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
Thermo Scientific
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
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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
ii
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
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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Contents
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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
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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
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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
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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
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iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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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:
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•
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
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The flame atomization system
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The flame accessories
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The furnace atomization system
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The furnace accessories
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The vapor generation accessories
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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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:
1-2
•
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 ” 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 + ” means press and hold the key and then press the key.
•
Any button that you click on the screen is represented in bold face letters. For example, “click Close”.
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
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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)
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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 Information
www.thermofisher.com/aas
Service Contact
www.unitylabservices.com
Technical Documentation SharePoint
❖
To get user manuals for your product
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
[email protected].
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iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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Using this Manual Contacting Us
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iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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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
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Installation Kit including
•
-
Equipment for connecting the above components (hoses, cables)
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Computer equipment
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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.
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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:
2-2
•
Thermo Scientific™ GFS33 Graphite Furnace and autosampler for iCE™ 3300 AA spectrometer
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Thermo Scientific GFS35 or GR35Z Graphite Furnace and autosampler for iCE 3500 AA spectrometer
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Thermo Scientific SOLAAR Validator Package
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Thermo Scientific SOLAARSecurity Software
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Thermo Scientific ID100 Auto Dilutor
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Thermo Scientific VP100 Continuous Flow Vapor System (includes T-cell and mercury cell)
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Thermo Scientific EC100 Electrically Heated Atomization Cell
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Thermo Scientific Slotted Tube Atom Trap
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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
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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3 System Description This chapter provides an overview of the functional elements of the iCE 3000 Series atomic absorption spectrometer. Contents
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Description of AA Systems on page 3-2
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Spectrometer System on page 3-7
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iSQ Module on page 3-9
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Flame System on page 3-10
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Furnace on page 3-15
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VP100 Continuous Flow Vapor System on page 3-19
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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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.
3-2
iCE 3000 Series system
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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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
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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.
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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
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512 MB RAM
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CD ROM drive
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Fixed disk drive with at least 1 GB free space
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19 in SVGA color monitor
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USB port
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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
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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.
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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.
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•
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.
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System Description Spectrometer System
1
2
5
3
4
Labeled Components: 1=adjustment screw, 2=accessory mounting pin, 3=location plate, 4=mounting pads, 5=spring retainer Figure 3-2.
3-8
Right hand sample compartment with universal mount
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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:
Thermo Scientific
•
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
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
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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.
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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
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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.
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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
Thermo Scientific
The extraction system must be switched on and must be operating correctly before the furnace is used.
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.
1 2
3
Labeled Components: 1=cooling water outlet, 2=cooling water filter, 3=cooling water inlet Figure 3-5.
3-16
Furnace power supply connections panel
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 5
13
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.
3-18
GFS autosampler
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. 1
2
3 6
4 5
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
5
2
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.
3-20
Front panel of EC100
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 CAUTION Hot surfaces. Risk of burn. See manual for safety instructions.
WARNING Read and fully understand operator‘s manual before using this machine. Failure to follow operating instructions could result in death or serious injury.
Label description
Label position
Hot Surface. Risk of Burn. See manual for instructions.
This label is attached to the furnace.
Also refer to “Furnace Safety” on page 4-24. Read and fully understand This label is attached inside the flame operator’s manual before you use compartment. The label is attached this machine. Failure to follow at the bottom left hand side. operating instructions could result in death or serious injury. Also refer to “Flame System Safety” on page 4-12.
WARNING Read and fully understand operator‘s manual before using this machine. Failure to follow operating instructions could result in death or serious injury.
Read and fully understand This label is attached inside the flame operator’s manual before you use compartment at the right hand side this machine. Failure to follow wall near the drain tube. operating instructions could result in death or serious injury. Also refer to “Flame System Safety” on page 4-12.
WARNING Read and fully understand operator‘s manual before using this machine. Failure to follow operating instructions could result in death or serious injury.
