Aa83321-06 Ref Man PDF

ARL 3460
Reference Manual
AA83321
REFERENCE MANUAL
ARL 3460
Report MANUAL
No AA83321-06
Language E
Date April 2005
Department Doc
Author RTh
AA83321-06
The information in this document is subject to change without
notice.
We assume no responsibility for any errors that may appear
in this document.
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Information gendert werden.
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in diesem Dokument.
Les informations contenues dans ce document sont sujettes

changement sans pravis.
Nous nassumons aucune responsabilit pour toutes erreurs
ventuelles contenues dans ce document.
Ci riserviamo il diritto di modificare le informazioni contenute

nel presente manuale senza preavviso e non ne assumiamo
nessuna responsabilit quanto ad eventuali errori che
potrebbero esservi accidentalmente introdotti.
Las informaciones contenidas en este documento pueden

ser modificadas sin previo aviso.
Nosotros declinamos toda responsabilidad sobre los
eventuales errores contenidos en este documento.
AA83321-06
PAGE DE MODIFICATION
NDERUNGSANGABEN
REVISION CONTROL SHEET
Date Modification Description

Datum nderung Beschreibung
Date Revision Description
1996
October 00/RTh Creation. Valid from 3460 - 2000, MA - 050 or 2460 -
500
1997
June 01/RTh Updated according to OM3081, 3100, 3101 and WinOE
V2.0-1.
December 02/RTh Updated according to OM3186
1999
August 03/RTh Updated according to OM3322, 3344, Hot-Line OE-92.
2000
December 04/RTh Updated according to OM3401, 3423.
2002
February 05/RTh Updated according to OM3503.
2005
April 06/RTh Updated according to OM3449, 3629, 3675, 3700, 3762,
3836, 3838, WinOE 3.2.
AA83321-06
TABLE OF CONTENTS
Table of Content
1. INTRODUCTION ........................................................................... 1-1
1.1 CONFORMITY TO STANDARDS ................................................. 1-2
1.2 SAFETY......................................................................................... 1-3

1.2.1 SPARES PARTS LABEL .................................................................................1-4
1.3 DOCUMENTATION....................................................................... 1-5

1.3.1 CUSTOMER DOCUMENTATION....................................................................1-5
1.3.2 SERVICE DOCUMENTATION.........................................................................1-6
2. SIMPLIFIED TECHNICAL DESCRIPTION ................................... 2-1
2.1 FUNCTION PRINCIPLE ................................................................ 2-1
2.2 STRUCTURE OF THE INSTRUMENT.......................................... 2-3
2.3 ANALYTICAL PROGRAM AND OPTICAL LAYOUT..................... 2-4
2.4 THE EXCITATION......................................................................... 2-5

2.4.1 THE SOURCE .................................................................................................2-5
2.4.2 THE STAND.....................................................................................................2-5
2.4.2.1 The Argon Stand..............................................................................................2-5
2.4.2.2 Stand Safety Circuit .........................................................................................2-6
2.5 THE SPECTROMETER ................................................................ 2-7
2.6 THE ELECTRONIC RACK ............................................................ 2-9
2.7 THE COMPUTER........................................................................ 2-11

2.7.1 COMPUTER CONFIGURATION ...................................................................2-11
2.7.1.1 Visual Display ................................................................................................2-11
2.7.1.2 Keyboard .......................................................................................................2-11
2.7.1.3 Mouse ............................................................................................................2-11
2.7.1.4 Central Unit ....................................................................................................2-12
2.7.2 PRINTER .......................................................................................................2-12
2.7.3 SOFTWARE...................................................................................................2-12
2.8 THE INTERCONNECTIONS ....................................................... 2-13
3. LAYOUT AND CONTROLS .......................................................... 3-1
3.1 CABINET, GENERAL VIEW.......................................................... 3-2
3.2 UNIT AND SUB-ASSEMBLIES ..................................................... 3-4
AA83321 Reference Manual - ARL 3460 I

Table of Content
3.3 STAND .......................................................................................... 3-9
3.4 HI-REP SOURCE ........................................................................ 3-14
3.5 POWER DISTRIBUTION RACK.................................................. 3-16
3.6 ELECTRONIC RACK .................................................................. 3-18
3.7 VACUUM PUMPING LINE .......................................................... 3-21

3.7.1 STANDARD SYSTEM FOR INTERMEDIARY VACUUM...............................3-21
3.7.2 SPECIAL SYSTEM FOR HIGH VACUUM .....................................................3-23
3.8 WATER COOLER ....................................................................... 3-25
3.9 ARGON CIRCUIT........................................................................ 3-26
3.10 OVEN AND SPECTROMETER ................................................... 3-28

3.10.1 COMMON ITEMS ..........................................................................................3-29
3.10.2 PARTICULAR ITEMS ....................................................................................3-34
3.10.2.1 Reflected beam..............................................................................................3-34
3.10.2.2 Direct beam....................................................................................................3-35
4. ROUTINE MAINTENANCE ........................................................... 4-1
4.1 FOREWORDS............................................................................... 4-1
4.2 APPLICATION DOMAINS OF PROCEDURES............................. 4-2
4.3 SUMMARY TABLE........................................................................ 4-3
4.4 ANALYSIS ELECTRODE .............................................................. 4-4

4.4.1 ELECTRODE EXCHANGE AND ADJUSTMENT ............................................4-5
4.5 CLEANING OF THE STAND AND THE SPARKING CHAMBER.. 4-6

4.5.1 CLEANING OF THE INSULATOR AND THE SPARKING CHAMBER ............4-6
4.5.2 CLEANING OF THE TABLE AND THE INSIDE...............................................4-7
4.5.2.1 Dismantling ......................................................................................................4-7
4.5.2.2 Cleanings .........................................................................................................4-7
4.5.2.2.1 Table's Block Support ................................................................................................................ 4-7
4.5.2.2.2 Electrode .................................................................................................................................... 4-7
4.5.2.2.3 Analysis Table............................................................................................................................ 4-7
4.5.2.2.4 Glass Insulator ........................................................................................................................... 4-8
4.5.2.3 Reassembling ..................................................................................................4-8
4.5.2.4 Remarks ..........................................................................................................4-8
4.6 ARGON OUTLET FILTER............................................................. 4-9

4.6.1 STANDARD SYSTEM......................................................................................4-9
II Reference Manual - ARL 3460 AA83321

Table of Content
4.6.2 VUV OPTION SYSTEM .................................................................................4-10

4.6.2.1 Intermediary Oil filter......................................................................................4-10
4.6.2.2 Argon Outlet Filter..........................................................................................4-10
4.7 VACUUM PUMPING LINE .......................................................... 4-11

4.7.1 STANDARD PUMPING LINE FOR INTERMEDIARY VACUUM....................4-11
4.7.1.1 Checking the Vacuum Pump Oil Level...........................................................4-11
4.7.1.2 Changing the Oil and the Vacuum Pump Gaskets.........................................4-12
4.7.2 SPECIAL PUMPING LINE FOR HIGH VACUUM ..........................................4-12
4.8 PROFILE CHECK........................................................................ 4-13

4.8.1 DIRECT (OR MANUAL) PROFILE.................................................................4-14
4.8.1.1 Basic Advice ..................................................................................................4-14
4.8.1.2 Direct Profile Taking.......................................................................................4-16
4.8.2 PROFILE BY INTEGRATION ........................................................................4-23
4.8.2.1 Basic Advice ..................................................................................................4-23
4.8.2.2 Measuring the Profile by Integration ..............................................................4-24
4.9 GREASING OF THE STAND DOOR'S HINGES......................... 4-30
4.10 LENS CLEANING........................................................................ 4-30

4.10.1 LENS HOLDER EXTRACTION......................................................................4-30
4.10.2 CLEANING.....................................................................................................4-31
4.11 CHANGING OR CLEANING OF THE DUST FILTERS ............... 4-32
4.12 CHECK OF THE CABINET FANS............................................... 4-33
4.13 ANALYTICAL CHECKS............................................................... 4-33

4.13.1 CONTROL SAMPLE......................................................................................4-33
4.13.2 STANDARDISATION .....................................................................................4-33
4.14 BACKUP...................................................................................... 4-33
4.15 ACCESSORIES........................................................................... 4-34

4.15.1 SIRCAL ARGON PURIFIER ..........................................................................4-34
A. SAMPLE PREPARATION ............................................................A-1
A.1 SAMPLE TAKING - MOULDS ....................................................... A-2

A.1.1 NON FERROUS METALS .............................................................................. A-2
A.1.2 FE, NI, CO BASES ......................................................................................... A-2
A.1.3 CAST IRONS .................................................................................................. A-3
A.1.4 TRACES ......................................................................................................... A-3
AA83321 Reference Manual - ARL 3460 III

Table of Content
A.1.5 SPEMIS PROBE............................................................................................. A-4
A.2 SURFACE PREPARATION - SAMPLE PREPARATION

MACHINES.................................................................................... A-5
A.2.1 DISK SANDER................................................................................................ A-5
A.2.2 SURFACE GRINDER ..................................................................................... A-6
A.2.3 MILLING MACHINE OR LATHE ..................................................................... A-6
A.2.4 PRESS MACHINE .......................................................................................... A-7
A.2.5 INDUCTIVE FURNACE .................................................................................. A-7
B. PLACING THE SAMPLE ON THE ANALYTICAL TABLE ...........B-1
B.1 PUTTING THE SAMPLE ............................................................... B-1
B.2 MULTIPLE MEASUREMENTS...................................................... B-2
B.3 SAMPLE STOP ............................................................................. B-3
C. SPECIAL PROCEDURES.............................................................C-1
C.1 MAGNESIUM ALLOY MATRIX .....................................................C-2

C.1.1 GENERAL CONSIDERATION ........................................................................ C-2
C.1.2 WORKING CONSTRAINTS............................................................................ C-2
C.1.3 PARTICULAR EQUIPMENT AND TOOLS ..................................................... C-2
C.1.4 PARTICULAR PROCEDURES ....................................................................... C-3
C.1.4.1 Stand and Special Filtering Device Maintenance............................................ C-3
C.1.4.2 Cleaning of Stand Components ...................................................................... C-3
C.1.4.3 Other Subjects ................................................................................................ C-4
IV Reference Manual - ARL 3460 AA83321

