 21
CFR Part 11 Rule Electronic Records, Electronic Signatures.

3-6 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
System Description
Spectrometer System

Spectrometer System

Hollow Cathode Lamps


Hollow cathode lamps (HCLs) are high intensity, stable light sources
that emit the element specific spectral lines required for Atomic
Absorption spectrometry. Up to six hollow cathode lamps can be
installed in the iCE 3000 Series spectrometer.

The iCE 3000 Series spectrometers provide automatic lamp alignment


facilities, with manual overrides if required. You can access these
facilities from the Lamp page of the Data Station software (Edit >
Lamp).

See “Hollow Cathode Lamp Hazards” on page 4-9 for information


about the hazards associated with hollow cathode lamps. Ensure that the
hazards involved and the necessary precautions are understood before
you install such a lamp.

NOTICE Coded or uncoded lamps supplied by Thermo Fisher Scientific are


recommended.

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.

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

Universal Mount in Right Hand Sample Compartment


In the right hand sample compartment of the iCE 3400 and iCE 3500
systems, an universal mount serves to fit several accessories. See
Figure 3-2.

• If a graphite furnace on a tilt mount is fitted in the right hand


sample compartment, it can be tilted forward to allow the universal
mount to be fitted.

• If you want to use a graphite furnace and other accessories on the


universal mount in the right hand sample compartment, Thermo
Fisher Scientific strongly recommends using the tilt mount. If a
graphite furnace on a fixed mount is fitted, the furnace and the
mount must be removed before the universal mount can be fitted.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-7
System Description
Spectrometer System

1 2

4 3

Labeled Components: 1=adjustment screw, 2=accessory mounting pin,


3=location plate, 4=mounting pads, 5=spring retainer
Figure 3-2. Right hand sample compartment with universal mount

3-8 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
System Description
iSQ Module

Universal Mount in Left Hand Sample Compartment


In the left hand sample compartment of the iCE 3300 and the
iCE 3500 systems, an universal mount serves to fit several accessories.

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.

NOTICE Observe the electrical safety precautions described in “Safety” on


page 4-1

The iSQ package consists of the following parts:

• The iSQ Module

• A calcium/magnesium data-coded hollow cathode lamp

• Support and accessory brackets

• An right hand accessory mount or universal accessory mount

• An in-line power supply unit

• A serial data lead

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.

The flame system consists of:

• The fuel and oxidant gas supplies and connectors

• The spectrometer automatic gas control system

• The nebulizer and impact bead

• The spray chamber

• The spray chamber drain assembly

Gas Connections
Three gas inlet connections are provided on the spectrometer.

• Air

• Acetylene

• Nitrous Oxide

Figure 3-3 shows the spectrometer gas connection panel.

Figure 3-3. Spectrometer gas connection panel

Burners
Two types of burners are available for iCE 3000 Series spectrometers:

• 50 mm slot universal finned titanium burner suitable for general


purpose use with all flame types

• 100 mm slot titanium burner suitable for air/acetylene flames only

The sensitivity for elements measured with this flame is improved


compared to the universal finned titanium burner.

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.

A filter/regulator unit is included to remove particles and moisture, and


to ensure that a stable air pressure to the spectrometer is maintained.

The performance is reduced at high altitude.

1 2 3

Labeled Components: 1=air outlet, 2=carrying handle, 3=mains lead


Figure 3-4. Air compressor

CETAC ASX-560 and ASX-280 Flame Autosamplers


• The CETAC ASX-560 is a high capacity autosampler with integral
wash facilities, capable of handling up to 360 samples.

• The CETAC ASX-280 is a medium capacity autosampler capable of


handling up to 180 samples.

They are compatible with:

• normal flame operation

• flame dilution with the ID100 Autodilutor accessory

• vapor operation with the VP100 accessory

Tip Also refer to the ASX-560 and ASX-280 Autosampler Operator’s


Manual for more information.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-11
System Description
Flame System

ID100 Autodilutor Accessory


The ID100 Autodilutor accessory provides automatic sample dilution
and standard preparation for flame AAS.

It can be used manually or with any of the flame autosamplers. It is not


compatible with the VP100 Vapor Generation accessory.

Slotted Tube Atom Trap (STAT)


The Slotted Tube Atom Trap (STAT) is an accessory that enhances the
flame sensitivity for certain elements by 2 to 5 times. It consists of a
slotted tube held in the flame by a simple holder.

Variable Flow Auxiliary Oxidant Accessory


An auxiliary supply of oxidant gas to the air/acetylene flame is necessary
to maintain the optimum flame chemistry when using non-aqueous
solvents.

The standard configuration of the flame instruments provides a fixed


auxiliary oxidant flow that is suitable for use with common solvents such
as white spirit and methyl isobutyl ketone (MIBK).

This accessory provides a variable flow of auxiliary oxidant to allow the


flame chemistry to be optimized for other less common solvents.

If you use your instrument to analyze this type of sample on a regular


basis, Thermo Fisher Scientific recommends fitting your instrument also
with the Solvent Resistant Flame Kit, see “Solvent Resistant Flame Kit”.

The accessory must be installed by a trained Thermo Fisher Scientific


field service engineer.

Solvent Resistant Flame Kit


The Solvent Resistant Flame Kit has been designed for the Thermo
Scientific Flame Atomic Absorption spectrometers. It provides
replacements for certain parts in the standard flame atomization system
that can be susceptible to damage if subject to long term exposure to
certain organic solvents.

3-12 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
System Description
Flame System

Components of the Solvent Resistant Flame Kit

Spray Chamber

The Solvent Resistant Flame Kit includes a modified spray chamber.


The top of the spray chamber stem has been modified with a Teflon™
sleeve. This prevents the top of the stem from softening when ketone
solvents, such as methyl isobutyl ketone, di-isobutyl ketone and methyl
ethyl ketone, are run for long periods with a high temperature nitrous
oxide supported flame.

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

The Solvent Resistant Flame Kit includes an extended length of the


convoluted PTFE drain that extends down to the drain vessel, and does
not require a joint between the PTFE tube and the standard polythene
drain tube. This prevents leakage of certain low viscosity solvents at the
joint and prevents degradation of the standard polythene 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.

0.4 mm ID Sample Uptake Tube

It is often desirable to reduce the sample uptake rate when measuring


samples in organic solvents, as this can make it easier to optimize the
flame chemistry. This can be conveniently achieved by replacing the
standard 0.5 mm ID sample uptake tubing with the 0.4 mm ID tubing
supplied in the Solvent Resistant Flame Kit.

Auxiliary Oxidant

When an organic solvent is sprayed into a flame, the solvent combusts


and so increases the effective fuel supply to the flame. This causes a
change in the flame chemistry that can result in reduced sensitivity and
increased interferences for certain elements. This problem affects only
air/acetylene flames.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-13
System Description
Flame System

With nitrous oxide supported flames, the oxidant is sufficiently


powerful that compensation for the additional fuel effect of the solvent
can be achieved with the normal fuel flow rate adjustments available.

With an air supported flame, an additional supply of oxidant is


normally required to obtain the optimum flame chemistry. The flame
capable iCE 3000 Series spectrometers fitted with fully automatic gas
handling systems provide a facility known as the Auxiliary Oxidant that
provides this additional oxidant supply. It can be selected on the Flame
Parameters page of the SOLAAR Data Station software.

The standard Auxiliary Oxidant feature supplies a fixed flow rate of


additional oxidant that will be suitable for flame measurements with the
solvents commonly used in AAS, such as methyl isobutyl ketone and
white spirit.

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

Spray Chamber Drain

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

GFS35 and GFS35Z Graphite Furnace Systems


The GFS35 and GFS35Z graphite furnace systems are major accessories
that are fitted in the right hand sample compartment of the
iCE 3400/3500 Series spectrometers.

The GFS35 and GFS35Z use an electrically heated graphite cuvette,


enhancing the analytical sensitivity compared to flame atomization by
100-1000 times, and reduce the sample volume required to a few
microliters.

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

Smoke and fumes from the sample decomposition must be extracted


away from the vicinity of the instrument. Refer to the iCE 3000 Series
Pre-Installation Requirements Guide for the specifications of a suitable
extraction system.

NOTICE The extraction system must be switched on and must be operating


correctly before the furnace is used.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-15
System Description
Furnace

Cooling Water

A supply of reasonably clean water, at a temperature of 5 °C below


ambient (and less than 30 °C) and a pressure of 1.4 to 6.9 bar (20 to
100 psi), capable of providing a minimum flow rate of ≥ 1.1 L/min is
required.

NOTICE Do not allow the pressure to exceed 6.9 bar (100 psi).

The recommended water quality is distilled or deionized water of


approximately 18 M/cm³. If the use of water of lower quality cannot
be avoided, at least a suitable fungicide or biocide should be added to
the water.

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.

Labeled Components: 1=cooling water outlet, 2=cooling water filter,


3=cooling water inlet
Figure 3-5. Furnace power supply connections panel

3-16 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
System Description
Furnace

Recirculation Chillers

The specifications of a suitable recirculation chiller are given in the


iCE 3000 Series Pre-Installation Requirements Guide.

GFS33 Graphite Furnace System


The GFS33 graphite furnace system is a major accessory that can be
fitted in the sample compartment of the iCE 3300 Series spectrometers.

It uses an electrically heated graphite cuvette, enhancing the analytical


sensitivity by 100-1000 times compared to flame atomization and
reducing the sample volume required to a few microliters.

The GFS33 accessory includes an integrated furnace autosampler to


automatically inject the sample solutions into the graphite furnace.

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

Labeled Components: 1=wash position, 2=autosampler arm, 3=adjustment


control A, 4=capillary height control, 5=capillary tip, 6=supporting arms,
7=adjustment control B, 8=waste container, 9=wash liquid container,
10=syringe cover, 11=carousel cover, 12=carousel handle, 13=reagent cup
position, 14=sample cup position
Figure 3-6. GFS autosampler

3-18 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
System Description
VP100 Continuous Flow Vapor System

VP100 Continuous Flow Vapor System


The VP100 is an accessory for measuring hydride-forming elements and
mercury with better analytical sensitivity than can typically be obtained
with flame or furnace atomization. See Figure 3-7.

Labeled Components: 1=reagent bottles, 2=measurement cell connection,


3=mains switch, 4=gas liquid separator, 5=connection panel, 6=peristaltic
pump
Figure 3-7. VP100 - general view

The analyte elements in the sample solution are reduced to volatile


hydrides using sodium borohydride and are carried in a carrier gas
stream to a heated measurement cell for measurement.

The measurement cell is normally heated by an air supported acetylene


flame. The EC100 Electrically Heated Atomization Cell accessory can
also be used.

The VP100 can be used to measure mercury as well as the hydride


group elements. Because is it not necessary to use heat for mercury
measurements, the VP100 includes a mercury absorption cell that can
be used in place of the normal T-cell. The mercury absorption cell
improves the sensitivity of the system for mercury measurements by a
factor of about 1.3 relative to the standard T-cell.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 3-19
System Description
VP100 Continuous Flow Vapor System

EC100 Electrically Heated Atomizer


The EC100 Electrically Heated Atomizer is an accessory for use with the
VP100 Continuous Flow Vapor accessory. It replaces the flame heated
measurement cell with an electrically heated atomization cell, so that
vapor measurements can be performed without a flame. It can be fitted
in either sample compartment, using either the right hand or the left
hand sample compartment universal mount.

The accessory consists of two parts:

• EC100 furnace head

• EC100 power supply

1 2

5 4 3

Labeled Components: 1=set temperature (green), 2=actual temperature (red),


3=heat switch, 4=increase/decrease set temperature, 5=mains switch
Figure 3-8. Front panel of EC100

3-20 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
4
Safety

This chapter contains information that is important or your own safety


or the safety of others, and that prevents damage to the instrument.
Read this chapter carefully before you install or operate the instrument
and its accessories, or come into contact with it.

Contents

• Safety Symbols and Signal Words in this Manual on page 4-2

• Safety Symbols on the Instrument on page 4-3

• Intended Use on page 4-6

• Electrical Safety on page 4-8

• Equipment Cleaning and Decontamination on page 4-8

• Spectrometer Safety on page 4-9

• Flame System Safety on page 4-12

• Furnace Safety on page 4-24

• Vapor Safety on page 4-27

• In Case of Emergency on page 4-29

• Residual Hazards on page 4-30

The instrument and accessories described in this manual are designed


to be used by properly trained personnel only.

Adjustment, maintenance and repair of equipment that involves the


removal of covers must only be carried out by qualified Service
Engineers who are aware of the hazards involved.

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

Safety Symbols and Signal Words in this Manual


Notices that concern the safety of the personnel operating the
iCE 3000 Series spectrometers appear different from the main flow of
text. Safety notices include the following:

Always be aware of what to do with and the effect of safety


information.

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.

Observing this Manual


This manual must always be kept near the instrument to be available for
quick reference.

Be sure to read and comply with all precautions described in this


manual.

System configurations and specifications in this manual supersede all


previous information received by the purchaser.
Safety Precautions
For the correct and safe use of the instrument and its accessories, it is
essential that the operating and service personnel follow generally
accepted safety procedures in addition to the specific precautions
specified in this manual. Specific warning and caution statements and
symbols are included in the relevant sections of this manual.

A safety warning triangle means that when operating or exchanging


parts, the correct operating steps, as described in the user
documentation, must be adhered to. Non-observance can cause
accidents, injuries and/or damage to the instrument and accessories.

4-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Safety
Safety Symbols on the Instrument

Safety Symbols on the Instrument


Table 4-1 lists all safety labels on the instrument and their respective
positions. See the indicated safety notices to prevent risk of harm to the
operator and to protect the instrument against damage. If they are
present, read and obey the instructions on the label.

Table 4-1. Safety labels on the instrument


Label Label description Label position

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.

Also refer to “Flame System Safety”


on page 4-12.
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 at the right hand side
using this machine.
Failure to follow operating
instructions could result in
this machine. Failure to follow wall near the drain tube.
death or serious injury.
operating instructions could result in
death or serious injury.

Also refer to “Flame System Safety”


on page 4-12.
WARNING Read and fully understand This label is attached to the inside of
Read and fully understand
operator‘s manual before
operator’s manual before you use the door of the spectrometer.
using this machine.
Failure to follow operating
instructions could result in
this machine. Failure to follow
death or serious injury.
operating instructions could result in
death or serious injury.

Also refer to “Spectrometer Safety”


on page 4-9.
WARNING Read and fully understand This label is attached near the gas
Read and fully understand
operator‘s manual before
operator’s manual before you use connection panel at the left hand side
using this machine.
Failure to follow operating
instructions could result in
this machine. Failure to follow of the instrument.
death or serious injury.
operating instructions could result in
death or serious injury.

Also refer to “Flame System Safety”


on page 4-12.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 4-3
Safety
Safety Symbols on the Instrument

Table 4-1. Safety labels on the instrument


Label Label description Label position

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.

Also refer to “Installation of the


Spectrometer” on page 5-6.
WARNING Hazardous Radiation. Can cause This label is attached to the D2 lamp
Hazardous radiation.
Can cause severe eye
severe eye injury. See manual for cover.
injury.
See manual for safety safety instructions.
instructions.
This label is only applicable for the
Also refer to “Spectrometer Safety” iCE 3400 and iCE 3500
on page 4-9. instruments.
Electric Shock Hazard. Hazardous This label is attached to the rear side
electric voltage capable of causing of the instrument.
personal injury is used in the
instrument. To make sure that the
instrument is free from all electric
current, always disconnect the power
cord of the instrument before you try
any type of maintenance.

Also refer to “Electrical Safety” on


page 4-8.
Hot Surface. Risk of Burn. See This label is attached to the flame
manual for instructions. compartment door.

Also refer to “Flame System Safety”


on page 4-12.

Other Warning Symbols

Other warning symbols may be used on accessories and should be


adhered to.

The covers of the instrument and accessories must only be removed by


qualified, trained Thermo Fisher Scientific Service personnel.

All spare parts and consumable items used must be approved by


Thermo Fisher Scientific.

Some of the chemicals used in Atomic Absorption spectrometry are


corrosive and/or flammable, and samples might be radioactive, toxic
or potentially infective.

Normal laboratory procedures and regulations for handling such


materials should be followed. A complete risk assessment must be
completed for all operations and analysis.

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.

Figure 4-1. Example of rating plate

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.

Observe the following usage guidelines when you operate your


iCE 3000 Series instrument.

• The instrument is designed to be placed on a bench in the


laboratory. It is not designed for the use outdoors.

• The instrument is not designed for use in diagnostic or medical


therapeutic procedures.

If the iCE 3000 Series instrument is used in a manner that is not


specified by Thermo Fisher Scientific, the protection provided by the
instrument could be impaired. Thermo Fisher Scientific assumes no
responsibility and will not be liable for instrument damage and/or
operator injury.

When the safety protection of the instrument has been compromised,


disconnect the instrument from all power sources and secure the unit
against unintended operation.

Notice on the Susceptibility to Electromagnetic Transmissions

Your instrument is designed to work in a controlled electromagnetic


environment. Do not use radio frequency transmitters, such as mobile
phones, in close proximity to the instrument.

4-6 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Safety
Intended Use

Qualified Personnel

Personnel that install or operate iCE 3000 Series atomic absorption


spectrometer must have the following qualifications:

• 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.

Observe the following safety precautions when you operate or perform


service on your instrument:

• The instrument is properly grounded in accordance with


regulations when shipped. You do not need to make any changes
to the electrical connections or to the chassis of the instrument to
ensure safe operation.

• 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.

• Do not turn the instrument on if you suspect that any kind of


electrical damage has incurred. Instead, disconnect the power
cords of atomic absorption spectrometer and accessories and contact a
Thermo Fisher Scientific field service engineer for a product
evaluation. Do not try to use the instrument until it has been
evaluated. Electrical damage may have occurred if the system
shows visible signs of damage, or has been transported under
severe stress.

• Do not place any objects on the instrument—especially not


containers with liquids—unless it is requested by the user
documentation. Leaking liquids might get into contact with
electronic components and cause a short circuit.

Equipment Cleaning and Decontamination


It is the user's responsibility to carry out appropriate cleaning and decon-
tamination of the equipment if hazardous material is spilt on or inside the
equipment.

• Cleaning and decontamination procedures are specified in the


relevant sections of this manual. Also see “Returning Parts” on
page 7-34.

• Before using any other procedures, users should check with the
manufacturers that the proposed method will not damage the
equipment.

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Spectrometer Safety

Spectrometer Safety

Hollow Cathode Lamp Hazards


Hollow cathode lamps present several hazards, which you must be aware
of before using them.

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.

CAUTION Intoxication Hazard. Certain hollow cathode lamps might release


hazardous chemicals if the lamp envelope is broken. Handle and
dispose the hazardous material according to your local regulations for
safe procedures.

Table 4-2. Cathode Material Hazards


Lamp Cathode material hazard
Aluminum N/A
Antimony Toxic by inhalation, skin contact and Ingestion.
Irritant.
Arsenic Toxic by inhalation and ingestion.
Barium Toxic. Flammable on contact with water.
Beryllium Toxic. Serious health damage from prolonged
exposure by inhalation. Irritant to eyes, skin and
respiratory system.
Bismuth Harmful by ingestion.
Boron Harmful by ingestion and contact with open
wounds.
Cadmium Toxic.