Read and fully understand This label is attached to the inside of operator’s manual before you use the door of the spectrometer. this machine. Failure to follow operating instructions could result in death or serious injury. Also refer to “Spectrometer Safety” on page 4-9.
WARNING Read and fully understand operator‘s manual before using this machine. Failure to follow operating instructions could result in death or serious injury.
Read and fully understand This label is attached near the gas operator’s manual before you use connection panel at the left hand side this machine. Failure to follow of the instrument. 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 WARNING Heavy object. Can cause back injury during transportation. See manual for instructions.
Label description
Label position
Heavy Object. Can cause back injury during transportation. See manual for instructions.
This label is attached near the rating plate to the rear side of the instrument.
Also refer to “Installation of the Spectrometer” on page 5-6. WARNING Hazardous radiation. Can cause severe eye injury. See manual for safety instructions.
Hazardous Radiation. Can cause severe eye injury. See manual for safety instructions. Also refer to “Spectrometer Safety” on page 4-9.
This label is attached to the D2 lamp cover. This label is only applicable for the iCE 3400 and iCE 3500 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 manual for instructions.
This label is attached to the flame 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.
Thermo Scientific
Example of rating plate
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:
Thermo Scientific
•
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.
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 decontamination of the equipment if hazardous material is spilt on or inside the equipment.
4-8
•
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.
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
Thermo Scientific
Safety 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.
Thermo Scientific
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.
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
4-9
Safety Spectrometer Safety
Table 4-2.
4-10
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
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
Thermo Scientific
Safety Spectrometer Safety
Table 4-2.
Thermo Scientific
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.
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
4-11
Safety 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
4-12
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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Safety Flame System Safety
Flame Safety
CAUTION
Risk of Eye Injury. Nitrous oxide supported flames emit intense radiation which can damage your eyes if viewed directly. Visible and invisible radiation according to EN 12198 might cause retinopathy. Category 2. Avoid long exposure of several hours. Wear safety goggles that include an UV filter and provide protection against brightness.
CAUTION
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).
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.
Flashback
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Safety Flame System Safety
CAUTION
Only align the burner with an air/acetylene flame. Do not align the burner with a nitrous oxide/acetylene flame. Do not attempt to adjust the impact bead with a nitrous oxide supported flame burning. 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
4-14
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.
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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Safety Flame System Safety
Perchloric Acid
CAUTION
Explosion Hazard. Take the measures described below to reduce the risk of an explosion or a flashback. Aspiration of solutions of perchloric acid and metal perchlorates into a nitrous oxide supported flame can increase the risk of an explosion or a flashback. Consequently, Thermo Fisher Scientific does not recommend using perchloric acid in sample preparation for nitrous oxide supported flame analyses. If the use of perchloric acid is essential, you minimize the hazards if you: •
Ensure that the burner is kept clean, and do not allow deposits to accumulate around the slot.
•
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:
Thermo Scientific
•
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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Safety Flame System Safety
•
Thoroughly flush the spray chamber, and empty and refill the drain trap with clean water at the end of the analysis.
Organic Solvents
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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Safety 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.
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.
Acetylene
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Safety 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
4-18
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.
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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Safety Flame System Safety
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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Safety 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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Thermo Scientific
Safety Flame System Safety
The lower end of the drain extension must always be above the level of the liquid in the drain vessel/waste container! Do not use a glass or metal drain vessel. The drain extension tube must provide a vertical free-flowing drain outlet to prevent formation of any additional U-traps, and must be free of kinks, obstructions and sharp bends. Once out of the instrument, it must be oriented straight down in a vertical position. Empty and clean the waste container regularly. If you have used an organic solvent, do not let the solvent accumulate in the waste container, as vapor might cause a fire hazard.
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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
4-22
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.
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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Safety Flame System Safety
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
NOTICE
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. 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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Safety Furnace Safety
Flame Atomizer
CAUTION
Fire Hazard. Do not leave solvent in the spray chamber when you do not use the instrument. Solvent vapor can accumulate in and around the spectrometer, creating a fire hazard and potentially damaging plastic and other components.