1
INTRODUCTION
Introduction Chapter 1
1. INTRODUCTION
This is the ARL 3460 Reference Manual; additionally to the Operator Manual, you will find here more
details about the instruments functionality and some operations that are not part of routine analysis. You
will find the following subjects:
Chapter 1: The references to other technical documents supplied with the instrument, as well
as important instructions concerning the safety and the conformity to the
international standards.
Chapter 2: An introduction to the spectroscopy and a simplified technical description of the
instrument.
Chapter 3: A description of units and sub-assemblies contained in the ARL 3460, with in-
structions concerning some handling and controls.
Chapter 4: The list of routine maintenance operations, as well as the corresponding
procedures and the recommended frequency.
General comment
This manual, and its pictures, stands for an ARL 3460 in the most usual configuration
sold. Illustrations and drawings may therefore show noticeable differences with the
configuration of your own instrument.
The VUV option is more detailed in a separate manual.
AA83321 Reference Manual - ARL 3460 1-1

Chapter 1 Introduction
1.1 Conformity to standards

Our instruments are developed according to the most common international standards.
We declare the ARL 3460 instrument conforms with the following standards:
EN292-1,-2 (1991) Safety of machinery: basic concept

EN60204-1 (1984) Electrical equipment of industrial machines.
EN60947-1 (1991) Low voltage switchgear and controlgear.
CEI1010-1 (1990) Safety requirements for electrical equipment for measurement, regu-
lation and laboratory use.
CEI 950 (1986) Safety of information technology equipment.
EN50081 (1992) Electromagnetic compatibility: generic emission standard
EN50082 (1993) Electromagnetic compatibility: generic immunity standard
This according to European directive provisions:
89/392/CEE Machinery.
73/23/CEE Low voltage.
89/336/CEE Electromagnetic compatibility
1-2 Reference Manual - ARL 3460 AA83321

1.2 Safety
As we declare it in the previous section, the instrument conforms to the CEI1010-1 safety standard.
The only two areas where an ill-advised operator could access to hazardous voltage by a simple manual op-
eration are protected by safety contacts ("forced opening") that switches off the power supply of the con-
cerned areas.
The other inside parts of the instrument, around or into which ones hazardous voltage may exist, can be ac-
cessed only by the mean of a tool. Although the power supplies are closed or protected, and the wires ade-
quately insulated, a little electrocution risk can remain around these components. The hazardous modules, or
the accesses to them, are mentioned with the danger label:
Risk of electrocution
Non qualified personnel should never approach

these modules when the instrument is powered.
Only our Service Engineers, or your maintenance technicians advised

and trained by our care should approach these modules, with the custom
precautions when they are under power.
Switch off the power before removing this panel or part.
Figure 1.1
Also some modules can be labelled with the attention sign:
Warning!
This label points out if there is a risk to affect the

alignment of the concerned module in case of a wrong
handling.
Follow exactly the procedures described in this manual when operating

around or inside this module.
Figure 1.2
The routine maintenance procedures (for example the profile taking) that require the operator to execute an
operation around or inside such a module are clearly described in the Maintenance chapter of this manual. If
they are scrupulously followed, the alignment and the calibration of the instrument will not be affected.
Furthermore the handlings indicated in the procedures do not expose the operator to hazardous voltage and
electrocution risk.

1.2.1 Spares Parts Label

Some spare parts are marked with a blue label containing the following text:
This component was developed and tested by Thermo Electron to comply with our instrument's technical
specifications in order to guarantee and maintain analytical performances as well as safety standards.
For safety reasons, this part must be provided only through Thermo distribution companies. Any attempt to fit a
part provided by another supplier than Thermo Electron may result in damages and loss of performances, and
thus render Thermo Electron warranty and responsibility void.
Figure 1.3
These parts have been modified by Thermo Electron, or our supplier is manufacturing this part especially
dedicated for our applications. Replacement by a similar part from another supplier may damage the instru-
ment as well as to deteriorate the performances. Therefore a part marked with such a label can only be re-
placed by an equivalent one supplied by the Thermo Electron distribution network.
Thermo Electron declines any responsibility in the event of attempting the replacement of a part
by another one, which is not provided by the Thermo Electron distribution network, and conse-
quently the guarantee of the instrument will become void.

1.3 Documentation
The instrument documentation is composed by several manuals, lists, catalogues, drawings, schematics, etc.
They are split into two distinct documentation sets:
The documents intended for the operator and the laboratory personnel, as well as for your maintenance
technicians. We call this basic documentation, supplied as standard with each instrument, "Customer
Documentation". See thereunder Customer Documentation.
The documents intended for our Service Engineers and of our Distributors and agreed Agents. This
reserved documentation is called "Service Documentation"; it is not supplied as standard with the in-
strument. See thereunder Service Documentation.
1.3.1 Customer Documentation

The Reference documentation of the instrument is composed by:
SUBJECT CONTENT / USE

A set of catalogue sheets Component or part number and name identification.
The Operator Manual Start-up and routine operations on the instrument.
The Reference Manual References to other documents, simplified technical description, con-
trols and sub-assemblies' description, routine maintenance operations,
troubleshooting. It is this manual!
The Vacuum Pump Manual Operating and maintenance. It is the manual of the pump manufacturer.
The possible Option Manuals Description and use of the concerned option.
An electrical diagrams set Troubleshooting.
Additionally, you will find the specific documentation of the application software, that are the WinOE
Configuration Manual, the WinOE Operator Manual, as well as manuals of software options, if applicable.
Apart from the WinOE software, the remaining computer software and hardware is not manufactured by
Thermo Electron. For all these modules (software and hardware) you will find the documentation supplied
by the manufacturer(s) in their original packing.
Optional accessories (for example: sample preparation machine, voltage stabiliser, etc.) can be delivered with
the instrument. In such a case, a documentation is also supplied for those options.

1.3.2 Service Documentation

As said above, this documentation does not belong to the standard documentation supplied with our instru-
ments. These documents are intended to be used by our Service Engineers and those of our Distributors and
agreed Agents.
The understanding of the content of these documents requires a strong technical basic knowledge as well as
practical experience on our instruments.
These documents are usually available in English only, but some of them may be available in French.
They are:
SUBJECT CONTENT / USE

A supplementary set of catalogue sheets Component or part number and name identification.
The ARL 3460 Technical Description Detailed technical description.
Manual
The TICS software Troubleshooting and test software.
The Tool list Recommended tools for troubleshooting and miscellaneous
jobs.
IMPORTANT:
The information in the documentation was true at the time of printing, but
could include technical inaccuracies or typographical errors. Thermo
Electron assumes no responsibility for any errors that may appear in the
Service documentation set described above.
As well the responsibility of Thermo Electron cannot be engaged in the case

of the use of this documentation by non qualified people and not agreed by
Thermo Electron. This is valid for the injury to persons as well as for mate-
rial damage to the instrument that may result in a financial loss to the busi-
ness user of the instrument.

2
SIMPLIFIED TECHNICAL
DESCRIPTION
Chapter 2 Simplified Technical Description
2. SIMPLIFIED TECHNICAL DESCRIPTION
2.1 Function Principle

The ARL 3460 is a simultaneous Quantometer. This means the instrument measures the intensity of several
spectral lines simultaneously in the light emitted by the sample, when the atoms that compose it are exited by
an external energy source. The analysed light is located approximately into the 130 nm to 800 nm
wavelength range.
The whole measuring system is therefore based on the physical phenomenon that is summarised as follows:
When a certain energy is applied to an atom, some of its electrons change their orbit. When these electrons
return to their initial orbit, a precise energy is restored in the form of a light at a determined wavelength. This
is an atomic phenomenon, and consequently it is practically unaffected by the chemical or crystalline form of
the atom. This means the instrument can determine, for example the quantity of silicon in a steel; but will not
give information about the form under this silicon is to be found. The figure 2.1 gives a rough representation
of this excitation.
Excitation of an atom Emission of photon of

c
wavelength : E2 - E1 = h = h
Supplied energy +E
+4 +4 +4
Initial energy E1 Energy E2 Return to energy E1

Figure 2.1
A sample containing several different elements will therefore produce light composed of wavelength specific
to each of the elements. By separating these wavelengths by a dispersion system, we can determine which
elements are present, the intensity of each of these wavelengths being a function of the concentration of the
considered element. By measuring this luminous intensity (with a photomultiplier) and by processing this
information with a digital analogue converter and a computer, we can thus determine the concentration of the
considered element.

Simplified Technical Description Chapter 2
An instrument that allows such analysis is therefore composed of the four following parts (figure 2.2):
1) A source of excitation which supplies energy to the samples.
2) A dispersion device which discriminates the different wavelengths.
3) Electronics which measure the luminous intensity of each of the wavelengths.
4) A computer which processes the measurements and controls the instrument.
2
Spectrometer
3 4
1
Computer
Excitation Electronics
Figure 2.2

2.2 Structure of the Instrument
3
1 Stand
2 Oven cover (spectrometer in-
side)
2 3 Keyboard support
(detachable)
11 4 230 VAC mains distribution
10 5 Source
1 6 Electronic rack
15 7 Watercooler
8 Argon filter
9 -
4 10 Access to the scanning screw
6 5
Figure 2.3
11 Multimeter (for vacuum and

profile check)
12 Input RS232
2 13 Dust filter (fan inside)
1
14 230 VAC output sockets (for
computer and peripherals)
15 13 15 Argon inlet
13 16 230 VAC mains input
12 8 17 Vacuum pump
4 18 18 Vacuum pipe
14 7
16 17
Figure 2.4

2.3 Analytical Program and Optical Layout

Each instrument is different to another one of the same model, at least by its analytical program (spectral
wavelengths installed according to specific application of each customer); the optical layout is a workshop
document elaborated on the basis of the analytical program.
The useful information for the operator (analytical program, optical layout, etc.) is to be found in the first
pages of the QC/QA/Calibration report, between them:
The channel number (the same for the attenuator also) and the spectral line used for a chemical element.
Incidentally, it can also be important to know the sensitivity of the photomultiplier used for this line. This
information is shown in the "Pmt" columns of the optical layout. The sign -1 corresponds to the less
sensitive photomultiplier and the -3 sign to the most sensitive photomultiplier.
Depending of the type of grating installed, some of the spectral lines are seen in higher order (order 2, 3,
4). This information is shown in the "A line" column.
In the case where a line is measured in a higher order, selecting filters are placed in front of the
photomultiplier. Those filters are indicated in the "Filt" columns, and the relevant information concerning
those filters is shown in the "Interference filter" table of the first page of the optical layout.

