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ATOMIC SPECTROMETRY

THGA
Graphite Furnace
Including the AS-800 Autosampler

User’s Guide
Release history

Part Number Release Publication Date Release Publication Date

0993-5259 1 February 1998 6 August 2000


2 May 1998
3 September 1998
4 April 1999
5 April 2000

Any comments about the documetation for this product should be addressed to:

User Assistance
PerkinElmer, Inc.
710 Bridgeport Avenue
Shelton, Connecticut 06484-4794
U.S.A.
Or emailed to info@perkinelmer.com

Notices
The information contained in this document is subject to change without notice. Except as specifically set forth in its
terms and conditions of sale, PerkinElmer makes no warranty of any kind with regaed to this document, including,
but not limited to, the implied warranties of merchantability and fitness for a particular purpose. PerkinElmer shall
not be liable for errors contained herein for incidental consequential damages in connection with furnishing, performance
or use of this material.
Copyright information
This document contains proprietary information that is protected by copyright.
All rights are reserved. No part of this document may be reproduced in any form whatsoever
or translated into any language without the prior written permission of PerkinElmer, Inc.
or one of its affiliates.
Copyright ©1998–2000 by affiliates of PerkinElmer, Inc.
Produced in Singapore
Trademarks
PerkinElmer is a trademark of PerkinElmer, Inc.
AA WinLab, AAnalyst, Lumina, and THGA are trademarks of affiliates of PerkinElmer, Inc.
Windows is a trademark and Microsoft is a registered trademark of Microsoft Corporation.
Registered names, trademarks, etc. used in this document, even when not specifically marked as such, are not to be consid-
ered unprotected by law.
Table of Contents

page

Chapter 1 Safety Information


Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Correct use of analytical instruments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Warning markings on the graphite furnace . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
Chapter 2 THGA Graphite Furnace: Preparing for Analyses
Atomizer compartment door . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Raising and lowering the door . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Removing and refitting the door . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
Installing the furnace autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
The first installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Fitting the autosampler to the spectrometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Removing the autosampler from the spectrometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Connecting the rinse feed tubes and the rinse bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
Connecting the drain tube and waste bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-10
Installing sample trays and containers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-11
Types of sample tray . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-11
To install the sample tray and cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-11
Sample cups and reagent containers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12
Quick Reference . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12
Setting up the system for analyses
using the furnace technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-13
Selecting the atomizer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-14
Setting up the autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15
Perform these steps before the start of every analysis run . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15
Filling and flushing the rinsing system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15
Rinsing solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-16
Aligning the autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-17
Checking the solution droplet delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-22

0993-5259 C-1
Contents

page

Chapter 3 THGA Graphite Furnace: System Maintenance


Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-3
Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-3
Checklists for regular maintenance tasks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4
Tilting the furnace in and out of the atomizer compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6
Dual-atomizer spectrometer systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6
Graphite furnace spectrometer systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8
Opening the furnace and removing the graphite tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-10
Inserting the graphite tube and closing the furnace . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12
Graphite furnace maintenance procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-14
Cleaning the graphite tube and graphite contacts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-14
Heating the graphite tube to remove contamination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-15
To clean the contact surfaces of the graphite tube and contacts . . . . . . . . . . . . . . . . . . . . . . . . . . 3-16
To condition the graphite tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-17
To heat the graphite furnace manually . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-18
Changing the graphite contacts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-19
Checking and cleaning the furnace windows . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-32
Cooling system maintenance procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-34
Emptying the cooling system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-34
Refilling the cooling system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-36
Changing the cooling system fuse . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-37
Autosampler maintenance procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-38
Routine maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-38
Valve maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-39
Routine maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-39
Rinsing solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-40
Checking the valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-41
Removing the rinse pump valves and sample pump
tube connectors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-42
Cleaning the valves, tube connectors and pump heads . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-44
Assembling and installing the valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-44
Repairing a pipet . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-47
Installing a new pipet assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-49
Aligning the pump heads . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-52

C-2 0993-5259
Contents

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Chapter 4 THGA Graphite Furnace: Parts and Supplies


Obtaining supplies, replacement parts, and accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-3
Furnace system supplies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-4
Furnace . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-4
Furnace gas and cooling systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-5
Matrix modifiers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-5
AS-800 furnace autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
Parts provided with the furnace autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
Supplies and replacement parts for the furnace autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-7
Pump parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8
Chapter 5 THGA Graphite Furnace: System Description
THGA Graphite Furnace . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
Furnace design . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
The graphite tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
The graphite contacts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5
Furnace heating and temperature profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Maximum power heating . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7
Time-controlled heating . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7
Temperature control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7
The furnace gas system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
Principle of the gas purging system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
Inert gas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
The external protective gas flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-10
The internal purge gas flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-10
Cooling the furnace system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11
Cooling system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11
Zeeman-effect background correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-12
The Zeeman effect . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-12
Applying Zeeman-effect background correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-14
Longitudinal configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-15
Transverse configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-16
Analyte signals and background correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-17
Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-18
Graphite furnace . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-18
Cooling system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-20

0993-5259 C-3
Contents

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AS-800 Furnace Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-21


Autosampler design . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-21
Sample and rinse pumps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-21
The sample table . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-21
Sample and reagent containers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-23
Controlling the autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-23
The autosampler operating cycle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-24
Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-25
AS-800 Furnace Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-25
Literature on electrothermal atomization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-26
Chapter 6 Translations of Warnings
Warning Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3
Index
Customer Service

C-4 0993-5259
Safety Information 1
1Safety Information

Contents page

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Correct use of analytical instruments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Warning markings on the graphite furnace . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4

0993-5259 1-1
Safety Information

1-2 0993-5259
Safety Information

Introduction

The guides provided with your analytical instrument contain information and
warnings that you must follow to ensure safe operation and to maintain the
instrument in a safe condition. This advice is intended to supplement, not
supersede, the normal safety code of behavior prevailing in the country of
operation.
General safety practices for atomic spectroscopy and potential hazards with
various atomic absorption techniques are described in the User’s Guide for the
atomic absorption spectrometer. Please refer to that guide before you operate the
system.
The information provided does not cover every safety procedure that should be
practiced. Ultimately, maintenance of a safe laboratory environment is the
responsibility of the user and the user’s organization.

Correct use of analytical instruments

Before you install or use your instrument, and in order to get the best results, you
should be familiar with all of the instruments in the system and know how to
operate them. You should also be aware of the safety procedures in force in your
laboratory, especially those concerning atomic spectroscopy instruments. Read
the guides supplied with the instruments before you start.
If you use the instrument in a manner not specified in the guides, or if you use it
for a purpose other than that intended, you may damage the instrument, or
compromise your own, or someone else’s, safety.
Analytical instruments should only be operated by persons who are suitably
qualified and have received adequate training.

0993-5259 1-3
Safety Information

Warning markings on the graphite furnace

Risk of hot surfaces


Risque de surfaces chaudes
Gefahr durch heiße Oberflächen

B A
0.6 m

B Strong Magnetic Field


Champ Magnétique Intense
Starkes Magnetfeld

C
C

0.6 m THGA furnace

Strong Magnetic Field Warning: Moving Parts – Risk of Injury


Anyone wearing a heart pacemaker or having Some moving parts of the instrument are accessible in
metallic implants should remain at least 0.6 normal operation. Keep hands, clothing and other
meter away from the furnace – in any direction – objects away from the moving parts of the instrument.
while the furnace is operating. Danger: Parties en mouvement – Risque d'accident
Champ magnétique intense corporel
Tout personne ayant un stimulateur cardiaque Certaines parties en mouvement de l'instrument sont
ou des implants métalliques doit rester éloignée accessibles en fonctionnement normal. Tenir les
d'au moins 0,6 m du four pendant le mains, vêtements et autres objets éloignés des parties
fonctionnement de celui-ci. en mouvement de l'instrument.
Starkes Magnetfeld Warnung: Bewegliche Teile – Verletzungsgefahr
Herzschrittmacherträger und Personen mit Bei normalem Betrieb sind bewegliche Teile des Geräts
Metall-Implanten müssen zum Magneten einen zugänglich. Hände, Kleidung und andere Gegenstände
Sicherheitsabstand von mindestens 0,6 m in von den beweglichen Teilen des Geräts fernhalten.
jeder Richtung um den Magneten einhalten.

1-4 0993-5259
THGA Graphite Furnace:
Preparing for Analyses 2
2THGA Graphite Furnace: Preparing for Analyses
Marker for header

Contents page

Atomizer compartment door . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3


Raising and lowering the door . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Removing and refitting the door . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
Installing the furnace autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
The first installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Fitting the autosampler to the spectrometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Removing the autosampler from the spectrometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Connecting the rinse feed tubes and the rinse bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
Connecting the drain tube and waste bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-10
Installing sample trays and containers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-11
Types of sample tray . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-11
To install the sample tray and cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-11
Sample cups and reagent containers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12
Quick Reference . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12
Setting up the system for analyses
using the furnace technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-13
Selecting the atomizer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-14
Setting up the autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15
Perform these steps before the start of every analysis run . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15
Filling and flushing the rinsing system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15
Rinsing solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-16
Aligning the autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-17
Checking the solution droplet delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-22

0993-5259 2-1
THGA Preparing for Analyses

2-2 0993-5259
THGA Preparing for Analyses

Atomizer compartment door

Raising and lowering the door


Perform the steps below to raise or lower the atomizer compartment door:

Grip

Latch button

Figure 2-1. Raising or Lowering the Atomizer Compartment Door


1. Place the fingers of your left hand behind the grip and press the latch button
with your thumb.
2. Keeping the latch button pressed in, raise or lower the atomizer compartment
door to the end stop, preferably holding the door with both hands.
You can also leave the door in any intermediate position when you release the
latch button.

0993-5259 2-3
THGA Preparing for Analyses

Removing and refitting the door


To operate the graphite furnace with the autosampler you must remove the
atomizer compartment door. Follow the steps below to remove and refit the door.

Door securing knob

Figure 2-2. Removing the Atomizer Compartment Door

Caution Risk of damage to the furnace autosampler


The sampler arm on the autosampler can strike the door when the door is in the
lowest position.
 Always remove the atomizer compartment door before you operate the
graphite furnace with the autosampler.

To remove the door:


1. Slide the door to the lowest position.
2. Unscrew the door securing knob.
3. Carefully pull the 2 door pins out of the door slide on the left-hand side.
4. Pull the door retainer strip out of the door slide on the right-hand side.
Removal is complete.
To refit the door:
1. Insert the door retainer strip into the slot in the door slide on the right-hand
side.
2. Slide the door up or down until the 2 door pins line up with the holes in the
door slide on the left-hand side.
Push the pins into the holes.
3. Screw in the door securing knob.
Refitting is complete.

2-4 0993-5259
THGA Preparing for Analyses

Installing the furnace autosampler

The first installation


A PerkinElmer service engineer will install the furnace autosampler at the same
time as the spectrometer system. The following instructions are provided for
those occasions when you may need to remove and refit the autosampler.
Usually there is no need to remove the autosampler. When you are working with
a different atomizer, or when you wish to perform graphite furnace maintenance
procedures, you swivel the autosampler away from the atomizer compartment to
the standby position at the right.
Note: The AS-800 autosampler functions with the HGA graphite furnace (as
used in the AAnalyst 700) and the THGA graphite furnace (as used in the
AAnalyst 600 and 800). Due to differences in these furnaces, the swing arm
supporting the autosampler is specific to the given furnace type and is not
interchangeable.

0993-5259 2-5
THGA Preparing for Analyses

Fitting the autosampler to the spectrometer

Caution Risk of damage to the autosampler


The autosampler assembly with the metal swing arm is quite heavy.
 Do not lift the autosampler by the motor, the autosampler arm, or any of the
plastic components. This can cause irreparable damage.
 Always lift the autosampler by the metal swing arm.

1. Make sure that the spectrometer is switched off.


2. Hold the autosampler assembly by the metal swing arm and carefully insert
the hinge pin on the swing arm into the hinge on the spectrometer to the right
below the atomizer compartment. Lower the autosampler assembly to the
stop.
3. Carefully swivel the autosampler to the standby position at the right.
4. Connect the control cable:
1. Feed the female connector on the cable from underneath through the slot
at the rear of the swing arm and insert it into the right-hand (as seen from
the rear) connector on the base of the autosampler.
2. Lead the cable to the accessory ports at the front of the spectrometer and
insert the plug into port 1.
5. Fit the rinse bottle and the waste bottle in the brackets on the swing arm.
6. Carefully swivel the autosampler to in front of the atomizer compartment and
secure it with the large securing knob.

Removing the autosampler from the spectrometer


1. Make sure that the spectrometer is switched off.
2. Disconnect the control cable at the spectrometer (it can remain attached to the
autosampler).
3. Unscrew the large securing knob and carefully swivel the autosampler to the
standby position at the right.
4. Remove the rinse bottle and the waste bottle from the brackets on the swing
arm.
5. Hold the autosampler assembly by the metal swing arm and carefully lift the
assembly vertically upward until the hinge pin comes out of the hinge.

2-6 0993-5259
THGA Preparing for Analyses

6. Put the autosampler in a safe place where its components will not be damaged
or strained.

Metal
swing arm
Hinge

Hinge
pin

Connector

Control cable

Figure 2-3. Fitting the Furnace Autosampler to the Spectrometer

0993-5259 2-7
THGA Preparing for Analyses

Connecting the rinse feed tubes and the rinse bottle


The basic rinse bottle provided with the instrument is made from polyethylene
(PE). PE is resistant to most rinsing solutions that are commonly used. A PTFE
rinse bottle is offered as an option. If you are performing trace analyses, you may
prefer to use the PTFE bottle to reduce the risk of contamination. If you are using
an aggressive rinsing solution, use the PTFE rinse bottle.
Note: New plastic components may be contaminated with copper as a result of
the production process. We recommend that you rinse all new components in
dilute nitric acid and then in deionized water before you use them.
Refer to Figure 2-4 while performing the following procedure.
1. You require:
– a rinse bottle and the cap with the small hole,
– the rinse feed assembly, consisting of a flexible PTFE tube with two
screw fittings and a rigid FEP tube with a complementary screw thread.
2. Push the notched end of the rigid tube through the bottle cap until the tube
touches the base of the bottle.
3. Connect one end of the flexible tube to the rigid tube.
4. Slide the rinse bottle into the right-hand bracket on the swing arm.
5. Connect the other end of the flexible tube to the inlet fitting of the rinse pump.

2-8 0993-5259
THGA Preparing for Analyses

Rinse Pump

Rinse feed: flexible


Rinse feed: rigid

Rinse feed
tube

Tube
Port 1
Waste Rinse Control cable Nut
bottle bottle
Back ferrule
Front ferrule

Tube fitting
on the pump

Figure 2-4. Connecting the Rinse Feed Tubes and Rinse Bottle

0993-5259 2-9
THGA Preparing for Analyses

Connecting the drain tube and waste bottle


The basic waste bottle provided with the instrument is made from polyethylene
(PE). PE is resistant to most commonly-used solutions. A PTFE waste bottle is
offered as an option. If you are using an aggressive rinsing solution, particularly
if it attacks PE, you should use the PTFE waste bottle.
You may have to change the drain tube more often if you are using an aggressive
rinsing solution.
1. Push one end of the drain tube onto the drain outlet on the rinsing port.
2. Slot the rinsing port onto the guides on the left-hand side of the circular trough
for the sample tray.
3. Slide the waste bottle into the left-hand bracket on the swing arm.
4. Place the end of the drain tube into the mouth of the waste bottle.
If necessary, shorten the drain tube so that it protrudes only about 30 mm into
the waste bottle. Do not put a cap on the bottle.
The drain tube must hang straight down, without any loops, and the end must
never be immersed in the liquid in the bottle.

Rinsing Circular
port trough

Drain
tube

Securing
knob Waste Rinse
bottle bottle

Figure 2-5. Connecting the Drain Tube and Waste Bottle

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THGA Preparing for Analyses

Installing sample trays and containers


Types of sample tray
Two sample trays are provided with the autosampler: one tray has 88 locations
while the other has 148 locations.
You select the type of sample tray you are going to use in the software. The
procedure is described in the AA WinLab Online Help.

To install the sample tray and cover


1. Grip the hub of the sample tray and lower it onto the drive spindle.
2. Rotate the tray gently until the tab on the hub locates in the slot on the drive
spindle. There is a notch in the outer ring of sample locations to mark the
position of the tab.
3. Place the sample tray cover over the hub and line it up so that the tabs on the
sample tray trough engage in the notches in the cover. The ports in the cover
are on the left.
Note: Always place the cover on the sample tray to protect the samples from
contamination and to reduce the rate of evaporation of the solvent. You can
reduce the rate of evaporation further by pouring a small volume of water into the
trough; the water level in the trough must always be below the top of the central
ring around the drive spindle.

Hub

Notch

0993-5259 2-11
THGA Preparing for Analyses

Sample cups and reagent containers

Cup or container 88-location tray 148-location tray


volume, material locations locations
1.2 mL; polypropylene not suitable 1–120
122, 123, 125, 127, 128,
130, 132, 133, 135, 137,
138, 140
2.5 mL; polypropylene 1–80 121, 124, 126, 129, 131,
134, 136, 139
7 mL; polypropylene 81–88 141–148

 Polypropylene containers are suitable for organic solvents

Quick Reference
A slot is provided underneath the autosampler into which you can insert the
Quick Reference. We recommend that you keep the Quick Reference with the
autosampler at all times since it contains important maintenance information,
particularly maintenance of the valves.

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THGA Preparing for Analyses

Setting up the system for analyses


using the furnace technique

Summary of the procedure:


1. Switch on the system (see ‘Switching on the system’ in the Spectrometer
User’s Guide).
2. If necessary, move the graphite furnace into the atomizer compartment
(procedure: page 2-14).
3. Carefully swivel the autosampler to in front of the atomizer compartment and
secure it with the large securing knob (procedure: page 2-5).
4. Create or open a method (see the Online Help in AA WinLab).
5. Install the lamps that you require (see ‘Installing lamps’ in the Spectrometer
User’s Guide).
6. If required, install and condition a graphite tube (see ‘Inserting the graphite
tube and closing the furnace’, page 3-12).
7. Set up the furnace autosampler (see the Online Help in AA WinLab).
You should now optimize the analytical conditions. Refer to the Online Help in
AA WinLab.