Furnace Safety 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
CAUTION
4-24
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. 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.
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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Safety Furnace Safety
CAUTION
Heavy Load. The magnet and head assembly is heavy. Take care if you have to lift or move the assembly. Ensure that it is securely attached to the spectrometer before use
CAUTION
Danger of Bruises. When tilting the GFS35Z on the tilt mount, avoid trapping your fingers in the moving mechanism.
Fume Extraction
CAUTION
Hazardous Fumes. Hot, potentially toxic and corrosive fumes derived from the sample are vented above the furnace head and must be removed by a suitable fume extraction system. Fire the furnace only when the furnace head is securely attached to the spectrometer, it is not tilted, and there is suitable extraction.
Gases
CAUTION
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:
CAUTION
4-26
•
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.
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.
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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
NOTICE
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. 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
Thermo Scientific
Do not mix the waste from vapor analysis with waste from other analyses.
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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
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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
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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.
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.
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).
Gases
Waste
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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.
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Safety Residual Hazards
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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.
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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
5-2
For operation of the furnace, both power supply units must be connected to line power.
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
Thermo Scientific
•
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.
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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
5-4
•
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.
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Thermo Scientific
Installation Laboratory Conditions
•
NOTICE
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.
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.
1
2
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.
5-6
Spectrometer dimensions and weights
Spectrometer
Width
Depth
Height
Weight
iCE 3500
780 mm (30.1 in)
577 mm (22.7 in)
595 mm (23.4 in)
54 kg (119 lbs)
iCE 3400
780 mm (30.1 in)
577 mm (22.7 in)
520 mm (20.5 in)
54 kg (119 lbs)
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 (22.3 in)
589 mm (23.2 in)
595 mm (23.4 in)
45 kg (99 lbs)
iCE 3300GF
567 mm (22.3 in)
589 mm (23.2 in)
510 mm (20.1 in)
38 kg (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.
1
2
3
4
Labeled Components: 1=hollow cathode lamp, 2=lamp clip, 3=lamp ejection lever, 4=lamp socket Figure 5-2.
5-8
Lamp compartment - general view
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.
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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
5
3
4
Labeled Components: 1=adjustment screw, 2=accessory mounting pin, 3=location plate, 4=mounting pads, 5=spring retainer Figure 5-3.
Thermo Scientific
Right hand sample compartment with universal mount
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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.
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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.
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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. 2 1
4
3
6
5
Labeled Components: 1=ISQ module, 2=serial port, 3=power connector, 4=shutter, 5=RH accessory mount, 6=support bracket Figure 5-4.
5-14
iSQ Module assembly (iCE 3400/3500 systems)
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.
Thermo Scientific
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
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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 type
Pressure and gas
support gases
nominal pressure of compressed air 2.4 to 2.75 bar (35 to 40 psi)
fuel gases
NOTICE CAUTION
Gas pressures at spectrometer inlet ports Pressure value
nominal pressure of nitrous oxide
2.70 to 2.75 bar (39 to 40 psi)
maximum allowed pressure of acetylene
0.57-0.62 bar (8.5-9 psi)
The gas pressures on the gas box are maximum pressures. 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.
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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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Thermo Scientific
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:
Thermo Scientific
•
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:
NOTICE
•
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.
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.
Thermo Scientific
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.
5-22
CETAC ASX-560 autosampler - front view (Source: ASX-560/ASX-280 Autosampler Operator’s Manual, Teledyne Cetac)
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 3 4 5 8
7
6
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
2
1
3
Labeled Components: 1=RS232C serial port, 2=power inlet, 3=power switch Figure 5-9.
Thermo Scientific
ID100 Autodilutor - rear view
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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.
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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.
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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 8
7 7 6
5
4
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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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. 2 1
3
4
9
8
5 7
6
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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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
1 1
3
2
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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2. Locate the capillary tip adjustment controls A and B. See Figure 5-15. 1 2
3
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 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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❖
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
3
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.