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Table 4-2. Cathode Material Hazards, continued


Lamp Cathode material hazard
Cesium Highly toxic (contains lead). Flammable.
Calcium Contact with water releases flammable gas.
Harmful to eyes and skin by contact.
Chromium Might cause sensitization by skin contact.
Cobalt Might cause sensitization by skin contact.
Copper Toxic by ingestion.
Dysprosium Harmful by ingestion.
Erbium Harmful by ingestion.
Europium Contact with water releases flammable gas.
Gadolinium Harmful by ingestion.
Gallium Might cause sensitization by skin contact.
Germanium N/A
Gold N/A
Hafnium Toxic. Mild irritant.
Holmium Harmful by ingestion.
Indium N/A
Iridium N/A
Iron N/A
Lanthanum Contact with water releases flammable gas.
Lead Highly toxic.
Lithium N/A
Lutetium Harmful by ingestion.
Magnesium Contact with water releases flammable gas.
Spontaneously flammable in air.
Manganese Toxic. Might cause sensitization by contact.
Mercury Toxic by inhalation. Cumulative. Prolonged
exposure causes serious health damage.
Molybdenum N/A
Neodymium Harmful by ingestion.
Nickel Might cause sensitization by skin contact.
Niobium N/A
Osmium Highly toxic.
Palladium N/A

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Spectrometer Safety

Table 4-2. Cathode Material Hazards, continued


Lamp Cathode material hazard
Phosphorus N/A
Platinum N/A
Potassium Spontaneously flammable in air. Reacts violently
with water to release flammable gases.
Causes burns on contact with skin.
Praseodymium N/A
Rhenium N/A
Rhodium N/A
Rubidium Highly toxic. Flammable.
Ruthenium N/A
Samarium N/A
Scandium Harmful by ingestion. Irritant.
Selenium Toxic by inhalation and ingestion. Cumulative.
Prolonged exposure causes health damage.
Silicon N/A
Silver N/A
Sodium Spontaneously flammable in air. Reacts violently
with water to release flammable gas.
Causes burns on contact with skin. Highly toxic
(contains lead).
Strontium Contact with water releases flammable gas.
Tantalum N/A
Tellurium Highly toxic.
Terbium Harmful by ingestion.
Thallium Highly toxic by inhalation and ingestion.
Cumulative. Prolonged exposure causes health
damage.
Thorium Radioactive. Irritant.
Thulium N/A
Tin N/A
Titanium N/A
Tungsten N/A
Uranium Radioactive. Highly toxic by inhalation and
ingestion. Cumulative. Prolonged exposure causes
health damage.
Vanadium Might cause sensitization by skin contact.

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Flame System Safety

Table 4-2. Cathode Material Hazards, continued


Lamp Cathode material hazard
Ytterbium Harmful by ingestion.
Yttrium N/A
Zinc Toxic by ingestion.
Zirconium N/A

Flame System Safety


Flame Atomic Absorption Spectrometry (AAS) involves the use of
large quantities of inflammable, explosive and toxic gases, and high
temperature flames. To minimize the hazards involved, read and
understand the contents of this section before using the equipment.

Do not leave a flame AAS instrument unattended while the flame is


burning.

CAUTION Risk of Eye Injury. 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 small explosion associated with noise, flying


debris and fright might take place. In the event of a flashback, the
sound level might reach 145 dBC (peak)/127 dBA. The risk of a
short-time acute hearing loss is given. Wear ear protection. Keep the
door of the flame compartment closed in all occasions when the flame
is burning.

To prevent the occurrence of flashbacks always turn off the flame


before maintenance or adjustment works on the gas supply or drain
system (drain tubing and waste vessel).

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.

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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 Burn Hazard. Nitrous oxide supported flames burn at a high


temperature, and emit large amounts of heat. Keep a safety distance to
the flame to avoid severe burns.

CAUTION Risk of Flashback. Nitrous oxide/acetylene flames can deposit carbon


along the edges of the burner slot, which can build up and partially
block the slot. The probability of a flashback is increased.

A whistling sound can be the precursor of a flashback. Turn off the


flame immediately and verify the requirements for a safe operation of
the flame.

Carbon build up can be reduced by ensuring that the burner is clean,


and by warming up the burner with a fuel lean nitrous oxide flame for
at least 10 minutes before use.

If carbon deposits appear, extinguish the flame immediately and


remove the deposits carefully without causing damage to the burner
slot. An enlarged slot width makes carbon build up more likely.

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

CAUTION Risk of Flashback. A small explosion associated with noise, flying


debris and fright might take place. In the event of a flashback, the
sound level might reach 145 dBC (peak)/127 dBA. The risk of a
short-time acute hearing loss is given. Wear ear protection. Keep the
door of the flame compartment closed when the flame is burning.

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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.

In the event of a flashback, a small explosion occurs in the spray


chamber, rupturing the over-pressure disc at the rear of the spray
chamber. Disconnect all gas and power lines and contact your local
Thermo Fisher Scientific field service engineer. A list of Thermo Fisher
Scientific organizations and agents is given at www.thermofisher.com. A
Flashback Report form must be completed and returned to the address
on the form.

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.

• Avoid perchloric acid in nitrous oxide flames or reduce its


concentration to the minimum acceptable level.

• Avoid silver, gold and copper in samples or reduce their


concentrations to the minimum acceptable level.

• Avoid organic solvents.

• Check for leaks in gas lines and fittings.

• Ensure that the acetylene cylinder is changed when the cylinder


pressure drops to 7 bar (100 psi) to prevent an acetone carryover.

• 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.

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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.

• Reduce the perchlorate ion concentration as much as possible before


aspirating the solution.

• Aspirate the solution for the minimum time necessary.

• Flush the spray chamber thoroughly with deionized water between


measurements.

• Do not allow the spray chamber to run dry.

• Do not allow perchlorate solutions to come into contact with


organic solvents. If organic solvents have previously been aspirated,
ensure that all traces have been removed from the spray chamber
before aspirating perchlorate solutions.

• Thoroughly flush the spray chamber, and empty and refill the drain
trap with clean water at the end of the analysis.

Silver, Gold and Copper Samples


Certain elements, notably silver, gold and copper, form unstable
acetylides, increasing the risk of an explosion or a flashback. To
minimize these hazards when aspirating solutions containing these
elements:

• 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.

• Flush the spray chamber thoroughly with deionized water between


measurements.

• Do not allow the spray chamber to run dry.

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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

CAUTION Risk of Explosion. Many common laboratory solvents are unsuitable


for use in 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.

Do not store organic or volatile solvents near the instrument, not even
for a short time.

Using organic solvents in flame AAS is hazardous. To protect yourself,


carry out a comprehensive risk assessment before performing the
analysis. As a minimum, take the following precautions:

• 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.

• Confirm that the hazards associated with the flashpoint, combustion


products, volatility and toxicity of the solvents are acceptable.

• Use the minimum possible quantity of solvent in the vicinity of the


spectrometer.

• 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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Flame System Safety

Use gloves that are resistant to organic solvents when handling the waste
bottle.

If you use organic solvents on a regular basis, Thermo Fisher Scientific


recommends having the Solvent Resistant Flame Kit fitted to your
instrument.

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.

CAUTION Explosive Components. Risk of injuries. Acetylene and nitrous oxide


in combination with oxygen are highly flammable and can form
explosive compounds. If the gas lines are not appropriate or leak, the
gas can escape unchecked and can cause explosion of the gas line. Be
sure the gas lines are appropriate. Regularly check them for leaks.

Turn off the flame before maintenance or adjustment operations on


the gas supply system. Steady flow rates at the required pressures (as
described in the following) are important for flame safety.

CAUTION When operating the instrument with hazardous gas, an external


warning sensor must be installed in the vicinity of the instrument.

Acetylene

CAUTION An acetylene sensor must be installed in the vicinity of the instrument


for the rare gas of leaks within the gas supply to the instrument.

CAUTION Flammable or Explosive Components. Risk of injuries. Acetylene is


a highly inflammable gas that can form an explosive mixture with air.
It also forms explosive compounds with copper or silver. Contact with
copper, silver, and alloys containing these metals must be avoided.
Fittings, filters, or tubing containing copper, silver, or other
acetylide-forming metals, must not be used.

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Flame System Safety

Acetylene has a strong garlic-like odor caused by inherently present


impurities. Follow the local safety guidelines provided by local
standards and regulation of authorities. Refer to your supplier's
Material Safety Data Sheet (MSDS) for proper handling of acetylene.

The following materials must not be used for parts that will come into
contact with the gas:

• Pure copper metal

• Copper alloys with a copper content above 70%

• Copper alloys with a copper content lower 70%, if used as


- Filters or sieves
- Silver and silver alloys, except where used as brazing materials.
Silver alloys used as a braze must contain less than 43% of silver
and less than 21% of copper. The width of the braze gap
exposed to the acetylene gas must be less than 0.3 mm.
Acetylene is supplied in cylinders dissolved in acetone. As the cylinder
pressure falls, acetone carryover increases.

CAUTION Hazardous Material. Increased carryover of solvents from the


acetylene cylinder might cause severe damage to the instrument and
can cause dangerous situations, like flashbacks, explosions etc.

Although iCE 3000 Series spectrometers can operate with lower


pressures, the acetylene cylinder must be replaced when the internal
pressure drops below 6.9 bar (100 psi). Do not operate the instrument
below 6.9 bar (100 psi)!

NOTICE Some specialist grades of acetylene may be supplied in solvents other


than acetone. The iCE 3000 Series gas control system has not been
designed to withstand carryover of these solvents, which might cause
severe damage to the instrument.

Nitrous Oxide

CAUTION A nitrous oxide sensor must be installed in the vicinity of the


instrument for the rare case of leaks within the gas supply to the
instrument.

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CAUTION Nitrous oxide is an anesthetic, which causes drowsiness,


unconsciousness and eventual death if inhaled. It is a powerful
supporter of combustion, and allows many materials to ignite and
burn more readily than they would in air. Refer to your supplier's
Material Safety Data Sheet (MSDS) for proper handling of nitrous
oxides.

Flame Sample Compartment Door


The door to the flame sample compartment is an important part of the
safety features of your instrument. The flame can be ignited only when
the door is closed. During normal operation the door should be kept
close. If the door is opened during flame operation, an interlock will
shut off the flame automatically for safety reasons.

CAUTION Risk of Flashback. A small explosion associated with noise, flying


debris and fright might take place. In the event of a flashback, the
sound level might reach 145 dBC (peak)/127 dBA. The risk of a
short-time acute hearing loss is given. Wear ear protection. Keep the
door of the flame compartment closed when the flame is burning.

CAUTION Risk of Eye Injury. 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 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

Do not operate the spectrometer without an effective fume extraction


system installed above the sample compartments. The fume extraction
hood must not be attached to the chimney and the air gap between
chimney and fume extraction hood must be 150 mm (6 in.) to
230 mm (9 in.). For dual atomizer instruments with two sample
compartments, two separate extractions are required.

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Flame System Safety

The extraction system must not be affected by external weather


conditions or other equipment connected to the same exhaust system.

Ensure that your laboratory is properly vented and that fresh air for
the exhaust is continuously provided.

Ensure that the exhaust is correctly positioned above the LH


compartment (flame, EC100, T-Cell or mercury cell) and RH
compartment (furnace). Make sure that the ventilation is on before
igniting the flame, using the EC100, T-Cell or mercury cell or before
firing the furnace. Do not run any of those when the ventilation is
turned off.

If the instrument has been mounted on a rolling cart, ensure that it is


positioned below the fume extraction.

All flames produce large quantities of heat and toxic combustion


products. These must be removed by a suitable fume extraction system.
Specifications of a suitable extraction system are provided in the
iCE 3000 Series Pre-Installation Requirements Guide.

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.

The drain must discharge to a low level waste system capable of


handling acidic solutions, or a suitable, wide necked plastic container.
Do not use a glass or a narrow necked plastic waste container. Use
wide neck containers with a volume of 5 L or more that are
standardized for laboratories.

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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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.

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Safety
Flame System Safety

Safety Guidelines for Flame Measurements in Organic Solvents


Before you use your instrument, read the guidelines described at “Flame
Safety” on page 4-13 that concern the safe use of the spectrometer and
the flame atomization system.

If you use organic solvents on a regular basis, Thermo Fisher Scientific


recommends having the Solvent Resistant Flame Kit fitted to your
instrument. See “Solvent Resistant Flame Kit” on page 3-12.

Risk Assessment

The use of organic solvents in flame AAS is a hazardous procedure. As a


minimum:

1. Use the minimum possible quantity of solvent in the vicinity of the


spectrometer.

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.

5. Ensure that the extraction system is operating properly to minimize


the risk of solvent vapors accumulating 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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To minimize the hazards to personnel and equipment, Thermo Fisher


Scientific recommends carrying out a comprehensive risk assessment
before you perform the analysis. At a minimum, this should include
measures to reduce the hazards associated with the risk of:

• accidental spillage of solvent in and around the instrument

• accidental ignition of solvent

• a flashback in the spray chamber

Drain Vessel

Waste solvent draining from the instrument accumulates in the drain


vessel. To minimize the associated hazards, ensure that:

• The drain vessel is made of a material that is resistant to the solvent


used.

• The drain vessel is located in a secure position such that it cannot be


accidentally overturned or its contents spilt.

• The capacity of the drain vessel is no greater than 500 mL, to


prevent accumulation of large volumes of waste solvent. Empty it
frequently.

• 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.

Alternatively, vapors can be removed from the vessel with a suitable


venting system, but it is still important that the vessel has a large
opening and is not sealed in any way.

Slotted Tube Atom Trap

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.

NOTICE Use the STAT only with the 50 mm universal burner.

Do not use nitrous oxide supported flames with this accessory because
this can impede flame safety and result in a flashback.

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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

GFS33/35 and GFS35Z Furnace Heads

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.

GFS35Z Zeeman Furnace Head

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.

CAUTION Strong Magnet. Strong magnetic fields can be harmful to pacemaker


wearers and others with medical implants. If you use a heart
pacemaker, do not stand closer than one meter from the magnet when
the system is operating. Keep all magnetic material and magnetic
storage media at least 30 cm away from the magnet when it is
operating.

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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 Hazardous Gases. Risk of suffocation. Nitrogen and argon might


cause suffocation at high concentrations. Take appropriate care.

CAUTION Hazardous Gases. Risk of injuries. Nitrous oxide is an anesthetic and


if inhaled in large amounts can be fatal. The gas supports combustion
to a higher degree than air and produces highly combustible mixtures
very readily.

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).

Follow the local safety guidelines provided by local standards and


regulation of authorities. All gas lines, fittings and regulators must be
free from oil or grease. Gas cylinders must be fitted with suitable
pressure reducing regulators.

Furnace Measurements in Organic Solvents


If you use organic solvents on a regular basis, Thermo Fisher Scientific
recommends using PTFE sample cups and PTFE sampling capillaries.

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Safety
Furnace Safety

The use of organic solvents in furnace AAS is a hazardous procedure. As


a minimum, take the following precautions:

• Remove any aqueous solutions from the autosampler before


introducing the solvent unless the solvent that you are planning to
use is freely miscible with water.

• Use the minimum possible quantity of solvent in the vicinity of the


spectrometer.

• 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 autosampler has been purged five times.

• 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.

• Empty the waste bottle frequently to minimize the quantity of


solvent in the vicinity of the spectrometer.

• Ensure that the extraction system is operating properly to minimize


the risk of solvent vapors accumulating in the vicinity of the
spectrometer.

• Ensure that the autosampler is leak free.

• 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 The sodium borohydride reagent used is unstable, and gradually


evolves hydrogen on standing. Ensure that any containers used for this
reagent are suitably vented.

NOTICE Do not store the reagent for any length of time.

Flame Heated Atomization Cell

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.

VP 100 Continuous Flow Vapor System

The use of organic solvents with flame AA spectrometry is hazardous.


Ensure that you read and fully understand the hazards and precautions
described at “Flame System Safety” on page 4-12.

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 Hazardous Accumulation. Risk of injuries, flying debris and hearing


loss. All kinds of toxic, corrosive and organic samples can accumulate
in the waste container. The pressure in the waste container can cause
the waste container to burst, or the liquids in the waste container can
return back to the flame compartment with a loud flashback. Use only
waste containers with a wide neck.

CAUTION Hazardous Mixture. Risk of injuries. The mixture in the waste


container might be toxic and/or corrosive, and can be harmful in
contact with the skin. Pay attention to the Material Safety Data Sheets
(MSDS).

CAUTION Hazardous Chemical. Mercury is toxic by inhalation and cumulative.


The exhaust vapors must be extracted from the mercury absorption
cell via a suitable tubing that is connected to a free port of the mercury
absorption cell. Keep the door closed during operation at all times.

EC100 Electrically Heated Atomizer

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.

❖ To shut down the system in case of emergency

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.

flame off button

Figure 4-2. Main switch at spectrometer


P

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.

CAUTION Hazardous Chemicals. Samples and solvents might contain toxic,


carcinogenic, mutagenic, or corrosive/irritant chemicals. Avoid
exposure to potentially harmful materials. Always wear protective
clothing, gloves, and safety glasses when you handle solvents or
samples. Also contain waste streams and use proper ventilation. Refer
to your supplier's Material Safety Data Sheet (MSDS) for proper
handling of a particular compound.

Gases

CAUTION Hazardous Gases. Risk of asphyxiation. Nitrogen and argon gas


might cause asphyxiation at high concentrations. Take appropriate
care.

CAUTION Hazardous Gases. Risk of injuries. Nitrous oxide is an anesthetic and


if inhaled in large amounts can be fatal. The gas supports combustion
to a higher degree than air and will produce highly combustible
mixtures very readily.

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.

CAUTION When operating the instrument with hazardous gas, an external


warning sensor must be installed in the vicinity of the instrument.

Waste

CAUTION Hazardous Accumulation. Risk of injuries, flying debris and hearing


loss. All kinds of toxic, corrosive and organic samples can accumulate
in the waste container. The pressure in the waste container can cause
the waste container to burst, or the liquids in the waste container can
return back to the flame compartment with a loud flashback. Use only
waste containers with a wide neck.

CAUTION Hazardous Mixture. Risk of injuries. The mixture in the waste


container may be toxic and/or corrosive, and can be harmful in
contact with the skin. Pay attention to the material safety data sheets
(MSDS).

4-30 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Safety
Residual Hazards

Personal Protective Equipment


Appropriate safety clothing must be worn at all times while you operate
the instrument, particularly when you handle hazardous material.

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

For handling chemical compounds and organic solvents, Thermo Fisher


Scientific recommends white nitrile clean room gloves from Fisher
Scientific or Unity Lab Services.

For handling hot objects, gloves made of heat-resistant materials (for


example, leather) should be available.

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

This chapter describes the conditions for an operating environment that


will ensure continued high performance of your iCE 3000 Series system
and describes the main installation procedures.

Contents

• Laboratory Conditions on page 5-2

• Installation of the Spectrometer on page 5-6

• Installation of a Hollow Cathode Lamp on page 5-8

• Universal Mount in Right Hand Side Compartment on page 5-10

• Fitting the Left Hand Sample Compartment Universal Mount on


page 5-12

• Installation of the iSQ Module on page 5-14

• Flame System on page 5-17

• Installation of GFS35 and GFS35Z Furnace System on page 5-27

• Installation of the GFS33 Graphite Furnace System on page 5-31

• Installation of VP100 Continuous Flow Vapor System on page 5-38

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

The spectrometer will require an electrical supply at 100 to 240 VAC,


300 VA, 50/60 Hz. The spectrometer will be supplied with a 2 m mains
cord with USA type or Non USA (rest of world) type coding. USA
coding is black (X - ac high), white (Y - ac low), green
(G - earth/ground). Rest of World coding is blue (neutral), brown (live),
green/yellow (earth/ground).