0993-5259 2-13
THGA Preparing for Analyses

Selecting the atomizer

Note: This procedure applies only to dual-atomizer (flame/furnace)


spectrometer systems.
If the atomizer you require is not currently located in the atomizer compartment,
follow the steps below to move it into the compartment:

W9.1
Warning: Moving Parts – Risk of Injury
Some moving parts of the instrument are accessible in normal operation.
 Keep hands, clothing and other objects away from the moving parts of the
instrument.
1. If the flame is burning, extinguish it, shut down the gases (except the air
supply), and bleed the gas supply lines (see ‘Extinguishing the flame’ in the
Burner System User’s Guide).
2. Make sure that the air supply is turned on since this provides the pneumatic
pressure required to change the atomizers.
3. Make sure that the furnace autosampler is swivelled from in front of the
atomizer compartment to the standby position at the right, and that the
nebulizer sample tube is not connected to an external accessory.
4. In the File menu, click on Change Technique.
–or–
On the Toolbar, click on Technique.
The Select Technique dialog appears.
5. Select the atomizer that you require:
Flame for the burner system.
Furnace for the graphite furnace.
6. Click on OK.
The system changes over the atomizers. Further information on changing the
atomizer is also provided in the Online Help in AA WinLab.
Note: While the atomizers are being changed, do not put your hands or other
objects into the atomizer compartment.

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THGA Preparing for Analyses

Setting up the autosampler

Perform these steps before the start of every analysis run


1. Fill and flush the rinsing system (procedure: page 2-15).
2. Align the autosampler arm (procedure: page 2-17 ).
3. Adjust the penetration depth of the pipet tip in the graphite tube (procedure:
page 2-19).
4. Adjust the immersion depth of the pipet tip in the sample cup (procedure:
page 2-21).
5. Check delivery of the solution droplet (procedure: page 2-22 ).

Filling and flushing the rinsing system


 You must fill the rinsing system before the start of every analysis run to make
sure that the tubes are completely filled with fresh rinsing liquid, to remove
entrained air bubbles, and as part of routine valve maintenance.
 You must flush the rinsing system at the end of every analysis run as part of
routine valve maintenance.
Follow the steps below to fill and flush the rinsing system:
1. Make sure that the rinsing system components are correctly installed, in good
condition, and suitable for the rinsing liquid you will use.
2. Prepare the rinsing solutions that you require, see following page.
3. Fill the rinse bottle with the first, clean, particle-free, rinsing liquid.
If there are particles in the rinsing liquid they can lodge in the valves, causing leaks
and non-reproducible results.
4. Fill and flush the system:
1. In the Furnace Control window, click on Flush Sampler.
This activates a rinse cycle.
2. Repeat substep 1 as often as required to completely fill the rinsing system
with rinsing liquid and flush all the air out.
5. Empty the waste bottle. Dispose of any hazardous waste correctly.
6. Repeat steps 2 through 4 for each further rinsing solution.
Note: Make certain there are no air bubbles in the rinsing system. Air
bubbles can lead to non-reproducible results.

0993-5259 2-15
THGA Preparing for Analyses

Rinsing solutions
Use the following rinsing solutions in the given sequence:

Before the start of every analysis series:


If the rinsing solution you intend to use is miscible with the solution currently in
the system, use your intended rinsing solution. If the rinsing solution you intend
to use is not miscible with the solution in the system, you must use intermediate
rinsing liquids.
For example, to change from an acidic liquid to an organic solvent, you could use:
1. Deionized water.
2. Isopropanol or other water-miscible solvent.
3. Final organic solvent.

After an analysis series:


1. If you have been using an organic rinsing liquid, use isopropanol or other
water-miscible solvent.
2. Dilute nitric acid. This is especially important for elements with a tendency to
carryover.
3. Isopropanol.
4. Deionized water.

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THGA Preparing for Analyses

Aligning the autosampler


 You must align the autosampler to make sure that:
– the delicate tip of the sampling pipet enters the sample injection hole in
the graphite tube without striking the edge of the hole;
– the pipet tip does not strike the integrated platform;
– the measurement solution is correctly dispensed.

 You must check alignment of the autosampler:


– before the start of every analysis run;
– every time you change the graphite tube or contacts, or open and close the
furnace;
– every time you realign the furnace.

To align the autosampler arm and preadjust the penetration depth:


A summary of the procedure is presented below. For detailed information, refer
to the Online Help in AA WinLab.

Caution Risk of damage to the autosampler


You can cause irreparable damage to the gears if you attempt to move the
autosampler arm by hand.
 Never attempt to move the autosampler arm by hand.
Move it only with the depth control wheel.

Refer to Figure 2-6 for the alignment controls.


1. Raise the pipet tip out of the rinsing port:
1. In the Furnace Control window, click on Align Tip.
The Align Autosampler dialog appears.
2. In this dialog, click on Unlocked Above Tube. The autosampler arm is
unlocked and the pipet tip moves to a position directly above the graphite
tube.
2. Using the depth control wheel, very carefully lower the pipet tip to just above
the graphite contact.
Do not allow the pipet tip to touch any part of the furnace.
3. Adjust the forward/backward and left/right controls on the autosampler until
the pipet tip is more or less directly above the injection hole.

0993-5259 2-17
THGA Preparing for Analyses

Depth control
wheel

Left/right
alignment
control

Forward/backward
alignment control

Figure 2-6. Alignment controls on the autosampler

W3.3
Warning: UV Radiation – Risk of Eye Damage
The lamps may emit UV radiation which can damage your eyes.
 Always wear UV-absorbing safety glasses when aligning the autosampler.
4. View the inside of the furnace:
1. Swing down the white background plate on the left-hand side of the
furnace.
2. Swing down the mirror on the right-hand side of the furnace.
You can view the inside of the graphite tube in the mirror.
Wear UV-absorbing glasses when viewing the graphite tube.

2-18 0993-5259
THGA Preparing for Analyses

5. Then very carefully lower the pipet tip with the depth control wheel into the
tube to check that the pipet tip does not strike the edge of the injection hole.
Do not lower the pipet tip so far that it could strike the integrated platform (see
Figure 2-7). View the inside of the graphite tube while you are doing this.
6. In the Align Autosampler dialog, click on Unlocked Above Tube again, and in
the dialog that appears save the new position.
Saving can take several seconds.
7. Swing up the mirror and the background plate.
Note: Once you have saved this depth position, do not inadvertently change it
by clicking on Yes to the query Do you want to save this position? in the Unlock
Above Tube and In Tube commands. Only click on Yes when you have readjusted
the depth.

To check and fine-adjust the penetration depth of the pipet tip in the
graphite tube:
A summary of the procedure is presented below. For detailed information, refer
to the Online Help in AA WinLab.

W3.3
Warning: UV Radiation – Risk of Eye Damage
The lamps may emit UV radiation which can damage your eyes.
 Always wear UV-absorbing safety glasses when aligning the autosampler.

Caution Risk of damage to the pipet tip


The pipet tip enters the graphite tube when you issue the In Tube command. The
pipet tip can strike the edge of the injection hole if the autosampler arm has not
been aligned.
 Make sure that the autosampler arm has been aligned before you issue the
In Tube command.

1. Before you use this procedure, align the autosampler arm as described in the
procedure above.
2. In the Furnace Control window, click on Align Tip.
The Align Autosampler dialog appears.
3. In this dialog, click on In Tube. The autosampler arm is unlocked and the pipet
tip enters the graphite tube.

0993-5259 2-19
THGA Preparing for Analyses

4. View the inside of the furnace:


1. Swing down the white background plate on the left-hand side of the
furnace.
2. Swing down the mirror on the right-hand side of the furnace.
You can view the inside of the graphite tube in the mirror.
Wear UV-absorbing glasses when viewing the graphite tube.
5. Use the depth control wheel to move the pipet tip into the tube until it is at the
correct distance above the integrated platform.
Do not allow the tip to touch any part of the furnace.
6. In the Align Autosampler dialog, click on In Tube again, and in the dialog
that appears save the new position.
Saving can take several seconds.
7. Swing up the mirror and the background plate.
Note: Once you have saved this depth position, do not inadvertently change it
by clicking on Yes to the query Do you want to save this position? in the Unlock
Above Tube and In Tube commands. Only click on Yes when you have readjusted
the depth.

Detail in mirror

2 mm

Figure 2-7. Penetration depth of pipet tip in the graphite tube

2-20 0993-5259
THGA Preparing for Analyses

To adjust the immersion depth of the pipet tip in the sample cup:
A summary of the procedure is presented below. For detailed information, refer
to the Online Help in AA WinLab.
1. Preliminary procedure
1. Align the sampler arm (procedure: page 2-17).
2. Put a sample cup in location 1 of the sample tray (for visual comparison).
3. In the Furnace Control window, click on Align Tip.
The Align Autosampler dialog appears.
4. In this dialog, click on Unlock Above Rinse. The pipet tip moves to a position
directly above the rinsing port.
5. Adjust the depth control wheel to lower the arm so that the depth of the pipet
tip in the rinsing port is approximately the correct depth for the tip inside the
sample cup.
6. In the Align Autosampler dialog, click on Unlock Above Rinse again, and in
the dialog that appears save the new position.
2. Finely adjusting the depth in the sample cup
1. Make a preliminary adjustment as described above.
2. Put a sample cup in location 1 of the sample tray.
3. In the Align Autosampler dialog, click on In Sample Cup. The pipet tip moves
into the sample cup.
4. Adjust the depth control wheel so that the pipet tip is at the correct depth
inside the cup.
5. In the Align Autosampler dialog, click on In Sample Cup again, and in the
dialog that appears save the new position.
Note: Once you have saved this depth position, do not inadvertently change it
by clicking on Yes to the query Do you want to save this position? in the Unlock
Above Rinse command.

0993-5259 2-21
THGA Preparing for Analyses

Checking the solution droplet delivery


Once you have aligned the autosampler as described in the preceding sections,
you can check that solutions will be correctly dispensed by injecting blank
solution into the graphite tube.

W3.3
Warning: UV Radiation – Risk of Eye Damage
The lamps may emit UV radiation which can damage your eyes.
 Always wear UV-absorbing safety glasses when aligning the autosampler.
1. Create a furnace program comprising drying, pyrolysis, atomization, and
clean-out.
Enter the total volume of solution that you will use in the subsequent analyses.
Refer to the Online Help in AA WinLab on how to create a method.
2. Place a sample cup containing blank solution in location 1 in the autosampler.
Use an identical blank solution to the one that you will use for the subsequent
analyses.
3. In the Automated Analysis window, on the Setup page, in the Locations
column, enter the autosampler location of the blank solution.
4. View the inside of the furnace:
1. Swing down the white background plate on the left-hand side of the
furnace.
2. Swing down the mirror on the right-hand side of the furnace.
You view see the inside of the graphite tube in the mirror.
Wear UV-absorbing glasses when viewing the graphite tube.
5. Start the method:
In the Automated Analysis window, on the Analyze page, click on Analyze
Samples.
6. Look into the mirror and watch the delivery of the solution droplet onto the
platform.
7. Swing up the mirror and the white plate before the atomization step starts and
allow the furnace program to run to completion.

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THGA Preparing for Analyses

8. If the solution droplet delivery was unsatisfactory, make the appropriate small
adjustments to the penetration depth of the pipet tip (see page 2-19 ).
9. Repeat step 4 through step 8 to dispense further aliquots of blank solution
until you are satisfied with the delivery.
The pipet tip is at the correct height when the solution droplet contacts the
graphite surface just before leaving the tip.
If the pipet tip is too far above the platform and the droplet does not contact
the graphite surface, liquid may remain in the tip, leading to pipetting errors.
If the pipet tip is too near to the platform, liquid may hang up on the tip,
leading to pipetting errors

Detail in mirror

Wrong: Tip too far above platform Wrong: Tip too near platform

Correct

Figure 2-8. Checking the solution droplet delivery

0993-5259 2-23
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THGA Graphite Furnace:
System Maintenance 3
3THGA Graphite Furnace: System Maintenance
Marker for header

Contents page

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-3
Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-3
Checklists for regular maintenance tasks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4
Tilting the furnace in and out of the atomizer compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6
Dual-atomizer spectrometer systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6
Graphite furnace spectrometer systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8
Opening the furnace and removing the graphite tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-10
Inserting the graphite tube and closing the furnace . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12
Graphite furnace maintenance procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-14
Cleaning the graphite tube and graphite contacts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-14
Heating the graphite tube to remove contamination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-15
To clean the contact surfaces of the graphite tube and contacts . . . . . . . . . . . . . . . . . . . . . . . . . . 3-16
To condition the graphite tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-17
To heat the graphite furnace manually . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-18
Changing the graphite contacts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-19
Checking and cleaning the furnace windows . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-32
Cooling system maintenance procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-34
Emptying the cooling system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-34
Refilling the cooling system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-36
Changing the cooling system fuse . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-37

0993-5259 3-1
THGA System Maintenance

Contents page

Autosampler maintenance procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-38


Routine maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-38
Valve maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-39
Routine maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-39
Rinsing solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-40
Checking the valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-41
Removing the rinse pump valves and sample pump
tube connectors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-42
Cleaning the valves, tube connectors and pump heads . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-44
Assembling and installing the valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-44
Repairing a pipet . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-47
Installing a new pipet assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-49
Aligning the pump heads . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-52

3-2 0993-5259
THGA System Maintenance

Introduction

W1.2
Warning: Unauthorized Adjustments and Servicing
Only a PerkinElmer service engineer or similarly trained and authorized person
should be permitted to service the instrument.
 Do not attempt to make adjustments, replacements, repairs, or modifications
to this instrument except as described in the documentation supplied with the
instrument.

If the spectrometer system does not function correctly…


 Switch off the spectrometer system and make sure it cannot be operated.
 Contact your local PerkinElmer office.
You should only perform the maintenance procedures described in this guide.
For any other maintenance or service contact your local PerkinElmer office to
arrange for a service engineer to visit.
In particular you should only allow a PerkinElmer service engineer or similarly
trained and authorized person to perform any work on:
 Electrical components inside the instrument;
 The monochromator and all other optical system components.
Before the service engineer arrives:
1. Make sure that the instrument and work area are clean.
2. Empty the furnace autosampler waste bottle and remove the samples and
reagents from the autosampler.

Troubleshooting
See the Troubleshooting guide supplied with the system. This guide includes
information about problems that can arise with both the software and the
spectrometer system.

0993-5259 3-3
THGA System Maintenance

Checklists for regular maintenance tasks

It is not possible to say exactly how often you must perform the procedures described here. This
depends on the number and type of samples that you analyze. At first you should perform most of
the checks before each batch of samples (one autosampler tray). You will soon be able to decide
how often you need to perform the checks and maintenance procedures for each type of sample
that you analyze.

Furnace, maintenance checklist

If you analyze samples that have ‘dirty’ matrices, such as blood, sugar or oil, you will probably
have to clean the components more often than if you were analyzing ‘clean’ samples, such as
drinking water.
Graphite tube If the tube is contaminated, for example by deposits around the injection hole
or on the integrated platform, you may be able to clean the tube (procedure:
page 3-14). If the contact surfaces on the tube are pitted or cracked, install a
new tube.
Graphite contacts Check the condition of graphite contacts. If they are pitted or cracked, install
new ones (procedure: page 3-19 ).
Every time that the furnace is opened, remove any particles from inside the
contacts using a small vacuum cleaner or a cleaning swab.
Furnace windows Clean the windows regularly (procedure: page 3-32 ).
How frequently depends on the type of samples being analyzed.

Cooling system, maintenance checklist

Water level Make sure that the water level is always at the MAX. mark. Fill up the system
when necessary (procedure: page 3-36).

3-4 0993-5259
THGA System Maintenance

Autosampler, maintenance checklist

Autosampler Wipe over the surfaces with a lint-free cloth moistened with a dilute solution
external surfaces of laboratory detergent.
The autosampler surfaces are resistant to dilute acids and alkalis, and to a
lesser extent to strong acids and alkalis and organic solvents.
Complete rinsing Fill and flush the rinsing system before the start of every analysis run
system (procedure: page 2-15).
Flush the rinsing system when you have finished an analysis run (more
information: page 3-39).
Valves The valves must function correctly to maintain the precision of the dispensed
volumes. If the precision of the analytical results deteriorates, this can be an
indication that a valve is not functioning correctly.
If a valve seizes or leaks, for example because the pump has been idle for a
long time, or because of particles lodged in the valve, or because of worn
seals, you can remove the valves to clean or change them (more information:
page 3-42).
Waste bottle Empty the autosampler waste bottle regularly. Never allow it to overflow or
allow the liquid to reach the end of the drain tube.
If the bottle contains hazardous, toxic, or flammable substances, dispose of
the waste properly, according to the local safety regulations.
Rinse bottle Make sure that the rinse bottle is always filled with clean, particle-free
rinsing liquid.
All tubes Make sure that all the tubes are clean and free from kinks.
Change any tubes that may be damaged or contaminated.
Pipet tip Make sure that the pipet tip is not damaged. If the tip is damaged you may
get pipetting errors during the analyses. Repair the tip or install a new pipet
assembly if necessary (more information: page 3-47).
Pump heads Make sure that the pump heads are not loose. Tighten the pump head
retaining ring if necessary. Make sure that the pump head remains vertical,
with the arrow aligned vertically (procedure: page 3-52).

0993-5259 3-5
THGA System Maintenance

Tilting the furnace in and out of the atomizer


compartment

To perform maintenance procedures on the graphite furnace, you must tilt the
furnace out of the atomizer compartment. The procedures for the two types of
spectrometer system are described below.

Dual-atomizer spectrometer systems


With dual-atomizer spectrometer systems (flame and furnace) you drive the
graphite furnace to the maintenance position and then tilt it out of the atomizer
compartment for easy access to the components.

To tilt the furnace out:

W4.3
Warning: High Temperatures – Risk of Burns
The graphite furnace can generate very high temperatures.
 Do not touch any parts of the furnace, especially the graphite components,
until they have cooled to room temperature.

Caution Risk of damage to the instrument


1. You can damage the graphite furnace if you tilt it forward when it is located in
the operating position.
 Always drive the graphite furnace to the maintenance position before you tilt
it out of the atomizer compartment.
2. The graphite furnace is heavy.
 Grasp it firmly as you tilt it and support its weight until it reaches the end stop.