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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 3
2
4
5
6
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
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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. 1
2
3
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)
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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
Thermo Scientific
Do not overtighten the pressure screw. This would shorten the life of the pump tubing and may damage the pump mechanism.
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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. 1 2 3 4
5 6 7
8 9
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
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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. 1 2
3
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.
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2. Orientate the burner with the burner handle to the right and the ignition electrode to the left. 1
5 4
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.
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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. ❖
CAUTION
To fit the mercury absorption cell to the universal accessory mount
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.
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1
2
3
4
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.
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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.
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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
7
6 4
5
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. 5-50
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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.
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Installation Installation of VP100 Continuous Flow Vapor System
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iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
Thermo Scientific
6 Operation This chapter outlines the basic system operations and checks before operation. Contents
Thermo Scientific
•
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
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. Standby
FC3
FC2
FC1
Halt
Comment
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
On
a
Spectrometer status indicators
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.
6-2
Connection panel with spectrometer status indicators
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
Thermo Scientific
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.
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.
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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.
CAUTION
•
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.
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:
Thermo Scientific
•
Empty any aqueous liquids from the drain.
•
Refill the drain with clean solvent. See “Maintenance of Drain” on page 7-15.
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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
NOTICE
•
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.
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: •
6-6
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.
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
Thermo Scientific
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.
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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.
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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.
1
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.
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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:
6-10
•
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.
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
Thermo Scientific
Operation Operation of Flame System
1 1
3 3 4 2
6
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.
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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
6-12
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.
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.
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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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Thermo Scientific
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
NOTICE
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. 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.
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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.
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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.
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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.
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iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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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
Thermo Scientific
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.
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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 5
2
6 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.
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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
4
2
5
6
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.
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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.
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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 Reagent
This reagent is suitable for mercury analyses only. 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.
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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: •
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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.
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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:
6-30
•
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.
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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.
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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.
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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.
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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
Arsenic (As) Antimony (Sb) Selenium (Se) Germanium (Ge) Tellurium (Te) Lead (Pb) Tin (Sn) Mercury (Hg)
Operation temperature
900 °C
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:
6-34
•
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.
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Operation Vapor Operation
Thermo Scientific
•
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.
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Operation Vapor Operation
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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.”
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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:
7-2
•
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:
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Maintenance General Advice for Maintenance
Thermo Scientific
-
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.
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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
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 hoses
If required
page 7-16
Perform gas leak test
every 6 months and after moving the instrument
page 7-16
Inspect and clean external surfaces of air compressor
Regularly
page 7-17
Flame system
Replace all gas supply hoses every three years.
Compressor filter/regulator unit: Inspect filter trap
Regularly
Drain our any liquid collected
Regularly
Clean filter bowl Drain liquid in the hose
If required
“Maintenance of the Air Compressor” on page 7-17
Inspect rubber components Regularly for deterioration and damage Autosampler
7-4
Refer to manufacturer’s manual
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Maintenance Inspection- and Servicing Plan
Table 7-1.
User maintenance procedures, continued
Component
Procedure
Variable Flow Auxiliary Oxidant accessory
Check the for wear and damage at regular intervals.
Graphite Inspect all graphite furnace system components
Frequency
Procedure Location
Weekly
page 7-20
Inspect all other head components Leak test water cooling and gas handling system
NOTICE
Thermo Scientific
page 7-26
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.
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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.
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Maintenance Maintenance of the Spectrometer
2
1 5 4
3
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.
NOTICE
Thermo Scientific
Mains inlet and fuse
Replace fuses only with same type and rating: 2 × 2.5 AF H 250 V IEC60127-2, Littelfuse 216 02.5, or equivalent type.
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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.
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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
Thermo Scientific
Do not dismantle the while it is still plugged to the spectrometer.
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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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
3 8 7 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.
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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.