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.

The furnace power supply unit should be connected to a supply with an


impedance of 0.124  or less. It is the responsibility of the user of the
unit to ensure by consultation with the local supply authority if
necessary, that the unit is connected to this type of supply.

Others

An additional 200/208/220-240 VAC, 1.5 kVA, 50/60 Hz supply is


required for the Zeeman furnace power supply unit (see label near
appliance inlet for individual voltage setting).

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.

Tip As the laboratory temperature increases, system reliability


decreases. All electronic components generate heat while operating.
This heat must be dissipated to the surrounding air for the
components to continue to operate reliably.

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.

Thermo Fisher Scientific recommends that your laboratory be equipped


with a temperature/humidity monitor to ensure that your laboratory is
always within the required temperature and humidity specifications.

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 exhaust system must fulfill the following requirements:

Over the Flame

• The entire extraction system must not be made of flammable


material.

• 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).

• The extraction system and ducting up to the fan must be made of


stainless steel.

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.

• No cables, plastics or other materials that can melt at temperatures


below 100 °C must be in contact with the outer surface of the duct
(even within suspended ceilings or behind other covers).

• A centrifugal fan, preferably with plastic coated metal blades, must


be fitted into ducting connected to the hood over the flame.

• The fan must be at least 6 m away from the hood (measured


through the duct).

• A flow rate of at least 2800 L/min (100 ft3/min) through the duct
over the flame must be ensured.

• Thermo Fisher Scientific strongly recommends installing an


automatic supervision of the air flow.

• If it can be ensured that the flow rate is at least 10000 L/min


(355 ft3/min) and/or that only acetylene flames are used, the
distance between hood and fan can be reduced to 3.5 m.

• The temperatures that effectively appear within the duct depend on


several factors. Therefore, Thermo Fisher Scientific strongly
recommends measuring the resulting temperatures within the duct
and at the fan under worst case conditions in the final installation,
to ensure proper dimensioning of the exhaust system.

Additional Considerations

Additional considerations for multiple installations where the tubes end


up into a single fan or duct are:

• The overall sum of temperatures must be taken into account.

• 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.

For Dual Atomizer

• For instruments with two sample compartments, two separate


extractions are required. Also see “Additional Considerations” on
page 5-4.

• 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.

CAUTION Hazardous Gases. Risk to health. The instrument must not be


installed in a normal chemical fume cupboard as the ventilation is
likely to be inadequate, and any other chemical operation may damage
the spectrometer.

Local regulations may require to perform a risk analysis.

Air

The spectrometer requires clean dry compressed air at a steady pressure


of 2.75 bar (40 psi). If the graphite furnace is using air as an oxidant, it
requires a pressure of 1.1 bar (15 psi).

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-5
Installation
Installation of the Spectrometer

Installation of the Spectrometer


Figure 5-1 shows a schematic front view of a Thermo Scientific
iCE 3000 Series spectrometer with important instrument controls.

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.

Table 5-1. Spectrometer dimensions and weights


Spectrometer Width Depth Height Weight
iCE 3500 780 mm 577 mm 595 mm 54 kg
(30.1 in) (22.7 in) (23.4 in) (119 lbs)
iCE 3400 780 mm 577 mm 520 mm 54 kg
(30.1 in) (22.7 in) (20.5 in) (119 lbs)

5-6 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of the Spectrometer

Table 5-1. Spectrometer dimensions and weights, continued


Spectrometer Width Depth Height Weight
iCE 3300 567 mm 589 mm 595 mm 45 kg
(22.3 in) (23.2 in) (23.4 in) (99 lbs)
iCE 3300GF 567 mm 589 mm 510 mm 38 kg
(22.3 in) (23.2 in) (20.1 in) (84 lbs)

The installation of an iCE 3000 Series spectrometer consists of the


following procedures:

• Installation

Your spectrometer must be installed and tested by a Thermo Fisher


Scientific field service engineer.

The boxed spectrometer, the graphite furnace and the power


supply should be moved with a mechanical lift. To distribute the
weight, two people should lift the equipment from the box. Take
care in doorways, corridors or when lowering to avoid trapping
fingers.

• Data Station installation

For instructions about installing the data station, refer to the iCE
3000 Series AA Spectrometers SOLAAR Software Manual.

• Data Station printer installation

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

Installation of a Hollow Cathode Lamp


❖ To install a hollow cathode lamp

1. Turn on the system.

2. Start the Data Station software.

3. Use the Lamp commands in the system software to rotate the


carousel to bring an empty lamp position to the front.

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.

6. Align the lamp correctly.

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.

9. Close the lamp carousel door.

Labeled Components: 1=hollow cathode lamp, 2=lamp clip, 3=lamp ejection


lever, 4=lamp socket
Figure 5-2. Lamp compartment - general view

5-8 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of a Hollow Cathode Lamp

Removal of a Hollow Cathode Lamp


❖ To remove a hollow cathode lamp

1. Turn on the system.

2. Start the Data Station software if required.

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.

5. Open the lamp carousel door.

6. Press the lamp ejection lever downward to eject the lamp.

7. Release the lamp from the clip and remove it.

8. Close the lamp carousel door.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-9
Installation
Universal Mount in Right Hand Side Compartment

Universal Mount in Right Hand Side Compartment

Fitting an Accessory to the Universal Mount


Fit the accessory to the universal mount before installing the assembly in
the right hand sample compartment.

❖ To fit the accessory to the universal mount

1. Tilt the graphite furnace forward on the tilt mount or remove the
graphite furnace on its fixed mount.

2. Place the universal mount assembly in the right hand sample


compartment, locating the adjustment screws on the sample
compartment mounting pads. See Figure 5-3.

3. Use the supplied tool to push the spring retainer into the location
plate.

4. Give it one quarter turn to lock the assembly in position.

Reverse this procedure to remove the assembly.

Alignment of a Fitted Accessory


Accessories fitted to the universal mount normally require alignment
with the spectrometer optical system. Once the alignment has been set
up and locked, the universal mount and accessory assembly can be
removed and replaced without disturbing the alignment.

❖ To align an accessory fitted to the universal mount

1. Ensure that the right hand sample compartment optical path is clear
of obstruction.

2. Fit a suitable hollow cathode lamp.

3. Use the system control software to set up the optical system in the
right hand sample compartment.

NOTICE Do not select any form of background correction.

4. Use the system control software to display the live absorbance signal
from the right hand sample compartment.

5. Fit the universal mount and accessory assembly.

6. If necessary, fit a suitable absorption cell in the accessory.

7. Use a piece of white card to locate the optical beam in the sample
compartment.

5-10 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Universal Mount in Right Hand Side Compartment

8. Adjust the position of the assembly using the adjustment screws


until the light beam passes through the accessory.

The long-handled, ball-ended hex key tool is helpful when adjusting


the rear adjustment screw.

9. Make fine adjustments to the position of the assembly to obtain a


minimum in the displayed absorbance signal.

1 2

4 3

Labeled Components: 1=adjustment screw, 2=accessory mounting pin,


3=location plate, 4=mounting pads, 5=spring retainer
Figure 5-3. Right hand sample compartment with universal mount

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

Fitting the Left Hand Sample Compartment Universal Mount


The accessory mount is fitted in the left hand sample compartment.

❖ To fit the left hand sample compartment universal mount

1. If necessary, use the appropriate software commands to move the


burner to the Parked position.

2. If necessary, remove the burner head as described in “Flame System”.

3. Orientate the universal mount correctly.

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.

Reverse this procedure to remove the assembly.

Alignment of a Fitted Accessory


Accessories fitted to the universal mount should be aligned with the
optical system of the spectrometer before the accessory is used. When
the alignment has been completed, it is possible to remove and replace
the mount and accessory without re-alignment.

❖ To align an accessory fitted to the universal mount

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.

2. Fit a suitable hollow cathode lamp.

3. Use the appropriate software commands to set up the optical system


in the left hand sample compartment.

NOTICE Do not select any form of background correction.

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.

6. If necessary, fit a suitable absorption cell in the accessory.

7. Use a piece of white card to locate the optical beam in the sample
compartment.

5-12 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Fitting the Left Hand Sample Compartment Universal Mount

8. Adjust the position of the assembly using the adjustment screws


until the light beam passes through the accessory.

You need the 3 mm ball-ended hex key to adjust the screws.

9. Make fine adjustments to the position of the assembly to obtain a


minimum in the displayed absorbance signal.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-13
Installation
Installation of the iSQ Module

Installation of the iSQ Module


NOTICE Observe the electrical safety precautions described in Chapter 4,
“Safety.”

❖ To prepare the iSQ Module for use

1. Fasten the iSQ Module to the support bracket using the two
supplied screws.

2. Attach the assembly to the relevant mount using the accessory


mounting points.

3. Connect one end of the 9-way data lead to the data socket on the
iSQ Module.

4. Tighten the locking screws.

5. Fit the round plug from the power supply in the power socket on
the iSQ Module.

6. Connect the mains lead to the power supply.

4 3

Labeled Components: 1=ISQ module, 2=serial port,


3=power connector, 4=shutter, 5=RH accessory mount,
6=support bracket
Figure 5-4. iSQ Module assembly (iCE 3400/3500
systems)

5-14 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of the iSQ Module

❖ To install the iSQ Module in the spectrometer

1. If a graphite furnace is fitted to the system:

• iCE 3300 system

Remove the GFS33 Furnace and autosampler assembly.

• iCE 3400/3500 system

If the furnace head is fitted on a tilt mount, tilt the furnace head
forward out of the sample compartment.

If the furnace head is fitted on a fixed mount, remove the


furnace and the fixed mount from 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.

Check that the green LED on the power supply is illuminated.

During a normal start, the red LED 3 on the iSQ Module flashes
whereas LEDs 1 and 2 are extinguished.

Table 5-2 lists other LED indications.

Table 5-2. Other LED indications


Behavior of LED Indication
LED 1 lit flash checksum test failed
LED 2 lit RAM test failed
LED 3 lit continuously fatal error has occurred

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-15
Installation
Installation of the iSQ Module

Alignment of the iSQ Module


The iSQ wizard in the SOLAAR Data Station software provides
facilities for aligning the iSQ Module. When the iSQ Module has been
correctly installed, you can carry out the alignment and the suite of
iSQ Test procedures by running the iSQ wizard.

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

1. Turn on the spectrometer.

2. Turn on the power to the iSQ Module.

3. Open the shutter of the iSQ Module.

4. Start the SOLAAR Data Station software.

5. Start the iSQ wizard.

6. Follow the instructions on screen until you reach the Install and
Align Lamps page.

7. Install the Ca/Mg lamp supplied with the iSQ Module.

8. Use the commands on the wizard to perform an optical setup.

9. Carry out the alignment procedure described in the RH Accessory


Mount section.

If the assembly is a long way out of alignment, it may be necessary to


remove the iSQ Module and universal mount assembly to allow the
initial optical setup to be completed successfully.

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.

Gas Supply Inlet Pressures


Adjust the gas supply regulators to deliver the gases at the spectrometer
inlet ports at the pressures listed in Table 5-3.

Table 5-3. Gas pressures at spectrometer inlet ports


Gas type Pressure and gas Pressure value
support gases nominal pressure of compressed air 2.4 to 2.75 bar
(35 to 40 psi)
nominal pressure of nitrous oxide 2.70 to 2.75 bar
(39 to 40 psi)
fuel gases maximum allowed pressure of 0.57-0.62 bar
acetylene (8.5-9 psi)

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

CAUTION When operating the instrument with hazardous gas, an external


warning sensor must be installed in the vicinity of the instrument.

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

Three gas inlet connections are provided on the spectrometer.


Figure 5-5 shows the spectrometer gas connection panel.

Figure 5-5. Spectrometer gas connection panel

Air/Acetylene Flame

NOTICE An acetylene sensor must be installed in the vicinity of the instrument


for the rare case of leaks within the gas supply to the instrument.

❖ To establish air and acetylene supply

1. Connect the air supply to the connector marked Air using the clear
hose supplied.

2. Connect the acetylene supply to the connector marked Fuel using


the red hose supplied.

Nitrous Oxide/Acetylene Flame

NOTICE A nitrous oxide sensor must be installed in the vicinity of the


instrument for the rare case of leaks within the gas supply to the
instrument.

❖ To establish nitrous oxide and acetylene supply

1. Connect the air supply to the connector marked Air using the clear
hose supplied.

2. Connect the acetylene supply to the connector marked Fuel using


the red hose supplied.

3. Connect the nitrous oxide supply to the connector marked N2O


using the blue hose supplied.

Installation of Burner
❖ To install a burner

1. Open the left hand sample compartment door.

2. Orientate the burner so that the ignition electrode is to the rear of


the burner.

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Installation
Flame System

3. Fit the burner to the spray chamber stem. Push firmly home.

NOTICE Avoid damaging the O-ring seals.

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.

2. Disconnect the burner plug from the burner socket.

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.

Installation of the Air Compressor


❖ To install the air compressor

1. Confirm that your compressor is suitable for the mains supply in


your laboratory. See Table 5-4.
Table 5-4. Part numbers and mains voltages of compressors
P/N of compressor mains voltage
9423 393 34225 220 V/50 Hz nominal
9423 393 34226 220 V/60 Hz nominal
9423 393 34115 110 V/50 Hz nominal
9423 393 34116 110 V/60 Hz nominal

2. Fit a suitable plug to the mains cable.

3. Place the compressor in a well ventilated position close to the


spectrometer.

4. Use the black connecting hose to connect the compressor outlet to


the filter/regulator inlet.

5. Position the hose so that it is:

• free from bends

• away from heat sources

• not possible for condensation to run back into the compressor.

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Installation
Flame System

6. Connect the clear air hose from the outlet of the filter/regulator unit
to the spectrometer air inlet connector.

7. The compressor is now ready to use.

NOTICE Do not shorten the pipe.

Installation of the CETAC ASX-560 and ASX-280 Flame Autosampler


❖ To assemble the autosampler

1. Unpack and assemble the unit as described in the user


documentation of the autosampler supplied with the unit.

The user documentation of the autosampler may be provided in


electronic form on a CD together with the parts sent with the
autosampler.

2. Position the autosampler on the accessory trolley or on the bench in


front of the appropriate sample compartment.

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.

Two types of uptake tube are supplied - one with an internal


diameter of 0.5 mm and one with an internal diameter of 0.8 mm.
The 0.5 mm ID uptake tube is suitable for general purpose use, but
causes some loss of analytical sensitivity, particularly when longer
lengths are used. In these circumstances, using the 0.8 mm ID
uptake tube restores the sensitivity.

4. Connect the rinse station. Either configuration may be used.

❖ To establish the system interconnections

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.

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Installation
Flame System

Figure 5-6 shows the CETAC ASX-560 autosampler in rear view.

serial port

Figure 5-6. CETAC ASX-560 - rear view (Source: ASX-560/ASX-280


Autosampler Operator’s Manual, Teledyne Cetac)

2. Connect a suitable mains cable to the in-line mains power supply.

3. Connect the power supply output to the power connection on the


unit.

❖ To connect the capillary tubing

1. Select the appropriate sample transfer tube interface.

2. Connect the sample transfer tube to the autosampler.

3. Connect the free end of the tube as follows:

• Normal flame operation: cut back the tube to the minimum


convenient length and connect the free end to the nebulizer.
• Other accessories: refer to the appropriate accessory page.

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

❖ To prepare the sample racks

1. Assemble the sample racks required. Place them in the sample tray.
All the sample racks must be of the same type.

2. Place the appropriate sample tubes into the racks as listed in


Table 5-5.

Table 5-5. Placement of sample tubes in racks


Sample positions in rack Tube diameter
21 30 mm
24 25 mm

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Installation
Flame System

Table 5-5. Placement of sample tubes in racks, continued


Sample positions in rack Tube diameter
40 20 mm
60 16 mm
90 13 mm

3. Place the standard tubes into the rear standards rack.

Figure 5-7 shows the CETAC ASX-560 sample changer in front view.

2
1

4 3

Labeled Components: 1=arm, 2=rinse station, 3=sample tray, 4=sample rack


Figure 5-7. CETAC ASX-560 autosampler - front view (Source:
ASX-560/ASX-280 Autosampler Operator’s Manual, Teledyne
Cetac)

5-22 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Flame System

Installation of the ID100 Autodilutor


Before installing your autodilutor, familiarize yourself with the parts
shown in Figure 5-8 and Figure 5-9.

1 1
2

Labeled Components: 1=port labels, 2=nebulizer tube, 3=port A, 4=port B,


5=mixing piece, 6=diluent uptake tube, 7=sample uptake tube, 8=power
indicator
Figure 5-8. ID100 Autodilutor - general view

1 2

Labeled Components: 1=RS232C serial port, 2=power inlet, 3=power switch


Figure 5-9. ID100 Autodilutor - rear view

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 5-23
Installation
Flame System

❖ To install the ID100 autodilutor

1. Place the ID100 autodilutor in a convenient position in front of the


spectrometer flame compartment.

2. Connect a suitable power lead between the power inlet socket and a
power outlet.

3. Connect an RS-232C cable between the RS-232C port on the


accessory and an accessory port on the Spectrometer Connection
panel.

4. Nebulizer tubing

Locate the 1.5 mm OD, 0.5 mm ID polyethene nebulizer tubing:


Connect one end to the mixing piece using one of the white finger
nut and ferrule connectors in the plumbing kit. Cut the tube to
length, and fit the free end to the nebulizer.

5. Mixing Piece - Port B


Locate the 1.5 mm OD, 0.8 mm ID PTFE tubing. Fit a suitable
length between the Port B of the Autodilutor and port 2 of the
mixing piece. Use a white finger nut and ferrule connector at the
mixing piece, and a gray 10/32 miniature fitting at the Autodilutor
end.

6. Diluent tubing

Locate the 3.2 mm OD wide bore PTFE tubing supplied. Fit it to


the remaining free port of the mixing piece, using the red finger nut
and ferrule connector. Trim the tube to a suitable length and place
the free end in the diluent container.

Manual Sampling

Fit a suitable length of 0.8 mm ID PTFE tubing to Port A of the


autodilutor using a gray miniature 10/32 connector.

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.

❖ To fit a miniature 10/32 connector

1. Use a sharp blade to trim the end of the 1.6 mm OD tubing to a


shallow taper.

2. Slide the nut over the tubing.

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.

7. Tighten the nut until the assembly is secure.

Installation of the Slotted Tube Atom Trap


The STAT tube is held in the flame by the STAT holder, which clips to
the burner.

❖ To install the STAT holder

1. Remove the burner from the spectrometer.

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.

6. Re-fit the burner to the spectrometer.

❖ To fit a STAT tube to the STAT holder

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

operating position parked position

Figure 5-10. STAT tube and STAT holder

Figure 5-11. STAT assembly

Alignment of the STAT Tube


❖ To align the STAT tube

1. With the burner and the STAT holder fitted to the spectrometer, fit
a STAT tube to the holder.

2. Move the holder to the Parked position.

3. Install a suitable hollow cathode lamp. Perform an optical setup.


4. Move the holder to the Operating position.

5. Use a piece of white card at the right hand side of the sample
compartment to locate the light beam.

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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.