1. Make sure that the furnace is cool.


2. Carefully swivel the autosampler to the standby position at the right.
3. Drive the graphite furnace to the maintenance position:
1. In the Tools menu, click on Diagnostics.
2. Click the Furnace tab at the bottom of the Diagnostics window.
3. Click on Change Contacts.
4. A warning message appears.
When you are ready, click on OK.

3-6 0993-5259
THGA System Maintenance

4. Wait until the graphite furnace has been driven to the maintenance position.
5. Grasp the graphite furnace with both hands and carefully tilt it forward.
Support its weight until it reaches the end stop. Never allow the graphite
furnace to swing down with force.
The graphite furnace is now accessible and you can perform maintenance
procedures.

To tilt the furnace in:


When you have completed maintenance procedures, tilt the graphite furnace back
into the atomizer compartment and drive it to the operating position as follows:
1. Grasp the graphite furnace with both hands and carefully tilt it back into the
atomizer compartment. Support its weight until it reaches the end stop.
Never allow the graphite furnace to swing back with force.
2. Drive the graphite furnace back to the operating position:
1. If the Diagnostics window is not currently open, in the Tools menu, click
on Diagnostics.
2. Click the Furnace tab at the bottom of the Diagnostics window.
3. Click on Restore Position.
4. A warning message appears.
When you are ready, click on OK.
The graphite furnace is driven back to the operating position.

0993-5259 3-7
THGA System Maintenance

Graphite furnace spectrometer systems


With graphite furnace spectrometer systems (fixed furnace) you tilt the graphite
furnace out of the atomizer compartment to the maintenance position for easy
access to the components.

To tilt the furnace to the maintenance position:

W4.3
Warning: High Temperatures – Risk of Burns
The graphite furnace can generate very high temperatures.
 Do not touch any parts of the furnace, especially the graphite components,
until they have cooled to room temperature.

Caution Risk of damage to the instrument


The graphite furnace is heavy.
 Grasp it firmly as you tilt it and support its weight until it reaches the end stop.

1. Make sure that the furnace is cool.


2. Carefully swivel the autosampler to the standby position at the right.
3. Grasp the graphite furnace with both hands and carefully tilt it forward.
Support its weight until it reaches the end stop (the latch clicks into the detent
position). Never allow the graphite furnace to swing down with force.
The graphite furnace is now accessible and you can perform maintenance
procedures.

To install a quartz tube atomizer:


If you intend to install the quartz tube atomizer (QTA) of a flow-injection system,
you must tilt the graphite furnace completely out of the atomizer compartment.
Do this as follows:
1. Perform steps 1 through 3, above, to tilt the furnace to the maintenance
position.
2. Supporting the weight of the graphite furnace, depress the latch tab and
carefully lower the furnace to the end stop. Support its weight until it reaches
the end stop. Never allow the graphite furnace to swing down with force.

3-8 0993-5259
THGA System Maintenance

To tilt the furnace in:


When you have completed maintenance procedures, or if you have finished work
with the QTA, tilt the graphite furnace back into the atomizer compartment as
follows:
1. From the maintenance position:
Supporting the weight of the graphite furnace, depress the latch tab and
carefully tilt the furnace back into the atomizer compartment.
Support its weight until it reaches the end stop.
Never allow the graphite furnace to swing back with force.
2. When the furnace is tilted fully out of the atomizer compartment:
Grasp the graphite furnace with both hands and carefully tilt it up to the
maintenance position.
Then, tilt it back into the atomizer compartment as described in step 1, above.

0993-5259 3-9
THGA System Maintenance

Opening the furnace and removing the graphite tube

W4.3
Warning: High Temperatures – Risk of Burns
The graphite furnace can generate very high temperatures.
 Do not touch any parts of the furnace, especially the graphite components,
until they have cooled to room temperature.
1. Make sure that the furnace is cool.
2. Tilt the graphite furnace out of the atomizer compartment:
1. Dual-atomizer spectrometer systems: Drive the furnace to the
maintenance position and tilt it out of the atomizer compartment
(procedure: page 3-6).
–or–
2. Graphite furnace spectrometer systems: Tilt the graphite furnace to the
maintenance position (procedure: page 3-8).
3. Release the pressure holding the furnace closed:
In the Furnace Control window, click on Open/Close.

3-10 0993-5259
THGA System Maintenance

4. Swing the support lever


to the side (1).

Tilt the front contact


housing downward (2).

(1) (2)

Support Front contact


lever housing

5. The graphite tube is now visible in


the rear contact.
Use the grips provided to remove the
graphite tube.
Do not touch the tube with bare
fingers.

0993-5259 3-11
THGA System Maintenance

Inserting the graphite tube and closing the furnace

Note: Do not touch the graphite tube or


contacts with your fingers. Use the grips
provided to hold the graphite tube.
Perspiration can affect the tube lifetime
and the analytical results by
contaminating and damaging the surface
of the graphite.

1. When you insert the graphite tube, Rear contact


make sure that: Sample
injection hole
 The sample injection hole is
uppermost.
 The side of the tube to which the
platform is attached faces the Radiation beam
rear of the furnace.
The platform is then higher
toward the rear.

2. Use the grips provided to insert the


graphite tube into the rear contact.

3-12 0993-5259
THGA System Maintenance

3. Carefully tilt the front contact


housing up into the closed position
(1).
4. Swing the support lever underneath
the front contact housing (2).
5. Activate the pressure that holds the
furnace closed:
In the Furnace Control window, click
on Open/Close. (2) (1)
6. Return the furnace back to the
operating position in the atomizer
Support Front contact
compartment (see page 3-7 or page lever housing
3-9).
7. If you have installed a new graphite
tube, perform the procedure outlined
in ‘To condition the graphite tube’ (procedure: page 3-17).
If you are reusing a previously conditioned graphite tube, heat manually at
2500 °C for 5 seconds to remove contamination ( procedure: page 3-18).
Note: Every time you open the furnace, subsequently always heat it out
manually at 2500 °C for approximately 5 seconds.
8. Check alignment of the furnace autosampler (procedure: page 2-17).

0993-5259 3-13
THGA System Maintenance

Graphite furnace maintenance procedures

Procedures described
 Cleaning the graphite tube and contacts.
 Conditioning ( page 3-17) and manually heating ( page 3-18) the graphite
tube.
 Changing the graphite contacts (procedure: page 3-19 ).
 Checking and cleaning the furnace windows (procedure: page 3-32).

Cleaning the graphite tube and graphite contacts


Good, reproducible analytical results depend on good electrical contact between
the graphite contacts and the graphite tube. The contact surfaces of the graphite
tube and the contacts must be smooth and clean to allow good electrical contact.
After prolonged use the contacts may become contaminated with remnants of
samples and small particles of graphite. Even quite small particles can spoil the
contact and cause poor analytical results.
Every time that you open the furnace, clean the contacts as described below.
Note: Do not touch the graphite tube or contacts with your fingers. Perspiration
can affect the tube lifetime and the analytical results by contaminating and
damaging the surface of the graphite.
If a graphite tube breaks inside the furnace you must remove all the remnants and
thoroughly clean the contacts.

3-14 0993-5259
THGA System Maintenance

Rear contact

Graphite tube

Aperture for the Front contact


radiation beam

Contact surfaces

Contact surfaces

Figure 3-1. Graphite Components

Heating the graphite tube to remove contamination

W3.5
Warning: UV Radiation – Risk of Eye Damage
When the graphite furnace is heated to incandescence, e.g. during the
atomization step, the furnace can emit UV radiation which can damage your
eyes.
 Always wear UV-absorbing safety glasses when looking at the furnace.

You can sometimes remove contamination from the graphite tube by heating the
tube. Heat the graphite tube manually at 2500 °C for approximately 5 seconds.
(procedure: page 3-18). If there are stubborn deposits in the tube that you cannot
remove, discard the tube and use a new one.

0993-5259 3-15
THGA System Maintenance

To clean the contact surfaces of the graphite tube and contacts

W4.3
Warning: High Temperatures – Risk of Burns
The graphite furnace can generate very high temperatures.
 Do not touch any parts of the furnace, especially the graphite components,
until they have cooled to room temperature.

1. Open the furnace and use the grips to remove the graphite tube (procedure:
page 3-10).
2. Use a dry, clean swab to clean the contact surfaces of the graphite tube. If the
surfaces of the graphite tube are pitted or cracked, discard the graphite tube
and use a new one.
3. Use a dry, clean swab to clean the inside of the contacts, especially around the
apertures where the radiation beam enters and exits.
Be careful not to scratch the inner surfaces of the contacts.
Remove any particles from inside the contacts using a small vacuum cleaner.
If the surfaces of the contacts are pitted or cracked, remove the contacts and
install new ones (procedure: page 3-19).
4. Use the grips to insert the graphite tube into the rear contact and close the
furnace (procedure: page 3-12).
5. Heat out the graphite tube to remove contamination (procedure: page 3-18).
6. Check alignment of the furnace autosampler (procedure: page 2-17).

3-16 0993-5259
THGA System Maintenance

To condition the graphite tube


We recommend that you run the graphite tube conditioning program every time
that you change the graphite tube. The conditioning procedure removes adsorbed
gases and surface contamination from the graphite, and ensures reproducible
performance.
After conditioning it is good practice to verify that the tube and/or platform are
sufficiently clean for the element you wish to determine.
In order to do this, run your method for this element, but do not inject a sample.
Perform a ‘dry fire’ instead. Evaluate the results obtained. If the absorbance value
is too high for this element, heat the tube manually at 2500 °C for 10 seconds
(procedure: page 3-18).

W4.3
Warning: High Temperatures – Risk of Burns
The graphite furnace can generate very high temperatures.
 Do not touch any parts of the furnace, especially the graphite components,
until they have cooled to room temperature.
W3.5
Warning: UV Radiation – Risk of Eye Damage
When the graphite furnace is heated to incandescence, e.g. during the
atomization step, the furnace can emit UV radiation which can damage your
eyes.
 Always wear UV-absorbing safety glasses when looking at the furnace.
W6.1
Warning: Toxic Gases
If you use nitrogen as the inert gas, toxic cyanogen gas (CN)2 will be produced
when the furnace temperature is above 2300 °C.
 Make sure that the main laboratory fume ventilation system removes all
gases and fumes emitted by the furnace.

1. On the Toolbar, click on Furnace.


2. In the Furnace Control window, click on Condition Tube.
The system uses a special furnace program to heat the tube to successively
higher temperatures.

0993-5259 3-17
THGA System Maintenance

To heat the graphite furnace manually


Note: Do not heat the graphite furnace for longer than about 10 s when the
temperature exceeds 2000 °C. Heating for longer periods will markedly reduce
the lifetime of the graphite tube.
To enter the temperature manually and heat the furnace:
1. On the Toolbar, click on Furnace.
2. In the Furnace Control window, click on the Cleanout Temp. entry field and
type the required temperature (e.g. 2500 °C).
3. Click on Start to heat the furnace.
The furnace is heated to the selected temperature and continues to heat until
you stop it.
4. After about 10 s, click on Start again to stop furnace heating.

3-18 0993-5259
THGA System Maintenance

Changing the graphite contacts


Change the graphite contacts when one or both contacts are badly contaminated
or show visible pits and small cracks. Always change both contacts at the same
time.

W4.3
Warning: High Temperatures – Risk of Burns
The graphite furnace can generate very high temperatures.
 Do not touch any parts of the furnace, especially the graphite components,
until they have cooled to room temperature.

Summary of the procedure


Always change the graphite contacts in the following sequence:
1. Tilt the furnace to the maintenance position (procedure: page 3-6).
2. Open the furnace and remove the graphite tube (procedure: page 3-20).
3. Exit AA WinLab and switch off the spectrometer.
4. If the furnace has a fume extraction unit attached to the rear contact housing,
remove the fume extraction unit; the procedure is described in the
spectrometer guide.
5. Remove the front contact (procedure: page 3-21).
6. Remove the rear contact ( procedure: page 3-23).
7. Insert a new front contact (procedure: page 3-26).
8. Insert a new rear contact (procedure: page 3-28 ).
9. Where applicable, attach the fume extraction unit to the rear contact housing.
10. Switch on the spectrometer and then start AA WinLab.
11. Insert the graphite tube and close the furnace (procedure: page 3-31 ).
12. Return the furnace to the operating position (procedure: page 3-6).
13. Condition the graphite tube (procedure: page 3-17).
14. Align the furnace autosampler (procedure: page 2-17).
Special tools to change the contacts are provided with the furnace.

0993-5259 3-19
THGA System Maintenance

To open the furnace for contact change:


1. If the Automated Analysis Control window is open, select the Setup page and
then close the window.
2. Make sure that the furnace is cool.
3. Tilt the furnace out of the atomizer compartment, open the furnace and
remove the graphite tube (procedure: page 3-10).
4. Display the Automated Analysis Control window:
On the Toolbar, click on Auto.
5. Click on the Analyze tab on the bottom of the window.
Click on Reset and then on OK.
6. In the File menu, click on Exit to exit AA WinLab.
7. Switch off the spectrometer at the operational on/off switch on the front panel.

3-20 0993-5259
THGA System Maintenance

To remove the front contact:


1. If the furnace has a fume extraction unit attached to the rear contact housing,
remove the fume extraction unit; the procedure is described in the
spectrometer guide.
2. From the tools provided, you Contact removal tool
require the contact removal
tool, the hex-driver, and the
Torx driver (star-shaped
cross-section).

3. Loosen the two socket-head


screws that secure the pressure
cylinder to the front contact
housing.
Carefully pull the pressure
cylinder out of the front
contact housing. Make sure
that you do not damage the
O-ring.
Put the pressure cylinder and
screws in a safe place.

Pressure cylinder

0993-5259 3-21
THGA System Maintenance

4. Attach the removal tool to the


front contact housing with the
two captive screws on the tool.

Removal tool

5. Use the hex-driver to screw


the bolt on the removal tool
into the tool to push out the
contact.

6. Unscrew the two screws that secure the tool to the contact housing and
remove the tool.

3-22 0993-5259
THGA System Maintenance

To remove the rear contact:


1. From the tools provided, you Contact removal tool
require the contact removal
tool, the short hex-driver, and
the Torx driver (star-shaped
cross-section).

2. Inspect the temperature sensor


attached to the rear contact
housing. It should be rotated
to the side as far as possible. If
it is not:
– Carefully slacken the
socket-head screw that
secures the temperature
sensor to the rear contact
housing. Temperature
– Carefully rotate the sensor sensor
to the side, then retighten
the screw.
Note: Make sure that you do
not bend or twist the
temperature sensor
connector. Also, do not
damage the insulating
washers.

0993-5259 3-23
THGA System Maintenance

3. Unscrew the two captive, Optical sensor


socket-head screws that secure
the optical sensor to the rear
contact housing.

Carefully pull the optical


sensor out of the rear contact
housing. Make sure that you
do not damage the O-ring.
Move the optical sensor to the
side.

4. Attach the removal tool to the


rear contact housing with the
two captive screws on the tool.

3-24 0993-5259
THGA System Maintenance

5. Use the hex-driver to screw


the bolt on the removal tool
into the tool to push out the
contact.

6. Unscrew the two screws that


secure the tool to the contact
housing and remove the tool.

0993-5259 3-25
THGA System Maintenance

To insert the front contact:


Note: Do not scratch the new contact and do not touch it directly. Perspiration
can contaminate the contact and cause poor analytical results.
1. Make sure that the contact housing is completely clean and free from
particles. If necessary, blow out any graphite particles from the contact
housing with clean, dry compressed air.
Wear safety glasses when doing this.
2. From the tools provided, you require:
 the hex-driver and the Torx driver (star-shaped cross-section).
 the long bolt, front contact guide, and threaded cylinder as shown below.
3. Slide the guide and the
front contact onto the long
bolt as shown.
Threaded cylinder
Bolt
Guide
Front contact

4. Put the bolt into the front


contact housing such that
the new contact sits in the
opening of the housing.
5. Put the threaded cylinder
into the opposite end of the
contact housing and screw
the bolt into the cylinder
until the contact is pressed
up against the housing.

3-26 0993-5259
THGA System Maintenance

6. Use the hex-driver to screw the


Hex-driver
bolt into the threaded cylinder
and push the contact into the
contact housing.
Screw in the bolt until the rim of
the contact is flush with the
contact housing.
Note: There must be no gap
between the rim of the contact
and the housing.
Do not use excessive force to
push the contact into the
housing, otherwise the contact
may shatter.
If there is substantial resistance,
check that the parts are aligned
correctly.
7. Screw the bolt out of the
threaded cylinder and carefully remove the tools.
Note: Do not scratch the contact when you remove the tools.
8. Blow out any graphite particles from the contact housing with clean, dry
compressed air. Wear safety glasses when doing this.

9. Check the O-ring on the


pressure cylinder; if it is
damaged, fit a new one. See the
chapter Parts and Supplies for
the part number.
10. Push the pressure cylinder
carefully into the front contact
housing. Make sure that you do
not damage the O-ring.
11. Tighten the two screws to secure
the pressure cylinder to the front
contact housing.

Pressure cylinder

0993-5259 3-27
THGA System Maintenance

To insert the rear contact:


Note: Do not scratch the new contact and do not touch it directly. Perspiration
can contaminate the contact and cause poor analytical results.
1. Make sure that the contact housing is completely clean and free from
particles. If necessary, blow out any graphite particles from the contact
housing with clean, dry compressed air.
Wear safety glasses when doing this.
2. From the tools provided, you require:
 the hex-driver and the Torx driver (star-shaped cross-section).
 the long bolt, rear contact guide, and threaded cylinder as shown below.

3. Slide the rear contact into


the guide and slide these
two parts onto the long
bolt as shown.
Threaded
cylinder
Bolt
Contact
Guide

4. Put the bolt into the rear


contact housing such that the
new contact sits in the opening
of the housing.
Make sure that the graphite
contact is correctly orientated,
with the sample injection hole
at the top.
5. Put the threaded cylinder into
the opposite end of the contact
housing and screw the bolt
into the cylinder until the
contact is pressed up against
the housing.