Thermo Scientific
Alignment of ignition electrode
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Maintenance Maintenance of the Flame System
Maintenance of Spray Chamber Figure 7-5 schematically shows the parts of the spray chamber and the nebulizer. 3
2 1 19
standard impact bead adjustment
4
18 17 16
5
15 1
14
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.
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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
Thermo Scientific
Do not re-assemble the spray chamber with damaged parts.
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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.
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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.
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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.
•
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OQ Test Software/Automated Test Sequence/Start Test Sequence
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.
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iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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Maintenance Maintenance of the Flame System
Maintenance of the Slotted Tube Atom Trap
CAUTION
NOTICE
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. 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.
7-18
Flame compartment valance with Variable Flow Auxiliary Oxidant accessory fitted
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
Thermo Scientific
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.
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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
3
1
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
6
9
7
8
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.
7-20
GFS35Z furnace head - interior view
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.
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iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
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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
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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.
Thermo Scientific
•
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.
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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.
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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.
2
1
3
removal
4 8
8
5 6
6 4 7 insertion
3 2 1
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
1 2
removal
3 4 5 5 4 3 2 1
insertion
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.
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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.
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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.
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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.
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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. 1 2
3 4 5
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.
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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:
7-30
•
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.
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.
Thermo Scientific
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
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
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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
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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 instrument
Replace deuterium lamp
if necessary
see page 7-6
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
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Thermo Scientific
A Legal Documents Contents
Thermo Scientific
•
WEEE Compliance on page A-2
•
Declaration of Conformity on page A-3
•
Health and Safety Form on page A-5
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
[email protected] 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).
Health and Safety Form
1. General information
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 shipping packaging or in contact with - pump fluids - service fluids - samples - standard solutions - other chemicals - hazardous materials
Tick the applicable check box. Yes Æ go to section 3 No Æ go to section 5
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’. toxic
flammable
serious health hazard
corrosive
hazardous to environment
explosive
gas under pressure
other harmful substances
biological contaminated
radioactive contaminated
Thermo Scientific Health and Safety Form (P/N 1342350, Revision H)
oxidizing
Yes Æ go to section 4 No Æ go to section 5 iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
A-5 Page 1 of 2
Health and Safety Form
Legal Documents 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 third-party personnel?
Yes
No
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)
A-6
Date
Signature
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
Health and Safety Form (P/N 1342350, Revision H)
Company stamp
Thermo Scientific Page 2 of 2
B Specifications Contents
Thermo Scientific
•
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
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 spectrometer
512 kB Flash PROM 256 kB RAM three general purpose RS-232C ports USB port
B-2
Data Station
See “Data Station Control” on page 3-5.
Optics iCE 3400 configuration
Self-referencing single beam Zeeman system
Optics iCE 3500 configuration
Double Beam Stockdale optical system
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
Thermo Scientific
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.
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 spectrometer
512 kB Flash PROM 256 kB RAM three general purpose RS-232C ports USB port
Data Station
Refer to “Data Station Control” on page 3-5.
Optics iCE 3300 configuration
Double Beam Stockdale Optical system
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
B-4
Grating
1800 L/mm
Absorbance range
-0.150 A to 3.000 A (including background signal)
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
Thermo Scientific
none
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
B-6
Necessary additional items
none
Power
100-240 V at 50 or 60 Hz
Power consumption
50 VA
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.
Thermo Scientific
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
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
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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.
B-10
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
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
Thermo Scientific
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
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
B-14
Power consumption
720 VA
Dimensions [mm]
280 W × 140 H × 290 D (power supply)
Weight
approximately 13 kg
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 (depends on kit type)
SOLAAR Validator Logbook 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
Thermo Scientific
Necessary additional items
none
Power
110-240 V at 50 or 60 Hz
Power consumption
10 VA
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 •
Thermo Scientific
Maintenance of the CETAC ASX-560 and ASX-280 Flame Autosampler on page C-2
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
C-2
•
Observe electrical safety precautions.