2.4 The Excitation

The excitation is composed by two distinct parts:
The source (or generator)

The stand
The source, called Hi-Rep 2+, is located in the right bay of the instrument (see figure 2.3, position 5). The
source is linked to the stand through a high voltage wire and a signal cable. The stand is called MBS201I and
contains the igniter of the source, protected inside a Faraday cage.
2.4.1 The Source

The analysis is done by creating a low voltage arc between the surface of the sample to be analysed and a
counter electrode. The sparking energy is supplied by a generator called the "SOURCE".
The source into the ARL 3460 is a classical source of the RLC discharge type and its frequency can rise up
to 400 Hz. Our Analytical Specialists have looked for the best analytical conditions for each of the material
types to be analysed. Our sources are delivered with a certain number of conditions already pre-programmed
and optimised for the various matrix required by the customer.
The various available pre-programmed source conditions are indicated in the first pages of the
QC/QA/Calibration report.
The selection procedure of one or more of these conditions is explained into the WinOE Configuration
Manual.
A more detailed technical description can be found into the manual Technical Description ARL 3460. This
description is however meant for our Service Engineers.
2.4.2 The Stand

The purpose of the stand is to place the sample in a reproducible way relatively to the optical device located
into the spectrometer.
2.4.2.1 The Argon Stand
To avoid any interaction between the air atmosphere and the sample surface, the discharge is made in a
sparking chamber under argon atmosphere. The stand therefore constitutes an enclosure in which an argon
flow circulates.
The energy dissipated by the sparks heats the sample and the table on which it is placed. The table is cooled
by a closed water cooled circuit. This device is composed of a water pump, a tank, and flexible pipes for
bringing the cooled water to the analytical table. The separation between the spectrometer under vacuum and
the stand under argon is made by an airtight lens, which can be removed for cleaning without breaking the
spectrometer vacuum.
During an analysis, two types of sparks are usually created. During a given time, a high energy spark is pro-
duced in order to prepare (melt and homogenise) the sample surface. Then a lower energy spark is produced,
and the light emitted at this time is measured. In order to avoid the photomultiplier dazzling during the first
phase, and also to prevent to make the lens dirty with particles extracted from the sample, a shutter remains
closed. This shutter is opened during the measuring phase by an electromagnetic valve.

The argon system that supplies the stand is built so as to allow a small argon flush to circulate permanently
around the stand and the sparking chamber, even if the instrument is not running an analysis. The stand-by
flow is fixed to about 0.2 - 0.5 l/min. During sparking, this flow is automatically increased. The relation be-
tween the stand-by flow and the analytical flow is fixed by restrictors and cannot be altered.
2.4.2.2 Stand Safety Circuit
The safety circuit protects the operator and the instrument. It is not possible to perform an analysis when the
stand door is open. This circuit conforms with the international norm CEI 1010-1.

2.5 The Spectrometer

The spectrometer is the mechanical housing that contains the optical dispersion system. The geometry of this
system has to be stable in order to guarantee the analytical performances of the instrument. The spectrometer
itself is placed into a controlled thermo insulated cabinet called oven (at 38 0.1 C) in order to avoid any
deformation by dilatation. The temperature adjustment is achieved by a heating device whose switching is
controlled by a temperature sensor. A certain equilibrium is thus achieved between the heat lost from the
enclosure in the ambient air and the heat produced by the heating device.
The light path into the spectrometer is approximately 2 meters long. As air will absorb ultraviolet light, it is
necessary to put the spectrometer under vacuum to avoid this effect.
The vacuum system is composed of a pumping line, a manual aeration valve for the spectrometer and a vac-
uum gauge.
For the VUV option, the high vacuum pumping line is composed of a dry membrane pump after which a mo-
lecular pump is connected. Such a clean vacuum system allows the vacuum working pressure into the spec-
trometer to reach 10-4 mbar.
In the other case (normal UV only) the pumping line consists of a classical blades vacuum pump. This latter
includes an anti suck back device that allows to stop the pump and prevents oil from returning into the spec-
trometer.
The manual aeration valve is used to fill the spectrometer with air when it must be opened. The Pirani gauge
(thermo-couple) permits to measure the vacuum level.
The lens is heated to avoid condensation, and to prevent oil vapour deposit a small air flow is introduced into
the spectrometer (the oil vapour particles will be dragged by the air flow and sucked by the pump). This air
flow is to be adjusted by a pin-valve in order to keep a vacuum at around 50 mHg / 0.05 Torr. The pin-
valve should be closed when the pump is stopped. With the high vacuum system (VUV option) the air leak
must be suppressed by closing permanently the pin-valve.
The optical system is composed of five main parts: the primary slit, the grating, the secondary slits, the mir-
rors and the photomultipliers.
The primary slit is to be considered as the object in terms of optical geometry, each spectral line is an image
of that slit. It has 20 m width. The grating has a dual feature: it diffracts the light and focuses it on the sec-
ondary slits. The grating is a spherical mirror (to focus) marked with extremely thin and narrow grooves
(2160, 1080 and 1667 grooves/mm), which does the diffraction.
The secondary slits (around 20 to 150 m width) constitute the mask that lets only narrow wavelength bands
to pass. The slits are fixed to the slit frame holder and an eccentric axle allows to adjust very precisely their
position (to 2 m). The light going through the slit is reflected by a mirror that focuses on the photomulti-
plier.
The photons (light) hit the photomultiplier's photocathode and extract electrons from it. These electrons are
captured by the electric field existing between the dynodes of the tube, and then they hit again one of these
dynodes, extracting again more electrons. These electron sets are multiplied from dynode to dynode and
reach finally the tube's anode. All electron sets reaching the anode constitute the current to be measured. A
serial resistor network fixes the potential of each dynode.
The primary slit, the grating and the secondary slits are located on a circle; this is a necessary condition to
obtain a proper focus on the secondary slits.

The wavelength crossing each secondary slit depends on the angle formed by the incident beam and the dif-
fracted beam of the grating. The grating curvature is aligned on this circle.
Concave
grating
Photomultiplier
Concave
mirror
Secondary
Ro
la
w
nd slits
cir
cle
Primary
slit
Light from the stand
Figure 2.5
By moving the primary slit on the Rowland circle, the wavelength crossing a fixed secondary slit on the
circle is modified. This is how the instrument is profiled, i.e. the position of the primary slit is adjusted so
that a given wavelength passes through a given secondary slit. This can be achieved, of course, only if
relative position between each of the secondary slits is absolutely correct. The primary slit can be manually
driven from the exterior of the spectrometer by a micro metrical screw called the "scanning screw".

2.6 The Electronic Rack

The electronic rack contains all the necessary circuit for the communication between the computer and the
spectrometer. The C-MOS technology is used for the control and interface cards.
The principle is based on control by a microprocessor connected to the main computer. This microprocessor
needs an adaptation card to manage the various readout lines, the stand and the source signals.
The low voltage power supplies are produced by two separate modules, one for the +24 VDC, and another
one for the +5 VDC and the 12 VDC.
The rack dimensions are normalised according to the "Europa rack" type. The boards and modules of this
rack are:
The ICS34B; this sandwich module contains two boards, the MMB88 microprocessor board, and the
adaptation board; this assembly is the brain of the instrument.
The converter and counter boards for the measure of the signals. One card contains six channels. It is pos-
sible to install up to ten IVFC cards.
The Vacuum and Profile board. This board allows the analogue display of the vacuum value or the ana-
logue display of the profile of one channel. Both can be watched on the multimeter on the front of the in-
strument roof.
The Status board; it allows the reading of a certain number of check points, tied to the good operation of
the instrument.
An optional Dual Attenuator Control board can be found too.
The Low Voltage Power Supplies (LVPS) are located at the back of the rack. They power the
instrument's electronics, except the excitation (source and stand).
The High Voltage Power Supply (HVPS) is also located at the back of the rack. The photomultipliers are
polarised at -100 V and power by -1000 V through attenuator circuits (resistor networks).

To external Vacuum
ICS34B Internal bus
Computer and Profile
(ACS)
Signals
cable
Status
Stand and
Source
Reserved for ex-

tension (not used)
Spectrometer
IVFC
and PMT's Light from
Stand
HVPS LVPS
Figure 2.6
A more detailed technical description can be found into the manual Technical Description ARL 3460. This
description is however meant for our Service Engineers.

2.7 The Computer

The computer fulfils two different tasks:
The instrument control on one end and the calculation of the concentration on the other end.
All data information exchanged between the computer and the instrument is driven on a RS232 serial line
type. Data reach directly the instrument's microprocessor that processes it. Analytical results are transmitted
from the microprocessor to the computer in the same way.
2.7.1 Computer Configuration

The computer is usually composed by the following main modules:
the central unit

the visual display (screen)
the keyboard
the mouse
Figure 2.7
A printer is normally connected to the central unit.
2.7.1.1 Visual Display
The colour screen displays the dialogue between the operator and the computer; the results of the analysis
will also be shown on this screen.
2.7.1.2 Keyboard
The keyboard permits the operator to dialogue with the computer, and to enter the particular data to the
application software.
2.7.1.3 Mouse
Most of software programs are designed to accept command or parameter inputs through a mouse, which
can replace a certain number of operations normally done through the keyboard.

2.7.1.4 Central Unit
The central unit itself is usually composed by the following sub-assemblies:
the motherboard, including computer system microprocessor (the true brain of the system); the mother-
board also contains a part of the memory, interfaces and input/output ports for the screen, the keyboard,
the mouse, as well as a serial port (for the instrument) and a parallel port (for the printer).
the additional memory of the computer system.
one floppy disk reading unit, and its interface.
one hard disk reading unit, and its interface.
one CD-ROM reading unit, and its interface.
additional interfaces can also be found or been added, according to options bought with the equipment
(for example for options like COMPAC, NetARL, etc.).
Once the application software is loaded from floppies, it remains permanently into the hard disk; the micro-
processor manages and load, if necessary, parts or routines of the application software into the memory.
The computer start-up and loading procedures are explained in both the instruments Operator Manual and
the WinOE Software Configuration Manual.
2.7.2 Printer
Normally a parallel printer is connected on the input/output port of the central unit.
The utilisation and routine maintenance of this printer (ribbon or paper exchange, etc.) are explained in the
printer operating manual.
2.7.3 Software
The software contains all necessary information to control the instrument, to perform analysis or function
tests, as well as to treat results received from the instrument. Options like NetARL, COMPAC, etc., allow to
transmit results to other remote units or systems.
The standard application software supplied with the instrument is named WinOE.
The manuals delivered with the software (and the option's ones if applicable) should give you all necessary
information for its loading procedure, its utilisation, and parameter input which will be particular for your
tasks.
If your instrument has been calibrated by ourselves, the installed software will already contain a certain
number of data (or parameter) files allowing you to proceed to routine analysis right after the end of the
instrument installation. In the other way round, it will be your job to create your own tasks and programs; in
that respect the WinOE Software Configuration manual should give you all necessary instruction for
entering data and parameters.