3-28 0993-5259
THGA System Maintenance

6. Use the hex-driver to screw


the bolt into the threaded
cylinder and push the contact
into the contact housing.
Screw in the bolt until the
contact is flush with the
contact housing.
Note: There must be no gap
between the contact and the
housing.
Do not use excessive force to
push the contact into the
housing, otherwise the
contact may shatter.
If there is substantial Hex-driver
resistance, check that the
parts are aligned correctly.
7. Screw the long bolt out of the threaded cylinder and carefully remove the
tools.
Note: Do not scratch the contact when you remove the tools.
8. Blow out any graphite particles from the contact housing with clean, dry
compressed air. Wear safety glasses when doing this.

0993-5259 3-29
THGA System Maintenance

Optical sensor
9. Check the O-ring on the
optical sensor; if it is
damaged, fit a new one. See
the Chapter Parts and
Supplies for the part number.
10. Push the optical sensor into the
rear contact housing. Make
sure that you do not damage
the O-ring.
11. Tighten the two screws to
secure the optical sensor to the
rear contact housing.
12. Where applicable, attach the
fume extraction unit to the rear
contact housing; the procedure
is described in the
spectrometer guide.

3-30 0993-5259
THGA System Maintenance

To close the furnace after contact change:


1. Insert a graphite tube into the furnace, close the front contact housing, and
swing the support lever under the contact housing (see step 1 through step 4
on page 3-12).
2. Switch on the spectrometer at the operational on/off switch on the front panel.
3. Start AA WinLab.
4. Activate the pressure that holds the furnace closed:
In the Furnace Control window, click on Open/Close.
5. Return the furnace back to the operating position in the atomizer compartment
(see page 3-7 or page 3-9).
6. If you have installed a new graphite tube, perform the procedure outlined in
‘To condition the graphite tube’ (procedure: page 3-17).
If you are reusing a previously conditioned graphite tube, heat manually at
2500 °C for 5 seconds to remove contamination ( procedure: page 3-18).
Note: Every time you open the furnace, subsequently always heat it out
manually at 2500 °C for approximately 5 seconds.
7. Check alignment of the furnace autosampler (procedure: page 2-17).

0993-5259 3-31
THGA System Maintenance

Checking and cleaning the furnace windows


The quartz furnace windows seal the ends of the furnace where the radiation beam
enters and exits.
Over a period of time sample constituents can accumulate on the windows. This
reduces the intensity of the radiation and the sensitivity and precision of the
analytical results.
Remove the windows and clean them regularly. How frequently depends on the
type of samples that are being analyzed.
If you analyze samples that have ‘dirty’ matrices, such as blood, sugar or oil, you
will probably have to clean the furnace windows more often than if you were
analyzing ‘clean’ samples, such as drinking water.

Window key

Caution Risk of damage to the furnace windows


 The quartz windows are precision optical components; handle them carefully
to prevent scratches, fingerprints or other contamination.

To remove the windows:


1. Make sure that the furnace is cool.
2. Drive the furnace to the maintenance position and tilt it out of the atomizer
compartment (see page 3-6 or page 3-8).
3. Use the key provided to unscrew the left-hand and the right-hand windows
from the furnace.

3-32 0993-5259
THGA System Maintenance

To clean the windows:


1. Remove the windows from the furnace.
2. Dismantle the window assemblies and carefully remove the quartz windows
from the mounts.

Seal Window Mount

3. Blow any dust or particles off the window surface with clean dry air before
you start.
4. Clean the windows carefully with a tuft of cotton moistened with a dilute
solution of mild laboratory detergent.
Rinse the windows several times with deionized water.
If the windows are not clean after this procedure, clean them with a soft lint
free cloth moistened with spectroscopic grade alcohol.
Note: To avoid scratching the windows, rub the surfaces of the windows as
little as possible. Discard scratched windows.
5. Reassemble the windows.
New seals and windows are available.
6. Screw the windows in the furnace.

To refit the windows:


1. Screw each window carefully into the ends of the furnace; make sure that the
threads are properly engaged.
The windows are designed to be slightly offset from the vertical.
2. Return the furnace back to the operating position in the atomizer compartment
(see page 3-7 or page 3-9).

0993-5259 3-33
THGA System Maintenance

Cooling system maintenance procedures

Note: The following directions are only relevant if you have installed the
(optional) cooling system.

Procedures described
 Emptying the cooling system.
 Refilling the cooling system.
 Changing the cooling system fuse.

Emptying the cooling system


Usually there is no need to empty the cooling system. This may only be necessary
when you want to move the complete analysis system to a new location.
The hoses attached to the cooling system have automatic valves that shut when
you disconnect them from the inlet manifold of the spectrometer.
To empty the cooling system you require two drain fittings (P/N B019-3243) to
open the valves.

3-34 0993-5259
THGA System Maintenance

1. For each hose, carefully pull on the


knurled locking ring slightly to
release the lock on the connector,
then pull the connector off the fitting
on the inlet manifold of the Inlet manifold on
spectrometer. the spectrometer
2. Remove the stopper from the top of
the cooling system – twist and pull. Locking ring

3. Hold the hoses over a waste water


Cooling system

WATER IN

WATER OUT
container or drain, and insert drain
hoses
fittings into the automatic
connectors.
Allow the water to drain out of the
hoses.
Drain fittings
4. Temporarily disconnect the cooling
system line cord from the special
outlet at the rear of the spectrometer Locking ring
and connect it to one of the other
outlets.
WATER IN

WATER OUT

5. Switch on the cooling system and


pump out the remaining liquid in the
system.
6. If there is sediment in the water when
you empty the cooling system, fill
the system with water and pump it
out again several times to completely
flush the system.
7. For each hose, carefully pull the locking ring on the drain fitting down slightly
to release the lock, then pull the drain fitting out of the connector.
8. Reconnect the cooling system hoses to the spectrometer.
9. Reconnect the line cord to the special outlet at the rear of the spectrometer.

0993-5259 3-35
THGA System Maintenance

Refilling the cooling system


The cooling system is self-priming; air in the system is removed automatically as
the cooling system operates. The coolant is a 1:10 solution of glycerol in water
(1 part glycerol plus 9 parts water). Do not use antifreeze.

1. Reconnect the cooling system hoses to


the spectrometer.
Make sure that you remove the drain
fittings from the cooling system hoses as
described above.
2. Remove the stopper from the top of the
cooling system – twist and pull.
3. Pour 0.5 L of glycerol into the cooling
system. Max

Do not use antifreeze.


4. Fill the cooling system up to the MAX Min

mark with sediment-free drinking water


– about 4.5 L.
Do not use deionized water since this can
cause corrosion.
5. Replace the stopper securely.
Water level indicator

3-36 0993-5259
THGA System Maintenance

Changing the cooling system fuse


In addition to the fuse in the cooling system, shown here, there is a fuse in the
power outlet on the spectrometer.
1. Switch off the cooling system with On/off switch
the switch on the rear panel. Lift fuse cover here
2. Disconnect the line power cord
from the socket.
3. Behind this socket is the cover of
the fuse holder.
Use the tip of a small screwdriver
to carefully lever open the fuse
holder. Power cord
socket
4. Remove the blown fuse.
5. Insert a new fuse of the correct type
and rating.
Correct fuse: 230 V, 1.6 A, slow-
blow.
6. Close the fuse holder and reconnect
the line power cord.
7. Switch on the cooling system with
the switch on the rear panel.

0993-5259 3-37
THGA System Maintenance

Autosampler maintenance procedures

Routine maintenance
The autosampler is a precision instrument constructed from high quality
components. It is capable of dispensing volumes of liquid in the microliter range.
To maintain this high level of performance, you must treat the autosampler with
due care.

Procedures described
 Valve maintenance (procedure: page 3-39).
 Repairing the pipet tip (procedure: page 3-47).
 Installing a new pipet assembly (procedure: page 3-49).
 Aligning the pump heads (procedure: page 3-52).

Caution Risk of damage to the autosampler


You can cause irreparable damage to the gears if you attempt to move the
autosampler arm by hand.
 Never attempt to move the autosampler arm by hand.

3-38 0993-5259
THGA System Maintenance

Valve maintenance
The autosampler pumps dispense microliter volumes of liquid with high
precision. To maintain this high precision it is essential that the valves function
correctly. If there is a deterioration in the precision of the analytical results, and
other sources of error can be excluded, this is an indication that a valve may not
be functioning correctly.
Only the rinse pump contains valves. The sample pump contains inserts that are
a similar shape to the rinse pump outlet valve.

Routine maintenance
The only routine maintenance that the valves require is to flush them thoroughly
before and after every analysis.

Flushing the valves and rinsing system


1. Make sure that the rinsing system components are correctly installed, in good
condition, and suitable for the rinsing liquid you will use.
2. Prepare the rinsing solutions that you require, see following page.
3. Fill the rinse bottle with the first, clean, particle-free, rinsing liquid.
If there are particles in the rinsing liquid they can lodge in the valves, causing
leaks and non-reproducible results.
4. Flush the system:
1. In the Furnace Control window, click on Flush Sampler.
This activates a rinse cycle.
2. Repeat substep 1 as often as required to completely flush the rinsing
system with rinsing liquid and flush all the air out.
5. Empty the waste bottle. Dispose of any hazardous waste correctly.
6. Repeat steps 2 through 4 for each rinsing solution.
Note: Make certain there are no air bubbles in the rinsing system. Air
bubbles can lead to non-reproducible results.

0993-5259 3-39
THGA System Maintenance

Rinsing solutions
Use the following rinsing solutions in the given sequence:

Before the start of every analysis series:


If the rinsing solution you intend to use is miscible with the solution in the system,
use your intended rinsing solution. If the rinsing solution you intend to use is not
miscible with the solution in the system, you must use intermediate rinsing
liquids.
For example, to change from an acidic liquid to an organic solvent, you could use:
1. Deionized water.
2. Isopropanol or other water-miscible solvent.
3. Final organic solvent.

After an analysis series:


1. If you have been using an organic rinsing liquid, use isopropanol or other
water-miscible solvent.
2. Dilute nitric acid. This is especially important for elements with a tendency to
carryover.
3. Isopropanol.
4. Deionized water.

Before performing maintenance on the system:


1. Isopropanol.
2. Deionized water.

After performing maintenance on the system:


1. Isopropanol.
2. The rinsing solution you intend to use next, or deionized water.

3-40 0993-5259
THGA System Maintenance

Checking the valves


If you experience problems such as poor precision or recovery, check to see if the
rinse pump valves are leaking.

Caution Risk of damage to the autosampler


You can cause irreparable damage to the gears if you attempt to move the
autosampler arm by hand.
 Never attempt to move the autosampler arm by hand.

To check the outlet valve


1. Raise the pipet tip out of the rinsing port:
1. In the Furnace Control window, click on Align Tip.
The Align Autosampler dialog appears.
2. In this dialog, click on Unlocked Above Rinse. The pipet tip rises to a
position directly above the rinsing port.
3. Click on Unlocked Above Rinse again. In the dialog that appears, click on
Yes to save this position.
4. Click on Exit to clear the Align Autosampler dialog.
2. Start a rinse cycle (procedure: page 3-39).
The rinsing pump performs three cycles. During the suction phase of each
cycle (pump plunger moves backward) a droplet of rinsing liquid hangs on the
end of the pipet tip; this droplet must remain stationary.
At the end of a rinse cycle the sample pump draws the rinsing liquid droplet
back into the pipet tip.

To check the inlet valve


1. Start a rinse cycle (procedure: page 3-39).
2. Remove the rinse feed tube briefly from the rinsing liquid so that an air bubble
is drawn in and then replace the tube in the rinsing liquid.
3. Watch the meniscus of the air bubble: It must remain stationary during the
expulsion phase of each cycle (pump plunger moves forward).
4. When you have finished checking the valves, in the Align Autosampler dialog,
click on Unlocked Above Rinse.
5. Adjust the depth control wheel so that the pipet tip is at the correct depth
inside the rinsing port.

0993-5259 3-41
THGA System Maintenance

6. Click on Unlocked Above Rinse again. In the dialog that appears, click on Yes
to save this position.
7. In the Align Autosampler dialog, click on Exit.
8. Thereafter repeat the rinse cycle as often as required to remove air bubbles.
Remove persistent bubbles by flushing the system first with isopropanol and
then with aqueous rinsing liquid.
If a valve is leaking, clean it as described on the following pages. If cleaning does
not remedy the problem, replace the complete valve.
Note: Do not attempt to repair the valves or change individual components
inside the valve. If any components are damaged or worn, discard the valve and
install a complete, new valve.

Removing the rinse pump valves and sample pump


tube connectors
Note: Avoid handling the internal valve components with bare fingers as much
as possible—grease from your fingers can interfere with the correct functioning
of the valves. Wear suitable gloves.

Caution Risk of damage to the autosampler


You can cause irreparable damage to the gears if you attempt to move the
autosampler arm by hand.
 Never attempt to move the autosampler arm by hand.

1. Disconnect the tubes from the pumps.


When you unscrew the nuts (A), make sure A A
that you do not lose any of the ferrules from
the ends of the tubes.

A A

Sample Pump Rinse Pump

3-42 0993-5259
THGA System Maintenance

2. Unscrew the valve retaining rings.


Carefully withdraw the valves from the rinse pump or the tube connectors
from the sample pump. Be very careful not to lose any of the parts from inside
the valves.

Sample Pump Components Rinse Pump Components

Retaining ring Retaining ring

Tube connector Outlet valve

Inlet valve
Tube connector
Tube connector

Retaining ring Retaining ring

3. Remove the components from inside the rinse pump valves.


Do not use sharp or pointed tools to remove them.
Handle the seals with especial care; they are very delicate and easily
damaged.
Keep the components from the different valves separate.

Outlet Valve Inlet Valve

1 2
1 Outlet valve body
2 Inlet valve body
3 Gasket 3
4 Ruby ball 4
5 Seal
5

0993-5259 3-43
THGA System Maintenance

Cleaning the valves, tube connectors and pump heads


Note: Never use any sharp tools to clean the pump components.
Avoid handling the internal valve components with bare fingers as much as
possible—grease from your fingers can interfere with the correct functioning of
the valves. Wear suitable gloves.
1. Clean the valve components in an ultrasonic bath.
Use a dilute solution of laboratory detergent.
Rinse them thoroughly with deionized water.
2. Rinse the sample pump tube connectors thoroughly C
with deionized water.
3. Rinse the inlet and outlet chambers (C) of the pump
heads thoroughly with deionized water.
Note: Do not remove the pump heads from the pumps.
This operation should only be performed by a PerkinElmer
service engineer or similarly trained person.
C
Assembling and installing the valves
1. If any of the valve components are damaged or worn, discard the valve and
install a complete, new valve.
2. Reassemble the valves.
Do not mix components from different valves. Make sure that the shiny side
of the seal is directed toward the ruby ball.

Outlet Valve Inlet Valve

1 2
1 Outlet valve body
2 Inlet valve body
3 Gasket 3
4 Ruby ball 4
5 Seal
5

3-44 0993-5259
THGA System Maintenance

3. Place the valves and tube connector in the Rinse Pump Components
rinse pump head. Screw on the retaining
rings finger-tight. Do not use tools or Retaining ring
overtighten the retaining rings; this may
deform the seals and cause leaks. Outlet valve
Make sure that you use the outlet valve,
which has a black seal, and not one of the
sample pump tube connectors.
Make sure that the black seal of the inlet Inlet valve
valve faces the tube connector. Tube connector

Retaining ring

4. Place the tube connectors in the sample Sample Pump Components


pump head.
Make sure that you do not use the rinse Retaining ring
pump outlet valve which has a black seal.
Tube connector
5. Screw on the retaining rings finger-tight.
Do not use tools or overtighten the retaining
rings; this may deform the connections and
cause leaks.
6. Make sure that all the tubes in the rinsing Tube connector
system are clean before you reconnect the
tubes to the pumps.
Retaining ring

0993-5259 3-45
THGA System Maintenance

7. Reconnect the tubes to the correct sides of the pumps.


Make sure that the ferrules are positioned correctly.
Screw on the nuts firmly by hand; do not use any tools.
The rinse feed tube has a larger diameter than the other tubes and uses larger
ferrules and a larger nut.
Sample Pump Rinse Pump

Tube Sample
tube
Nut

Back ferrule

Front ferrule

Tube fitting
on the pump Connecting
tube Rinse feed
tube

8. Make sure that the pump heads are correctly aligned (procedure: page 3-52).
9. Fill and flush the rinsing system (procedure: page 3-39 ):
1. Flush the rinsing system with isopropanol.
2. Flush the rinsing system well with the usual rinsing liquid.
Note: Always flush the rinsing system after you have performed any work on the
components.

3-46 0993-5259
THGA System Maintenance

Repairing a pipet
The complete pipet is an assembly that consists of the sample tube fitted through
a mount and a flexible sleeve. The mount is provided with a groove that locates
the mount in the correct position in the clip at the end of the autosampler arm. The
pipet tip is that portion of the sample tube protruding from the mount.
If the pipet tip becomes damaged you can repair it as given below:

Caution Risk of damage to the autosampler


You can cause irreparable damage to the gears if you attempt to move the
autosampler arm by hand.
 Never attempt to move the autosampler arm by hand.

1. Raise the pipet tip out of the rinsing port:


1. In the Furnace Control window, click on Align Tip.
The Align Autosampler dialog appears.
2. In this dialog, click on Unlocked Above Rinse. The pipet tip rises to a
position directly above the rinsing port.

2. Unthread the tube from the hooks on the


autosampler arm.
Hooks on
3. Pull the mount out of the clip at the end autosampler
of the autosampler arm. arm

Mount

4. Hold the plastic mount in one hand


and the end of the damaged pipet tip,
with grips, in the other hand. Pull the
tube through the mount until
approximately 10 mm of undamaged
PTFE tube are outside the flexible
sleeve.

0993-5259 3-47
THGA System Maintenance

5. Using a sharp blade, cut off the PTFE Flexible sleeve


tube at a slight angle to leave
approximately 7 mm of tube
extending out of the sleeve.