7. Close the lamp compartment door.

Installation of the Solvent Resistant Flame Kit


The Solvent Resistant Flame Kit will be installed at our factory, if you
specified it on your original spectrometer order.

Alternatively, it can be installed as a field upgrade by a Thermo Fisher


Scientific field service engineer who has been properly trained and
authorized to do this work by Thermo Fisher Scientific.

NOTICE Do not install the Solvent Resistant Flame Kit yourself.

Installation of GFS35 and GFS35Z Furnace System


The GFS33/GFS35 and GFS35Z furnace systems must be installed in
your spectrometer by a trained Thermo Fisher Scientific field service
engineer.

Furnace Head Mounts

The GFS35 furnace can be supplied with either a fixed head mount or
with a tilting head mount.

The GFS35Z furnace is always supplied 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

Fitting and Removing the GFS35 on the Fixed Mount

Occasionally, it may be necessary to remove the GFS35 furnace from


the fixed mount to gain better access to the head for cleaning and
maintenance, or to fit an accessory in the right hand sample
compartment.

1
2

9
3

7
7

Labeled Components: 1=clamping lever, 2=sample injection port,


3=right-hand window, 4=conduit, 5=head securing screws, 6=mounting pads,
7=alignment screws (not visible), 8=center block, 9=left hand window
Figure 5-12. GFS35 furnace head on a fixed mount

❖ To remove the GFS35 furnace head from the fixed mount

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.

To refit the head, reverse the procedure.

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Installation
Installation of GFS35 and GFS35Z Furnace System

Electrical Connections

❖ To establish the 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.

2. Connect the furnace power supply mains lead to a suitable mains


outlet (minimum 30 A).

NOTICE The GFS35Z unit requires a second mains power connection to


supply the Zeeman magnet drive board

Optical Alignment of the Furnace Head

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.

❖ To align the furnace head

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.

2. Install a suitable hollow cathode lamp.

3. Set up a furnace method.

4. Set up the optical system in the normal way.

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.

6. Return the furnace head to its normal operating position.

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Installation
Installation of GFS35 and GFS35Z Furnace System

7. Use the positioning controls to adjust the position of the furnace


head to obtain a minimum in the absorbance signal. See
Figure 5-13.

1 3

5
7

Labeled Components: 1=magnet pole pieces, 2=center block, 3=sample


injection port, 4=right hand window, 5=clamping lever, 6=conduit, 7=vertical
adjustment control, 8=magnet securing bolt, 9=transverse adjustment screw
(not visible)
Figure 5-13. GFS35Z furnace head on a tilt mount

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.

With the windows in place, you should be able to obtain a


minimum absorbance value of below 0.1 absorbance units when the
furnace head is correctly aligned.

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Installation
Installation of the GFS33 Graphite Furnace System

Installation of the GFS33 Graphite Furnace System


Your GFS33 graphite furnace system must initially be installed by a
trained Thermo Fisher Scientific field service engineer, who establishes
all the necessary connections to the services and aligns the instrument
ready for use. This information is useful if you have to move the system
to another location, or otherwise re-install it. See “Maintenance of the
GFS33 System” on page 7-27.

Removing and Fitting the GFS33


You have to remove the GFS33 assembly if you want to use the flame or
vapor atomization systems on your spectrometer. When not fitted in the
sample compartment of the spectrometer, the GFS33 should be parked
between the left hand side of the spectrometer and the furnace power
supply.

❖ To remove the GFS33

1. Identify the securing screw at the top rear of the mount.

2. Loosen the securing screw to release the assembly from the rear wall
of the sample compartment.

Do not disturb the setting of the transverse alignment nut.

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.

5. If applicable, fit the flame or vapor atomization system that you


want to use. See the appropriate section of this manual.

6. If appropriate, fit the sample compartment door.

❖ To fit the GFS33

1. If applicable, use the system software to move the burner to the


Parked position.

2. If applicable, remove the burner or the vapor atomization accessory.


See the appropriate section of this manual.

3. If applicable, remove the sample compartment door by lifting it off


its hinges.

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.

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Installation
Installation of the GFS33 Graphite Furnace System

5. Secure the GFS33 in the sample compartment with the securing


screw on the rear of the mounting assembly.

Do not disturb the setting of the transverse alignment nut.

6. The GFS33 is ready for use.

Alignment of the Furnace Head of the GFS33 System


Routine alignment of the GFS33 should seldom be required. However,
it is good practice to check the alignment if a component has been
replaced, and as part of the routine maintenance procedures for your
instrument.

❖ To align the furnace head of the GFS33 System

1. Remove the GFS33 from the sample compartment.

It is helpful to remove the furnace head windows, although this is


not essential. The windows are held in place on an O-ring seal.
Remove each window by grasping the window mount, and twisting
and pulling until the window mount is free.

2. Install a suitable hollow cathode lamp.

3. Set up a furnace method.

4. Set up the optical system in the normal way.

NOTICE Do not select any form of background correction.

5. Set up the system software to display the live absorbance signal.

6. Confirm that the display shows zero. Use the auto-zero command if
necessary.

7. Replace the GFS33 in its normal operating position.

8. Use the transverse and vertical position adjustment controls to


adjust the position of the furnace head so that the light beam passes
through the cuvette. See Figure 5-14.

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Installation
Installation of the GFS33 Graphite Furnace System

Labeled Components: 1=transverse adjustment control, 2=RHS vertical


adjustment access port, 3=LHS vertical adjustment access port
Figure 5-14. Furnace adjustment controls of GFS33

9. Make final adjustments of each of the controls to obtain a minimum


of the displayed absorbance signal.

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.

With the windows in place, you should be able to obtain a


minimum absorbance value of below 0.1 absorbance units when the
furnace head is correctly aligned.

❖ To align the autosampler capillary tip

1. Ensure that the graphite furnace is correctly aligned before you align
the capillary tip.

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Installation
Installation of the GFS33 Graphite Furnace System

2. Locate the capillary tip adjustment controls A and B. See


Figure 5-15.

Labeled Components: 1=capillary tip height adjuster, 2=autosampler


adjustment A, 3=autosampler adjustment B
Figure 5-15. Autosampler adjustments of GFS33

3. Use the Align Capillary Tip 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:

Control A moves the tip diagonally across the sample compartment


from the rear left to the front right.

Control B moves the tip diagonally across the sample compartment


from the rear right to the front left.

5. Use a dentists mirror or the GFTV image to view the capillary tip
inside the cuvette.

6. Loosen the adjustment lock nut.

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.

You may have to optimize the capillary depth setting further by


observing a sample injection.

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Installation
Installation of the GFS33 Graphite Furnace System

8. Lock the adjustment screw with the adjustment lock nut.

9. Use the Park Capillary Tip command to return the autosampler


arm to its normal parked position.

10. Align the probe automatically by selecting the Align Probe


command in the SOLAAR software.

You may need to make fine adjustments to the position of the


capillary tip. Repeat if necessary.

Fitting the Cuvettes


Handle new cuvettes carefully to avoid contamination.

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

1. Unclamp the furnace head by turning the clamping lever. See


Figure 5-13.

2. Remove the old 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.

5. Check that the cuvette injection hole is positioned correctly. If


necessary, unclamp the furnace head and rotate the cuvette slightly.
Use the cuvette tool to make the injection hole central in the furnace
head injection port.

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.

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Installation
Installation of the GFS33 Graphite Furnace System

Installation of the GFS Autosampler


❖ To fit the GFS autosampler (GFS35 and GFS35Z)

1. Fit and align the GFS35 or GFS35Z graphite furnace system.


Ensure that the furnace head is in the normal operating position.

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.

❖ To remove the GFS autosampler (GFS35 and GFS35Z)

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.

3. Place the autosampler upright on the bench.

Gas Connection

The autosampler wash facility is pressurized by an inert gas supply


routed through the furnace power supply unit.

❖ To connect the autosampler gas supply

1. Locate the autosampler gas inlet tube.

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.

❖ To connect the autosampler to the furnace power supply

1. Locate the autosampler connection cable.

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

❖ To connect a permanent drain

1. Remove the waste container.

2. Locate the waste tube that discharges into the waste container.

3. Use the connector and spare length of Tygon tubing supplied to


extend the waste tube as required.

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.

❖ To fit the carousel cover feet

1. Locate the three feet supplied.

2. Fit the feet to the carousel cover. See Figure 5-16.

feet

Figure 5-16. Carousel cover of GFS autosampler

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Installation
Installation of VP100 Continuous Flow Vapor System

Installation of VP100 Continuous Flow Vapor System


❖ To prepare the installation

• Power supply: connect the unit to a suitable mains supply via the
main cable supplied.

• Control signals: connect the serial cable supplied between the


RS-232C connection on the rear of the unit and a free accessory
port on the spectrometer connection panel.

• 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.

• Drain: Connect a suitable length of the 3.2 mm ID Tygon drain


tubing supplied, from the drain outlet on the front of the unit,
identified with a black connector, to a suitable low level drain or
wide necked plastic container.

CAUTION Do not mix the waste from vapor analysis with waste from other
analyses.

CAUTION Hazardous Accumulation. Risk of injuries, flying debris and


hearing loss. All kinds of toxic, corrosive and organic samples can
accumulate in the waste container. The pressure in the waste
container can cause the waste container to burst, or the liquids in
the waste container can return back to the flame compartment
with a loud flashback. Use only waste containers with a wide neck.

CAUTION Hazardous Mixture. Risk of injuries. The mixture in the waste


container might be toxic and/or corrosive, and can be harmful in
contact with the skin. Pay attention to the Material Safety Data
Sheets (MSDS).

• 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

The VP100 can conveniently be supported on the accessory trolley if


the bench is not deep enough.

1 2 3

4
7 6 5

Labeled Components: 1=gas liquid separator, 2=reagent bottles, 3=bottle


tray, 4=gas inlet, 5=RS232C connector, 6=mains inlet, 7=mains switch
Figure 5-17. VP100 - rear view

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.

Sample Uptake Capillary Tube


The sample uptake tubing must be attached to the green sample uptake
connector on the front panel of the VP100 using a short piece of the
thick-walled silicone tube supplied.

• Manual sampling. Take a suitable length of the PTFE sample


uptake tubing supplied and connect it to the VP100 sample uptake
connector.

• Autosampler. Connect the tube from the autosampler sample probe


to the VP100 sample uptake connector.

If you are using a CETAC autosampler, Thermo Fisher Scientific


recommends using the larger 0.8 mm ID sample probe and uptake
tube supplied with the autosampler.

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Installation
Installation of VP100 Continuous Flow Vapor System

❖ To connect the sample uptake tube

1. Locate the thick-walled silicone tubing supplied, and cut off a piece
15-20 mm long. See Figure 5-18.

1 2

Labeled Components: 1=connector, 2=thick walled silicone tubing, 3=PTFE


sample tubing
Figure 5-18. Sample uptake tubing connection

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.

Use a drop of water to lubricate the tubing, if necessary.

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.

Table 5-6. Four channel peristaltic pump and color-coded connectors


Channel Bridges Tubing ID Tubing OD
black channel (drain) black/white 3.17 mm 4.85 mm
green channel (sample) two green 1.85 mm 3.53 mm
red channel (reductant) two black 0.76 mm 2.43 mm
blue channel (acid) yellow/orange 0.50 mm 2.33 mm

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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 red (reductant reagent) channel must be fitted with pump


tubing with two black bridges. This tubing has an ID of 0.76 mm
and an OD of 2.43 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

Labeled Components: 1=clamp arms, 2=pressure screws, 3=plungers,


4=reductant channel RED connector BLACK/BLACK pump tubing, 5=acid
channel blue connector ORANGE/YELLOW pump tubing, 6=sample channel
BLACK connector BLACK/WHITE pump tubing, 7=drain channel BLACK
connector BLACK/WHITE pump tubing, 8=bridge retaining pillars, 9=drain
outlet BLACK connector, 10=sample inlet GREEN connector
Figure 5-19. VP 100 connection panel and peristaltic pump

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

connection panel. Fit a short length of the 1.6 mm ID Tygon tubing


supplied over the ends of the pump tubing. Then fit that to the VP100
connectors. See Figure 5-20.

Labeled Components: 1=ORANGE/YELLOW or BLACK/BLACK pump tubing,


2=1.6 mm ID Tygon tubing, 3=connector
Figure 5-20. Pump tubing connection

❖ To attach a 1.6 mm ID Tygon tubing to the pump tubing

1. Take a piece of 1.6 mm ID Tygon tubing and expand one end.

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.

3. Trim back the Tygon tubing to about 15 mm.

4. Repeat for the other end of the pump tubing.

❖ To fit the pump tubing

1. Fit the pump tubes from the rear of the connection panel towards
the front, in the following order:

a. Reductant channel (red connectors; pump tubing with black


bridges)

b. Acid channel (blue connectors; pump tubing with


yellow/orange bridges)

5-42 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of VP100 Continuous Flow Vapor System

c. Sample channel (green connectors; pump tubing with green


bridges)

d. Drain channel (black connectors; pump tubing with


black/white bridges)

2. Release the plungers to free the clamp arms.

3. Move the arms anti-clockwise to reveal the pump rollers.

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.

7. Move the clamp arm back over the rollers.

8. Confirm that the tubing is properly located beneath it.

9. Return the plunger to the normal position.

10. Adjust the pressure screw to release the pressure on the tubing.

❖ To adjust the peristaltic pump tube pressure

1. Turn on the spectrometer, data station and VP100.

2. Turn on the inert gas supply to the VP100.

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.

7. Set an appropriate value for the carrier gas flow rate.

8. Set the pump speed to 30 rpm.

9. Use the commands on the Action menu in the system software to


turn on 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.

Gas Liquid Separator


The reaction zone of the gas liquid separator contains 4 mm glass beads
which minimize the dead volume of the zone and ensure proper mixing
of the carrier gas and liquid reagents. It also contains an hydrophobic
Teflon membrane to prevent moisture and salts from being carried over
into the measurement cell.

These parts are supplied with the VP100. They must be fitted before the
accessory is used.

❖ To prepare the gas liquid separator

1. Unscrew the top cap of the gas liquid separator. See Figure 5-21.

Labeled Components: 1=top cap, 2=O-ring seal, 3=hydrophobic membrane,


4=Teflon coated face, 5=reaction zone, 6=drain channel BLACK connector,
7=reductant channel RED connector, 8=acid channel BLUE connector,
9=sample channel GREEN connector
Figure 5-21. VP100 gas liquid separator

5-44 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Installation
Installation of VP100 Continuous Flow Vapor System

2. Add a sufficient quantity of the 4 mm glass beads supplied to fill the


reaction zone. There should be no beads on the floor of the
expansion volume.

Prevent the glass beads from falling into the drain where they may
cause blockage.

3. Take one of the 47 mm Teflon membranes supplied. Orientate it


such that the Teflon covered face is on the underside and place it in
position.

4. Carefully re-fit the O-ring seal and the top cap, ensuring that the
position of the membrane is not disturbed.

Flame Heated Measurement Cell


The flame heated measurement cell (T-cell) is supported over the
universal burner by the T-cell holder. See Figure 5-22.

operating position parked position

Labeled Components: 1=T cell, 2=burner head, 3= T-cell holder


Figure 5-22. T-cell and T-cell holder

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.

❖ To fit the T-cell holder to the burner

1. Remove the burner from the spectrometer.

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

Labeled Components: 1= T cell, 2=location hole, 3=securing clips, 4=strap


clip, 5=T-cell clips,
Figure 5-23. T-cell holder assembly

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.

6. Re-fit the burner to the spectrometer.

7. Clip the T-cell into the T-cell holder clips.

❖ To align the T-cell

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.

3. Install a suitable hollow cathode lamp.

4. Perform an optical set up.

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.

8. Move the T-cell away from the burner slot.

Electrically Heated Atomization Cell


The EC100 electrically heated atomization cell can be fitted to either
sample compartment of the spectrometer. It must be mounted on the
appropriate universal mount.

Mercury Absorption Cell


You can measure mercury with the VP100 using the standard T-cell,
although it is not necessary to heat the cell. However, sensitivity and
precision are improved by using the mercury absorption cell that is
supplied with the VP100.

The mercury absorption cell can be fitted in either sample compartment


of the spectrometer. It should be mounted on the appropriate universal
mount.

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.

❖ To fit the mercury absorption cell to the universal accessory mount

CAUTION Hazardous Chemical. Mercury is toxic by inhalation and cumulative.


The exhaust vapors must be extracted from the mercury absorption
cell via a suitable tubing that is connected to a free port of the mercury
absorption cell. Keep the door closed during operation at all times.

1. Locate the mercury cell holder. See Figure 5-24.

2. Fit the mercury cell holder to the required universal mount.

3. Fit the assembly into the appropriate sample compartment.

See “Universal Mount in Right Hand Sample Compartment” on


page 3-7 and “Universal Mount in Left Hand Sample
Compartment” on page 3-9, respectively.

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

Labeled Components: 1=exhaust outlet (pointing upwards), 2=mercury


absorption cell, 3=cell clips, 4=sampler inlet
Figure 5-24. Mercury absorption cell and cell holder

Connection of the Mercury Absorption Cell

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.

❖ To connect the mercury absorption cell

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.

5. Align the assembly in the sample compartment.

See “Universal Mount in Right Hand Sample Compartment” on


page 3-7 and “Universal Mount in Left Hand Sample
Compartment” on page 3-9, respectively.

Conditioning of the T-cell

A new T-cell may require conditioning before you obtain stable


measurements.

❖ To condition a new T-cell

1. Run a high concentration standard (typically 1-10 mg/L) for at least


five complete measurement cycles.

2. Perform a blank to wash out the high concentration standard.

The signal may not return to baseline.

3. Wait for the signal to stabilize.

4. Perform an autozero.

Installation of the EC100


❖ To install the EC100 power supply

1. Place the power supply at the front or side of the spectrometer.

2. Confirm that the voltage selector on the rear panel matches your
mains voltage.

3. Connect the power supply to a mains socket.

❖ To install the EC100 furnace head

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

Labeled Components: 1=EC100 furnace, 2=head closure knobs, 3= T cell leg,


4=EC100 baseplate, 5=head securing screw, 6=power cable to power
module, 7=T cell
Figure 5-25. EC100 furnace head

2. Locate the pink sensor lead. Connect it to the pink sensor plug on
the furnace head.

3. Fit the furnace head and mount assembly in the required


compartment of the spectrometer. See “Fitting an Accessory to the
Universal Mount” on page 5-10.

4. Connect the power cable from the furnace head to the head socket
on the back of the power supply:

a. Push the plug into the socket.

b. Give it a quarter turn clockwise until it clicks into position.

c. To disconnect the plug from the socket, pull the metal locking
piece towards the cable to release the lock.

d. Rotate the plug anti-clockwise and pull it from the socket.

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.

7. Fit a quartz T-cell.

8. Close the furnace head.

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Installation
Installation of VP100 Continuous Flow Vapor System

9. Align the assembly with the optical system of the spectrometer.

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

• Operation of AA Systems on page 6-2

• Alignment and Operation of the iSQ Module on page 6-4

• Operation of Flame System on page 6-5

• Operation of the Graphite Furnace System on page 6-21

• Operation of the GFS Autosampler on page 6-23

• Vapor Operation on page 6-27

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

Spectrometer Status Indicators


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 Table 6-1 and Figure 6-1. An × denotes that the LED can be
in either state.