•
Read the Safety section of the user documentation of the autosampler supplied with the unit.
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
Thermo Scientific
I Index Numerics
C
21 CFR Part 11 3-6 3 mm ball-ended hex key 5-13
Calibration Validation Unit (CVU) B-16 carousel cover 5-37 cleaning burner 7-9 furnace system 7-20 nebulizer 7-15 spray chamber 7-12 cleaning tool 7-11 clothing 4-31 compressor 3-11 condensation 5-3 cone replacement tool 7-24 contaminated parts 7-34 cooling water 3-16 cuvette contact cones 7-23 fitting 5-35 cuvette life counter 5-35 cuvette tool 5-35, 6-23
A AA systems 3-2, 6-2 AA Validator Kits B-15–B-16 accessory trolley 5-39 acetone carryover 4-14, 4-18 acetylides 4-15 acid blank reagent 6-27 acid channel 7-31 air compressor 3-11 air/acetylene flame 3-13, 5-18 alignment burner 6-8 capillary tip 6-25 furnace head 5-29, 5-32 impact bead 6-10 iSQ Module 5-16, 6-4 lamp 3-7 LH Accessory Mount 5-12 RH Accessory Mount 5-10 STAT Tube 5-26 T-Cell 5-46 alignment and operation 5-16, 6-4 alternate gas 3-15 argon 3-15, 5-38 ASX-260 Flame Autosampler B-6 ASX-520 Flame Autosampler B-5 atomization temperature 6-33 autosamplers 3-11, C-2 auxiliary oxidant 3-14 auxiliary oxidant flow rate 6-16
D data station control 3-5 installation 5-7 printer installation 5-7 software 3-5 declaration of conformity A-3 decommissioning, the instrument 4-7 deuterium lamp 7-6 drain empty and refill 7-16 position drain tube 4-20 tube 3-13 vessel 4-23 drain channel 7-31
B ball valve 4-20 Biohazard symbol 4-16 black nylon tubing 5-38 borohydride reductant reagent 6-27 burner 3-3 alignment 6-8 maintenance 7-9 types 3-10 warm-up 6-7, 6-17 burner cleaning tool 7-9
Thermo Scientific
E EC100 description B-14 installation of furnace head 5-49 installation of power supply 5-49 usage 3-19 Echelle 3-3 electrical connections autosampler 5-36
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
I-1
Index: F–M
furnace 5-29 electrically heated atomization cell 5-47 electronics 3-4 emergency shutdown 4-29 equipment cleaning and decontamination 4-8
F flame heated measurement cell (T-cell) 5-45 flame optimization 6-18 flame sample compartment 4-19 flame system 3-3 flash checksum failure 6-2 flashback report 4-14 flashbacks 4-13–4-14 flow rates, check 7-31 fuel flow rate 6-16, 6-19 fuel gases 5-17 furnace control B-10 furnace window removal tool 7-21 fuse replacement 7-7, 7-27, 7-32
G gas leak test wizard 7-16 gas liquid separator 7-32 GFS Furnace Autosampler B-11 GFS33 graphite furnace system 3-17 GFS33 system maintenance 7-27 GFS33, GFS35 and GFS35Z Furnace Head and Power Supply B-8 GFS33/35 and GFS35Z Furnace Heads 4-24 GFS35 / 35Z System Maintenance 7-19 GFS35 and GFS35Z Graphite Furnace Systems 3-15 GFS35Z Zeeman Furnace Head 4-24 gloves 4-31, 7-3 goggles 4-31 graphite furnace 3-7 Graphite Furnace Systems 3-4 Graphite Furnace TeleVision (GFTV) 3-4
H hazardous contents 4-9 Health and Safety Form 7-34, A-5 heated measurement cell 3-19 high voltage 4-9 hollow cathode lamps hazards 4-9 installation 3-7, 6-3 humidity 5-3 hydride generation technique 6-30
I-2
hydroxylamine hydrochloride 6-27