7 mm

6. Push the mount into the clip at the end of the autosampler arm.
Make sure that the groove in the mount fits correctly in the clip.
7. Rethread the sample tube through the hooks on the autosampler arm such that
it forms a smooth loop from the mount (see ‘To install the new pipet
assembly’, page 3-50).
8. When you have finished, in the Align Autosampler dialog, click on Unlocked
Above Rinse.
9. Adjust the depth control wheel so that the pipet tip is at the correct depth
inside the rinsing port (more information: page 2-21).
10. Click on Unlocked Above Rinse again. In the dialog that appears, click on Yes
to save this position.
11. In the Align Autosampler dialog, click on Exit.
12. Fill and flush the rinsing system (procedure: page 3-39 ):
1. Flush the rinsing system with isopropanol.
2. Flush the rinsing system well with the usual rinsing liquid.
Note: Always fill and flush the rinsing system after you have performed any
work on the components.

3-48 0993-5259
THGA System Maintenance

Installing a new pipet assembly


The complete pipet is an assembly that consists of the sample tube fitted through
a plastic mount. The mount is provided with a groove that locates the mount in
the correct position in the clip at the end of the autosampler arm. The pipet tip is
that portion of the sample tube protruding from the mount.
If the pipet tip becomes damaged and cannot be further repaired or if the sample
tube is kinked or contaminated, you should replace the complete assembly.

Caution Risk of damage to the autosampler


You can cause irreparable damage to the gears if you attempt to move the
autosampler arm by hand.
 Never attempt to move the autosampler arm by hand.

To remove the old pipet assembly


1. Raise the pipet tip out of the rinsing port:
1. In the Furnace Control window, click on Align Tip.
The Align Autosampler dialog appears.
2. In this dialog, click on Unlocked Above Rinse. The pipet tip rises to a
position directly above the rinsing port.
2. Remove the pipet assembly:
1. Unscrew the knurled nut that connects the sample tube to the sample
pump. Remove the nut and ferrules from the tube and save the nut.
2. Unthread the tube from the hooks on the arm.
3. Pull the mount out of the clip at the end of the autosampler arm.
4. Remove the entire sample tube from the sample table.

0993-5259 3-49
THGA System Maintenance

H1

Hooks on H2 H3
autosampler
arm Knurled nut
on sample pump

To install the new pipet assembly


Note: Handle the sample tube with care. Do not damage the delicate pipet tip
and do not kink the tube.
1. Push the mount into the clip at the end of the autosampler arm.
Make sure that the groove in the mount fits correctly in the clip.
2. Take the sample tube in a smooth loop from the mount to the hooks on the
autosampler arm and then thread it through the hooks on the autosampler arm.
3. Pass the sample tube around the back of the motor assembly and thread it
through hook H1 on the sample table. Leave a sufficiently large loop so that
the autosampler arm can move freely.
4. Thread the sample tube through hooks H2 and H3 on the sample table and
pass it to the top of the sample pump.

3-50 0993-5259
THGA System Maintenance

5. Take two new ferrules from the ferrule kit provided with the autosampler.
Slide the knurled nut, the back ferrule, and then the front ferrule onto the tube.
Note: Make sure the ferrules are the correct way round.
6. Screw the knurled nut finger-tight onto the sample pump.
Do not use force.
7. When you have finished, in the Align Autosampler dialog, click on Unlocked
Above Rinse.
8. Adjust the depth control wheel so that the pipet tip is at the correct depth
inside the rinsing port (more information: page 2-21).
9. Click on Unlocked Above Rinse again. In the dialog that appears, click on Yes
to save this position.
10. In the Align Autosampler dialog, click on Exit.
11. Fill and flush the rinsing system (procedure: page 3-39):
1. Flush the rinsing system with isopropanol.
2. Flush the rinsing system well with the usual rinsing liquid.
Note: Always fill and flush the rinsing system after you have performed any
work on the components.

Sample
tube
Tube

Nut

Back ferrule

Front ferrule

Tube fitting Connecting Rinse feed


on the pump tube tube

0993-5259 3-51
THGA System Maintenance

Aligning the pump heads


To align the pump heads
1. Use the special wrench provided to loosen Arrows on the pump heads
the retaining ring that secures the pump
head.
2. Set the pump head so that the molded arrow
is pointing upward. The pump head has a
lug that engages in a notch on the pump
mount when the pump head is set correctly.
3. Use the special wrench provided to tighten
the retaining ring. Do not use excessive
force.
Note: Do not remove the pump heads from the
pumps. This operation should only be
performed by a PerkinElmer service engineer
or similarly trained person. Side view of pump head

Retaining ring

Pump head

3-52 0993-5259
THGA Graphite Furnace:
Parts and Supplies 4
4THGA Graphite Furnace: Parts and Supplies
Marker for header

Contents page

Obtaining supplies, replacement parts, and accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-3


Furnace system supplies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-4
Furnace . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-4
Furnace gas and cooling systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-5
Matrix modifiers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-5
AS-800 furnace autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
Parts provided with the furnace autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
Supplies and replacement parts for the furnace autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-7
Pump parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8

0993-5259 4-1
THGA Parts and Supplies

4-2 0993-5259
THGA Parts and Supplies

Obtaining supplies, replacement parts, and accessories

Supplies, replacement parts, and accessories can be ordered directly from


PerkinElmer, using the part numbers quoted in the guides provided with the
instrument.
e-ssentials
PerkinElmer Instruments on-line catalog, your single source for quality supplies
and accessories.
http://essentials.perkinelmer.com/

PerkinElmer’s catalog service offers a full selection of high-quality supplies.


To place an order for supplies and many replacement parts, request a free catalog,
or ask for information:
– If you are located within the U.S., call toll free 1-800-762-4002, 8 a.m. to
8 p.m. EST. Your order will be shipped promptly, usually within 24 hours.
– If you are located outside of the U.S., call your local PerkinElmer sales or
service office.

What is listed in this chapter


This chapter lists the most important replacement parts for your graphite furnace
system. Information about other parts and accessories is given in the current
PerkinElmer brochures and price lists.

0993-5259 4-3
THGA Parts and Supplies

Furnace system supplies

Furnace

Description Part No.

Graphite tubes, pack of 20 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B050-4033


pack of 5 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B300-0641
Graphite tubes, with end caps, pack of 20 . . . . . . . . . . . . . . . . . . B300-0655
pack of 5 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B300-0653
Graphite contacts, 5 sets . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B050-4036
O-ring, for the pressure cylinder in the front contact housing
and the optical sensor in the rear contact housing . . . . . . . . . . . . B013-2870
Insulating sleeve for temperature sensor on rear contact housing B019-9476
Insulating washer for temperature sensor on rear contact housing B008-3633
Set of tools,
for changing the contacts and the furnace windows . . . . . . . . . . . B019-3347
Key for furnace windows, separate . . . . . . . . . . . . . . . . . . . . . . . B050-5339
Grips for graphite tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0990-7925
Furnace window, quartz . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B019-8005
Furnace window seal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B050-1236

Graphite contacts Graphite tube

Front

Rear

Temperature sensor
Screw
Furnace window parts Insulating sleeve

Cable shoe

Insulating washer
Seal Window

4-4 0993-5259
THGA Parts and Supplies

Furnace gas and cooling systems

Description Part No.

Drain fitting for the automatic connectors, . . . . . . . . . . . . . . . . . B019-3243


to empty the cooling system hoses (2 required)
Gas tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B050-8264
Tube cutter for the gas tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0992-3183
Y-connector for the gas tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0992-0179
Recirculating cooling system, 230 V, 50/60 Hz . . . . . . . . . . . . . B019-8072
Water hose kit with pressure relief valve . . . . . . . . . . . . . . . . . . B313-0124
Glycerol (85%) for cooling systems . . . . . . . . . . . . . . . . . . . . . . B050-5133

Drain fitting

Y-connector

Matrix modifiers

Description Part No.

Magnesium nitrate modifier (10 g/L Mg, 100 mL) . . . . . . . . . . . B019-0634


Palladium nitrate modifier (10 g/L Pd, 50 mL) . . . . . . . . . . . . . . B019-0635

0993-5259 4-5
THGA Parts and Supplies

AS-800 furnace autosampler

Parts provided with the furnace autosampler


PerkinElmer reserves the right to alter the schedule of parts provided without prior notice.

Qty. Item Part No.

1 Furnace autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . B300-1500


together with the following components:
1 Sample tray, 148 locations . . . . . . . . . . . . . . . . . . . . . . . . B300-1506
1 Sample tray, 88 locations . . . . . . . . . . . . . . . . . . . . . . . . . B300-1507
1 Sample tray cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B300-1505
1 Sample cups, polypropylene, 1.2 mL, . . . . . . . . . . . . . . . B051-0397
pack of 2000
1 Sample cups, polypropylene, 2.5 mL, . . . . . . . . . . . . . . . B300-1566
pack of 1000
1 Sample cups, polypropylene, 7 mL, . . . . . . . . . . . . . . . . B300-1567
pack of 100
1 Rinsing port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B300-1512
1 Pipet assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B012-9258
2 Rinse and waste bottles, polyethylene, 2 L . . . . . . . . . . . B010-4344
1 Drain tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B300-2141
1 Rinse feed assembly:
Rigid tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B300-1363
Flexible tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B001-7998
Front ferrule, 2.45 mm . . . . . . . . . . . . . . . . . . . . . . . . B300-1333
Back ferrule, 2.45 mm . . . . . . . . . . . . . . . . . . . . . . . . . B300-1334
Nut . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B300-1335
1 Grips for 1.2 mL sample cups . . . . . . . . . . . . . . . . . . . . . B051-0398
1 Wrench for the pump head retaining ring . . . . . . . . . . . . B300-1365
1 Quick Reference . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0993-5260

4-6 0993-5259
THGA Parts and Supplies

Supplies and replacement parts for the furnace autosampler

Description Part No.

Sample cups, polypropylene, 1.2 mL,


pack of 2000 for the 148-location tray . . . . . . . . . . . . . . . . . . . . B051-0397
Sample cups, polypropylene, 2.5 mL,
pack of 1000 for the 88- or 148-location tray . . . . . . . . . . . . . . . B300-1566
Sample cups, polypropylene, 7 mL,
pack of 100 for the 88- or 148-location tray . . . . . . . . . . . . . . . . B300-1567
88-location sample tray . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B300-1507
148-location sample tray . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B300-1506
Rinse pump valve kit (contains both valves) . . . . . . . . . . . . . . . B300-1485
Inlet valve assembly (complete) . . . . . . . . . . . . . . . . . . . . . . . . . B300-2007
Outlet valve assembly (complete) . . . . . . . . . . . . . . . . . . . . . . . . B300-2006
Tube cutter, for PTFE tubing . . . . . . . . . . . . . . . . . . . . . . . . . . . . B051-0268
Solvent resistant rinse and waste bottle, 1 L, PTFE . . . . . . . . . . B300-1460
Pipet assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B012-9258
Connecting tube, PTFE, . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B002-9792
to connect the rinse and sample pumps

0993-5259 4-7
THGA Parts and Supplies

Pump parts

1 Nut, for 1/16'' tube B300-2089 1


2a
2 Ferrule kit, 1/16'' B008-6142 2b
contains 5 back ferrules (2a)
and 5 front ferrules (2b)
3
3 Valve and connector retaining ring B009-2450
for rinse pump and sample pump
inlets and outlets

4 Outlet valve (rinse pump) B300-2006


4 9
complete with ferrules (2a, 2b)
and nut (1)

5 Inlet valve (rinse pump) B300-2007


complete with valve (5a),
tube connector (5b),
ferrules (7, 8) and nut (9) Pump head

6 Front ferrule, 2.45 mm B300-1333

7 Back ferrule, 2.45 mm B300-1334

8 Nut, for 2.45 mm tube B314-0226


5a
9
9 Tube connector B300-2010
for the sample pump 5b

6 2b
7 2a
8 1

4-8 0993-5259
THGA Graphite Furnace:
System Description 5
5THGA Graphite Furnace: System Description
Marker for header

Contents page

THGA Graphite Furnace . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3


Furnace design . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
The graphite tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
The graphite contacts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5
Furnace heating and temperature profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Maximum power heating . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7
Time-controlled heating . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7
Temperature control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7
The furnace gas system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
Principle of the gas purging system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
Inert gas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
The external protective gas flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-10
The internal purge gas flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-10
Cooling the furnace system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11
Cooling system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11
Zeeman-effect background correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-12
The Zeeman effect . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-12
Applying Zeeman-effect background correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-14
Longitudinal configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-15
Transverse configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-16
Analyte signals and background correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-17
Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-18
Graphite furnace . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-18
Cooling system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-20

0993-5259 5-1
THGA System Description

page

AS-800 Furnace Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-21


Autosampler design . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-21
Sample and rinse pumps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-21
The sample table . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-21
Sample and reagent containers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-23
Controlling the autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-23
The autosampler operating cycle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-24
Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-25
AS-800 Furnace Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-25
Literature on electrothermal atomization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-26

5-2 0993-5259
THGA System Description

THGA Graphite Furnace

Furnace design
The THGA is a transversely-heated graphite furnace for electrothermal
atomization in atomic absorption spectrometry. The furnace incorporates the
electromagnet required for the application of the Zeeman effect for background
correction.
The furnace is electrically heated. The voltage is applied across the graphite tube,
perpendicular to the radiation beam. The electromagnet is orientated so that the
magnetic field is parallel to the radiation beam (more information: page 5-12).

Heating current

Radiation beam

Figure 5-1. Graphite Furnace Showing the Relationship between the Radiation
Beam, Furnace Heating, and Magnetic Field
In spectrometer systems with dual atomizers, the graphite furnace is mounted on
a carriage that can be driven into and out of the atomizer compartment by software
command. In this way you can change between electrothermal atomization and
flame atomization easily within a few seconds.
The power supply, system electronics, and the inert gas control pneumatics for the
furnace are incorporated in the spectrometer. The electrical cables and gas and
water tubes to the furnace are led via a flexible conduit. The gas and electrical
supplies for the furnace are controlled from the spectrometer.

0993-5259 5-3
THGA System Description

The graphite tube


The graphite tube with its integral platform is made from a single piece of
electrographite with a coating of pyrolytic graphite. The tube has precisely
engineered holes for the external gas flow.
The integral platform enables the sample and the atmosphere in the graphite tube
to be in thermal equilibrium during the atomization step. This is an important
requirement of the STPF concept (Stabilized Temperature Platform Furnace).

Inlet for external


protective gas flow

Platform

Figure 5-2. Cross-section through the Graphite Tube


Tubes with and without end caps are available. The end caps prevent the atomized
sample from dispersing too quickly. This is very useful for some applications. The
end caps are also made from electrographite with a coating of pyrolytic graphite.

End cap

Figure 5-3. Graphite Tubes With and Without End Caps

5-4 0993-5259
THGA System Description

The graphite contacts


The special graphite tube is held in position in the furnace by two graphite
contacts. These provide the electrical contacts for the heating. The contact
surfaces must be perfectly clean and smooth to allow consistent heating
conditions. You must periodically clean the contact surfaces and change the
graphite contacts when the contact surfaces deteriorate.

Graphite tube
Rear contact

Front contact

Figure 5-4. Graphite Tube and Contacts

0993-5259 5-5
THGA System Description

Furnace heating and temperature profile


The furnace is electrically heated. A low-voltage high-current supply is applied
across the graphite tube, perpendicular to the path of the radiation beam through
the tube. The front and rear graphite contacts provide the electrical contacts.

Temp

0
Tube
Heating current length

Figure 5-5. Graphite Tube Temperature Profile


The transverse heating provides a more uniform temperature profile within the
tube than longitudinal designs. There are no cooler parts of the tube where atoms
can recombine, condense, or interact with cooler matrix components during the
atomization step. This design offers a number of advantages:
 The efficiency of atomization is increased – there is a greater concentration of
atoms in the radiation beam.
 Less tailing of the analyte absorption signal.
 Reduced background attenuation.
 A major reduction of carryover and memory effects, which can be especially
important for multi-element analyses.
 Shorter heating times are required for the determination of refractory
elements.

5-6 0993-5259
THGA System Description

Maximum power heating


Maximum power heating provides the most rapid heating of the tube and thus
atomization of the sample. The heating rate is approximately 2000 °C/s. It is
recommended for most analyses and is an important component of the STPF
concept.
To select this method of heating, you enter 0 (zero) for the Ramp Time in the
atomization step of the furnace program.

Time-controlled heating
Time-controlled heating is used for program steps other than the atomization step,
except in special situations.
To select this method of heating you enter a time between 1 and 99 (seconds) for
the Ramp Time in the relevant furnace program step. The heating rate is always
lower than the maximum power heating rate.

Temperature control
The temperature regulation system of the THGA furnace continuously monitors
the effective voltage across the tube and uses this together with the initial and final
temperatures to control the heating.
During maximum power heating, the emission temperature of the tube, measured
by an optical sensor, is also used to control the heating.

0993-5259 5-7
THGA System Description

The furnace gas system


Principle of the gas purging system
To prevent the graphite tube from being oxidized during the atomization step of
a graphite furnace analysis, an inert gas atmosphere inside and outside the
graphite tube is essential.
The furnace gas system supplies two independently controlled flows: the external
protective flow and the internal purge flow.
The furnace gas system has two inlets, the Normal Gas inlet and the Special Gas
inlet, to allow you to connect two separate gas supplies to the furnace.
The Normal Gas inlet provides:
 The inert gas that prevents the graphite tube and sample from oxidizing at
high furnace temperatures.
 The pneumatic pressure that holds the furnace closed and ensures that the
graphite tube makes good electrical contact with the graphite contacts.
Even when the spectrometer is switched off, the furnace is held closed if there
is pressure in the gas supply line. If you release the pressure in the lines you
can open the furnace.
The Special Gas inlet supplies the furnace with a special gas during some steps
of a furnace program. This is optional but is useful for particular applications; for
example, air may produce more effective ashing of organic materials.
The gas connections are located on the rear panel of the spectrometer.
Note: The furnace will operate correctly only if there is gas pressure at both gas
inlets. If you are not using a special gas, you must connect the inert gas to both
inlets using the Y-connector provided.

Inert gas
Argon is the recommended inert gas. It does not react with either the graphite tube
or the sample at the temperatures used in the furnace.
Although nitrogen can be used, it is not recommended as an inert gas for the
furnace. It can react both with the graphite tube and samples at normal
atomization temperatures. Nitrogen does not provide such efficient protection for
the graphite tube as argon at temperatures above 2000 °C and can react with the
graphite tube to form toxic cyanogen gas, (CN)2, at temperatures above 2300 °C.