The flash checksum failure may be corrected by downloading the


spectrometer software. Refer to the iCE 3000 Series Operating Manual.
The other errors and the display of any code that is not shown in
Table 6-1 requires service attention.

Table 6-1. Spectrometer status indicators


Standby FC3 FC2 FC1 Halt Comment
a
On Off Off Off Off OK
× Off Off On Off boot checksum failure
× Off On Off Off RAM failure
× Off On On Off flash checksum failure
× On Off Off Off timer failure
× On Off On Off RS-232 crystal failure
× × × × On processor halt
a
When connected to a Data Station, the status LED instead flashes slowly, once a second.
Otherwise, it flashes rapidly (about five times a second).

STANDBY

FC1
GFTV
FC2

FC3

HALT

PRINTER

Figure 6-1. Connection panel with spectrometer status indicators

6-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of AA Systems

Hollow Cathode Lamps

See “Hollow Cathode Lamp Hazards” on page 4-9 for information


about the hazards associated with hollow cathode lamps. Ensure that
the hazards involved and the necessary precautions are understood
before you install such a lamp.

Lamp Types

Coded or uncoded lamps supplied by Thermo Fisher Scientific are


recommended.

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

Alignment and Operation of the iSQ Module


The iSQ wizard in the SOLAAR Data Station software provides
facilities for aligning the iSQ Module. When the iSQ Module has been
correctly installed, you can carry out the alignment and the suite of
iSQ Test procedures by running the iSQ wizard.

Tip Refer to the iCE 3000 Series AA Spectrometers SOLAAR Software


Manual to run a SOLAAR wizard.

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

1. Turn on the spectrometer.

2. Turn on the power to the iSQ Module.

3. Open the shutter of the iSQ Module.

4. Start the SOLAAR Data Station software.

5. Start the iSQ wizard.

6. Follow the instructions on screen until you reach the Install and
Align Lamps page.

7. Install the Ca/Mg lamp supplied with the iSQ Module.

8. Use the commands on the wizard to perform an optical setup.

9. Carry out the alignment procedure described in the RH Accessory


Mount section.

If the assembly is a long way out of alignment, it may be necessary to


remove the iSQ Module and universal mount assembly to allow the
initial optical setup to be completed successfully.

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

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.

• Inspect and, when you perceive a damage or scratches, replace the


over-pressure disc at the rear of the spray chamber.
Damage increases the risk of a flashback.
Inspect and, if necessary, clean the burner every time before
operating it. See “Silver, Gold and Copper Samples” on page 4-15.

• Inspect and, if soiled by soot particles, clean the spray chamber


and the nebulizer.

• Confirm that the fume extraction system is switched on and is


operating correctly.

• Check that the spray chamber drain is clear and that it discharges
freely into a suitable receptacle.

• Set all gases to the correct inlet pressures.

• Perform a gas leak test when the instrument has been moved or
rebuilt. See “Gas Leak Test” on page 7-16.

CAUTION When operating the instrument with hazardous gas, an external


warning sensor must be installed in the vicinity of the instrument.

Organic Solvents

Before you measure samples in an organic solvent, see page 4-12.

If you are certain that the solvent is safe to be used for Flame Atomic
Absorption measurements, check the following before lighting the
flame:

• Empty any aqueous liquids from the drain.

• Refill the drain with clean solvent. See “Maintenance of Drain” on


page 7-15.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-5
Operation
Operation of Flame System

If you are using methyl isobutyl ketone (MIBK) or similar solvents,


prevent the solvent from coming into direct contact with the top of
the spray chamber. Place a long stemmed funnel into the spray
chamber neck and pour the solvent through this until it flows freely
from the drain.

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.

Requirements for safe flame operation

• 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.

Lighting the Flame


Before lighting the flame, confirm that:

• the required fuel and oxidant gases (for example, air and acetylene)
- are connected to the spectrometer,
- have the correct pressure settings.

• the spray chamber is clean.

• an intact explosion disk is fitted in the back of the spray chamber.

• the drain trap is filled with clean water or solvent.

• the spray chamber drains freely to waste.

• the burner is clean and correctly fitted.

• the lamp compartment door is securely closed.

• the fume extraction system is turned on and working correctly.

6-6 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Operation of Flame System

❖ To light the flame

1. Confirm that the Ignition Ready light is flashing.

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.

2. Press and hold the Ignition Ready/Flame On switch until the


default flame is established.

The default flame is a stoichiometric air/acetylene flame.

If a flame is not established within 30 seconds, the automatic flame


ignition system stops. Wait approximately 30 seconds before trying
again.

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.

❖ To extinguish the flame

1. Aspirate clean water or solvent to remove all traces of sample


solution from the spray chamber and the drain.

2. Press the Flame Off button.

a. The oxidant gas changes to air, if necessary.

b. The fuel flow increases to give a fuel rich flame.

c. The flame is shut off.

Warming up the Burner

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

❖ To warm up the burner for use with an air acetylene flame

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.

2. Light the flame.

3. Confirm that it is burning correctly.

4. Aspirate an appropriate solution, such as deionized water.

5. Use the system software to execute a Flame Setup command.

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

1. Warm up the burner with an air acetylene flame, as described on


page 6-8.

2. Change the Flame Type to Nitrous Oxide Acetylene.

3. Set the fuel gas flow rate to 3.6-3.8 L/min.

4. Use the system software to execute a Flame Setup command.

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.

Alignment of the Burner

CAUTION Risk of Eye Injury. 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.

Burner alignment is achieved by aspirating a suitable sample solution


and adjusting the burner position to obtain the maximum absorbance
signal.

❖ To align the burner

1. Set up a suitable analysis using the system software, install a hollow


cathode lamp, and perform an Optical Setup. Ensure that the live
absorbance signal is displayed.

2. Adjust the angular position of the Burner by rotating the entire


spray chamber assembly through the access hole in the door.

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.

Labeled Components: 1=access hole in door


Figure 6-2. Flame compartment door

3. Light the flame and allow a few minutes for it to stabilize.

4. Aspirate deionized water and, if necessary, autozero the absorbance


signal.

5. Use the Transverse Adjustment control knob to adjust the


transverse position of the burner to maximize the signal from the
test solution.

6. Use the Burner Height controls in the system software to adjust the
height of the burner to maximize the test signal.

The SOLAAR software provides an automatic burner height


optimization function to optimize this adjustment.

Do not touch the burner support or height adjustment mechanism


when the height adjustment mechanism is operating.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-9
Operation
Operation of Flame System

Alignment of the Impact Bead


The impact bead is aligned by aspirating a suitable sample solution and
adjusting the impact bead position to obtain the maximum absorbance
signal.

❖ To align the impact bead

1. Set up a suitable analysis with the system software, install a hollow


cathode lamp, and perform an Optical Setup. Ensure that the live
absorbance signal is displayed.

2. Light the flame and allow a few minutes for it to stabilize.

3. Align the burner as described on page 6-8.

4. Aspirate deionized water and, if necessary, autozero the absorbance


signal.

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.

Flame capable iCE 3000 Series spectrometers may be fitted with


either a micro-adjustable impact bead control or a standard impact
bead control. See Figure 6-3 to identify the type of adjustment
required:

• Adjust the standard impact bead control by pulling or pushing it


into and out of the spray chamber cap. Ensure that the handle
remains in contact with the guide pin at all times.

• Adjust the micro-adjustable impact bead control by rotating the


micro-adjuster.

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.

Venting the Gas System


Venting the gas system releases the gas pressure in the lines to the
spectrometer. The gas system should be vented at the end of the working
day or when the instrument will not be used again immediately.

❖ To vent the gas system

1. Turn off the flame.

2. Shut off the gas supplies at the source.

3. Press and hold the Flame Off button for 30 seconds.

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

Operation of the Air Compressor

Handling the Air Compressor

Pay attention to the following safety guidelines:

• Observe the electrical safety precautions.

• Use the accessory in a well ventilated position.

• Ensure that the accessory is not close to a heat source.

This could result in poor removal of water vapor from the


compressed air, causing flame instability.

• Do not use the accessory as a pump for combustible liquids or


vapors.

• This accessory is an oil-free pump and does not require


lubrication. Do not let hydrocarbons come into contact with the
diaphragm.

• Do not operate the accessory without the fan guards in place.

❖ To operate the air compressor

1. Ensure that the drain plug at the base of the filter/regulator unit is
closed and that the system is leak free.

2. Switch on the compressor.

3. Set the filter/regulator to 2.75 bar (40 psi).

4. Let the unit run for 30 minutes to achieve normal operating


temperature.

5. Check and reset the pressure if necessary.

6. Switch on the spectrometer.

7. Carry out your analysis.

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

Operation of the Autosampler

Observe electrical safety precautions.

Read the safety section of the user documentation of the autosampler


supplied with the unit.

❖ To operate the autosampler

1. Switch on and set up the spectrometer and the accessories.

2. Switch on the autosampler. Wait for it to initialize.

3. Use the Data Station software facilities to define the type and
number of sample racks, and the number of solutions required.

4. Refer to the Autosampler Loading Guide facility in the software,


and place the solutions in the correct positions in the racks.

5. The system is now ready to start the analysis.

Operation of the ID100 Autodilutor

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.

❖ To operate the ID100 autodilutor

1. Prepare a sufficient quantity of diluent solution. Place the diluent


uptake tube in this solution.
The diluent solution should be similar in composition to the sample
solution matrix.

2. Turn on and set up the spectrometer and lamps in the normal way.
Light the flame.

The diluent solution is then drawn up through the mixing piece


into the nebulizer.

3. Use the appropriate wizards to optimize the burner and the


nebulizer.

4. Otherwise, disconnect the nebulizer uptake tubing between the


autodilutor mixing piece and the nebulizer at the nebulizer end, and
replace it with a standard piece of nebulizer tubing, then optimize
the burner position and the impact bead as usual.

5. Replace the tube connecting the autodilutor to the nebulizer.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-13
Operation
Operation of Flame System

6. Set the Pre-Fill Volume on the Sampling tab of the View.Options


dialog.

A Pre-Fill volume of 1200-1500 mL is suitable for use with manual


sampling with the ASX280 autosamplers. Up to 2000 mL are
needed for the larger ASX-560 autosampler.

If you notice memory effects when measuring solutions with widely


different concentrations, increase the Pre-Fill volume.

7. Set up the analysis parameters in the normal way.

8. When working at high dilutions, small bubbles in the sample can


disturb the operation of the autodilutor, resulting in poor
measurement precision and incorrect results.

Take precautions to remove as much dissolved gas from the sample


as possible, but it is not practicable to completely prevent the
formation of such bubbles. Thermo Fisher Scientific therefore
recommends using the RSD Test facility in the SOLAAR Data
Station software to identify and automatically repeat any
measurements with poor (> 5% RSD) precision.

9. Set the Nebulizer Delay Flame parameter to a value of 10 seconds.

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.

13. Load the samples into the autosampler, if required.

14. Start the analysis in the normal way.

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.

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Operation
Operation of Flame System

Do not leave any sample or diluent in the dilutor. If you do not


intend to use the autodilutor again immediately, remove the sample
and diluent uptake tubes from the liquid containers and perform
another wash cycle. This removes all the fluid from inside the
autodilutor.

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.

Prolonged exposure to mineral acids at concentrations above 10% can


cause degradation of the material used in the ID100 high precision
piston pump. Avoid using samples containing high concentrations of
mineral acid if possible. Otherwise, ensure that you wash the ID100
autodilutor with clean water between each measurement, and at the
end of the analysis.

Operation of the Slotted Tube Atom Trap

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.

NOTICE Use the STAT only with the 50 mm universal burner.

Do not use nitrous oxide supported flames with this accessory because
this can impede flame safety and result in a flashback.

❖ To operate the STAT

1. Set up your method as required.

The STAT does not require any additional parameters to be set.

2. Light the flame.

3. Aspirate deionized water.

4. Allow the STAT tube to stabilize for 5 minutes.

5. Start your analysis in the normal way.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-15
Operation
Operation of Flame System

Operation of the Variable Flow Auxiliary Oxidant Accessory

The use of organic solvents with flame AA spectrometry is hazardous.


Ensure that you read and fully understand the hazards and precautions
described at “Flame System Safety” on page 4-12.

❖ To operate the Variable Flow Auxiliary Oxidant Accessory

1. Set up the instrument in the normal way.

It may be beneficial to use a longer and/or narrower length of


nebulizer uptake tube to reduce the aspiration rate of the sample,
although this reduces the chemical sensitivity.

2. Ensure that the Auxiliary Oxidant parameter on the Flame page of


the Method is selected.

3. Normally set the Fuel Flow Rate parameter to its minimum value.

4. Confirm that the Variable Flow Auxiliary Oxidant needle valve is


closed.

5. Light the flame.

6. Use the Flame Setup command in the system software to set your
chosen flame parameters.

7. Aspirate a typical sample solution.

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.

10. Use the system software to display the analytical signal.

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

Operation of the Solvent Resistant Flame Kit

Before you use your instrument, read the guidelines described at


“Flame System Safety” on page 4-12 that concern the safe use of the
spectrometer and the flame atomization system.

If you use organic solvents on a regular basis, Thermo Fisher Scientific


recommends having the Solvent Resistant Flame Kit fitted to your
instrument. Also see “Solvent Resistant Flame Kit” on page 3-12.

Flame Atomizer

Spray Chamber Drain

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.

Warming up the Burner when Using an Organic Solvent

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.

❖ To warm up the burner when using an organic solvent

1. Perform the normal flame safety checks described at “Flame Safety”


on page 4-13 and “Requirements for safe flame operation” on
page 6-6. Ensure that any additional checks and actions associated
with your risk analysis have been properly performed.

2. Fill the spray chamber drain with clean solvent as described at


“Spray Chamber Drain” on page 6-17.

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.

4. Ignite the flame, and perform a flame setup.

NOTICE Do not aspirate solvent into the nebulizer at this time.

5. Let the flame burn for at least ten minutes.

6. If you intend to use an air supported flame, proceed with the


optimization of the flame described at “Flame Optimization” on
page 6-18.

7. If you intend to use a nitrous oxide supported flame:

a. Set the flame type to Nitrous Oxide Acetylene, with a Fuel


Flow Rate of 4.2 L/min.

b. Perform a flame setup.

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.

NOTICE Do not aspirate solvent into the nebulizer at this time.

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).

8. Let the flame burn for at least ten minutes.

9. Optimize the flame as described on page 6-18.

Flame Optimization

Initial Optimization of Air Supported Flames

❖ To initially optimize air supported flames

1. When the burner has been properly warmed up (see “Warming up


the Burner when Using an Organic Solvent” on page 6-17), set the
Auxiliary Oxidant option on the Flame Parameters page of the
SOLAAR software. Perform a flame setup.

The appearance of the flame changes as the oxidant flow is


increased.

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Operation
Operation of Flame System

2. Aspirate clean solvent into the flame.

If the flame color changes to yellow, indicating a fuel rich flame,


reduce the fuel flow rate until a clear flame is obtained.

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.

It may be necessary to make further minor adjustments to the fuel


gas flow rate and sample uptake rate to obtain a clean flame that is
stable when no solvent is being aspirated.

Variable Flow Auxiliary Oxidant Kit

If you have a Variable Flow Auxiliary Oxidant accessory fitted to your


spectrometer, optimize the flame as follows:

❖ Optimizing the flame if a Variable Flow Auxiliary Oxidant accessory is


fitted

1. Having warmed up the burner (see “Warming up the Burner when


Using an Organic Solvent” on page 6-17), confirm that the auxiliary
oxidant flow control needle valve is fully closed.

Turn on the Auxiliary Oxidant facility on the Flame Parameters


page as described at “Auxiliary Oxidant” on page 3-13.

When you execute a flame setup command, the appearance of the


flame should not change.

2. Aspirate the clean solvent.

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

Initial Optimization of Nitrous Oxide Supported Flames

Auxiliary oxidant is not required with nitrous oxide supported flames.


The facility cannot be selected in the software when the Flame Type is
Nitrous Oxide/Acetylene.

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.

Final Optimization of All Flames

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.

Be careful when optimizing the transverse position and rotational


positions of the burner. There are flammable solvents in the vicinity of
the exposed flame.

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.

NOTICE The On-Line Cookbook and other documentation list typical


performance data, such as characteristic concentration, that you
should be able to obtain from your instrument. This data is always
measured with aqueous samples and is not applicable when
performing measurements in non-aqueous solvents.

Adjustment of the Impact Bead

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.

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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!

Operation of the Graphite Furnace System


NOTICE The graphite furnace system is not capable of detecting the type of
cuvette you have fitted. Select the correct type on the Furnace
Parameters software page. If you select the wrong type of cuvette,
incorrect heating regimes will be applied, which may damage the
furnace head and/or the cuvette.

Operating the GFS33 Graphite Furnace System


The GFS33 furnace head and autosampler will have been aligned with
each other and with the spectrometer optical system at installation. The
mounting arrangements have been designed so that the alignment is not
lost when the assembly is removed from and replaced in the sample
compartment.

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

The GFS33 accepts all types of cuvettes supplied by Thermo Fisher


Scientific for use in this furnace head.

NOTICE • Do not use cuvettes from any other source, nor those not
specifically designed for this furnace head.

• Handle new cuvettes carefully to avoid contamination.

❖ To fit a cuvette

1. Unclamp the furnace head by turning the clamping lever. See


Figure 6-4.

3 4

2 5

Furnace window
1

RHS electrode

Labeled Components: 1=center block, 2=sample injection port, 3=clamping


lever, 4=cuvette, 5=contact cone, 6=gas seal
Figure 6-4. GFS33 graphite furnace head

2. Remove the old cuvette.

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.

4. Position the cuvette fully in the furnace head.

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Operation
Operation of the GFS Autosampler

5. Carefully close the head with the clamping lever.

6. Check that the cuvette injection hole is positioned correctly. If


necessary, unclamp the furnace head and rotate the cuvette slightly.
Use the cuvette tool to make the injection hole central in the furnace
head injection port.

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.

Operation of the GFS Autosampler

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.

Wash liquid contamination can be a serious problem, affecting the


accuracy and precision of your results. Check that the wash liquid is
acceptable by analyzing a sample of the liquid before use.

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

Labeled Components: 1=capillary connector, 2=wash liquid connector,


3=syringe, 4=syringe plunger, 5=syringe handling strap, 6=internal capillary
tube
Figure 6-5. Syringe assembly of GFS autosampler

Sample Cups

Three types of sample cups are available for use with the GFS
autosampler:

• Polypropylene cups for general use. They contain approximately


2 mL of liquid and are normally not re-used.

• Fluoroplastic cups for ultra-trace applications. They also contain


approximately 2 mL and can be subjected to rigorous cleaning
procedures when necessary.

• Reduced volume cups for analyses where the available sample


volume is limited. They are Polypropylene cups and contain
approximately 1.5 mL. The bottom of these cups is V-shaped,
allowing sample volumes down to 100 L to be sampled reliably.

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.

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Operation
Operation of the GFS Autosampler

Cleaning Autosampler Cups


❖ To clean autosampler cups

1. Soak them in 5-10% v/v nitric acid.

2. Rinse them with clean water.

NOTICE More rigorous cleaning procedures may be necessary for ultra-trace


applications

Alignment of Capillary Tip


The autosampler capillary tip must be aligned with the cuvette injection
hole before use. The capillary tip depth adjustment must be set correctly
so that the sample is injected properly onto the floor of the cuvette.