2.8 The Interconnections

See the detailed interconnections diagram in your technical documentation (diagram set). The 230 VAC
power distribution is summarised on the next figure.
Mains
230 VAC
Filter Fan
MAINS 16 A (left bay)
Source
FUSE
T 10 A Air Pulser
Water
Filter
WATER PUMP Cooler
Vacuum
VACUUM PUMP System
Auxiliary
LVPS
Plugs ELECTRONICS
HVPS
HVPS
Fan
(right bay)
Heating
Fans
(oven)
POWER
DISTRIBUTION
PANEL
Safety
Figure 2.8
By lifting the instrument top roof the safety switches off the photomultiplier's power supply, as well as the
heating and fans' power supply. This permits to access the attenuators and other oven items without
electrocution risk.

3
LAYOUT AND CONTROLS

Layout and Controls Chapter 3
3. LAYOUT AND CONTROLS

This section is a purely topographical description of the instrument. It is limited to those items, which the
user should be familiar under normal circumstances.
The items are identified by groups of numbers, which are shown in this section. The descriptions are grouped
by illustrations.
The text is subdivided into four following categories:
D description
U use (purpose and/or how to use, access)
C comment
M maintenance (not troubleshooting)
If a description is followed by an F!, a further description and figure exist.

Chapter 3 Layout and Controls
3.1 Cabinet, General View

The figures 3.1 and 3.2 show two of several alternatives for the arrangement of the complete equipment.
14 15 16 13 12 4 6 2 3 5 7
Figure 3.1
2 3 4 5
12
15 16
14 13
Figure 3.2

Key to figures 3.1 and 3.2:
D : System terminal with keyboard.
2 D : Computer (central unit).
3 D : Monitor for computer.

U : Display the dialogue between the operator and the software driving the instrument.
4 D : Keyboard for personal computer.

U : The operator uses the keyboard or the mouse to control the instrument.
5 D : Mouse for personal computer.

U : The operator uses the keyboard or the mouse to control the instrument.
6 D : Printer.
U : Prints analysis results or parameters of the analytical program.
7 D : Table holding the computer, monitor, keyboard and printer.
D : ARL 3460 instrument complete cabinet.
12 D : Stand door (F!). See also key figure 3.7.

C : Access to the analytical table (F!).
U : To open, simply push the handle to the right.
13 D : Right-hand front panel.

C : Access to the source (F!) and to the power supply distribution panel (F!).
U : For removal, either with an Allen key or a screwdriver with an Allen key head, unscrew partly
the four "camlock" screws accessible through the holes at the panel corners, lift a little bit the
panel and pull it towards you.
14 D : Left-hand front panel.

C : Access to the electronic rack (F!).
U : As above, pos. 13.
15 D : Lid.
C : Access to the thermo-controlled housing (oven) (F!), to the spectrometer (F!) and to the at-
tenuators (F!).
U : To open, either with an Allen key or a screwdriver with an Allen key head, unscrew suffi-
ciently the screw accessible by the hole, then simply lift from the front upwards. If the screw is
not enough unscrewed, it is not possible to lift the lid.
16 D : Support for keyboard (pos. 4).

C : Access to the control multimeter (F!) and to the scanning screw (F!).
U : To open, simply lift the support upwards.

3.2 Unit and Sub-Assemblies

Figures 3.3 to 3.6 show the different units and sub-assemblies that make up the instrument. Certain of these
sub-assemblies are described in further detail in the following paragraphs.
7 1
6
6
8
17
2
5
3
4
Figure 3.3
18
10
11 11
16 9
19
12 14
2
13
15
Figure 3.4

1 D : Stand. F!
2 D : Power distribution panel. F!

U : For access, remove the right-hand panel (figures 3.1 and 3.2, pos. 13) or open it from the back
of the instrument.
3 D : Electronic rack. F!
U : For access, remove the left-hand panel (figures 3.1 and 3.2, pos. 14).
4 D : Source rack.
U : For access, remove the right-hand panel (figures 3.1 and 3.2, pos. 13).
5 D : Air pulser. F!
U : This little compressor is use to send pulsed air into the igniter auxiliary gap.
6 D : Fans.
U : Cooling by air of the lower cabinets of the instrument.
For access, open the front panels (figures 3.1 and 3.2, pos. 13 and 14).
M : Check its operation by observing the fans from the front of the instrument, with the front pan-
els removed (figures 3.1 and 3.2, pos. 13 and 14).
7 D : Lid's blocking screw.

U : Closes the user safety and prevents the lid to be open.
M : If the lid must be open (e.g. for maintenance purpose), that screw must be sufficiently un-
screwed. The safety will open and the lid can be lifted. The access to inside components is
therefore without danger for the operator.
WARNING: Out of alignment risks!
Handling inside the oven must only be done by qualified personal.
8 D : Argon inlet.
9 D : Argon outlet filter. F!

U : The filter retains the metal dust particles, which are drawn from the sample during the analysis.
M : To be cleaned regularly. Unscrew the container slowly as the dust can catch fire upon contact
with the oxygen of the air. Clean the filter cartridge with a vacuum cleaner or change it. See
complete procedure, section Argon Outlet Filter chapter Routine Maintenance.
10 D : Argon outlet.
C : It is recommended to evacuate the argon from the instrument outlet to the outside of the
laboratory.
11 D : Dust filters.
U : Prevents dust from entering the instrument's lower cabinets.
M : Should be cleaned regularly. See complete procedure, section Changing or Cleaning of the
Dust Filters chapter Routine Maintenance.
C : Behind the filters (on the inside) is a fan (F!) (figure 3.3, pos. 6).

12 D : 230 VAC output sockets.

U : For connection of the computer and its peripherals.
C : These sockets remain supplied, even if the main switch-breaker (figure 3.12, pos. 2) is off.
This permits to switch off the instrument with keeping the computer powered.
13 D : 230 VAC mains power supply cable.
14 D : Water cooler. F!
U : The analytical table is cooled by a closed circuit of circulating water.
M : Check the water level by time to time, see (figure 3.18, pos. 1).
15 D : Vacuum pump. F!
C : Depending if the version is with or without the VUV option the pump models are different, see
the later section Vacuum Pumping Line. The vacuum pump is switched on by the switch
(figure 3.12, pos. 5). However, it can never be powered if the main switch-breaker (figure
3.12, pos. 2) is off.
16 D : RS232 input.
U : Connection between the computer and the instrument.
17 D : High vacuum system control board.

U : This board is present only with the VUV option. It controls the molecular drag pump.
18 D : Molecular drag pump. F!

C : This object is installed only when the VUV option is present. See later section Special System
for High Vacuum.
19 D : Intermediary oil filter. F!

C : This object is installed only when the VUV option is present. See later section Argon Circuit.

Figure 3.5
1
4
Figure 3.6

1 D : Scanning screw. F!
U : This screw is used for finding a spectral line and its intensity peak (in terms of divisions of the
scanning screw's scale).
For access, lift the keyboard support (figures 3.1 and 3.2, pos. 16).
M : For the analysis, the scanning screw must be put on the position found during the profile
check. See section Profile Check chapter Routine Maintenance.
C : In order to correct the play on the screw, the final movement of the scanning screw must al-
ways be made in the same direction (clockwise).
2 D : Pilot lamp for heating of the oven (F!).

U : Gives an indication on the heating cycle operation. The lamp is lit when the heating is operat-
ing and it goes out when it stops. In normal operation, the lamp lights and goes out alternately
about one time every three seconds.
3 D : Control multimeter.
U : This multimeter has two purposes:
1. Check the intensity peak of a spectral line, for the direct profile method of profile taking;
there are four scales of sensitivity that can be selected on the vacuum and profile card (F!)
of the electronic rack (F!). See figure 4.7 for the vacuum and profile card, and the section
Direct (or Manual) Profile chapter Routine Maintenance for the direct profile procedure.
2. Check of the vacuum in the spectrometer; there are two sensitivity scales that can be se-
lected from the vacuum and profile card (F!) of the electronic rack (F!). See figure 4.7 for
the vacuum and profile card.
One of these scales gives the absolute value (real) of the vacuum inside the spectrometer; it
will be used to check the value of this vacuum and to adjust the air leak by micro-valve
(figure 3.8, pos. 15) if necessary.
The other vacuum value indicates a relative value (differential) allowing vacuum leak re-
search during repair.
4 D : Spectrometer. F! See section Oven and Spectrometer.

U : The spectrometer contains the optical elements for wavelength dispersion.
For access, lift the lid.
C : If the lid must be open (e.g. for maintenance purpose), the blocking screw (figure 3.3, pos. 7)
must be sufficiently unscrewed. The safety will open and the lid can be lifted. The access to in-
side components is therefore without danger for the operator.
WARNING: Out of alignment risks!
Handling inside the oven must only be done by qualified personal.

3.3 Stand
The figure 3.7 shows the stand with a sample in position ready for analysis. The figure 3.8 shows the stand
open for cleaning or maintenance purpose. The figure 3.9 shows several separate parts subject to mainte-
nance or cleaning.
4 11
5
3
7
6
1
2
8
10
9
12
Figure 3.7
Key to figure 3.7:
D : Stand.
1 D : Stand door.
U : The stand door is for closing the sample analysis housing. No analysis can be started when the
door is open. Likewise, the analysis is interrupted when the door is opened. This safety device
complies with the international standard CEI 1010-1.
M : The door's hinges should be greased from time to time. See section Greasing of the Stand
Door's Hinges chapter Routine Maintenance.
2 D : Safety contact.
U : Safety that prevents analysis when the door is open.
3 D : Safety tab.
U : Frees the safety when the door is closed.
4 D : START button.
U : Analysis start-up.
C : The software can do without the START button if the automatic start is selected. However the
analysis will start only if the door is closed.
5 D : STOP button.
U : By pressing this button, the analysis cycle will be stopped at any moment.