5-8 0993-5259
THGA System Description

Cross-section through
the furnace showing
the external purge flow

Longitudinal section
through the furnace
showing the internal
protective flow

External flow
Internal flow
The internal and external
flows in and around the
graphite tube

Internal flow
External flow

Figure 5-6. Schematic of Furnace Gas Flows (not to scale)

0993-5259 5-9
THGA System Description

The external protective gas flow


The external gas flow protects the outside of the graphite tube from being
oxidized when the graphite tube is heated. Usually argon is used. The gas enters
the furnace through the rear of both contacts and flows into the space between
these and the graphite tube. It flows over the outside of the graphite tube and exits
through the sample injection hole and through the gap between the two contacts.
The external gas flow, 2 x 100 mL/minute, starts when power to the system is
switched on and stops automatically when the furnace has been idle for 10
minutes. During a furnace program the external gas flows continuously.

The internal purge gas flow


The internal gas flow enters the graphite tube at both ends and exits through the
sample injection hole. The flow starts as soon as you start a furnace program and
stops automatically when the furnace has been idle for 10 minutes.
Usually an inert gas, argon, is used to protect both the inside of the graphite tube
and the sample from being oxidized. The internal flow also purges vapors and
fumes, produced during the drying and pyrolysis steps, out of the tube.
You can also use a special gas for the internal gas flow. This is optional but is
useful for particular applications. For example, air may produce more effective
ashing of organic materials.
For each step of the furnace program you must select either the inert gas or the
special gas and the required flowrate.
The flow values are valid for argon. If you use nitrogen they will differ slightly
from the values quoted.
During each step of the furnace program the gas flows at the rate specified for that
step. For any step where you specify a lower flowrate than that for the previous
step, the system reduces the flow five seconds before the step starts. This ensures
that the flow is stable when the step starts.
Selecting zero flow for the atomization step ensures that the graphite tube and
sample are in thermal equilibrium; an important requirement of the STPF
concept.

5-10 0993-5259
THGA System Description

Cooling the furnace system


For rapid and accurate temperature control, the furnace must be both heated and
cooled. Cooling is achieved using water flowing through tubes that are integrated
into the furnace. At optimum water temperature and flow rate, the furnace can be
cooled in about 20 seconds from its maximum temperature to that of the incoming
cooling water. The temperature of the furnace housing is measured during
operation and the furnace is shut down if the temperature rises to above 120 °C.
The spectrometer also incorporates cooling coils to maintain the electronic
components at a comfortable working temperature.

Cooling system
PerkinElmer offers a recirculating cooling system; it is included with certain
spectrometer systems and offered as an option for others. It provides coolant at a
constant temperature and flow, to allow the most reproducible analytical
conditions. It also makes the system independent of external water supplies and
saves water. Electrical power to the cooling system is provided by the
spectrometer. The system shuts down automatically if the furnace has been idle
for more than 10 minutes.
The cooling system uses a 1:10 solution of glycerol in sediment-free drinking
water.
The cooling system also includes a pressure-sensitive safety device. If the
pressure in the circulatory system increases to above a factory-preset value an
internal bypass opens. This feature eliminates the risk of damage to the furnace
system through excess pressure. A pressure increase could be caused, for
example, if one of the hoses is kinked.

Max

Min

Figure 5-7. Furnace cooling system

0993-5259 5-11
THGA System Description

Zeeman-effect background correction

The spectrometer system uses the inverse, longitudinal Zeeman effect to correct
the analyte signal for background attenuation.
In this context ‘inverse’ means that the magnetic field acts on the atomized
sample in the graphite tube and ‘longitudinal’ means that the magnetic field is
aligned parallel to the radiation beam. The Zeeman effect is described briefly
below.

The Zeeman effect


Normal Zeeman splitting
The Zeeman effect refers to the splitting of atomic spectral lines into three or more
components when the emitting or absorbing species are subjected to a magnetic
field. The extra lines arise through the splitting of electron energy levels within
the atoms. In the simplest case this splitting produces two extra spectral lines, the
″ + and ″ – components, at each side of a nonshifted line, the ↓ component. The
magnitude of the shift depends on the strength of the magnetic field.
The THGA furnace uses a magnetic field strength of approximately 0.8 Tesla.
This shifts the ″ + and ″ – components by approximately 0.01 nm to each side of
the ↓ component.

↑Ν ↑Μ ↑Ο
shifted ″+ ↓ component shifted ″– magnetic
component at original component field direction
wavelength
Figure 5-8. Normal Zeeman splitting of a spectral line

5-12 0993-5259
THGA System Description

The ↓ component is linearly polarized, with the electric vector (polarization


direction) parallel to the magnetic field.
The two shifted lines (″ components) are circularly polarized, in opposite
directions, with the axes of polarization parallel to the magnetic field.
The different intensities of the lines (the nonshifted line has twice the intensity of
the shifted lines) are due to quantum selection rules governing the probability of
transitions between the energy levels available to the electrons.

Anomalous Zeeman splitting


The brief description given above is for the simplest case of Zeeman splitting for
a singlet spectral line.
For many atoms, the actual relationship between the shifted and nonshifted lines
is much more complicated and produces complex or anomalous Zeeman splitting
patterns. In these, the ″ and ↓ lines can each be split into many components, but
the basic principle of the Zeeman-effect still explains these phenomena.

Normal splitting

Anomalous splitting Anomalous splitting

Figure 5-9. Comparison of Normal and Anomalous Zeeman Splitting

0993-5259 5-13
THGA System Description

Applying Zeeman-effect background correction


Two methods of observing and using the Zeeman effect are generally used:
 The longitudinal configuration where the magnetic field and radiation beam
are parallel. This system is used in the AAnalyst 600 and 800 spectrometers.
 The transverse configuration where the magnetic field and radiation beam are
perpendicular to each other. This system is described for comparison.

Magnetic field OFF


Longitudinal and transverse

↑Μ
Magnetic field ON
″– ″Η ↓ Magnetic field ON
Longitudinal ″ –
″ Η Transverse

↑Μ ↑Μ

Figure 5-10. Comparison of the Longitudinal and Transverse Directions of


Observation for Normal Zeeman Splitting

5-14 0993-5259
THGA System Description

Longitudinal configuration
This system is used in the AAnalyst 600 and 800 spectrometers.
In this arrangement only the two shifted lines are seen.
These appear to be, and are, circularly polarized, because of the direction of
viewing, which is parallel to the axis of circular polarization.
The nonshifted line cannot be seen because its electric vector is aligned with the
radiation beam (an electromagnetic wave does not propagate in the direction of
its electric vector).
With the longitudinal configuration no polarizer is needed.

Radiation beam
″ components
shifted lines,
circularly polarized

↓ component
nonshifted line,
linearly polarized
Magnetic field

↓ not seen
Η
″ –

Observed spectrum

↑Ν ↑Μ ↑Ο

Figure 5-11. The Zeeman Effect Observed in the Longitudinal Direction

0993-5259 5-15
THGA System Description

Transverse configuration
With this arrangement, the nonshifted line and the two shifted lines are seen.
The shifted lines appear to be linearly polarized (although in fact they are
circularly polarized) because of the direction of viewing, which is perpendicular
to the axis of the circular polarization.
A polarizer is required in the optical system in order to use the transverse
configuration for background correction.

Observed spectrum

″ components ↓
appear to be ″– ″Η
horizontally
polarized

″ components
↑Ν ↑Μ ↑Ο
shifted lines,
circularly polarized

↓ component
nonshifted line,
linearly polarized
Magnetic field
Radiation beam

Figure 5-12. The Zeeman Effect Observed in the Transverse Direction

5-16 0993-5259
THGA System Description

Analyte signals and background correction


Each measurement cycle contains two light phases. The magnetic field is on
during one of them and off during the other.
With the magnetic field on, the analyte signal is split into the two shifted ″
components and the ‘unseen’, nonshifted ↓ component. The two ″ components
cannot absorb energy at the analytical wavelength, and the ↓ component, not
having an effect in the longitudinal direction, also cannot absorb energy at the
analytical wavelength.
Any attenuation of radiation at the analytical wavelength is thus due only to the
background (structured and/or continuous).
With the magnetic field off, any attenuation of radiation at the analytical
wavelength is due to absorption by the single analyte signal in addition to any
attenuation due to the background; structured, continuous, or both.
This procedure of rapidly alternating measurements of [analyte+background] and
[background only] at exactly the same wavelength during the measurement cycle
gives the system its ideal double-beam characteristics.

Magnetic field OFF Magnetic field ON

Atomized sample

Radiation
beam
Magnetic field parallel
to radiation beam
Source emission line

″–
″Η
Absorption
Absorption
profile
Absorption

↑Μ ↑Μ
↑0 – analytical wavelength

Figure 5-13. Background Correction Using the Longitudinal Zeeman Effect

0993-5259 5-17
THGA System Description

Technical data

Graphite furnace
Principle Transversely-heated graphite furnace.
Temperature Ambient temperature (20 °C) to 2600 °C, programmable in steps of 10 °C.
range
Heating rate Programmable up to approx. 2000 °C/s (maximum power heating).
Gas Inert gas supply required for operation (not provided); argon recommended.
requirements A second, special gas can also be used.
Automatic gas shutdown when the furnace has been idle for 10 minutes.
Pressure: 350–400 kPa (3.5–4 bar, 51–58 psig)
Gas flow: max. 700 mL/min
Gas flows Internal flow, selectable flow rates: 0, 50, 250 mL/min
External flow, fixed: 2 x 100 mL/min
Cooling The use of the optional Recirculating Cooling System is recommended
(see page 5-20 for the technical data).
Furnace Up to twelve independent steps.
program Parameters:
Isothermal temperature holding time: 0–99 s, in steps of 1 s
Isothermal temperature: 20–2600 °C in steps of 10 °C
Heating rate: programmable, time-dependent or maximum power
Internal gas flow
Read delay
Read time
Magnetic field is automatically switched on and off by the system at the
correct times

5-18 0993-5259
THGA System Description

Safety features Automatic circuit breaker to prevent the furnace drawing too much current.
Safety lock to prevent operation with the furnace open or with a defective
tube.
Protection against overheating of the furnace, electromagnet, or transformer.
Safety lock to prevent operation with low gas pressure.
The software continuously monitors the status of the system and informs the
user of any problems. If the user attempts to perform an action that could
have serious consequences, suitable messages appear on the screen.
Power Integrated into the spectrometer; see the Technical Data for the spectrometer.
requirements
Electrical As defined in EN 61010-1-1993 (IEC 1010-1):
protection Insulation: Class I
Insulation category (Overvoltage category): II
Pollution degree: 2

Safety standards As defined in EN 61010-1-1993 (IEC 1010-1: 1990 + A1 + A2) and


EN 61010-2-061:1996.
CSA standards: CAN/CSA-C22.2 No. 1010.1-92, Amendment 1 (1992),
2 (1995), and CAN/CSA 61010-2-061 (1995).
UL standards: UL 3101-1 1993 and UL 3111-1 1994.
Compliant to the requirements of Canadian Standards Association (CSA)
and Underwriters Laboratory (UL) as listed in File No. LR 45111.
Certificate of Approval and GS mark from the LGA Bavaria, FRG, Institute
of Equipment Safety Testing and Certification, and CSA-NRTL/C mark
from CSA, Canada, File No. LR 45111.
EMC standards As defined in EN 61326-1:1997.
Environmental Ambient temperature +15 C to +35 C (+59 F to +95 F), with a
requirements maximum change not exceeding 2.8 C (5 F) per hour.
20–80% relative humidity; non-condensing.

0993-5259 5-19
THGA System Description

Cooling system
The recirculating cooling system is included with certain spectrometer systems and is offered as
an option for others.

Principle Self-priming recirculating system with fan-assisted heat exchanger.


Coolant 1:10 mixture of glycerol in sediment-free drinking water.
Volume Approx. 5 L
Water Output: 36 °C ± 5 °C
temperature Inlet max: 90 °C
Fan cut-in temp: 40 °C
Flow 2.5 L/min
Air flow Approx. 400 m3/hour
Water pressure 300 kPa, (3 bar, 43 psig).
Pressure-sensitive safety device opens if the internal pressure increases to
above a factory-preset value.
Connections Reinforced hose, i.d. 8 mm; automatic connectors with integral
shut-off valves.
Power 230 V, 50/60 Hz
requirements Power consumption: approx. 140 VA

Safety standards As defined in EN 61010-1-1993 (IEC 1010-1: 1990 + A1 + A2) and


EN 61010-2-061:1996.
CSA standards: CAN/CSA-C22.2 No. 1010.1-92, Amendment 1 (1992),
2 (1995), and CAN/CSA 61010-2-061 (1995).
UL standards: UL 3101-1 1993 and UL 3111-1 1994.
Compliant to the requirements of Canadian Standards Association (CSA) and
Underwriters Laboratory (UL) as listed in File No. LR 45111.
Certificate of Approval and GS mark from the LGA Bavaria, FRG, Institute
of Equipment Safety Testing and Certification, and CSA-NRTL/C mark from
CSA, Canada, File No. LR 45111.
EMC standards As defined in EN 61326-1:1997.
Dimensions Width: 200 mm
Height: 375 mm
Depth: 500 mm
Mass (Weight) Approx. 18 kg with coolant.

5-20 0993-5259
THGA System Description

AS-800 Furnace Autosampler

Autosampler design
The autosampler contains all the mechanical and electrical components required
to withdraw the correct volume of solution from a selected container, inject it into
the graphite tube, and rinse the pipet tip. Using the autosampler to inject solutions
into the graphite tube considerably improves the precision of the analytical results
compared to that for manual pipetting. The volumes pipetted and the positioning
of the droplet inside the graphite tube are much more reproducible when
performed by the autosampler.
The autosampler is mounted on a swing arm directly in front of the atomizer
compartment. Although you can easily remove and refit it, this is usually not
necessary.

Sample and rinse pumps


The sample and rinse pumps are mounted on the side of the sample table. They
are driven by stepping motors to guarantee the precision and accuracy of the
selected volumes.
The rinse pump contains ball valves at the inlet and outlet. The sample pump
contains no valves.
The rinse pump delivers a fixed volume of rinsing liquid. The sample pump
delivers the volume that you select in the application program.

The sample table


The autosampler arm moves the pipet tip between the pipetting location and the
sample injection hole of the graphite tube. The autosampler arm and motor
assembly is fixed to the sample table. The sample tray trough and the overflow
rinsing port are mounted on a movable plate on the sample table. A stepping
motor slews the plate to position the correct reagent or sample container, or the
rinsing port, at the pipetting location.
The sample tray sits in the sample tray trough, which has a plastic cover. The
cover protects the samples from contamination and reduces the rate of
evaporation of the solvent. You can reduce the rate of evaporation further by
pouring a small volume of water into the sample tray trough.
The sample tray is removable. It is useful to have several trays so that you can load
trays while one tray of samples is being analyzed.
There are two types of sample tray available, with either 88 or 148 locations for
samples and reagents.

0993-5259 5-21
THGA System Description

Sample tube

Rinsing port

Connecting Rinse feed


Forward/backward tube tube
alignment control

Left/right Pumps
alignment control
Rinse feed
tube
Drain tube
Metal swing arm

Control cable

Hinge pin

Waste bottle Rinse bottle

Figure 5-14. AS-800 Furnace Autosampler (1)

5-22 0993-5259
THGA System Description

Motor assembly

Depth control

Rinse pump

Sample tube
Sample pump

Autosampler arm

Rinsing port

Sample tray

Sample table

Figure 5-15. AS-800 Furnace Autosampler (2)

Sample and reagent containers


These containers are available with volumes of 1.2 mL, 2.5 mL or 7 mL. They are
made of polypropylene.
As well as for samples, you can use the containers for calibration solutions,
modifier solutions, or sample solutions for special applications.

Controlling the autosampler


Via the AA WinLab application, you control exactly how and when the solutions
will be taken up and injected into the graphite tube. For example you can select:
 The order in which the solutions will be taken up.
 To pipet some or all of the solutions one after another and inject them into the
graphite tube together.
 To pipet some or all of the solutions separately and inject them separately into
the graphite tube.

0993-5259 5-23
THGA System Description

The autosampler operating cycle


1. You start the analysis with a software command.
The furnace program starts. The pipet tip is in the rinsing port.
2. The rinse pump performs three cycles, rinsing the pipet tip with 4.5 mL of
rinsing liquid.
3. The autosampler arm rises and the movable plate positions the requested
solution at the pipetting location.
Simultaneously, the sample pump draws a small bubble of air into the pipet
tip to separate the rinsing liquid from the solution being pipetted.
4. The autosampler arm lowers the pipet tip into the solution and the sample
pump draws the selected volume of solution into the tip. The autosampler arm
rises.
5. If you selected to pipet more than one solution in one step:
– The container with the next solution is brought to the pipetting location.
– A small bubble of air is drawn into the pipet tip.
– Step 4 is repeated for this solution.
– Step 5 is repeated until all the solutions you selected have been taken up
into the pipet tip.
6. The autosampler arm swings over to the graphite furnace and injects the
solutions into the graphite tube.
7. The autosampler arm swings back to the sample table and simultaneously the
movable plate positions the rinsing port at the pipetting location. The rinse
pump rinses the pipet tip with rinsing liquid.
8. Steps 3 to 7 are repeated for each step of the analysis program that requires
solutions to be pipetted.
9. When all the solutions have been injected into the graphite tube, the pipet tip
returns to the rinsing port and the rinse pump rinses the pipet tip with rinsing
liquid.
10. The furnace program continues to the end and the analyte signal is measured.
11. The preceding steps are carried out for each replicate of every sample and
calibration solution.