❖ To align the capillary tip

1. Ensure that the graphite furnace is correctly aligned before you align
the capillary tip.

2. Locate the capillary tip adjustment controls A and B. See


Figure 7-12 on page 7-29.

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.

Control A moves the tip diagonally across the sample compartment


from the rear left to the front right.

Control B moves the tip diagonally across the sample compartment


from the rear right to the front left.

5. Use a dentists mirror or the GFTV image to view the capillary tip
inside the cuvette.

6. Loosen the adjustment lock nut.

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.

You may have to optimize the capillary depth setting further by


observing a sample injection.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-25
Operation
Operation of the GFS Autosampler

8. Lock the adjustment screw with the adjustment lock nut.

9. Use the Park Capillary Tip command to return the autosampler


arm to its normal parked position.

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.

Table 6-2. Reagents for analysis of simple aqueous solutions


Reagent Description
Acid Blank Reagent This reagent is suitable for all type of measurement.

50% v/v (6M) hydrochloric acid solution.


Borohydride Reductant Reagent This reagent is suitable for all hydride elements, and for mercury.

0.5% m/v sodium tetrahydroborate (sodium borohydride, NaBH4),


stabilized in 0.5% m/v sodium hydroxide (NaOH).

Filter the reagent through a coarse filter paper immediately after


preparation.

The reagent slowly evolves hydrogen gas, and so must be stored in a


vented container.

The reagent remains usable for 2-3 days if it is stored in a refrigerator at


4 °C, but Thermo Fisher Scientific recommends preparing it daily,
immediately before use.
Stannous Chloride Reductant This reagent is suitable for mercury analyses only.
Reagent
0.1-10% m/v of stannous chloride (SnCl2) in 1-10% v/v hydrochloric
acid.

If you have pre-reduced your sample with hydroxylamine


hydrochloride, or if your sample contains little or no oxidizing residues,
you can use the lower concentrations of stannous chloride.

Thermo Fisher Scientific strongly recommends using low mercury


grades of stannous chloride which are available from most major
chemical suppliers.

Dissolve the stannous chloride in the concentrated hydrochloric acid,


with gentle heating. The stannous chloride should dissolve to form a
clear solution. Cool, and make to volume with deionized water. The
final solution should be clear. A milky suspension indicates hydrolysis
of the stannous chloride and should not be used.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-27
Operation
Vapor Operation

Parameter Optimization of the VP100


Three parameters control the operation of the VP100:

• Carrier gas flow rate

• Pump speed

• Measurement delay time

Default values for these parameters are provided. If required, you can
edit them in the system software, on the Vapor page of the method.

VP100 Carrier Gas Flow Rate

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.

VP100 Pump Speed

As the VP100 pump speed is increased, the analytical sensitivity


increases, but so does the consumption of samples and reagents. The
measurement delay required is decreased at higher pump speeds.
Reducing the pump speed reduces the reagent consumption at the
expense of the analytical sensitivity and increased measurement delay
time. The default pump speed is 30 rpm, and good results can be
obtained with pump speeds up to 45 rpm.

VP100 Measurement Delay Time

A certain amount of time is required to allow the sample solution to


reach the gas liquid separator and for the reduction reaction to stabilize,
so that a stable analytical signal can be measured. This is the
measurement delay time. The optimum measurement delay is
determined by the carrier gas flow rate and the pump speed, but is
typically 40-60 seconds.

❖ To optimize the VP100 parameters

1. Prepare the following items:

• Freshly prepared reagents

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Operation
Vapor Operation

• A blank solution

• A test sample that gives a signal of between 0.1 and 0.4 A

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.

3. Install a suitable hollow cathode lamp.

4. Set up or load a suitable method.

5. If you are using flame heating:

a. Move the T-cell to the Parked position.

b. Light the flame.

c. Move the T-cell to the Operating position.

If you are using electrical heating:

a. Turn on the EC100.

b. Set the furnace temperature.

c. Wait until the furnace temperature stabilizes.

6. Perform an optical setup operation and open the Spectrometer


Status window to display the live absorbance signal.

7. Open the Vapour Status window.

8. Use the commands on the VP100 submenu on the Actions menu to


start the VP100.

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.

If necessary, perform an autozero to reset the signal display to


0.000 A.

10. Place the sample uptake tube in your test sample.

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.

Wait until the displayed signal returns to the baseline.

13. Place the uptake tube into the test solution.

Measure the time required for the signal to stabilize.

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 Measurement Using the VP100


When you have successfully set up the VP100, and optimized the
measurement parameters, you can use the system to measure your
samples.

Sample Preparation

Successful analyses using the hydride generation technique depend


critically on the sample preparation procedure used. It is not possible in
this Operating Manual to provide details for all types of samples, but
consider the following factors:

• It is normal practice to acidify samples for trace metal analysis, and


many types of sample require acid digestion to bring them into a
suitable form for analysis. The hydride generation technique is most
successful when the samples are presented in a hydrochloric acid
solution, and every effort should be made to design a sample
preparation procedure that ends with the final solution in
hydrochloric acid.

• The acid concentration in the samples affects the size of the


analytical signal. Samples, blanks and standards should therefore all
contain the same acid concentration. A final acid concentration of
10% v/v (1.2M) is suitable for many analyses.

6-30 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Operation
Vapor Operation

• The sensitivity of the hydride generation technique depends on the


oxidation state of the analyte element. The lower oxidations states
[As(III), Sb(III), Bi(III) Se(IV), and Te(IV)] are more sensitive. It is
therefore normal practice to pre-reduce the analytes before analysis.
- As and Sb can be pre-reduced with a potassium iodide/ascorbic
acid mixture.
- Se and Te can be pre-reduced by boiling in 6M hydrochloric
acid for ten minutes.
- The Bi(V) oxidation state is unstable, and all bismuth solutions
contain Bi(III). Bismuth analyses therefore do not normally
require pre-reduction.

• Many transition metals (such as copper and nickel) interfere with


the reduction reaction. Refer to the SOLAAR On-line Cookbook for
further information.

• Some samples may contain mercury in the form of organo-mercury


compounds. The stannous chloride reductant reagent only reduces
ionic mercury. The degree to which the borohydride reductant
reacts with organo-mercury compounds varies with the type of
compound. It is therefore normal practice to use an oxidative
digestion for samples for mercury analyses, to convert the
organo-mercury compounds to ionic mercury.

❖ To measure samples with the VP100 Vapor Kit

1. Install and align all parts of the VP100 Vapor Kit.

2. Prepare your samples, standards and blank solutions.

3. Prepare the reagents required and place them in the reagent bottles.

4. Turn on the spectrometer, Data Station and VP100.

5. Install suitable hollow cathode lamps in the spectrometer.

6. Turn on the gas supplies to the spectrometer and VP100.

7. Confirm that the VP100 drain discharges into a suitable container.

8. Set up a suitable method. Turn on the hollow cathode lamp, and/ or


perform an optical setup, and let the lamp warm up.

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.

10. Optimize the method parameters if necessary.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-31
Operation
Vapor Operation

11. If you are using an autosampler, refer to the Autosampler Loading


Guide. Place your samples and standards in the autosampler racks.

12. Start the VP100. Let it run until the reagents reach the gas liquid
separator and are pumped away through the drain channel.

13. Start your analysis by clicking the Analyze button, or by selecting


the Analyze command on the Actions menu in the usual way.

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.

Shutdown of the VP100


When your analysis is finished, shut down the VP100 properly if you do
not use it again immediately.

❖ To shut down the VP100

1. Extinguish the flame. Move the T-cell to the Parked position or


turn off the power to the EC100 furnace.

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.

5. Empty and rinse the reagent bottles.

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.

Operation of the EC100

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.

❖ To perform a vapor analysis with the EC100

1. Set a suitable atomization temperature (typically 900 °C).

2. Turn on the EC100 furnace and allow the temperature to stabilize.

3. Set up the VP100.

4. Perform the analysis.

❖ To set the atomization temperature

1. Ensure that the Heat power switch is turned off.

2. Turn on the main power switch on the front panel of the power
supply.

The controller display is illuminated.

3. On the lower (green) display, set the required temperature using the
Up and Down arrow buttons.

Recommended values for the atomization temperature for each


element are provided in the On-Line Cookbook and Method Manual.

The upper (red) display indicates the approximate ambient


temperature.

4. Ensure that the vapor system carrier gas is flowing through the
atomization cell.

5. Turn on the Heat power switch.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 6-33
Operation
Vapor Operation

Power is applied to the furnace head. The red temperature display


increases.

When the red and the green temperature displays are the same, the
furnace head is ready to use.

Optimization of the EC100

Furnace Operation Temperature

Table 6-3 lists default operation temperatures for your particular


analysis using the EC100 when determining hydride forming elements
by vapor generation.

Table 6-3. Default operation temperatures for the EC100


Element Operation temperature
Arsenic (As)
Antimony (Sb)
Selenium (Se)
Germanium (Ge) 900 °C
Tellurium (Te)
Lead (Pb)
Tin (Sn)
Mercury (Hg) ambient EC100 non operational

Further improvements in system performance may be possible through


manual optimization of the atomization temperature: using a standard
solution expected to yield an absorbance of approximately 0.20, vary the
furnace operation temperature until the maximum signal response is
observed. Ensure that the furnace temperature has achieved equilibrium
before each vapor measurement.

Troubleshooting of the EC100


If the furnace is non operational, check that the:

• Power supply is connected and is switched on.

• Power cable is connected between the furnace head and the back of
the furnace power supply/control box.

• Thermocouple cable is connected between the furnace head and the


rear of the furnace power supply/control box.

• Correct operating temperature is programmed at the local


controller.

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

This chapter describes maintenance procedures that the user must


perform to ensure optimum performance of the iCE 3000 Series atomic
absorption spectrometer.

Contents

• Safety Guidelines for Maintenance on page 7-2

• General Advice for Maintenance on page 7-2

• Inspection- and Servicing Plan on page 7-4

• Maintenance of the Spectrometer on page 7-6

• Maintenance of the Flame System on page 7-9

• Maintenance of the Furnace System on page 7-19

• Maintenance of the VP100 on page 7-30

• Thermo Fisher Scientific Service on page 7-34

Before performing any maintenance on the system, read and


understand the safety sections in this manual. See Chapter 4, “Safety.”

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-1
Maintenance
Safety Guidelines for Maintenance

Safety Guidelines for Maintenance


When you perform maintenance on the iCE 3000 Series system, pay
attention to the following general safety guidelines.

It is the user’s responsibility to maintain the system properly by


performing the system maintenance procedures on a regular basis.

Service by the customer must be performed by trained qualified


personnel only and is restricted to servicing mechanical parts. Service
on electronic parts must be performed by Thermo Fisher Scientific
field service engineers only.

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.

CAUTION When operating the instrument with hazardous gas, an external


warning sensor must be installed in the vicinity of the instrument.

General Advice for Maintenance


When you perform maintenance on the iCE 3000 Series atomic
absorption spectrometer, observe the following advice:

• Accurate results can be obtained only if the system is in good


condition and properly calibrated.

• Preventive maintenance must start with installation, and must


continue during the warranty period to maintain the warranty.
Thermo Fisher Scientific offers maintenance and service contracts.
Contact your local Thermo Fisher Scientific representative for more
information. Routine and infrequent maintenance procedures are
listed in Table 7-1.

• The user maintenance procedures described in this manual do not


require removing the instrument housing. Thermo Fisher Scientific
assumes no responsibility and will not be liable for instrument
damage and/or operator injury that might result from using the
instrument without the housing attached. Therefore, a Thermo
Fisher Scientific field service engineer must be called if removal of
the instrument housing is required.

• To successfully carry out the procedures listed in this chapter, obey


the following rules:

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

Inspection- and Servicing Plan


Routine and infrequent maintenance procedures to be performed by the
user are listed in Table 7-1.

Table 7-1. User maintenance procedures


Component Procedure Frequency Procedure Location
Spectrometer Clean the surface If required page 7-6
Replace fuse If required page 7-7
Flame system Clean burner If required page 7-9
Clean spray chamber If required page 7-12
Clean the nebulizer If required page 7-15
Clean the drain If required page 7-15
Empty and refill the drain If required page 7-15
Inspect the gas supply hoses Regularly page 7-16
Replace cracked or damaged If required page 7-16
hoses
Replace all gas supply hoses every
three years.
Perform gas leak test every 6 months and after moving page 7-16
the instrument
Inspect and clean external Regularly page 7-17
surfaces of air compressor
Compressor filter/regulator
unit:

Inspect filter trap Regularly

Drain our any liquid Regularly


collected

Clean filter bowl “Maintenance of the Air


Compressor” on
page 7-17
Drain liquid in the hose If required

Inspect rubber components Regularly


for deterioration and damage
Autosampler Refer to manufacturer’s manual

7-4 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Inspection- and Servicing Plan

Table 7-1. User maintenance procedures, continued


Component Procedure Frequency Procedure Location
Variable Flow Check the for wear and
Auxiliary damage at regular intervals.
Oxidant
accessory
Graphite Inspect all graphite Weekly page 7-20
furnace system components

Inspect all other head


components

Leak test water cooling and page 7-26


gas handling system

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

Maintenance of the Spectrometer


Before performing any maintenance on the system, read and
understand the spectrometer safety sections in this manual. See
“Spectrometer Safety” on page 4-9.

To ensure that the instrument operates safely and reliably, carry out
routine maintenance periodically.

Cleaning the Spectrometer

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.

• Clean up any spillage on the external covers or within the kitchen


areas immediately, using appropriate safety protection if necessary.

• Remove stains and marks on the covers using a soft cloth moistened
with dilute detergent solution.

• Do not use any type of solvent based cleaners. ▲

Deuterium Lamp of the iCE 3300 Spectrometer


The deuterium lamp (D2; see Figure 7-1) is a consumable part and may
eventually reach the end of its useful life. Signs of this include:

• The lamp fails to strike.

• Zero absorbance baseline drifts when Quadline Background


Correction is selected.

• Repeated warnings are displayed that the intensity of the deuterium


lamp is low.

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

Labeled Components: 1=securing bolts, 2=lamp base, 3=plug and socket,


4=cable, 5=adjustment controls
Figure 7-1. Deuterium lamp assembly on iCE 3400/3500 spectrometer

Replacement of a Spectrometer Fuse


The iCE 3000 Series spectrometers have twin mains fuses in the power
supply module. If the instrument does not turn on when the mains
switch is pressed, check these fuses. Figure 7-2 shows the mains inlet and
fuse in the upper rear right corner of the right hand side of the
spectrometer.

Figure 7-2. Mains inlet and fuse

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

1. Disconnect the spectrometer from the mains.

2. Locate the combined power inlet connector and the fuse holder on
the Power Supply unit.

3. Pull out the fuse holder tray.

4. Remove the two fuses.

5. Fit the new fuses.

6. Push the fuse holder tray back into place.

7. Re-connect the mains supply.

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.

Maintenance of the iSQ Module


Thermo Fisher Scientific strongly recommends using the hollow
cathode lamps supplied with the iSQ Module only for iSQ validation
purposes, but not for routine analysis. The iSQ test software
automatically monitors and records lamp usage in milliampere hours,
provided that the lamp serial numbers are registered in the lamp
database.

Thermo Scientific hollow cathode lamps are guaranteed to emit spectra


for a period of 24 months from date of dispatch or 5000 milliampere
hours usage, whichever occurs first. If either of these limits are exceeded,
a new hollow cathode lamp should be obtained.

The iSQ Module is designed to ensure reliable operation and must


only be serviced by Thermo Fisher Scientific. If the module needs
repair, it must be returned to Thermo Fisher Scientific, via your local
sales representative.

The iSQ Module is a high precision optical instrument. Handle and


store it carefully. When the module is not in use, place the shutter over
the measurement aperture to prevent dust falling on the filters. Store
the module in its original packing material to prevent damage to the
delicate operating parts.

7-8 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Flame System

Maintenance of the Flame System


Before performing any maintenance on the system, read and
understand the flame safety sections in this manual. See “Flame
System Safety” on page 4-12.

Turn off all gas supplies and disconnect the spectrometer and
accessories from the mains before you carry out any maintenance
procedures.

Maintenance of the flame system must be performed at regular intervals


to ensure safe and reliable operation.

Flame AAS involves high temperatures and corrosive solutions.


Therefore, system maintenance is essential.

Maintenance of the Burner

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.

❖ To clean the external surfaces of the burner

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.

CAUTION Do not dismantle the while it is still plugged to the spectrometer.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-9
Maintenance
Maintenance of the Flame System

❖ To dismantle the burner

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

Labeled Components: 1=ignition electrode, 2=burner slot, 3=burner handle,


4=burner cables, 5=burner cleaning tool, 6=burner rotation scale, 7=locking
clips, 8=burner base clip
Figure 7-3. Universal finned titanium burner head

❖ To clean the internal surfaces of the burner

Use an ultrasonic bath filled with deionized water, dilute detergent


solution or 5% v/v solution of nitric acid to clean the internal
surfaces of the burner head. Dry the burner thoroughly before use.

NOTICE Do not put the plastic burner base and ignition electrode assembly
into the ultrasonic bath.

❖ To re-assemble the burner

1. Orientate the burner base so that it is upright, with the burner


handle to the right.

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.

The burner must always be fitted to the correct burner base, as


supplied with the burner.

❖ To align the ignition electrode

1. Place the cleaning tool/setting jig as shown in Figure 7-4, aligning


the bottom corner of the chamfer with the edge of the ignition well.

2. Gently bend the electrode until the tip touches the top corner of the
chamfer on the setting jig. See Figure 7-4.

Figure 7-4. Alignment of ignition electrode

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-11
Maintenance
Maintenance of the Flame System

Maintenance of Spray Chamber


Figure 7-5 schematically shows the parts of the spray chamber and the
nebulizer.

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

❖ To clean the spray chamber

1. Aspirate a solution of dilute (1% v/v) hydrochloric acid, or a


solution of laboratory detergent, whichever is most appropriate.

Aspirate the solution for five minutes. Then aspirate deionized


water.

2. For a more thorough cleaning, dismantle the spray chamber, clean


the individual components with laboratory detergent, rinse
thoroughly with deionized water, dry and re-assemble.

7-12 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Flame System

❖ To remove and dismantle the spray chamber

1. Use the system software commands to raise the burner until the
burner height is less than 10 mm.

2. Remove the burner.

3. Empty the spray chamber drain.

Tip To empty the drain safely, see “Maintenance of Drain” on


page 7-15

4. Disconnect the gas lines to the spray chamber.

5. Disconnect the drain tube.

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.

❖ To dismantle the cap assembly

1. Slacken the impact bead clamp adjusting screw. Withdraw the bead
from the alumina disc side of the cap.

2. Remove the seal and the alumina disc.

3. Undo the securing screws. Remove the bead adjustment assembly.

4. Slacken the nebulizer retaining clip screw. Withdraw the clip.


Remove the nebulizer and the O-ring.

NOTICE Do not re-assemble the spray chamber with damaged parts.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-13
Maintenance
Maintenance of the Flame System

❖ To re-assemble the cap assembly

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.

❖ To position the impact bead

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.

3. Set the bead adjuster to the fully out position.

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.

5. Tighten the bead clamp screw.

6. Refit the alumina disc and the seal.

❖ To re-assemble the spray chamber

1. Inspect, clean and replace any damaged components.

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.