6 D : Sample in analysis position.

C : The sample must completely cover the hole in the table. It is necessary that the surface be flat.
See also Sample Preparation and Placing the Sample on the Analytical Table appendixes of
this manual.
7 D : Sample clamp.
U : This device maintains the sample firmly in place on the analysis table.
8 D : Analytical table. F!
U : This is a support for the sample and a cover for the sparking chamber.
C : The analytical table is also commonly called "Petrey table".
M : Clean the table and the chamber regularly. The complete procedure is described in the section
Cleaning of the Stand and the Sparking Chamber chapter Routine Maintenance.
9 D : Electrode's (figure 3.9, pos. 11) clamping screw.

U : Secures a reproducible position of the electrode in relation to the sample. The adjustment of
the position is to be made with a gauge (figure 3.9, pos. 13). It is useless and even harmful to
tighten the electrode excessively.
10 D : Camlocs screws (2x).

U : Fastening of the analytical table. To free the table, see section Cleaning of the Stand and the
Sparking Chamber chapter Routine Maintenance.
11 D : Protection plate.
U : Access to the top inside part of the stand. To remove, pull up. See also section Lens Cleaning
chapter Routine Maintenance.
C : The plate must be removed to proceed to some maintenance operations, for example the lens
cleaning.
12 D : Stand housing.
U : To have access to the inside of the stand enclosure, for example for troubleshooting or compo-
nent exchange, the complete housing must be removed.
C : Routine maintenance operations do not require the operator to remove the stand housing.

8 9 7 6 14
15
2 5
3 4
Figure 3.8
13
4 1
3
9
5 8
10
11
12
Figure 3.9

1 D : Analytical table. F!
U : This is a support for the sample and a cover for the sparking chamber.
C : The analytical table is also commonly called "Petrey table". The table is run by a closed water
circuit that allows to stabilise the table at a constant temperature.
M : Clean the table and the chamber regularly. The complete procedure is described in the section
Cleaning of the Stand and the Sparking Chamber chapter Routine Maintenance.
2 D : Analytical table's base.

U : Thermal stabilisation support for the table.
3 D : Light channel with shutter controlled by solenoid.

U : Passage of light between sparking chamber and lens.
C : A shutter is in place all the time, except during the integration time of the measurement. It cuts
out a part of the light during the pre-spark period so as not to dazzle the photomultipliers.
4 D : Solenoid.
U : Opens the shutter during the integration time of the measurement.
5 D : Lens holder and heated lens.

U : The lens acts as a focalisation lens and as a vacuum-tight entrance window.
M : Clean the lens regularly. The complete procedure is described in the section Lens Cleaning
chapter Routine Maintenance.
6 D : Primary channel manual shutter.

U : The purpose of this shutter is to open and close the primary optic chamber airlock (between the
lens and the spectrometer. The analysis position is "open". The "closed" position permits to re-
move the lens holder (pos. 5) for cleaning purposes, without breaking the vacuum inside the
spectrometer. See the complete procedure, section Lens Cleaning chapter Routine
Maintenance.
Positions: open <> closed.
IMPORTANT:
Do not open the shutter if the lens holder is not correctly in place.
The non-observation of this rule can cause serious damages to

your instrument.
7 D : Knurled knobs and clamps (2x).

U : Fastening for lens holder (pos. 5).
8 D : Lens heater connector.
9 D : Knurled knob (1x).

U : Is used for the extraction of the lens holder (pos. 5).
C : The plastic knurled knob is red in colour.

10 D : Glass insulator.
U : Used for electric insulation and recuperation of metal dust drawn from the sample.
M : The insulator must be cleaned regularly, see section Cleaning of the Stand and the Sparking
Chamber chapter Routine Maintenance.
11 D : Large tungsten electrode (6/2 mm ).

U : The analytical discharge is made between the sample and the electrode. Ensure that only elec-
trodes delivered by Thermo Electron are used.
M : Clean the electrode's tip with a small metal brush (pos. 12), see procedure, section Analysis
Electrode chapter Routine Maintenance.
C : Depending on the application another electrode type may be used.
12 D : Small metal brush.

U : Cleaning the electrode tip (for large electrodes only).
M : Brush the electrode vigorously (pos. 11). Take care to not damage the table's hole border. A
worn brush must be thrown away and replaced by a new one.
C : There are three types of brushes: the ones with a yellow handle (steel strands) are for Fe, Ni,
Co and Ti bases; the ones with a black handle (Mo strands) are for Ag, Al, Au, Cu, Cd, Mg,
Sn, Pb, Pd, Pt, Sb, Bi and In bases; the ones with a red handle (W strands) are for Ag, Al, Au,
Cu, Cd, Mg, Sn, Pb, Pd, Pt, Sb, Bi and In bases when the black brush is not suitable (Mo
analysis).
13 D : 3 mm adjustment gauge.
U : Set reproducibly the electrode (pos. 11) position. The procedure is described in the section
Analysis Electrode chapter Routine Maintenance.
14 D : Fittings for water pipes (2x).

U : The water cools the analysis table and the sample. See also section Water Cooler.
15 D : Micro-valve for inlet of spectrometer air leak.

U : To be adjusted to obtain a vacuum of 30 milli-Torr, reading on the multimeter (figure 3.5, pos.
3).
C : When the VUV lines option (nitrogen, oxygen, etc.) with a high vacuum pumping line is in-
stalled, the air leak is useless. In such a case the micro-valve must remain completely closed.

3.4 Hi-Rep Source

The figure 3.10 shows the front side and the figure 3.11 the back side of the Hi-Rep 2+ source. Its ignition
module is inside a Faraday cage into the stand enclosure.
2 1 3 4 5 6
Figure 3.10
7 9 13
8 10 11 12
Figure 3.11

1 D : Hi-Rep 2+ source rack.

U : The source generates sparks between the electrode and the sample to be analysed. The energy
brought by the sparks extracts atoms from the sample that emits light to be analysed.
2 D : Switch-breaker (6 A) for the source.

U : Switching on the source.
C : The switch breaker is not powered if the main switch breaker (figure 3.12, pos. 2) of the in-
strument is off.
3 D : Power supply board.
4 D : Pulse generator board.
5 D : Condition selection board.
6 D : Logic control board.
7 D : 230 VAC power supply connector.
8 D : Control signal connector.
9 D : High voltage signal connector cable.
10 D : Safety connector.
11 D : Voltage output connector.

U : Discharge voltage check.
12 D : Current output connector.

U : Discharge current check.
13 D : Label.
U : Safety wiring directions.

3.5 Power Distribution Rack

The figure 3.12 shows the external side of the power distribution panel, seen from the back side of the in-
strument.
3 4 2 5 6
1
8
Figure 3.12

Key to figure 3.12:
1 D : Power distribution panel (seen from back).
2 D : Main switch-breaker 16 A.
U : Switching on the instrument.
C : In the off position, the whole instrument is switched off, but the external output sockets (pos.
7) remain powered.
3 D : Electronics' switch.
U : Switching on the low voltages for the electronics.
4 D : High voltage switch.

U : Switching on the high voltage for the photomultipliers.
5 D : Vacuum pumping line switch.

U : Starting the vacuum pumping line.
6 D : Water cooling circuit switch.

U : Switching on the water cooling pump.
7 D : 230 VAC output sockets.

U : For connection of the computer and its peripherals.
C : These sockets remain supplied, even if the main switch-breaker (pos. 2) is off. This permits to
switch off the instrument with keeping the computer powered.
8 D : Fuse 10 A.
U : Output sockets (pos. 7) safety.
M : To check or change the fuse, unscrew the cap.
C : Only replace a fuse by an identical one (value and size).
9 D : Mains power cord input (230 VAC).

3.6 Electronic Rack

The figure 3.13 shows the front of the rack including the electronic boards, and the figure 3.14 shows an
overall view (modules and connections).
1 17 3 2 5 6 4
Figure 3.13
8 7 15 17 14 13 16
9 11 10 12
Figure 3.14

1 D : Electronic rack.
C : Boards other than those shown in the figures and described below may be installed in the elec-
tronic rack; in principle these will be optional boards or ones covering specialities. They will
be described in documents other than this manual.
2 D : ICS34 assembly (ICS = Instrument Controller System).

U : Instrument management centre.
C : The sandwich assembly consists in two boards. One is called MMB88 and it contains the mi-
croprocessor, the firmware dedicated to the instrument, the signals management and the com-
munication ports. The other one is called the adaptation board; it serves as an interface be-
tween the microprocessor and the instrument, and is specific to the applications of the ARL
3460 instrument.
On the top right-hand side of the ICS34 is a square red button: this is the microprocessor reset
button. It may be that you will have to press this button, e.g. during a telephone assisted trou-
bleshooting. It is important to note that when the button is pressed, the microprocessor looses
its previous information and it will thus be necessary after a reset to reload the parameter into
the microprocessor using the appropriate software command.
M : In case of replacement, always change the entire ICS34 assembly; do not separate the two
boards.
3 D : IVFC board. Current-voltage-frequency converter board.

U : Acquisition of signals coming from the photomultipliers and conversion to frequency for
counting.
C : One board can control 6 channels. The rack can admit a maximum of 10 boards (60 channels).
4 D : Vacuum and profile board.

U : Control and measurement of "vacuum" and "profile" functions.
C : Two wires are directly connected onto the board; these wires supply the control multimeter
(figure 3.5, pos. 3).
M : A 6 positions switch is situated on the front of the board, its purpose is to select different scales
of the multimeter (see also section Direct (or Manual) Profile chapter Routine Maintenance).
The positions are:
Top 1 : Differential vacuum
2 : Absolute value of vacuum
3 : Profile, low sensitivity
4 : Profile, medium sensitivity
5 : Profile, high sensitivity
Bottom 6 : Profile, very high sensitivity
5 D : Status board.
U : Monitoring of the instrument's general operation. The following 10 parameters are automati-
cally checked at each analysis or by request from the operator through the software: the 4
LVPS (+24 V, +12 V, -12 V, +5 V), the HVPS and its polarisation (-1000 V, -100 V), the
spectrometer temperature, the electronic cabinet's temperature, the value of the vacuum inside
the spectrometer, and the voltage of the mains power supply (230 VAC).
6 D : Dual attenuator board. Option.