5-24 0993-5259
THGA System Description

Technical data

AS-800 Furnace Autosampler


Principle Random access furnace autosampler with programmable sample volume. Can
combine and dilute solutions automatically in the graphite tube and produce
calibration solutions from a stock solution.
Control From the spectrometer’s application program.
Sample trays Removable trays with 88 and 148 locations.
Rinsing A rinsing port is integrated with the sample table. This rinses the inside and
outside of the pipet tip.
Minimum 0.1 mL
required sample
volume
Pipetted volume Minimum: 1.0 µL; maximum: 99 µL.
For the best precision a minimum of 5 µL is recommended.
Maximum = volume of one solution or the sum of individual solution
volumes pipetted together; for example: [sample + matrix modifier + diluent
+ air bubble volumes]
Power The autosampler draws its power from the spectrometer.
requirements
Safety and As defined in EN 61010-1-1993 (IEC 1010-1: 1990 + A1 + A2) and
EMC standards EN 61010-2-061:1996.
Electromagnetic compatibility: EN 61326-1:1997.
Environmental Ambient temperature +15 C to +35 C (+59 F to +95 F), with a maximum
requirements change not exceeding 2.8 C (5 F) per hour.
20–80% relative humidity; non-condensing.
Dimensions Dimensions without swing arm
Width: 270 mm
Height: 200 mm
Depth: 340 mm
Mass approx. 7 kg including swing arm.
(weight)

0993-5259 5-25
THGA System Description

Literature on electrothermal atomization

The following monograph provides detailed information on electrothermal


atomization and other aspects of atomic absorption analyses:
B. Welz and M. Sperling, Atomic Absorption Spectrometry,
third, completely revised edition,
Wiley-VCH, New York and Weinheim, 1999,
ISBN 3-527-28571-7

5-26 0993-5259
Translations of Warnings 6
6Translations of Warnings
Marker for header

0993-5259 6-1
Translations of Warnings

6-2 0993-5259
Translations of Warnings

Warning Messages

This section contains translations of the warnings used in this guide.

dansk Oversættelser af advarsler


Denne del indeholder oversættelserne af de advarsler, som er indeholdt i denne håndbog.
Deutsch Übersetzungen der Warnungen
Dieser Abschnitt enthält die Übersetzungen der in diesem Handbuch verwendeten
Warnungen.
español Traducciones de las advertencias
Esta sección contiene traducciones de las advertencias utilizadas en el presente manual.
italiano Traduzione dei simboli di avvertenza
La presente sezione contiene la traduzione dei simboli di avvertenza utilizzati nel
presente manuale.
Nederlands Vertalingen van de Waarschuwingen
Dit gedeelte bevat vertalingen van de waarschuwingen gebruikt in dit handboek.
português Traduções de avisos
Esta secção contém traduções dos avisos usados no manual.
suomea Varoitusten käännökset
Tämä osa sisältää tässä käsikirjassa käytettyjen varoitusten käännökset.
svenska Översättning av varningstexter
Detta avsnitt innehåller översättningar av de varningstexter som används i handboken.

0993-5259 6-3
Translations of Warnings

6-4 0993-5259
Translations of Warnings

This symbol alerts you to situations that could result in personal injury to yourself or other
persons.
Details about these circumstances are in a box like this one.

dansk Dette symbol gør Dem opmærksom på situationer, som kan medføre kvæstelser af Dem
selv eller andre personer.
Detaljer vedrørende disse omstændigheder er indrammet på tilsvarende måde som
denne henvisning.

Deutsch Dieses Symbol warnt vor Situationen, in denen Sie oder andere Personen verletzt werden
können.
Einzelheiten darüber sind in einem Rahmen wie diesem angegeben.

español Este símbolo le advierte de situaciones que pueden provocar lesiones corporales a
usted o a otras personas.
En los recuadros como éste se proporciona información sobre este tipo de circunstancias.

français Ce symbole vous signale des situations pouvant occasionner des dommages corporels
à l'utilisateur ou à d'autres personnes.
Les détails sur ces circonstances sont données dans un encadré semblable à celui-ci.

italiano Questo simbolo segnala situazioni che possono generare incidenti a voi stessi o ad
altre persone.
Troverete informazioni su tali circostanze in un riquadro come questo.

Nederlands Dit symbool maakt U attent op situaties die tot verwondingen voor Uzelf of anderen
kunnen leiden.
Bijzonderheden over deze omstandigheden staan in een kader zoals dit.

português Este símbolo alerta para situações que poderão causar um ferimento ao usuário.
Detalhes referentes a estas circunstâncias encontram-se referidos numa caixa como
esta.

suomea Tämä symboli haluaa kiinnittää huomiotasi tilanteisiin, joiden seurauksena voi olla itsesi
tai muiden henkilöiden loukkaantuminen.
Yksityiskohtaisia tietoja tällaisista tapauksista on tämäntapaisessa ruudussa.

svenska Denna symbol används för situationer där det finns risk för personskador om användaren
inte följer anvisningarna.
Detaljerad information ges i en ruta som denna.

0993-5259 6-5
Translations of Warnings

This symbol alerts you to the risk of hot surfaces that could cause personal injury to
yourself or other persons.
Details about these circumstances are in a box like this one.

dansk Dette symbol gør Dem opmærksom på risikoen for varme overflader, som kan medføre
kvæstelser af Dem selv eller andre personer.
Detaljer vedrørende disse omstændigheder er indrammet på tilsvarende måde som
denne henvisning.

Deutsch Dieses Symbol warnt vor Gefahr durch heiße Oberflächen, durch die Sie oder andere
Personen verletzt werden können.
Einzelheiten darüber sind in einem Rahmen wie diesem angegeben.

español Este símbolo le advierte del peligro de que las superficies candentes provoquen
quemaduras a usted o a otras personas.
En los recuadros como éste se proporciona información sobre este tipo de circunstancias.

français Ce symbole vous avertit d'un risque de surfaces chaudes pouvant occasionner des
dommages corporels à l'utilisateur ou à d'autres personnes.
Les détails sur ces circonstances sont données dans un encadré semblable à celui-ci.

italiano Questo simbolo vi mette in guardia da superfici molto calde che possono causare
incidenti a voi stessi o ad altre persone.
Troverete informazioni su tali circostanze in un riquadro come questo.

Nederlands Dit symbool maakt U attent op het risico van hete oppervlaktes dat tot verwondingen
voor Uzelf of anderen kunnen leiden.
Bijzonderheden over deze omstandigheden staan in een kader zoals dit.

português Este símbolo alerta para um risco de superfícies quentes que poderão causar um
ferimento ao usuário.
Detalhes referentes a estas circunstâncias encontram-se referidos numa caixa como
esta.

suomea Tämä symboli haluaa kiinnittää huomiotasi kuumiin pintoihin, joiden seurauksena voi
olla itsesi tai muiden henkilöiden loukkaantuminen.
Yksityiskohtaisia tietoja tällaisista tapauksista on tämäntapaisessa ruudussa.

svenska Denna symbol används för situationer där det finns risk för varma ytor som kan ge
personskador om användaren inte följer anvisningarna.
Detaljerad information ges i en ruta som denna.

6-6 0993-5259
Translations of Warnings

This symbol alerts you to the risk of ultraviolet radiation that could cause eye damage
to yourself or other persons.
Details about these circumstances are in a box like this one.

dansk Dette symbol gør Dem opmærksom på risikoen for ultraviolet stråling, som kan medføre
ødelæggelse af øjnene for Dem selv eller andre personer.
Detaljer vedrørende disse omstændigheder er indrammet på tilsvarende måde som
denne henvisning.

Deutsch Dieses Symbol warnt vor Gefahr durch UV-Strahlung, die bei Ihnen oder anderen
Personen zu Augenverletzungen führen können.
Einzelheiten darüber sind in einem Rahmen wie diesem angegeben.

español Este símbolo le advierte del peligro de que usted u otras personas sufran lesiones en los
ojos a consecuencia de la radiación ultravioleta.
En los recuadros como éste se proporciona información sobre este tipo de circunstancias.

français Ce symbole vous avertit d'un risque de rayonnement ultraviolet pouvant occasionner
des lésions oculaires à l'utilisateur ou à d'autres personnes.
Les détails sur ces circonstances sont données dans un encadré semblable à celui-ci.

italiano Questo simbolo vi mette in guardia da radiazione ultravioletta che può causare lesioni
agli occhi a voi stessi o ad altre persone.
Troverete informazioni su tali circostanze in un riquadro come questo.

Nederlands Dit symbool maakt U attent op het risico van ultraviolette straling dat tot verwondingen
voor Uzelf of anderen kan leiden.
Bijzonderheden over deze omstandigheden staan in een kader zoals dit.

português Este símbolo alerta para um risco de radiação ultravioleta que poderá causar
ferimentos aos olhos do usuário.
Detalhes referentes a estas circunstâncias encontram-se referidos numa caixa como
esta.

suomea Tämä symboli haluaa kiinnittää huomiotasi ultraviolettisäteilyn vaaraan, jonka


seurauksena voi olla silmävammat itsellesi tai muille henkilöille.
Yksityiskohtaisia tietoja tällaisista tapauksista on tämäntapaisessa ruudussa.

svenska Denna symbol används för situationer där det finns risk för ultraviolett strålning som kan
ge ögonskador om användaren inte följer anvisningarna.
Detaljerad information ges i en ruta som denna.

0993-5259 6-7
Translations of Warnings

Caution:
The term CAUTION alerts you to situations that could result in serious damage to the
instrument or other equipment.
Details about these circumstances are described in a message similar to this one.

dansk Bemærk:
Angivelsen CAUTION (BEMÆRK) gør Dem opmærksom på situationer, som kan medføre
alvorlig ødelæggelse af apparatet eller andet udstyr.
Detaljer vedrørende disse omstændigheder er beskrevet i henvisninger svarende til
denne.

Deutsch Achtung:
Der Ausdruck CAUTION (ACHTUNG) warnt vor Situationen, die eine ernste
Beschädigung des Geräts oder anderer Systemteile zur Folge haben können.
Einzelheiten darüber sind auf die gleiche Weise wie dieser Text hervorgehoben.

español Advertencia:
El término CAUTION (ADVERTENCIA) le previene de situacones que pueden provocar
averías graves en éste u otros equipos.
En los recuadros como éste se proporciona información sobre este tipo de circunstancias.

français Attention:
Le terme CAUTION (ATTENTION) vous signale des situations susceptibles de provoquer
de graves détériorations de l'instrument ou d'autre matériel.
Les détails sur ces circonstances figurent dans un message semblable à celui-ci.

6-8 0993-5259
Translations of Warnings

=Caution (continued)
italiano Attenzione:
Con il termine CAUTION (ATTENZIONE) vi si mette in guardia da situazioni che possono
comportare il serio danneggiamento della strumentazione o di altre apparecchiature.
Troverete informazioni su tali circostanze in un riquadro come questo.

Nederlands Let op:


De term CAUTION (LET OP) maakt U attent op situaties die tot ernstige beschadigingen
aan het instrument of andere apparaten kunnen leiden.
Bijzonderheden over deze omstandigheden worden beschreven in een mededeling gelijk
aan.

português Atenção:
O termo CAUTION (ATENÇÃO) alerta para situações que poderão causar danificação
do aparelho.
Detalhes referentes a estas circunstâncias encontram-se referidos numa caixa como
esta.

suomea Huomio:
CAUTION (HUOMIO) haluaa kiinnittää huomiotasi tilanteisiin, joiden seurauksena voi olla
laitteen tai muiden varusteiden vakava vaurioituminen.
Tällaiset tapaukset selostetaan yksityiskohtaisesti tämäntapaisessa huomautuksessa.

svenska Observera:
Termen CAUTION (OBSERVERA) skall göra användaren uppmärksam på att apparaten
eller annan utrustning kan ta allvarlig skada om anvisningarna inte följs. Detaljerad
information ges i en ruta som denna.

0993-5259 6-9
Translations of Warnings

W1.2
Warning: Unauthorized Adjustments and Servicing
Only a PerkinElmer service engineer or similarly trained and authorized person should be
permitted to service the instrument.
• Do not attempt to make adjustments, replacements, repairs, or modifications to this
instrument except as described in the documentation supplied with the instrument.

dansk Advarsel: Ikke-tilladte indstillinger og arbejder på apparatet


Vedligeholdelse af apparatet er kun tilladt for PerkinElmer kundeservice-ingeniøren eller
tilsvarende uddannede og autoriserede personer.
• Prøv ikke på at foretage indstillinger, udskiftninger, reparationer eller ændringer af
apparatet, som ikke er beskrevet i den dokumentation, der er vedlagt apparatet.

Deutsch Warnung: Unzulässige Arbeiten am Gerät


Wartungs- oder Reparaturarbeiten oder Justierungen, die in der Benutzerdokumentation
zum Gerät nicht beschrieben sind, dürfen nur vom PerkinElmer Kundendienst oder von
entsprechend ausgebildeten und autorisierten Fachkräften ausgeführt werden.

español Advertencia: Ajustes y servicios sin autorización


Tan sólo un ingeniero de Servicio Técnico de PerkinElmer o una persona de formación y
autorización similares podrán realizar trabajos de revisión y mantenimiento del
instrumento.
• No intente realizar ningún tipo de ajuste, sustitución o reparación en este aparato, a
excepción de lo descrito en la Documentación del Usuario que se adjunta.

français Danger: Réglages et entretien non autorisés


Seul un ingénieur du service après vente PerkinElmer ou une personne autorisée et de
même formation sont autorisées à intervenir sur l'instrument.
• Ne pas essayer d'effectuer des réglages, des remplacements, des réparations ou des
modifications sur cet instrument d'une manière autre que celle décrite dans la
documentation fournie avec l'instrument.

6-10 0993-5259
Translations of Warnings

=Warning (continued) W1.2

italiano Pericolo: Regolazioni e manutenzione non autorizzati


L'asservimento dello strumento è permesso esclusivamente ad un tecnico di assistenza
della PerkinElmer oppure da simile persona addestrata e autorizzata.
• Non provare ad eseguire regolazioni, sostituzioni, riparazioni o modifiche a questo
strumento se non come descritto nella documentazione allegata allo strumento.

Nederlands Waarschuwing: Ongeautoriseerde aanpassingen en service


Alleen een PerkinElmer service-monteur of een gelijksoortig opgeleid en geautoriseerd
persoon mag service verlenen aan het instrument.
• Probeer niet zelf aanpassingen aan dit instrument aan te brengen, het te repareren of
te veranderen behalve zoals beschreven in de documentatie die bij het instrument
geleverd is.

português Aviso: Trabalhos não permitidos no aparelho


Trabalhos de manutenção apenas podem ser executados pelo Serviço Técnico da
PerkinElmer ou por pessoal especializado devidamente formado e autorizado.
• Não tente realizar ajustamentos, substituições, reparações ou modificações neste
aparelho que não estejam descritos na documentação fornecida com o aparelho.

suomea Varo: Luvattomat säätö - ja huoltotyöt


Laitteen huoltotyöt saa antaa vain PerkinElmer -huoltoteknikoiden tai vastaavasti
koulutettujen ja valtuutettujen henkilöiden tehtäväksi.
• Älä tee muita säätö-, vaihto-, korjaus- tai muutostöitä tässä laitteessa kuin sellaisia,
jotka on selostettu laitteen mukana toimitetussa dokumentaatiossa.

svenska Varning: Icke tillåtna arbeten på apparaten


Endast servicepersonal från PerkinElmer eller personal med liknande utbildning och
behörighet får utföra servicearbeten på apparaten.
• Underhålls- eller reparationsarbeten, justeringar eller ändringar som inte finns
beskrivna i användarmanualen till apparaten får inte utföras.

0993-5259 6-11
Translations of Warnings

W3.3
Warning: UV Radiation – Risk of Eye Damage
The lamps may emit UV radiation which can damage your eyes.
• Always wear UV-absorbing safety glasses when aligning the autosampler.
dansk Advarsel: Ultraviolet stråling – farligt for øjnene
Lamperne kan emittere ultraviolet stråling, som kan forårsage øjenskader.
• Bær altid beskyttelsesbriller, som absorberer ultraviolet stråling under prøveautomat-
justeringen.

Deutsch Warnung: UV-Strahlung – Gefährdung der Augen


Die Strahlungsquellen können UV-Strahlung emittieren und dadurch Augenschäden
verursachen.
• Tragen Sie während der Probenautomatjustierung eine Schutzbrille, die die emittierte
UV-Strahlung ausreichend absorbiert.

español Advertencia: Radiación ultravioleta – Peligro de daños a los ojos


Las lámparas pueden emitir radiación utravioleta que puede ser perjudicial para los ojos.
• Al realizar el ajuste del extractor de muestras automático, utilice siempre gafas de
seguridad que absorban este tipo de rayos.

français Danger: Rayonnement UV


Les lampes peuvent émettre des UV susceptibles de provoquer des lésions oculaires.
• Toujours porter des lunettes de protection absorbant les UV pour aligner
l'échantillonneur automatique.

6-12 0993-5259
Translations of Warnings

=Warning (continued) W3.3

italiano Pericolo: Radiazioni UV – Rischio di lesioni agli occhi


Le lampade possono emettere radiazioni UV che possono lesionare gli occhi.
• Durante l'allineamento dell'autocampionatore indossate sempre occhiali di sicurezza
in grado di assorbire le radiazioni UV.

Nederlands Waarschuwing: Ultraviolette straling – Risico’s voor de ogen


De lampen kunnen UV-straling emitteren en daardoor letsel aan de ogen veroorzaken.
• Draag tijdens de instelling van de automaat een veiligheidsbril die de geïmitteerde
straling voldoende absorbeert.

português Aviso: Radiação UV – perigo para os olhos


As lâmpadas emitem uma radiação UV com intensidades diferentes podendo assim
provocar ferimentos aos olhos.
• Durante o ajuste do automático de ensaio use óculos de protecção que absorvam
suficientemente a radiação UV emitida.

suomea Varo: UV-säteily – silmävammojen vaara


Lamput saattavat lähettää UV-säteilyä, joka voi vahingoittaa silmiä.
• Käytä aina UV-säteilyltä suojaavia suojasilmälaseja, kun säädät näyteautomaattia.
svenska Varning: UV-strålning – risk för ögonskador
Strålningskällorna/lamporna alstrar UV-strålning som kan ge ögonskador.
• Använd alltid skyddsglasögon som absorberar UV-strålar vid inställning av
provningsautomaten.

0993-5259 6-13
Translations of Warnings

W3.5
Warning: UV Radiation – Risk of Eye Damage
When the graphite furnace is heated to incandescence, e.g. during the atomization step,
the furnace can emit UV radiation which can damage your eyes.
• Always wear UV-absorbing safety glasses when looking at the furnace.
dansk Advarsel: Ultraviolet stråling – farligt for øjnene
Når grafitdelene fra den opvarmede grafitovn gløder, dvs. under forstøvningstrinet, kan de
emittere ultraviolet stråling, som kan forårsage øjenskader.
• Bær altid beskyttelsesbriller, som absorberer ultraviolet stråling, når De ser ind i
ovnen.