5. Re-fit the cap assembly. Tighten the thumbscrews.

6. Re-fit the spray chamber to the spectrometer mount.

7. Re-connect the gas lines, drain and burner.

8. Perform a leak test. Rectify any leaks before lighting a flame.

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.

❖ To clean the nebulizer

1. Extinguish the flame.

2. Remove the nebulizer uptake capillary.

3. Push the nebulizer cleaning probe through the nebulizer capillary to


remove any blockages.

NOTICE Do not use any other tool or wire to clean the nebulizer.

4. Replace the nebulizer uptake tube.

5. Light an air/acetylene flame.

6. Measure the nebulizer uptake rate as described on “To measure the


nebulizer uptake rate”.

❖ To measure the nebulizer uptake rate

1. Fill a 10 mL measuring cylinder with deionized water.

2. Fit a standard length (250 mm) of 0.5 mm ID nebulizer capillary.

3. Light an air/acetylene flame.

4. Aspirate the water from the measuring cylinder. Note the volume
aspirated in 1 minute.

The normal nebulizer uptake rate under these conditions should be


above 6 mL/min.

Maintenance of Drain
Periodically check the external drain tube. Replace it if it is cracked or
damaged.

❖ To clean the drain

1. If the drain is blocked, clean it by pouring dilute hydrochloric acid


(5% v/v) or laboratory detergent down the spray chamber stem.

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

❖ To empty and refill the drain

1. Turn off the fuel and nitrous oxide gas supplies at source, but leave
the air supply turned on.

2. Remove the burner.

3. Ensure that a suitable container is positioned to receive the contents


of the drain.

4. Block the top of the spray chamber with a suitable bung.

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.

Maintenance of Gas Supply Hoses


Inspect the gas supply hoses regularly. Replace any that are cracked or
damaged.

Thermo Fisher Scientific recommends replacing all gas supply hoses


every three years.

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.

Gas Leak Test

Tip The SOLAAR OQ Tests Data Station application includes a gas


leak test wizard with full on-screen instructions.

The gas leak test wizard can be started from the OQ Test software:

• OQ Test Software/View/Customer Diagnostics/Gas Leak Test

The result of the gas leak test is not stored in the results database
when the wizard is started manually.

• OQ Test Software/Automated Test Sequence/Start Test Sequence

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.

Maintenance of the Air Compressor


Regularly inspect and clean external surfaces.

❖ To maintain the filter/regulator unit

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.

3. If any liquid has collected in the hose, drain it into a suitable


container.

4. Inspect rubber components regularly for deterioration and damage.

Maintenance of the Autosampler

For a detailed description of the maintenance procedures, refer to the


user documentation of the autosampler supplied with the unit. Also
note “Maintenance of the CETAC ASX-560 and ASX-280 Flame
Autosampler” on page C-2.

Maintenance of the ID100 Autodilutor


❖ To maintain the ID100 autodiluter

1. Wipe up any leaks or spillages as soon as they occur.

2. Do not allow liquid to accumulate in the drip tray.

3. Periodically check for visible signs of leakage from the connectors.


Replace any that are faulty.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-17
Maintenance
Maintenance of the Flame System

Maintenance of the Slotted Tube Atom Trap

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.

NOTICE Use the STAT only with the 50 mm universal burner.

Perform the following maintenance routines for the Slotted Tube Atom
trap (STAT).

❖ To maintain the 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.

2. If necessary, rinse with water or dilute acid to remove internal


deposits.

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.

Maintenance of the Variable Flow Auxiliary Oxidant Accessory


Check the Variable Flow Auxiliary Oxidant Accessory for wear and
damage at regular intervals.

Figure 7-6. Flame compartment valance with Variable Flow Auxiliary


Oxidant accessory fitted

7-18 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Furnace System

Maintenance of the Furnace System


Perform furnace system maintenance regularly to ensure safe and reliable
operation.

Contamination is the major cause of problems with the graphite furnace


system. It is essential to maintain scrupulous cleanliness of the furnace
head, furnace autosampler and all sample handling apparatus.

Maintenance of the GFS35/35Z System


Perform furnace system maintenance regularly to ensure safe and reliable
operation.

Contamination is the major cause of problems with the graphite furnace


system. It is essential to maintain scrupulous cleanliness of the furnace
head, furnace autosampler, and all sample handling apparatus.

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

Cleaning the GFS35/35Z 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

6 cuvette alignment tool

Labeled Components: 1=left hand electrode, 2=sample injection port,


3=rubber seal, 4=right hand electrode, 5=right hand contact cone, 6=cuvette,
7=center block
Figure 7-7. GFS35 furnace head - interior view

5
2
4
3
1

8 7

Labeled Components: 1=left hand electrode, 2=rear magnet coil, 3=sample


injection port, 4=center block, 5=cuvette, 6=right hand contact cone,7=right
hand electrode, 8=magnet securing bolt, 9=front magnet coil
Figure 7-8. GFS35Z furnace head - interior view

7-20 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Furnace System

❖ To clean the furnace head

1. Open the furnace head and remove the cuvette.

2. Inspect all graphite components.

3. Use a cotton bud to remove any sample deposits or debris. If


required, use an air jet to blow out any dust.

4. Inspect all other head components.

5. Clean exterior surfaces with tissue or soft cloth moistened with


dilute detergent solution.

If the furnace head windows become dirty, they reduce the optical
energy passing through the cuvette and so increase the baseline noise.

❖ To remove and clean the furnace head windows

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.

Figure 7-9. Furnace Window Removal Tool

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.

c. Remove each window holder by pulling it from the body of the


furnace.

3. Remove any debris or deposits from the window holder gas ways.

4. Clean the windows with a moist cotton bud.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-21
Maintenance
Maintenance of the Furnace System

The windows can be removed from the window holders by pulling


out the O-ring seal.

NOTICE Avoid damaging the O-ring seals if you do this.

5. Refit the window holders. Do not damage the O-ring seals.

NOTICE Do not lubricate the window holder O-ring seals.

Cleaning the Optical Temperature Feedback System

Thermal radiation emitted by the hot cuvette is used to control the


cuvette temperature when the Temperature Control command is
selected. If the temperature control window or the lens are dirty,
temperature accuracy, analytical precision and cuvette lifetime are
degraded.

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.

❖ To clean the temperature feedback system

1. Remove the furnace head center block, to expose the temperature


control window in the base of the center block, and the lens in the
body of the furnace.

2. Clean the lens with a cotton bud.

3. Unscrew the window holder from the rear of the center block.

NOTICE Take care that the window does not fall out.

4. Inspect and clean the window.

5. Replace the window and the window holder.

6. Re-fit the center block.

❖ To remove the GFS33/35 center block

1. Open the furnace head.

2. Remove the cuvette.

3. Pull the center block gently to the right to free it from the locating
spigots.

4. Switch off the cooling water to minimize the consequences if


accidental leaks in the water supply occur.

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

6. Reverse the procedure to re-fit 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.

❖ To remove the GFS35Z center block

1. Open the furnace head.

2. Remove the cuvette.

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.

6. Remove the center block by pulling it gently to the right.

Switch off the cooling water to minimize the consequences if


accidental leaks in the water supply occur.

7. Gently pull the hoses and connections out from the furnace body
until you obtain good access to the rear of the center block.

8. Reverse the procedure to re-fit 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.

Cuvette Contact Cones

After typically six months of use, the cuvette contact cones may become
worn, causing poor contact with the cuvette and unreproducible cuvette
temperatures.

• Inspect the cones regularly. A shallow groove in the contact area is


normal, but if the contact areas show signs of pitting or burning,
the cones must be replaced.

• The contact cones must be replaced in pairs.

• The contact cones cannot be re-used when they have been


removed from the head.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-23
Maintenance
Maintenance of the Furnace System

❖ To remove used contact cones

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.

3. In the case of the GFS35Z, open the magnet.

4. Remove the center block.

5. Switch off the cooling water to minimize the consequences if


accidental leaks in the water supply occur.

6. Remove the rubber seal from the right hand electrode.

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.

10. Repeat the procedure for the other electrode.

7-24 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Furnace System

❖ To fit the new contact cones

1. Assemble the new cone on the cone replacement tool. See


Figure 7-10 or Figure 7-11.

1 2

removal 3
4
8 8 5
6

4
7
3 2 insertion

Labeled Components: 1=M4 x 50 screw, 2=washer, 3=PTFE washer, 4=LHS


contact cone, 5=clearance for dowel, 6=body, 7=inserter, 8=position of
furnace electrode
Figure 7-10. Replacing a contact cone - GFS33/35

removal 2
3
4
5
5

4
3
2
insertion
1

Labeled Components: 1=cone jig-nut, 2=LHS contact cone, 3=cone jig-jack,


4=washer, 5=M4 x 50 screw
Figure 7-11. Replacing a contact cone - GFS35Z

2. Insert the assembly into the electrode.

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.

4. Repeat the procedure for the other electrode.

5. Re-fit the rubber seal in the right hand electrode.

6. Re-fit the center block. Close the GFS35Z magnet.

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.

Leaks in the Gas System

❖ To check for gas leaks

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.

3. Monitor the line pressure shown by the cylinder gauge for


10 minutes.
4. If the pressure falls by more than 0.07 bar (1 psi), check each
connection by brushing dilute soap solution on it. Bubbles indicate
a leak.

Ensure that you wipe off the soap solution at the end of the test, so
that it does not cause corrosion of the fittings.

5. Rectify any leaks found.

7-26 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the Furnace System

Leaks in the Water Cooling System

Water leaks usually occur at connections and are often self-evident.


Rectify them by tightening or by re-making the connection.

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.

In addition, the GFS35Z power supply contains two user replaceable


fuses. These are located adjacent to the Zeeman magnet mains inlet, on
the rear left hand panel of the power supply module.

If these fuses fail, they can be replaced with suitable replacements.


Replace only with same type and rating: 8AT(H) according to
IEC60127-2 with high breaking capacity (for example, Bussmann
S505-8-R). If the replacement fuses fail, a serious fault is likely. Call a
Thermo Fisher Scientific field service engineer to diagnose and rectify
the fault.

Maintenance of the GFS33 System


Maintenance on the furnace system must be performed regularly to
ensure safe and reliable operation.

Contamination is the major cause of problems with the graphite furnace


system. It is essential to maintain scrupulous cleanliness of the furnace
head, furnace autosampler and all sample handling apparatus.

Maintenance of the GFS Autosampler

Syringe

If persistent bubbles or leaks occur, it may be necessary to remove the


syringe and inspect it for blockage or damage.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-27
Maintenance
Maintenance of the Furnace System

❖ To remove the syringe

1. Ensure that the autosampler arm is in the Parked position by using


the Park Autosampler command in the system software.

2. Locate the syringe compartment on the autosampler front panel.

3. Remove the syringe from its mount by carefully pulling the syringe
handling strap.

NOTICE Do not cause damage to the syringe or plunger during this


operation.

4. Unscrew the capillary tube connections and remove the syringe.

Reverse this procedure to re-fit the syringe.

NOTICE Do not let any of the capillary tubing getting trapped between the
syringe or connector bodies and the autosampler.

Internal Capillary Tubing

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.

❖ To replace the internal capillary tubing

1. Remove the capillary tip and locking cap.

2. Pull the exposed capillary tubing gently from the arm and remove
the PTFE cone.
3. Remove the syringe.

4. Disconnect the capillary tubing connector.

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.

Autosampler Capillary Tip

The autosampler capillary tip, Figure 7-12, can be replaced if it becomes


bent or contaminated.

Labeled Components: 1=capillary tip height adjuster, 2=locking collar, 3=cone


seal, 4=capillary tip and cone, 5=locking cap
Figure 7-12. Autosampler capillary tip

❖ To replace the autosampler capillary tip

1. Gently lift the autosampler arm.

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.

3. Fit a new capillary tip into the locking cap.

4. Re-fit the cap to the arm.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-29
Maintenance
Maintenance of the VP100

Maintenance of the VP100


Routine maintenance mainly concerns keeping the apparatus clean. If it
is necessary to clean the casework, use a mild, water-based detergent.

The use of organic solvents with flame AA spectrometry is hazardous.


Ensure that you read and fully understand the hazards and precautions
described at “Vapor Safety” on page 4-27.

NOTICE Do not use any form of solvent-based cleaner, as it may damage the
plastic front cover.

Some of the reagents used are corrosive. To reduce potential corrosion


and hazards:

• Wipe up all spills immediately.

• Rectify all leaks immediately.

Problems can be caused by blockages formed from dried reagents and


sample solutions. To minimize these problems:

• Remove all reagents from the instrument when not being used.

• Flush all liquid paths with clean water at the end of the analysis.

CAUTION Hazardous Accumulation. Risk of injuries, flying debris and hearing


loss. All kinds of toxic, corrosive and organic samples can accumulate
in the waste container. The pressure in the waste container can cause
the waste container to burst, or the liquids in the waste container can
return back to the flame compartment with a loud flashback. Use only
waste containers with a wide neck.

CAUTION Hazardous Mixture. Risk of injuries. The mixture in the waste


container might be toxic and/or corrosive, and can be harmful in
contact with the skin. Pay attention to the Material Safety Data Sheets
(MSDS).

CAUTION Hazardous Chemical. Mercury is toxic by inhalation and cumulative.


The exhaust vapors must be extracted from the mercury absorption
cell via a suitable tubing that is connected to a free port of the mercury
absorption cell. Keep the door closed during operation at all times.

7-30 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the VP100

Maintenance of Peristaltic Pump


After extended use, the pump tubing becomes worn and must be
replaced.

❖ To inspect the tubing at regular intervals

1. Remove the tubing from the pump.

2. Examine the part of the tube that is in contact with the pump
rollers.

3. If the tubing appears to be stretched or does not appear to have a


circular cross section, it should be replaced.

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

1. Place the uptake tubes in a container of clean water.

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.

3. Take a 10 mL measuring cylinder and fill it to the 10 mL mark with


clean water.

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.

The flow rates should be as listed in Table 7-2.


Table 7-2. Flow rates in the different channels
Channel Flow rate
acid channel 0.7 mL/min
reductant channel 1.6 mL/min
sample channel 7.5 mL/min
drain channel 14 mL/min

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) 7-31
Maintenance
Maintenance of the VP100

❖ To check the flow rate in the drain channel

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.

3. Measure the volume of liquid discharged from the drain outlet in


1 minute.

It is unlikely that the drain becomes blocked in normal operation.

Maintenance of Gas Liquid Separator


The gas liquid separator is unlikely to become worn or damaged in
normal operation, but might become dirty and thus require cleaning.

❖ To clean the gas liquid separator

1. Remove the top cap and the hydrophobic membrane.

2. Inspect the internal volume of the gas liquid separator. Remove any
deposits.

3. Confirm that the reaction zone is filled with 4 mm glass beads.


4. Fit a new hydrophobic membrane.

5. Re-fit the O-ring seal and the top cap.

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.

If the replacement fuse fails immediately, or if the equipment does not


work normally after the fuse has been replaced, it is likely that a serious
fault exists. Isolate the unit from the mains power and gas supplies,
and ensure that it is not used until the fault has been diagnosed and
rectified by a trained Thermo Fisher Scientific field service engineer.

7-32 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Maintenance
Maintenance of the VP100

Maintenance of the EC100

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.

The EC100 power supply is fitted with thermal overload protection. If


this should trip, the power supply to the furnace head is cut off, and the
Overload Reset switch on the back of the power supply moves to the
Off position.

❖ To reset the thermal overload protection

1. Ensure that the Heat power switch is turned off.

2. Move the Overload Reset switch to the On position.

3. Turn on the Heat power switch.

If the thermal overload protection repeatedly trips out, it is likely that a


serious fault with the accessory exists.

❖ To react if the thermal overload protection repeatedly trips out

1. Disconnect all power to the accessory.

2. Remove the accessory from the spectrometer.

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

Thermo Fisher Scientific Service


This section contains information concerning maintenance work that
must be performed by Thermo Fisher Scientific personnel.

CAUTION Hazardous Chemicals. Hazardous material might contaminate


certain parts of your system during analysis. To protect our employees,
we ask you to adhere to special precautions when you send back parts
to the factory for exchange or repair.

If hazardous materials have contaminated instrument parts, then


Thermo Fisher Scientific can only accept these parts for repair if they
have been properly decontaminated.

Materials that due to their structure and the applied concentration


might be toxic or which are reported in publications to be toxic are
regarded as hazardous. Materials that will generate synergetic
hazardous effects in combination with other present materials are also
considered hazardous.

Parts contaminated by radioisotopes must not be returned to Thermo


Fisher Scientific—neither under warranty nor within the exchange
part program. If you are unsure whether parts of the system are
possibly contaminated by hazardous material, then make sure that the
Thermo Fisher Scientific field service engineer is informed before the
engineer starts working on the system.

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

Services to be Performed by Thermo Fisher Scientific Service Only


Table 7-3 lists services that must be performed by a Thermo Fisher
Scientific field service engineer only. Depending on the actual workload
of your iCE 3000 Series atomic absorption spectrometer, you may
increase the maintenance frequency.

Table 7-3. Thermo Fisher Scientific service procedures


MS Component Procedure Frequency Comments
iCE 3000 Series Replace deuterium lamp if necessary see page 7-6
instrument
iSQ module Repair module if necessary see page 7-8
Spray chamber Certificate instrument after flashback if necessary see page 7-12
Furnace system Rectify internal leak if necessary see page 7-26
Furnace power supply Replace fuse if necessary see page 7-27
EC100 power supply Check thermal overload protection if necessary see page 7-33

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

• WEEE Compliance on page A-2

• Declaration of Conformity on page A-3

• Health and Safety Form on page A-5

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:

Thermo Fisher Scientific is registered with B2B Compliance


(B2Bcompliance.org.uk) in the UK and with the European Recycling
Platform (ERP-recycling.org) in all other countries of the European
Union and in Norway.

If this product is located in Europe and you want to participate in the


Thermo Fisher Scientific Business-to-Business (B2B) Recycling
Program, send an email request to weee.recycle@thermofisher.com with
the following information:

• WEEE product class

• Name of the manufacturer or distributor (where you purchased the


product)

• Number of product pieces, and the estimated total weight and


volume

• Pick-up address and contact person (include contact information)

• Appropriate pick-up time

• Declaration of decontamination, stating that all hazardous fluids or


material have been removed from the product

This recycling program is not for biological hazard products or for


products that have been medically contaminated. You must treat these
types of products as biohazard waste and dispose of them in
accordance with your local regulations.

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).

1. General information Health and Safety Form


Thermo Fisher Scientific contact name for delivery
Thermo Fisher Scientific receiving site
Customer Instrument type
Address Instrument SN
Order number
Phone Return number
E-Mail Medical Device Research Use Only
SAP Service Notification

Part Number Quantity Material Description Error Description / Reason for Return Return Part Serial No

2. Condition of the material or instrument


Has the material or instrumentation been removed from the Tick the applicable check box.
shipping packaging or in contact with
- pump fluids Yes Æ go to section 3
- service fluids
- samples No Æ go to section 5
- standard solutions
- other chemicals
- hazardous materials

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

Health and Safety Form (P/N 1342350, Revision H) Page 1 of 2


Legal Documents
Health and Safety Form
Health and Safety Form
4. Description of process substances and/or compounds
Which substances have been in contact with the material or instrumentation? (trade name and/or chemical term of service
fluids and substances; properties of substances or compounds according to the Material Safety Data Sheet; e.g. toxic,
flammable, corrosive, radioactive)

Part Number Trade Name Chemical / Substance Name / Properties

a)

b)

c)

d)

e)

f)

5. Legally binding declaration

Has the material/instrument undergone a decontamination process? Yes Æ go to section 6 No


Is the material/instrument safe to handle for Thermo Fisher Scientific and Yes No
third-party personnel?