U : Driving the dual attenuators.
C : A maximum of 12 out of all the instrument channels can be switched on 2 attenuator selections
of a phototube. This allows to have two sensitivity ranges for 12 phototubes of the instrument.

7 D : LVPS module 12 VDC and +5 VDC.
8 D : LVPS module +24 VDC.
9 D : HVPS module (High Voltage Power Supply).

U : Power supply of photomultipliers' attenuators to around -1000 VDC and polarisation of the
photomultipliers to -100 VDC.
10 D : 230 VAC power supply connector for HVPS module (pos. 9).
11 D : 230 VAC power supply connector for LVPS modules (pos. 7 and 8).
12 D : Connection strip high voltage output.
13 D : Connector, electronic signals source/stand.
14 D : Connector serial link ACS-ICS

U : Links the instrument's microprocessor to the computer central unit.
C : An intermediary connector is to be found on the back side of the instrument (figure 3.4, pos.
16).
15 D : Connector, electronic signals oven/spectrometer.
16 D : Connector, channels' signals.

C : Signals coming from the photomultipliers.
17 D : Motherboard.
U : Receptacle for electronic boards and interconnections with other modules.

3.7 Vacuum Pumping Line
3.7.1 Standard System for Intermediary Vacuum

The figure 3.15 shows the standard pumping line that permits to obtain an intermediary vacuum. Such a sys-
tem is sufficient if the analysis in the VUV range is not required.
6 4
2 5
1
3
Figure 3.15

Key to figure 3.15:
1 D : Alcatel mechanical vacuum pump model 2005ARL-LS.

M : Change oil every six months; use only oil prescribed by Thermo Electron. See section Vacuum
Pumping Line chapter Routine Maintenance.
2 D : Oil level indicator.

U : The level must be visible; it can be easier to check this when the pump is stopped.
3 D : Oil drain plug.

C : The black plastic protection must be removed.
4 D : Outlet of air and possible oil vapours.
5 D : Air ballast valve.

U : After having changed the oil, run the pump for around 30 minutes with the valve open, then
close it.
6 D : Oil inlet cap.

C : The black plastic protection must be removed. One of the ends of the plastic protection can be
used as a tool for opening or closing the caps.
7 D : Pumping pipe.
U : Connects the vacuum pump's air inlet to the spectrometer.
IMPORTANT:
See ATTENTION under (figure 3.21, pos. 4).

3.7.2 Special System for High Vacuum

The figures 3.16 and 3.17 show the special pumping line that permits to reach a high vacuum. This system is
necessary if elements in the VUV range require to be analysed, in particular nitrogen and oxygen. When the
VUV option is purchased, this system is therefore automatically supplied with the instrument. In addition an
electronic board controls the system; it can be seen on the figure 3.3 and is described with the corresponding
legend.
Figure 3.16
Figure 3.17

1 D : Diaphragm pump
U : This pump produces a dry primary vacuum.
M : The diaphragm and the valves wear down and must be replaced at least once a year. The proce-
dure is described in the section Vacuum Pumping Line chapter Routine Maintenance.
C : This pump has a calibrated air ballast with a silencer, which must remain installed for routine
operation. The ballast can be replaced by a cork only for leakage test purpose.
2 D : Pumping pipe.
U : Connects mechanically the diaphragm pump to the molecular drag pump (pos. 4).
C : The volume of the pipe is a buffer, therefore the length and diameter should not be changed.
Do not use another pipe or do not shorten the supplied pipe.
3 D : Molecular drag pump.

U : This pump achieves the high vacuum into the spectrometer.
M : Bearings must be greased at least once a year. This subject is described in the section Vacuum
Pumping Line chapter Routine Maintenance.
C : This pump has a motor rotating at 27'000 turns per minutes and is therefore fragile. The motor
requires about 5 minutes to stop rotating once the circuit is switched off.
During operation, and even 5 minutes after switching off, shocks

against the molecular drag pump body must absolutely be avoided.
4 D : Spectrometer's manual aeration valve.

U : The atmospheric pressure can be restored into the spectrometer with this valve.
WARNING - VERY IMPORTANT
Wait at least 5 minutes after the high vacuum system switch off
before opening manually this valve.
C : This waiting time is necessary to let the molecular drag pump to stop completely.

3.8 Water Cooler

The figure 3.18 shows the water cooling system (closed circuit).
3
4
Figure 3.18
Key to figure 3.18:
1 D : Water pump and container.

M : The purge of the system is part of the preventive maintenance (revision) and is therefore done
in principle by a Thermo Electron or by our local agent service engineer.
The level must be between the half and the three quarters of the container. Use deionised water
in case of addition.
C : The liquid is a water-antifreeze mixture. In case of complete purge, only the Thermo Electron
mixture should be used.
2 D : Water inlet.
3 D : Water outlet.
4 D : Water pipes towards stand.

C : The water of the circuit is driven into the analytical table (figure 3.9, pos. 1).

3.9 Argon Circuit

The argon inlet is under the stand and can be located on the figure 3.3 pos. 8. The figure 3.19 shows the stan-
dard version of the outlet argon circuit, after the stand. The figure 3.20 shows the argon outlet in the case of
the VUV option.
Important: The analysis of magnesium alloys requires a special argon circuit and a special argon
filtering, different to circuits illustrated here below. In case of multiple bases analysis (Mg
bases and one or more other bases), a dual filtering system with a commutation valve is
installed. In that case a particular manual Mg Filter Kit describing this speciality is supplied.
For safety reasons tied to the presence of magnesium powders (highly flammable) it is
essential to understand and to follow the safety instructions of this manual.
2
5
1
3
Figure 3.19

Figure 3.20
1 D : Argon outlet filter.

U : The filter retains the metal dust particles, which are drawn from the sample during the analysis.
M : To be cleaned regularly. Unscrew the container slowly as the dust can catch fire upon contact
with the oxygen of the air. Clean the filter cartridge with a vacuum cleaner or change it. See
complete procedure, section Argon Outlet Filter chapter Routine Maintenance.
2 D : Fastening screws of the outlet argon filter assembly.

U : If the complete assembly must be removed for maintenance, just unscrew partially these four
screws so as to free the supporting square. The assembly can the be lifted and removed.
3 D : Argon pipe.
U : This pipe carries the argon evacuated from the stand to the outlet filtering device.
4 D : Intermediary oil filter (VUV option).

U : The oil maintains and regulates a slight over-pressure in the sparking chamber and also pre-
vents air from rising back through the pipes.
M : To be cleaned regularly. See complete procedure, section Argon Outlet Filter chapter Routine
Maintenance.
5 D : Argon outlet.
C : It is recommended to evacuate the argon from the instrument outlet to the outside of the
laboratory.

3.10 Oven and Spectrometer

The oven is the thermostatic controlled enclosure containing the spectrometer. The volume of the enclosure
is delimited by the interior of the instrument's lid.
A dual purpose safety switch (operator safety and safety for component function life span) automatically cuts
the high voltage power supply (of attenuators and photomultipliers) as well as the heating power supply for
the oven during lid opening.
Some objects, written in italics in the keys to figures, are indicated for information pur-
pose only. These are objects that should only be handled by duly qualified people. In case
of false manipulation of these objects, the replacement or repair of some of them would
lead to very delicate and expensive operations that can only be done with great difficulty
outside our factories. These objects are indicated so as to warn you of the care to be taken
near to them. In any case, shocks must be avoided to the outside and inside of the
spectrometer. Do not forget that the mechanical and optic components of the
spectrometer have been manufactured with the greatest care and adjusted with highest
precision to attain the analytical performances that you expect from your instrument.
Consequently, the spectrometer and its components are the most fragile and delicate to
handle in the instrument.

3.10.1 Common items

The figures 3.21 and 3.22 show two general views of the oven and the spectrometer. The figures 3.23 and
3.24 show close-ups that will help you to locate some objects in greater details. For these four figures, the
description is grouped just after them.
5
7
4
3 3
10 22 6 12 2
Figure 3.21
5 15 16
12
12 7
14
10
13
11
Figure 3.22

18
19
17
Figure 3.23
18
2 21
10
20
Figure 3.24

Key to figures 3.21, 3.22, 3.23 and 3.24:
1 D : Lid.
C : See key (figures 3.1 and 3.2, pos. 15).
2 D : Scanning screw.
C : See key (figure 3.5, pos. 1).
3 D : Spectrometer body.
U : The spectrometer serves as a support and as a box for the optic dispersive system.
C : Avoid all shocks against spectrometer body.
4 D : Spectrometer's manual aeration valve.
ATTENTION:
Before disassembling the vacuum circuit (pump oil change), this valve
must be used to restore atmospheric pressure in the spectrometer.
With a high vacuum pumping system you must wait at least 5

minutes after the pumping line system is switched off before to
open this aeration valve.
5 D : Photomultipliers.
U : Transforms the light photons into electric signals.
C : There are as many photomultipliers as there are element-channels installed in your instru-
ment; they can be situated indifferently above or below the spectrometer body.
Even though the damage which could occur through incorrect handling of the photomultipliers
is less important than that affecting the diffraction grating, access to them remains reserved to
qualified personnel.
6 D : Safety contact.
U : Cuts the high voltage power supply and heating when the lid is opened.
7 D : Attenuator board.
U : Adaptation of the high voltage individually on each photomultiplier.
C : Each photomultiplier has its attenuator, which has been pre-set in the factory according to dif-
ferent parameters (photomultiplier sensitivity, spectral line sensitivity, dynamic range to be
measured, etc.). The change of position of the attenuator directly affects the photomultiplier's
response, and because of this affects the previous analytical calibrations using the appropriate
channel. Only to be changed with full knowledge of the facts.

8 D : Diffraction grating holder.

U : The grating is the main optic part of the spectrometer; it separates the spark's light into all the
wavelength that composes it.
C : If it is handled with care, the grating should never need to be replaced during the life of the
instrument. Therefore in principle, it can only be damaged by accident or by a handling error;
its repair is almost impossible and its replacement is an operation that can only be carried out
by a few rare specialists outside our factories. There is no routine maintenance operation
requiring that you handle it or even approach it.
9 D : Lid and connection of fatigue lamps.