I iCE 3300 Series Spectrometer Specification B-4 ID100 Autodilutor accessory 3-12 specifications B-7 ignition electrode 7-11 impact bead adjustment 6-20 alignment 6-10 implosion 4-9 installing, hollow cathode lamps 3-7, 6-3 instrument cleaning 7-6 Intelligent Spectrometer Qualification module B-17 iSQ Module alignmnet and operation 5-16, 6-4 description 3-9 installation 5-14 location B-17 maintenance 7-8 iSQ package 3-9 iSQ wizard 5-16, 6-4
L lab coat 4-31 lamp alignment 3-7 installation 5-8 removal 5-9 types 6-3 lamp compartment 5-8 left hand sample compartment 3-9 long-handled, ball-ended hex key tool 5-11
M mains switch 7-7 maintenance autosampler C-2 ID100 7-17 iSQ Module 7-8 performed by Thermo Fisher Scientific 7-34 procedures 7-4 spectrometer 7-6 Material Safety Data Sheets 1-4 mercury absorption cell connection 5-48 fitting to universal mount 5-47 properties 3-19 methyl isobutyl ketone 6-6 mobile phones 4-6
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
Thermo Scientific
Index: N–V
MSDS 1-4
N nebulizer 7-12, 7-15 nitrogen 3-15, 5-38
O On-Line Cookbook 6-20 operating sound level 4-14 optical system 3-3 organic solvents 4-16, 6-5 O-rings 3-13 over-pressure disc 4-14, 6-5
P parameter optimization 6-28 parts, returning 7-34 perchloric acid 4-15 peristaltic pump 7-31 personal protective equipment (PPE) 4-31 potassium iodide/ascorbic acid mixture 6-31 Power Supply module 7-7
sample measurement 6-30 sample preparation 6-30 sample uptake tube 3-13, 5-39 setting up, the flame system 3-10 shutting down, the VP100 6-32 Slotted Tube Atom Trap (STAT) accessory 3-12 sodium borohydride reagent 3-19 SOLAARsecurity 3-6 Solvent Resistant Flame Kit components 3-13 installation 5-27 spray chamber 3-13 spectrometer cleaning 7-6 fuse replacement 7-7 installation 5-6–5-7 maintenance 7-6 operation 5-1, 6-1 status indicators 6-2 spray chamber drain 3-14, 6-17 stannous chloride reductant reagent 6-27 STAT holder 5-45 Stockdale 3-3 support gases 5-17
T Q Quadline 3-3 Quadline Background Correction 7-6
T-cell conditioning 5-49 holder 5-45 temperature feedback system 7-22 thermal overload protection 7-33 third party components 1-4
R reagents 6-27 recirculation chiller 3-17 reductant channel 7-31 returning, parts 7-34 right hand sample compartment 3-7 risk assessment 4-16, 4-22 room temperature 5-3
U universal accessory mount left sample compartment 3-9, B-16 right sample compartment 3-7, B-16 user maintenance 7-1, 7-4
V S safety glasses 4-31 safety information 4-8 safety precautions 4-2 sample channel 7-31 sample compartment left, universal accessory mount 3-9, B-16 right, universal accessory mount 3-7, B-16 sample cups 6-24
Thermo Scientific
Variable Flow Auxiliary Oxidant Accessory 3-12 Variable Flow Auxiliary Oxidant Kit 3-14, 6-6, 6-19 venting, the gas system 6-11 VP100 carrier gas flow rate 6-28 description 5-40, B-12 maintenance 7-30 measurement delay time 6-28 optimizing parameters 6-28 pump speed 6-28
iCE 3000 Series AA Spectrometers Operating Manual (P/N BRE0011709, Revision C)
I-3
Index: W–Z
shutdown 6-32 shutting down 6-32
Z
W warming up, the burner 6-7 wash facility 3-14 waste solvent draining 4-23
I-4
WEEE compliance A-2
Zeeman 3-3 Zeeman background correction 3-15 zero absorbance baseline 7-6
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