Deutsch Warnung: UV-Strahlung – Gefährdung der Augen


Die glühenden Graphitteile des aufgeheizten Graphitofens emittieren UV-Strahlung und
können dadurch Augenschäden verursachen.
• Tragen Sie eine Schutzbrille, die die emittierte UV-Strahlung ausreichend absorbiert,
wenn Sie in oder auf den heißen Ofen schauen.

español Advertencia: Radiación ultravioleta – Peligro de daños a los ojos


Cuando el horno de grafito se caliente hasta la incandescencia, p.ej. durante la fase de
atomización, este horno puede emitir radiación ultravioleta perjudicial para los ojos.
• Al mirar al horno utilice siempre gafas de seguridad que absorban este tipo de rayos.
français Danger: Rayonnement UV
Lorsque le four en graphite est porté à incandescence, par exemple pendant l'étape
d'atomisation, il peut émettre des UV susceptibles de provoquer des lésions oculaires.
• Toujours porter des lunettes de protection absorbant les UV pour regarder le four.

6-14 0993-5259
Translations of Warnings

=Warning (continued) W3.5

italiano Pericolo: Radiazioni UV – Rischio di lesioni agli occhi


Quando il forno a grafite è riscaldato sino all'incandescenza, per esempio durante la fase
di atomizzazione, esso può emettere radiazioni UV che possono lesionare gli occhi.
• Quando guardate nel forno indossate sempre occhiali di sicurezza in grado di
assorbire le radiazioni UV.

Nederlands Waarschuwing: Ultraviolette straling – Risico’s voor de ogen


De gloeiende grafietdeeltjes van de verhitte grafietoven emitteren UV-straling en kunnen
daardoor letsel aan de ogen veroorzaken.
• Draag altijd een veiligheidsbril, die de geëmitteerde UV-straling voldoende
absorbeert, wanneer U in of naar de hete oven moet kijken.

português Aviso: Radiação UV – perigo para os olhos


As peças de grafite em brasa dentro do forno de grafite aquecido (p. ex. durante a fase
de atomização) emitem radiações UV podendo assim provocar ferimentos aos olhos.
• Use sempre óculos de protecção que absorvam suficientemente a radiação UV
emitida ao olhar directamente para dentro do forno quente.

suomea Varo: UV-säteily – silmävammojen vaara


Kun grafiittiuuni kuumenee valkohehkuun asti, esim. sumutusvaiheen aikana, uuni
saattaa lähettää UV-säteilyä, joka voi vahingoittaa silmiä.
• Käytä aina UV-säteilyltä suojaavia suojasilmälaseja, kun katsot uuniin.
svenska Varning: UV-strålning – risk för ögonskador
De glödande grafitdelarna i den uppvärmda grafitugnen alstrar UV-strålning, t ex under
finfördelningsfasen, och kan därför skada ögonen.
• Använd alltid skyddsglasögon som absorberar UV-strålar när du tittar mot den varma
ugnen.

0993-5259 6-15
Translations of Warnings

W4.3
Warning: High Temperatures – Risk of Burns
The graphite furnace can generate very high temperatures.
 Do not touch any parts of the furnace, especially the graphite components, until they
have cooled to room temperature.
dansk Advarsel: Høje temperaturer – Fare for forbrændinger
Grafitovnen kan udvikle meget høje temperaturer.
 Berør aldrig nogen af ovnens dele, især ikke grafitdelene, før de er kølet ned til
stuetemperatur.
Deutsch Warnung: Verbrennungsgefahr
 Vergewissern Sie sich, daß der Ofen auf Raumtemperatur abgekühlt ist, bevor Sie Ihn
anfassen oder öffnen.
español Advertencia: Altas temperaturas – Riesgo de quemaduras
El horno de grafito puede alcanzar temperaturas muy altas.
 Asegúrese, antes de tocar cualquier parte del horno, sobre todo sus componentes de
grafito, de que éste se haya enfriado hasta alcanzar la temperatura ambiente.
français Danger: Températures élevées – Risque de brûlures
Le four en graphite peut générer de très hautes températures.
 Ne toucher aucun des éléments du four, en particulier les composants en graphite,
avant qu'ils n'aient refroidi à la température ambiante.
italiano Pericolo: Alte temperature – Rischio di ustioni
Il forno a grafite può generare temperature estremamente elevate.
 Non toccare nessun componente del forno, soprattutto i componenti in grafite, sino a
che essi non si sono raffreddati sino a raggiungere temperatura ambiente.
Nederlands Waarschuwing: Hoge temperaturen – Verbrandingsgevaar
De grafietoven kan zeer hoge tenperaturen bereiken.
 De oven en in het bijzonder de grafietonderdelen pas aanraken als ze tot
kamertemperatuur afgekoeld zijn.
português Aviso: Altas temperaturas – perigo de queimaduras
O forno de grafite pode alcançar temperaturas muito elevadas.
 Não toque em nenhuma peça do forno, especialmente nos componentes de grafite,
até terem alcançado a temperatura ambiente.
suomea Varo: Korkeat lämpötilat – palovammavaara
Grafiittiuuni voi kehittää erittäin korkeita lämpötiloja.
 Älä kosketa mitään uunin osia, tämä koskee erityisesti grafiittikomponentteja, ennen
kuin ne ovat jäähtyneet huoneenlämpötilaan.
svenska Varning: Höga temperaturer – risk för brännskador
Grafitugnen kan nå mycket höga temperaturer.
 Vidrör inte ugnen och framför allt inte grafitdelarna förrän de svalnat till
rumstemperatur.

6-16 0993-5259
Translations of Warnings

W6.1
Warning: Toxic Gases
If you use nitrogen as the inert gas, toxic cyanogen gas (CN)2 will be produced when the
furnace temperature is above 2300 °C.
• Make sure that the main laboratory fume ventilation system removes all gases and
fumes emitted by the furnace.

dansk Advarsel: Giftig forbrændingsgas


Ved anvendelse af kvælstof som inertgas dannes der giftig dicyan (CN)2 ved
ovntemperaturer over 2300 °C.
• Forvis Dem om, at hoved-udsugningsanlægget udsuger de forbrændingsgasser, som
emitteres af ovnen.

Deutsch Warnung: Giftiges Abgas


Bei Verwendung von Stickstoff als Inertgas bildet sich bei Ofentemperaturen über
2300 °C giftiges Dicyan (CN)2.
• Es muß sichergestellt sein, daß die aus dem Graphitofen austretenden Abgase von
der Haupt-Absauganlage sicher abgesaugt werdenΚ

español Advertencia: Gases tóxicos


Si se utiliza nitrógeno puro como gas inerte, al aumentar la temperatura del horno por
encima de 2300 °C se producirá gas cianógeno (CN)2, que es tóxico.
• Cerciórese de que el sistema principal de extracción de humos elimine todos los
gases y humos emitidos por el horno.

français Danger: Gaz toxiques


Si de l'azote est utilisé comme gaz inerte, du gaz cyanogène (CN)2 toxique se forme
lorsque la température du four dépasse 2300 °C.
• Vérifier que le système principal d'extraction des fumées élimine tous les gaz et
fumées émis par le four.

0993-5259 6-17
Translations of Warnings

=Warning (continued) W6.1

italiano Pericolo: Gas tossici


Se usate l'azoto quale gas inerte allora, quando il forno raggiunge temperature al di sopra
di 2300 °C, si formerà del gas cianogeno tossico (CN)2.
• Assicuratevi che l'impianto principale di estrazione fumi del laboratorio elimini tutti i
gas e le esalazioni emesse dal forno.

Nederlands Waarschuwing: Giftig afvoergas


Bij gebruik van stikstof als inertiegas wordt bij een oventemperatuur van meer dan
2300 °C het giftige dycyaan (CN)2 gevormd.
• Zorg ervoor dat alle gassen en dampen die uit de grafietoven komen, door de
hoofdafzuiging worden afgezogen.

português Aviso: Gás de escape venenoso


Ao utilizar nitrogénio como gás inerte a uma temperatura de forno superior a 2300 °C,
forma-se cianeto (CN)2 venenoso.
• Assegure-se de que os gases de escape que saem do forno são seguramente
aspirados pelo sistema exaustor principal.

suomea Varo: Myrkylliset kaasut


Jos käytät inerttikaasuna typpeä, syntyy myrkyllistä syaanikaasua (CN)2 , jos uunin
lämpötila on yli 2300 °C.
• Varmistu siitä, että laboratorion savunpoistojärjestelmä poistaa kaikki uunista lähtevät
kaasut ja savukaasut.

svenska Varning: Giftiga gaser


Om kväve används som inert gas bildas en giftig cyangas (CN)2 när ugnstemperaturen
överstiger 2300 C.
• Se till att utsugssystemet suger ut alla gaser och ångor som avges i ugnen.

6-18 0993-5259
Translations of Warnings

W9.1
Warning: Moving Parts – Risk of Injury
Some moving parts of the instrument are accessible in normal operation.
• Keep hands, clothing and other objects away from the moving parts of the instrument.
dansk Advarsel: Bevægelige dele – Fare for kvæstelser
Nogle af apparatets bevægelige dele er tilgængelige ved normal betjening.
• Hold hænder, tøj og andre genstande borte fra apparatets bevægelige dele.
Deutsch Warnung: Bewegliche Teile – Verletzungsgefahr
Bei normalem Betrieb sind bewegliche Teile des Geräts zugänglich.
• Hände, Kleidung und andere Gegenstände von den beweglichen Teilen des Geräts
fernhalten.

español Advertencia: Peligro mecánico


Algunas de las partes móviles del aparato son accesibles durante su funcionamiento
normal.
• Mantenga las manos, la ropa y otros objetos alejados de las partes móviles del
equipo.

français Danger: Parties en mouvement – Risque d'accident corporel


Certaines parties en mouvement de l'instrument sont accessibles en fonctionnement
normal.
• Tenir les mains, vêtements et autres objets éloignés des parties en mouvement de
l'instrument.

0993-5259 6-19
Translations of Warnings

=Warning (continued) W9.1

italiano Pericolo: Parti in movimento – Pericolo di infortunio


Alcune delle parti in movimento dello strumento sono accessibili anche durante il normale
funzionamento.
• Tenete le mani, gli indumenti e altri oggetti lontano dalle parti in movimento dello
strumento.

Nederlands Waarschuwing: Bewegende delen – Verwondingsgevaar


Sommige bewegende delen van het instrument kunnen aangeraakt worden tijdens de
normale werking.
• Handen, kleding en andere voorwerpen uit de buurt van de bewegende delen van het
instrument houden.

português Aviso: Peças móveis – perigo de ferimento


Algumas peças móveis do aparelho podem ser acedidas durante o funcionamento
normal.
• Mantenha afastados das peças móveis do aparelho as mãos, o vestuário e outros
objectos.

suomea Varo: Liikkuvat osat – loukkaantumisvaara


Muutamiin laitteen liikkuviin osiin on mahdollista päästä käsiksi normaalikäytön aikana.
• Pidä kädet, vaatteet ja muut esineet loitolla laitteen liikkuvista osista.
svenska Varning: Rörliga delar – risk för skador
En del rörliga delar på apparaten är åtkomliga vid normal användning.
• Se till att händer, kläder eller andra föremål inte kommer i närheten av apparatens
rörliga delar.

6-20 0993-5259
Index

0993-5259 In-1
Index

In-2 0993-5259
Index

A installing 2-5 C
installing a new pipet 3-49
aligning autosampler arm 2-17 changing fuses
installing sample tray cover
alignment controls cooling system 3-37
2-11
autosampler 2-18 changing graphite contacts 3-19
installing sample trays and
argon 5-8 containers 2-11 checking valves 3-41
atomizer maintenance 3-38 checklist
selecting 2-14 mass 5-25 autosampler maintenance 3-5
atomizer compartment door operating cycle 5-24 cooling system maintenance
raising and lowering 2-3 parts provided 4-6 3-4
removing and refitting 2-4 pumps 5-21 furnace maintenance 3-4
autosampler removing from spectrometer cleaning
adjusting immersion depth in 2-6 furnace windows 3-33
sample cup 2-21 removing rinse pump valves graphite contacts 3-14
adjusting penetration depth in 3-42 graphite tube 3-14
graphite tube 2-17 repairing a pipet 3-47 pump heads 3-44
aligning autosampler arm 2-17 replacement parts 4-7 valves 3-44
aligning pump heads 3-52 replacement pump parts 4-8 closing the furnace 3-12
alignment controls 2-18 rinsing solutions 2-16, 3-40
closing the furnace after contact
alignment procedures 2-17 sample and reagent containers
change 3-31
checking penetration depth in 5-23
controlling the autosampler 5-23
graphite tube 2-19 sample cups and reagent con-
tainers 2-12 cooling system (recirculating)
checking valves 3-41
sample table 5-21 changing the fuse 3-37
connecting drain tube and
setting up 2-15 to 2-23 description 5-11
waste bottle 2-10
types of sample tray 2-11 dimensions 5-20
connecting rinse feed tubes and
unlocking autosampler arm emptying 3-34
rinse bottle 2-8
2-17 maintenance 3-34
controlling 5-23
valve maintenance 3-39 mass 5-20
design 5-21
viewing inside graphite tube power requirements 5-20
dimensions 5-25
during alignment 2-18 refilling 3-36
electrical protection 5-25
weight 5-25 safety and EMC standards
environmental requirements
5-20
5-25 autosampler maintenance
technical data 5-20
filling the rinsing system 2-15 checklist 3-5
weight 5-20
fitting to spectrometer 2-6
flushing the rinsing system B cooling the furnace system 5-11
2-15, 3-39 background correction correct use of the instrument 1-3
flushing the valves 3-39 signal measurement 5-17 customer service – see end page
IEC 1010 compliance 5-25 Zeeman 5-12 cyanogen 5-8

0993-5259 In-3
Index

D opening 3-10 H
opening for contact change
dimensions heating
3-20
cooling system 5-20 furnace 5-7
principle of heating 5-3
furnace autosampler 5-25 maximum power 5-7
programs 5-18
time-controlled 5-7
E safety and EMC standards
electrical protection 5-19
5-19 I
safety features 5-19
autosampler 5-25 immersion depth of pipet tip in
technical data 5-18
electromagnetic compatibility sample cup 2-21
tilting in and out 3-6
5-19, 5-20 inert gas 5-8
viewing inside graphite tube
emptying the cooling system argon 5-8
2-18
3-34 nitrogen 5-8
windows
external protective gas flow 5-10 cleaning 3-33 inserting the graphite tube 3-12
furnace cooling 5-11 installing the autosampler 2-5
F internal purge gas flow 5-10
furnace heating
ferrules principle 5-3
fitting 3-46 L
furnace technique
filling the autosampler rinsing literature on electrothermal atom-
setting up 2-13
system 2-15 ization 5-26
fuses
fitting autosampler to spectrome- lowering the atomizer compart-
cooling system 3-37
ter 2-6 ment door 2-3
fitting ferrules 3-46 G
flushing the autosampler 2-15,
M
gas purging system 5-8
3-39 maintenance
gas requirements, furnace 5-18
autosampler 3-38
furnace graphite components autosampler valves 3-39
closing 3-12 replacements 4-4 checklists 3-4
closing after contact change
graphite contacts cooling system 3-34
3-31
changing 3-19 furnace 3-14
design 5-3
cleaning 3-14 maintenance position
gas requirements 5-18
tools 3-19 dual-atomizer systems 3-6
gas system, description 5-8
graphite tube furnace systems 3-8
heating 5-7
cleaning 3-14 mass
maintenance 3-14
inserting 3-12 autosampler 5-25
maintenance position
removing 3-10 cooling system 5-20
dual-atomizer systems 3-6
temperature control 5-7
graphite furnace systems matrix modifier 4-5
3-8 maximum power heating 5-7
temperature control 5-7

In-4 0993-5259
Index

N R sample tray cover


installing 2-11
nitrogen 5-8 raising the atomizer compartment
safety information 5-8 door 2-3 sample trays 2-11
normal gas 5-8 ramp time 5-7 selecting the atomizer 2-14
reagent containers 2-12 setting up
O refilling the cooling system 3-36
for furnace 2-13
opening the furnace 3-10 setting up the autosampler
refitting the atomizer compart-
for contact change 3-20 2-15 to 2-23
ment door 2-4
signal measurement
P regulatory information
using Zeeman backround cor-
penetration depth of pipet tip in electromagnetic compatibility
rection 5-17
graphite tube 2-17, 2-19 5-19, 5-20
special gas 5-8, 5-10
pipet removing autosampler from spec-
trometer 2-6 STPF concept
installing 3-49
removing the atomizer compart- maximum power heating 5-7
repairing 3-47
ment door 2-4 zero gas flow 5-10
pipet tip
immersion depth in sample cup removing the graphite tube 3-10 T
2-21 repairing a pipet 3-47 technical data
penetration depth in graphite replacement parts cooling system 5-20
tube 2-17, 2-19 autosampler 4-7 furnace 5-18
power requirements autosampler pumps 4-8 furnace autosampler 5-25
cooling system 5-20 furnace components 4-4 temperature control
pump heads graphite components 4-4 of the graphite tube 5-7
aligning 3-52 replacing fuses tilting the furnace
cleaning 3-44 cooling system 3-37 dual-atomizer systems
pumps on the autosampler 5-21 to tilt furnace in 3-7
purge gas 5-10
S to tilt furnace out 3-6
safety furnace spectrometer systems
Q correct use of the instrument to tilt furnace in 3-9
quartz tube atomizer (QTA) 3-8 1-3 to tilt furnace to install a
safety and EMC standards 5-19, QTA 3-8
5-20 to tilt furnace to mainte-
safety information nance position 3-8
cyanogen 5-8 time-controlled heating 5-7
nitrogen 5-8 tools for graphite contacts 3-19
sample cups 2-12 troubleshooting 3-3

0993-5259 In-5
Index

U W
unlocking autosampler arm 2-17 warning markings 1-4
weight
V autosampler 5-25
valves cooling system 5-20
assembling and installing 3-44
checking 3-41 Z
cleaning 3-44 Zeeman effect
maintenance 3-39 description 5-12
removing from rinse pump
3-42
viewing inside graphite tube 2-18

In-6 0993-5259

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