U : The fatigue lamps light up automatically in the absence of a spark in the stand. They are a
light source, which softly lights the photomultipliers so as to improve their stability (to avoid
dazzling). The fatigue lamps are also used for electronic function checks without sparking
analysis.
C : Owing to their proximity to the diffraction grating, only qualified personnel must have access
to the fatigue lamps. The checking operations with the fatigue lamps require no physical ac-
cess to the lamps themselves by the operator.
10 D : Oven's ventilation nozzle. F!

U : The nozzle carries the heating resistors (located inside the nozzle) and is used to run the warm
air propelled by the transverse fan (pos. 11).
11 D : Transverse fan.
U : To propel the warm air through the nozzle.
12 D : Radial fans.
U : Mixing the warm air inside the oven enclosure.
13 D : Heating regulation board.

U : Regulation of the spectrometer temperature.
C : The regulation operation can be observed by watching the heating pilot lamp (figure 3.5, pos.
2).
14 D : Thermostat.
U : Safety against fire risk, if the nozzle becomes overheated. The thermostat cuts the power of the
heating circuit if the temperature of the nozzle's plate exceeds 60 C.
C : If the thermostat starts to operate, there will be no further heating and the temperature of the
nozzle's plate will go down to about 54 C; at this temperature the thermostat rearms
automatically and lets the heating resistors be powered again.
15 D : Small board with temperature sensor.

U : This temperature sensitive circuit returns an instruction (under the form of an electrical signal
proportional to the temperature) to the regulation board.
16 D : Vacuum gauge.
U : This thermocouple returns a proportional voltage of the pressure into the spectrometer to the
vacuum and profile board (figure 3.13 pos. 4)
C : The pressure can be read on the control multimeter (figure 3.5 pos. 3), as long as the 6 posi-
tions switch of the vacuum and profile board (figure 3.13 pos. 4) is set on the position 2.
The reading is however approximate and the circuit is designed to read intermediary vacuum
pressure. Under a pressure of 5 mHg the reading is not anymore valid.

17 D : Side plate for access to the secondary optics.

U : For adjustment of spectrometer's secondary optic parts.
C : Qualified personnel only.
18 D : Spectrometer lid.
U : When opening the lid, access is gained to the primary and secondary optics of the spectrome-
ter.
C : The mechanical and optical components inside the spectrometer have been set with great pre-
cision. Only qualified personnel should have access to these parts. No routine maintenance
procedure requires the spectrometer to be opened by the operator.
19 D : Label.
U : Indicates several mechanical characteristics of the spectrometer's body (figure 3.21, pos. 3).
20 D : Silent-bloc (3x)
U : Vibration absorption.
21 D : Air leak inlet in the spectrometer.

C : The air leak is adjusted by the micro valve (figure 3.8, pos. 15). The micro valve must remain
closed with the high vacuum system (VUV option).
22 D : Dual attenuator relay board. Option.

U : Selects one of the attenuators for a given phototube (channel). The relays are controlled by the
dual attenuator board (figure 3.13, pos. 6) of the electronic rack.
C : A maximum of 12 channels can have this option.

3.10.2 Particular items
3.10.2.1 Reflected beam
The Reflected Beam (RB) can be used to install an external line that could not be easily installed inside the
spectrometer. This may be the case, for example, when an element such as the Li, Na or K must be installed.
The reflected beam is the total reflection of the grating, and it is necessary to install a narrow bandwidth in-
terference filter in order to measure only the desired light of the element to be analysed.
Note: Only one element can be installed on the reflected beam. If two particular elements are
needed, the direct beam (DB) will used. If three particular elements are needed, both the RB
and DB are used. For the Direct Beam, see the next section.
The figure 3.25 shows the spectrometer body with a reflected beam device installed.
Figure 3.25
Key to figure 3.25:
1 D : Support device for Reflected Beam.

C : Holds the RB photomultiplier and contains the interference filter corresponding to the
mounted external line.
2 D : RB Photomultiplier.
C : See legend of pos. 5 section Common items.

3.10.2.2 Direct beam
The Direct Beam (DB) can be used to install an external line that could not be easily installed inside the
spectrometer. This may be the case, for example, when an element such as the Li, Na or K must be installed.
The direct beam is a part of the primary light, reflected by two mirrors outside the spectrometer. This light is
then directed by optical fibres to photomultipliers. It is necessary to install a narrow bandwidth interference
filter in order to measure only the desired light of the element to be analysed.
Note: One or two elements can be installed on the direct beam. If only one element is needed, the
reflected beam (RB) will be preferred. If three particular elements are needed, both the RB
and DB are used. For the Reflected Beam, see the previous section.
The figure 3.26 shows the spectrometer body with a direct beam device installed.
1 3
Figure 3.26
Key to figure 3.26:
1 D : Support device for direct Beam.

U : Holds the DB photomultiplier and contains the interference filter corresponding to the
mounted external line.
C One or two PMT's can be mounted.
2 D : DB Photomultiplier.
C : See legend of pos. 5 section Common items.
3 D : Optical fibre.
U : Brings the light to the PMT.

4
ROUTINE MAINTENANCE
Routine Maintenance Chapter 4
4. ROUTINE MAINTENANCE
4.1 Forewords
Recent technologies let us build up instruments that require less maintenance as in the past time.
Some parts of the instrument, mainly the stand, are more subject to be used and it remains necessary to pro-
ceed to some operations that we call routine maintenance. These operations are usually performed by the
operator at regular intervals, or their frequency is depending on the sample throughput.
In order to guarantee a long term operation with a minimal breakdown risk, as well as to keep the initial ana-
lytical performances, it is highly recommended to overhaul completely the instrument at regular intervals, for
example once a year. This is called the service maintenance; that should be performed by an Thermo
Electron or agreed local agent service engineer.
Hereunder in this chapter, we will only talk about a routine maintenance guide foreseen for the operator.
Note: The standardisation (sometimes also called recalibration, or even normalisation), is considered
by some people as part of the routine maintenance. However we will not develop this subject in this
chapter. You can find explanation and procedures about the standardisation in the Operator
Manual.

Chapter 4 Routine Maintenance
4.2 Application Domains of Procedures

The routine maintenance procedures described in this chapter can be applied to most current application
cases.
In some particular cases, especially in domains requiring ultimate performances, different or more rigorous
procedures are necessary to achieve those performances.
For the particular application domains listed below, you must first consult the Special Procedures appendix
of this manual. This appendix shows the differences of procedures in relation to the ordinary procedures of
this chapter.
Magnesium alloy matrix
For the maintenance of the material for the analysis of VUV elements, the VUV Line Analysis manual must
also be consulted.
For all other cases not explicitly mentioned, the routine maintenance procedures described in this chapter
must be applied.

4.3 Summary Table

The few routine maintenance checks to be carried out periodically are pointed out in the table thereunder.
Further detailed explanations follow in the next sections of this chapter.
Maintenance subject Recommended frequency Details

section
Cleaning of the electrode Before each analysis 4.4
Cleaning of the insulator and the sparking chamber At least once a day, before standardisation 4.5.1
Cleaning inside the stand (table, block support) At least once a week 4.5.2
Argon outlet circuit At least once a week 4.6
Oil of argon circuit for the VUV option Every 6 months 4.6.2.1
Check pump oil level At least once a week 4.7.1.1
Change vacuum pump oil and gaskets Every 6 months 4.7.1.2
Profile check Monthly (at first weekly) 4.8
Greasing of stand's door hinges Once a month 4.9
Lens cleaning Once a month 4.10
Cleaning the dust filters Once a month 4.11
Changing the dust filters Once a year
Operation of cabinet fans Once a week 4.12
Running Control Sample and/or Once a day (optional) 4.13.1
Standardisation Once a week 4.13.2
Backup Once a week 4.14
Accessories in option According to manufacturer 4.15
Note: The cleaning of the lens, the profile check and the vacuum pump oil change, even taken
separately, can considerably affect the response of the instrument; they must thus be
followed by a standardisation and must be carried out before the standardisation started.
We recommend a waiting time of about 15 minutes between the cleaning of the lens and the
standardisation. This delay is necessary to flush out the air that is entered into the sparking
chamber and pipes during the cleaning. This delay can be reduced if the pipes and the
chamber are purged with the analytical flow rate, by choosing the direct profile mode for
example.

4.4 Analysis Electrode

The electrode should be cleaned with the small metal brush before (or after) each analysis.
Take care to not worn the analysis table and the border of the analysis hole with the brush.
A quick cleaning of the surface of the table is also advised, in order to remove metal dusts or possible greasy
deposits from fingers. Do it with a soft brush or a dry rag, lightly moisten with alcohol.
Figure 4.1
A worn metal brush does not do its job properly and must be replaced. Only use the brushes supplied by
Thermo Electron.
Your experience can bring you to the conclusion that an electrode cleaning is not necessary after each
analysis, but only perhaps after every 10, 50 or even 100 analyses, the choice is yours. By cleaning the elec-
trode after each analysis, you ensure a greater accuracy. It is necessary to clean the electrode when you
change the type of alloy analysed, and also between each sample during the standardisation or calibration of
a new program.