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.

6. Detailed description of the decontamination process used

Part Number Serial Number Describe the decontamination process

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

Health and Safety Form (P/N 1342350, Revision H) Page 2 of 2


B
Specifications

Contents

• Spectrometer on page B-2

• Autosampler on page B-5

• ID100 Autodilutor on page B-7

• Furnace Head and Power Supply on page B-8

• Furnace Control on page B-10

• GFS Furnace Autosampler on page B-11

• VP100 Continuous Flow Vapor System on page B-12

• EC100 Electrically Heated Atomization Cell on page B-14

• AA Validator Kits on page B-15

• Calibration Validation Unit on page B-16

• Left Hand Universal Accessory Mount on page B-16

• Right Hand Universal Accessory Mount on page B-16

• iSQ Module on page B-17

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-1
Specifications
Spectrometer

Spectrometer

iCE 3400/3500 Spectrometer


Table B-1. Specifications of iCE 3400/3500 spectrometer
Item Comment
iCE 3400 spectrometer Vapor atomization in the right hand
sample compartment

Zeeman Furnace AA spectrometer in right


hand sample compartment with wide range
photomultiplier
iCE 3500 spectrometer Dual Atomizer Zeeman AA spectrometer
with wide range photomultiplier

Flame atomization in left hand sample


compartment

Zeeman or standard Furnace atomization


in right hand sample compartment

Vapor atomization in either sample


compartment
Light source single or multi-element hollow cathode
lamps

uncoded and data coded hollow cathode


lamps

six independent lamp supplies, each


providing 0 to 20 mA
Wavelength range 180 nm to 900 nm
Data/Control systems 512 kB Flash PROM
spectrometer
256 kB RAM

three general purpose RS-232C ports

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

Table B-1. Specifications of iCE 3400/3500 spectrometer, continued


Item Comment
Monochromator Echelle monochromator and prism
post-monochromator

Nominal 1.0, 0.5 and 0.2 nm spectral


bandpass with 0.1 nm available below
400 nm

0.5 nm/mm reciprocal linear dispersion at


200 nm
Absorbance range -0.150 A to 3.000 A
(including background signal)
Background correction Quadline (continuum source) is standard
on all spectrometers

background signals < 2 A corrected to


< 2%

total signal up to 3 A
Gas control fuel flow range:

air/acetylene: - 0.8 to 2.3 L/min

nitrous oxide/acetylene: - 3.6 to 5.1 L/min


Power 100 to 240 V (±10%) at 50 or 60 Hz
Power consumption 300 VA
Dimensions and weight See Table 5-1 on page 5-6.

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-3
Specifications
Spectrometer

iCE 3300 Series Spectrometer


Table B-2. Specifications of iCE 3300 spectrometer
Item Comment
iCE 3300 spectrometer AA spectrometer with wide range
photomultiplier

six lamp automatic carousel

Flame and/or Furnace options available


Light source Single or multi-element hollow cathode
lamps

Uncoded and data coded hollow cathode


lamps

six independent lamp supplies, each


providing 0 to 20 mA
Wavelength range 180 nm to 900 nm
Data/Control systems 512 kB Flash PROM
spectrometer
256 kB RAM

three general purpose RS-232C ports

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

Half height slit settings available

Reciprocal linear dispersion 1.5 to


2.0 nm/mm

Focal length 270 mm


Grating 1800 L/mm
Absorbance range -0.150 A to 3.000 A
(including background signal)

B-4 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Specifications
Autosampler

Table B-2. Specifications of iCE 3300 spectrometer, continued


Item Comment
Background correction Quadline (continuum source) is standard
on all spectrometers

background signals < 2 A corrected to


< 2%

total signal up to 3 A
Gas control fuel flow range:

air/acetylene: - 0.8 to 2.3 L/min

nitrous oxide/acetylene: - 3.6 to 5.1 L/min


Power 100 to 240 V (±10%) at 50 or 60 Hz
Power consumption 300 VA
Dimensions and weight See Table 5-1 on page 5-6.

Autosampler

ASX-560 Flame Autosampler


The ASX-560 flame autosampler is a random access, large capacity
flame and vapor autosampler with 84 to 360 maximum sample capacity,
dependent on rack configuration. Optional racks for 21, 24, 40, 60 or
90 samples are available.

Table B-3. Specifications of ASX-560 flame autosampler


Item Comment
Standard items random access x-y autosampler
mechanism

standards rack (10 positions)

one sample rack (60 positions)

ten standard and 60 sample


polypropylene sample tubes

0.5 mm ID and 0.8 mm ID PTFE


sample probes

pumped wash facility

USB cable
Necessary additional items none

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-5
Specifications
Autosampler

Table B-3. Specifications of ASX-560 flame autosampler, continued


Item Comment
Power 100-240 V at 50 or 60 Hz
Power consumption 50 VA

ASX-280 Flame Autosampler


The ASX-280 flame autosampler is a random access, medium capacity
flame and vapor autosampler with 42 to 180 maximum sample capacity,
dependent on rack configuration. Optional racks for 21, 24, 40, 60 or
90 samples are available.

Table B-4. Specifications of ASX-280 flame autosampler


Item Comment
Standard items random access x-y autosampler
mechanism

standards rack (10 positions)

one sample rack (60 positions)


ten standard and 60 sample
polypropylene sample tubes

0.5 mm ID and 0.8 mm ID PTFE


sample probes

pumped wash facility

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.

Table B-5 lists the specifications of the ID100 autodilutor.

Table B-5. Specifications of ID100 autodilutor


Item Comment
Standard items ID100 autodilutor
Necessary additional items none
Power 110-240 V at 50 or 60 H
Power consumption 85 VA

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-7
Specifications
Furnace Head and Power Supply

Furnace Head and Power Supply


All cuvettes mount directly in an all-graphite containment with end
loaded contacts. Cuvettes are self aligning and can rapidly be exchanged
with a single lever movement.

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

tilt mount (GFS35Z) or


fixed mount (GFS35)

integrated furnace and autosampler


mount (GFS33)

ten normal electrographite cuvettes


Necessary additional items additional cuvettes (as required)
Contacts end-loaded graphite
Containment all graphite
Cuvettes normal electrographite

extended lifetime (ELC)

pyrolytically coated electrographite

Omega platform extended lifetime


Cuvette volume 0 to 70 L
Temperature control system choice of voltage control or optical
temperature control with a stabilized
sensor and fiber optic transmission
system
Gas system fixed external flow

adjustable internal flow with choice of


inert or alternate gas

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

0, 100, 200, 300 mL/min internal flow


Gas pressure 1.03 ± 0.14 bar (15 ± 2 psi)
Cooling water mains or recirculator

minimum flow rate 1.1 L/min

pressure 1.4 to 6.9 bar (20 to 100 psi)


Cooling time 20 s (fixed)
Interlocks water pressure and flow rate

inert gas pressure

power

power supply temperature

magnet temperature (GFS35Z only)

furnace open

magnet open (GFS35Z only)

cuvette present
Power 200/220/240 V at 50/60 Hz, 30 A
single phase

GFS35Z requires additional 200-240 V


50/60 Hz single phase supply
Power consumption 7.2 kVA

GFS35Z: additional 1.5 kVA


Dimensions [mm] 265 W × 390 H × 495 D
Weight GFS33: 58 kg

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.

A lifetime display enables the cuvette to be changed before failure


becomes likely. A pre-programmed cuvette clean cycle is available,
culminating in maximum temperature for five seconds to ensure
complete contamination removal.

Comprehensive storage of the furnace program, together with


spectrometer and autosampler parameters, is provided. Full furnace and
autosampler status can be displayed, together with the results during the
analysis. Complete monitoring of all furnace interlocks is provided.

Table B-7. Specifications of furnace control


Item Comment
Control system from Data Station
Program phases 20 time + temperature phases and 20 ramp
(five of each with local control)
Phase temperature range ambient to 3000 °C in 1 °C increments
Phase time 0 to 200.0 s in 0.1 s increments
Ramping modes linear and non-linear
Ramp rates 1 to 2000 °C/s in 1 °C/s increments
Injection temperature programmable up to 200 °C when used
with the furnace autosampler
Signal display Data Station VDU
Program storage unlimited disk storage with Data Station

B-10 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Specifications
GFS Furnace Autosampler

GFS Furnace Autosampler


The GFS furnace autosampler accommodates up to 60 samples in the
large carousel. Carousel changeover allows up to 120 samples per
element run. Six large reagent cups enable up to six matrix modifiers to
be employed. Using the cup reducing ring, smaller cups can be used to
reduce modifier consumption.

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.

Fast furnace operation provides concurrent operation of the furnace,


spectrometer, and autosampler sample uptake procedures, minimizing
overall furnace cycle time. The syringe is visible and easily accessible for
routine maintenance. A large, 1 L capacity wash vessel for long,
unattended analysis is complemented by an on-board waste vessel.
All facilities are programmed from the SOLAAR software. Sampling
facilities such as matrix modification (wet or dry mixing), standards
addition, dilution, re-concentration and automatic standards
preparation can be rapidly set up.

Automatic re-scaling and re-calibration functions are provided. If a


sample falls outside the calibration range, the system automatically and
intelligently calculates the most appropriate dilution factor required to
bring the sample back within range. Autosampler loading guides
indicate the optimum carousel layout.

Table B-8. Specifications of GFS furnace autosampler


Item Comment
Standard items 120 Polypropylene sample cups

12 Polypropylene reagent cups

10 spare capillary tips


Necessary additional items none
Carousel capacity 60 sample cups

six reagent cups


Cup types Polypropylene sample cups

Fluoroplastic sample cups

reduced volume sample cups

Polypropylene reagent cups

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-11
Specifications
VP100 Continuous Flow Vapor System

Table B-8. Specifications of GFS furnace autosampler, continued


Item Comment
Cup volumes (nominal) sample cups: 2 mL

reduced volume cups: 1.5 mL

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

VP100 Continuous Flow Vapor System


The VP100 Continuous Flow Vapor system performs hydride and
mercury vapor measurements with significant sensitivity improvement
over normal flame techniques. An air/acetylene flame or an electrically
heated cell is used for atomization.

The VP100 unit incorporates the reagent reservoirs, a variable speed


four channel peristaltic pump, control electronics and gas-liquid
separator. An integrated mass flow controller allows the carrier gas flow
to be controlled and monitored through the system software. The
continuous flow principle eliminates the need to clean the reaction
vessel after each sample.

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

Table B-9. Specifications of VP100 Continuous Flow Vapor system


Item Comment
Standard items two T-cells

spare pump tubing


Necessary additional items none
Absorption cell open ended, T-shaped silica cell

120 mm long

8 mm internal diameter

long path mercury absorption cell


Cell heating air/acetylene flame on 50 mm universal
burner

electrical heating using EC100


Carrier/purge gas argon or nitrogen
Gas inlet pressure 0.34 bar (5 psi)
Gas consumption up to 500 mL/min
Reducing agents sodium borohydride

Tin (II) chloride may be used for


mercury analysis
Solution transport variable speed

four channel peristaltic pump using


continuous flow principle
Solution flow rates reductant: 3.2 mL/min

sample: 7.8 mL/min


Carrier gas flow rates variable 50 to 500 mL/min

electronic control via mass flow


controller
Reagent containers two 1 L plastic bottles
Power 100-240 V, 50-60 Hz
Power consumption 30 VA
Dimensions [mm] 475 W × 300 H × 200 D

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-13
Specifications
EC100 Electrically Heated Atomization Cell

EC100 Electrically Heated Atomization Cell


The EC100 is an electrically heated atomization cell for flameless vapor
generation AAS. It provides improved analytical performance,
unattended operation and reduced operating costs.

The EC100 must be used with the VP100 and is suitable for all hydride
forming elements.

Table B-10. Specifications of EC100


Item Comment
Standard items EC100 furnace head

EC100 furnace power supply

two silica T-cells


Necessary additional items VP100 Continuous Flow Vapor System

appropriate accessory mount


Control system from external power supply
Temperature range ambient to 1000 °C in 1 °C steps
Power 200-240 V, 50 Hz or

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.

Table B-11. Specifications of AA Validator Kits


Item Comment
Major contents SOLAAR Validator Logbook
(depends on kit type)
Ca/Mg hollow cathode lamp

Ni/Cr/Mn hollow cathode lamp

pyrolytically coated cuvettes

manganese validation standard

nickel validation standard

chromium validation standard

Calibration Validation Unit (CVU)

water blank validation standard

Thermo Scientific iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) B-15
Specifications
Calibration Validation Unit

Calibration Validation Unit


The CVU is provided as part of the AA Validator Kits and contains a set
of traceable and certified filters. It is fitted in the spectrometer and
controlled by the OQ test software, and tests the spectrometer
resolution, wavelength accuracy, photometric accuracy and stability, and
D2 background correction efficiency.

The integrated PQ test software contains a complete set of SOPs and a


wizard to lead the user through the tests needed to validate the
instrument’s analytical performance against the manufacturer's
specification.
Table B-12. Specifications of Calibration Validation Unit
Item Comment
Standard items Calibration Validation Unit (CVU)

power supply

RS-232 data lead


Power 110-240 V at 50 or 60 Hz
Power consumption 10 VA

Left Hand Universal Accessory Mount


This accessory mount is for use in the iCE 3000 Series sample
compartments. This is necessary for mounting the EC100 furnace head,
the Calibration Validation Unit and the mercury absorption cell in these
sample compartments.

Right Hand Universal Accessory Mount


This accessory mount is for use in the right hand iCE 3400/3500 Series
sample compartment. It is necessary for mounting the EC100 furnace
head, the Calibration Validation Unit and the mercury absorption cell
in this sample compartment.

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.

Table B-13. Specifications of iSQ module


Item Comment
Standard items Intelligent Spectrometer Qualification
module

coded Ca/Mg hollow cathode lamp

right hand accessory mount


Necessary additional items none
Power 110-240 V at 50 or 60 Hz
Power consumption 10 VA

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

This chapter contains excerpts from component suppliers´ documents


with safety-relevant information that may concern users of the
iCE 3000 Series atomic absorption spectrometer.

Contents

• Maintenance of the CETAC ASX-560 and ASX-280 Flame


Autosampler on page C-2

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

Maintenance of the CETAC ASX-560 and ASX-280 Flame Autosampler


• Ensure that the autosampler is switched off and isolated from the
mains supply before carrying out any maintenance operations.

• Wipe the exterior surfaces with a soft cloth dipped in soapy water to
remove any marks.

• If a spillage occurs, isolate the autosampler from the mains supply


immediately. Wipe up the spillage with a dry cloth.

• The ASX-560 and ASX-280 autosamplers do not require routine


lubrication.

• Do not pick up the autosampler by either the vertical or horizontal


arms, but only by supporting the base of the device.

Safety Guidelines for Handling the Autosampler


• Observe electrical safety precautions.

• Read the Safety section of the user documentation of the


autosampler supplied with the unit.

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

furnace 5-29 hydroxylamine hydrochloride 6-27


electrically heated atomization cell 5-47
electronics 3-4
emergency shutdown 4-29 I
equipment cleaning and decontamination 4-8
iCE 3300 Series Spectrometer Specification B-4
ID100 Autodilutor
accessory 3-12
F specifications B-7
flame heated measurement cell (T-cell) 5-45 ignition electrode 7-11
flame optimization 6-18 impact bead
flame sample compartment 4-19 adjustment 6-20
flame system 3-3 alignment 6-10
flash checksum failure 6-2 implosion 4-9
flashback report 4-14 installing, hollow cathode lamps 3-7, 6-3
flashbacks 4-13–4-14 instrument cleaning 7-6
flow rates, check 7-31 Intelligent Spectrometer Qualification module B-17
fuel flow rate 6-16, 6-19 iSQ Module
alignmnet and operation 5-16, 6-4
fuel gases 5-17
description 3-9
furnace control B-10
installation 5-14
furnace window removal tool 7-21
location B-17
fuse replacement 7-7, 7-27, 7-32 maintenance 7-8
iSQ package 3-9
iSQ wizard 5-16, 6-4
G
gas leak test wizard 7-16
gas liquid separator 7-32 L
GFS Furnace Autosampler B-11 lab coat 4-31
GFS33 graphite furnace system 3-17 lamp
GFS33 system maintenance 7-27 alignment 3-7
GFS33, GFS35 and GFS35Z Furnace Head and Power installation 5-8
Supply B-8 removal 5-9
GFS33/35 and GFS35Z Furnace Heads 4-24 types 6-3
GFS35 / 35Z System Maintenance 7-19 lamp compartment 5-8
GFS35 and GFS35Z Graphite Furnace Systems 3-15 left hand sample compartment 3-9
GFS35Z Zeeman Furnace Head 4-24 long-handled, ball-ended hex key tool 5-11
gloves 4-31, 7-3
goggles 4-31
graphite furnace 3-7 M
Graphite Furnace Systems 3-4
mains switch 7-7
Graphite Furnace TeleVision (GFTV) 3-4
maintenance
autosampler C-2
ID100 7-17
H iSQ Module 7-8
hazardous contents 4-9 performed by Thermo Fisher Scientific 7-34
Health and Safety Form 7-34, A-5 procedures 7-4
heated measurement cell 3-19 spectrometer 7-6
Material Safety Data Sheets 1-4
high voltage 4-9
mercury absorption cell
hollow cathode lamps
connection 5-48
hazards 4-9
fitting to universal mount 5-47
installation 3-7, 6-3
properties 3-19
humidity 5-3
methyl isobutyl ketone 6-6
hydride generation technique 6-30
mobile phones 4-6

I-2 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C) Thermo Scientific
Index: N–V

MSDS 1-4 sample measurement 6-30


sample preparation 6-30
sample uptake tube 3-13, 5-39
N setting up, the flame system 3-10
shutting down, the VP100 6-32
nebulizer 7-12, 7-15
Slotted Tube Atom Trap (STAT)
nitrogen 3-15, 5-38
accessory 3-12
sodium borohydride reagent 3-19
SOLAARsecurity 3-6
O Solvent Resistant Flame Kit
On-Line Cookbook 6-20 components 3-13
operating sound level 4-14 installation 5-27
optical system 3-3 spray chamber 3-13
organic solvents 4-16, 6-5 spectrometer
O-rings 3-13 cleaning 7-6
fuse replacement 7-7
over-pressure disc 4-14, 6-5
installation 5-6–5-7
maintenance 7-6
operation 5-1, 6-1
P status indicators 6-2
parameter optimization 6-28 spray chamber drain 3-14, 6-17
parts, returning 7-34 stannous chloride reductant reagent 6-27
perchloric acid 4-15 STAT holder 5-45
peristaltic pump 7-31 Stockdale 3-3
personal protective equipment (PPE) 4-31 support gases 5-17
potassium iodide/ascorbic acid mixture 6-31
Power Supply module 7-7
T
T-cell
Q conditioning 5-49
Quadline 3-3 holder 5-45
Quadline Background Correction 7-6 temperature feedback system 7-22
thermal overload protection 7-33
third party components 1-4

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

shutdown 6-32 WEEE compliance A-2


shutting down 6-32

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

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