4.4.1 Electrode Exchange and Adjustment

If the electrode's tip becomes rounded, or if it breaks off, it must be replaced. Nevertheless we recommend to
exchange the electrode about every 6 months. Use only electrodes supplied by Thermo Electron.
Even if it is not necessary to replace the electrode, it is useful to check its adjustment by time to time.
By loosing the clamping screw (see d, figure hereunder) the electrode automatically lifts up. You can then
take it out with your finger or pliers. If the electrode does not lift up by itself, we recommend to change the
complete module (by a Service Engineer).
The electrode adjustment is done with a 3 mm gap gauge that is supplied with the instrument (see figure
hereunder):
c Press with one hand on the gauge in order to push down the electrode into the cylinder,
d Tighten the clamping screw.
Figure 4.2

4.5 Cleaning of the Stand and the Sparking Chamber

The sparking chamber is the argon flushed space inside which the electrical discharge between the electrode
and the sample takes place (see the Operator Manual, section Analysis Principle).
The sample material burned by the discharge lefts a dusty blackish deposit. A part of this deposit is
evacuated through the argon pipe towards the argon outlet filter. It is necessary to remove the remaining dust
deposit from the chamber regularly.
4.5.1 Cleaning of the Insulator and the Sparking Chamber

We recommend that these jobs be carried out at the end of each shift change or at the end of each working
day, but at least before each standardisation
However if your sample throughput is high, fast intermediate cleaning can be carried out. If these cleaning
sessions are carried out with care, they will not affect the instrumental response, so an intermediate
standardisation will not be necessary.
Remark: If the instrument is used for analysing various matrixes (bases), it is necessary to change the
analytical set (analytical table, electrode, brush, insulator) for each matrix change. Therefore
analytical sets must be kept separately and not mixed.
For removing the table, free the camlocs screws.
Slightly lift up the table, and pull softly towards you. The table becomes free from the optical primary
channel.
Warning! By acting too abruptly you may break the electrode.
Remove the o-rings of the base plate before they have been aspirated by the vacuum cleaner!
Remove the glass insulator by lifting it (take care not to break the electrode tip) and clean it first with a
vacuum cleaner, eventually with a piece of rag slightly moisten with alcohol so as to remove greases.
After the insulator is removed, remove the dust of the sparking chamber with a vacuum cleaner. Here again
take care not to hit the electrode tip. A broken electrode must be replaced.
Once these cleanings are done, put everything back into place and put a sample on the table so as to cover
the analysis hole.
Note: The oxygen in the air perturbs the creation of the plasma during the sparks. This is why we recom-
mend that you always leave a sample covering the analysis hole (see also Remarks).

4.5.2 Cleaning of the Table and the Inside

In this section we consider the analysis table and the inner space of the table's block support.
We recommend a weekly cleaning of these items. But here again, in case of a high (or low) sample
throughput, the frequency must be adapted to the use of the instrument.
4.5.2.1 Dismantling
For removing the table, free the camlock screws.
Slightly lift up the table, and pull softly towards you. The table becomes free from the optical primary
channel.
Warning! By acting too abruptly you may break the electrode.
Remove the o-rings of the base plate before they have been aspirated by the vacuum cleaner!
Unscrew the electrode clamping screw (see d of the figure 4.2), the released electrode should lift some milli-
metres. Take out the electrode, simply by pulling upwards with fingers.
4.5.2.2 Cleanings
4.5.2.2.1 Table's Block Support
Remove the metal dusts with a vacuum cleaner, if necessary with the help of a soft brush.
4.5.2.2.2 Electrode
The electrode brushing is explained in the section Analysis Electrode.
4.5.2.2.3 Analysis Table
Remove the metal dusts with a vacuum cleaner, if necessary with the help of a soft brush. Use pipe cleaners
for cleaning the inside of the primary optical channel and the other inner pipes. Do not use solvents.
The top of the table can be cleaned with a piece of rag slightly moisten with alcohol. Nevertheless avoid the
alcohol to pass on the inside of the table, or on the bottom part of it.
Note: The presence of water in the cleaning solvent has bad effects on the sparks. The alcohol used must
then be very pure, or you must use isopropyl alcohol containing less water.

4.5.2.2.4 Glass Insulator
The glass insulator can be cleaned, for example with alcohol. It has to be put back only once dry!
Finally clean and dry all parts with paper towels and arrange them on clean papers.
4.5.2.3 Reassembling
Put back together everything in the dismantling reverse order, take a particular attention:
to check if you don't forget to put back the o-ring of the table's block support,
to put back the glass insulator,
to insert well the front of the table around the primary channel's end,
to close the table's camlock screws without forcing them, otherwise it indicates that one of the pieces is
not in its place.
Check the electrode height adjustment with the gauge supplied with the instrument (see procedure in section
Analysis Electrode). Tighten the clamping screw normally, without forcing.
Cover the analysis hole with a sample.
4.5.2.4 Remarks
The oxygen in the air perturbs the creation of the plasma during the sparks. This is why we recommend that
you always leave a sample covering the analysis hole.
Like wise, during the maintenance operation and depending on how long it takes, air enters the sparking
chamber and the argon pipes. It is possible that the first two or three attacks on the sample (the attack being
the physical result of all the sparks of a measurement on the sample's surface) are insufficient (white or very
pale attacks) to allow an accurate measurement. If the problem persists one must nevertheless remember
there are many different reasons for bad attacks; the reasons can also be:
bad argon quality,

leaks in the pipes,
defects in the sparking source's electronics,
a bad sample which has inclusions of oxygen or another gas.

4.6 Argon Outlet Filter

If the instrument is used for Mg base analysis, it must be equipped with a special filter for Mg. In this case
the directions in this section are not valid, please consult the Magnesium base alloys section of the Special
Procedure appendix.
4.6.1 Standard System

he argon outlet passes through a filter cartridge in a container. This device takes place in the centre back of
the instrument (see chapter Layout and Controls, section Argon Circuit). Clean the cartridge and the con-
tainer at least once a week.
unscrew slowly
cartridge
to open
Figure 4.3
The synthetic filter cartridge retains the metal dust. For access, the container must be
unscrewed slowly from its support (slowly as the dust can catch fire upon contact with
the oxygen of the air) and, if necessary, with the adequate supplied key.
Leave the cartridge inside the container, in contact with the air, for at least 15
minutes before cleaning them.
The filtering cartridge and the container are cleaned with a vacuum cleaner. When the cartridge becomes
very dirty, it should be replaced.
After cleanings, put back all parts in reverse order.

4.6.2 VUV Option System

The device is located at the centre back of the instrument (see chapter Layout and Controls, section Argon
Circuit). In addition to the cartridge filter (see section Standard System), there is an intermediary oil filter,
commonly called bubbler.
IN OUT
Argon outlet filter
IN OUT
Outlet
From stand
Intermediary oil filter
About
0.5 liter of oil
Figure 4.4
4.6.2.1 Intermediary Oil filter
Change the oil each 6 months. Use a vacuum pump oil CPM Elite Z.
For the oil change, simply unscrew the container. Throw away the oil and clean the container. Fill with ap-
proximately 0.5 litre of oil.
Remark: Be very careful not to suck up in the stands outlet tube. this would the oil coming back to
the stand.
When remounting the filter bodies, make sure they are tightly screwed, otherwise air can
infiltrate into the argon circuit.
4.6.2.2 Argon Outlet Filter
This filter is the same also used for the standard version, therefore the cleaning method explained in the
section Standard System must be used.

4.7 Vacuum Pumping Line

Depending the kind of pumping line installed, the maintenance is different. Two cases can be applied:
a standard pumping line for an intermediary vacuum using an oil vacuum pump, without the VUV option,
see later section Standard Pumping Line for Intermediary Vacuum.
a special pumping line for a high vacuum, with a diaphragm pump and a molecular drag pump, for the
VUV option, see later section Special Pumping Line for High Vacuum.
4.7.1 Standard Pumping Line for Intermediary Vacuum
4.7.1.1 Checking the Vacuum Pump Oil Level
Check the vacuum pump oil level at least once a week. If necessary top up the oil. Only use oil
recommended by Thermo Electron.
Use only oil prescribed by Thermo Electron.
Maximum
level
Intermediary
level
Minimum
level
Figure 4.5
The oil level can be observed more easily if the pump is stopped for a short moment but still warm.
For oil addition, kindly refer to the pump supplier's manual that has been delivered with the instrument docu-
mentation.
Note: The pump performances and its life span are optimal when the oil level is between the maximum
level and the intermediary level.

4.7.1.2 Changing the Oil and the Vacuum Pump Gaskets
This operation is recommended every six months. The procedure is described in the pump supplier's manual
that has been delivered with the instrument documentation.
Use only oil prescribed by Thermo Electron.
Only the gaskets recommended by Thermo Electron should be used. Your local Thermo Electron after sales
service (or our agreed agents) are at you disposal for the supply of spare oil and gasket kits.
These operations can be carried out upon request, during a service maintenance visit by one of our service
engineers.
4.7.2 Special Pumping Line for High Vacuum

This system is necessarily mounted with the VUV option. This dry pumping line is derived from the Alcatel
Drytel system and adapted to our instruments. A primary vacuum is made by the diaphragm pump. Then a
molecular drag pump located between the diaphragm pump and the spectrometer is making the high
clean vacuum necessary for the analyses of very low wavelengths spectral lines.
This special high vacuum pumping line requires a yearly maintenance (replacing the diaphragms and valves
of the diaphragm pump and lubricating the molecular pump).
These operations must be done during a yearly servicing performed by a Thermo Electron Service Engineer
(or from one of our agreed Agents). Kindly contact your local Thermo Electron Service.

4.8 Profile Check

The ARL 3460 is a very stable instrument. The profile's drift should be very slow and almost imperceptible.
However, we recommend that you check the instrument's profile at least once a week, at the beginning and
that the mean positions of the elements whose profile you have checked be kept in writing (with the dates the
profiles where taken). By observing the evolution of these values, you will be able to judge for yourself if
you can space out the profile checks (once a month for example).
The profile check of an element consists of finding the mechanical position of the secondary slit of this
element relatively to the primary slit which is common to all of the elements (channels) installed in your
instrument. The position of the primary slit is given by the graduation of the scanning dial.
Figure 4.6
Your instrument has been profiled in our factory with the greatest care and all the secondary slits have been
positioned mechanically to correspond with one single position of the primary slit. For analytical and
mechanical reasons, all the elements do not require the same positioning precision. As a general rule, all the
secondary slits are placed in an interval corresponding to 1 dial division of the average position.
There are two ways to take the profile: the first is called direct profile (or manual profile) and is an
analogue way, the second is called profile by integration and is a digital way. The manual method is often
faster and just as accurate as the integration method if care is taken. Nevertheless the manual method is more
subject to error than that by integration as it calls for interpretations (and analogue readings on a multimeter)
by the user.
The procedures (commands from the software) for taking the direct profile or the profile by integration are
also described into the WinOE Software Configuration Manual.
We expose hereunder a particular case as an example, for both methods (direct profile and profile by integra-
tion).

4.8.1 Direct (or Manual) Profile
4.8.1.1 Basic Advice
We recommend that you take the profile regularly on three channels (elements) distributed regularly in the
working wavelengths range of your instrument (i.e. to check the position of 3 secondary slits distributed over
the slit holder's secondary slit frame). Always use the three same channels and note the profile positions
found in your profile log book. Feel free to check one or several other channels now and again.
Choose channels (elements) which are relatively "easy" to profile. For an analytical program with Fe base,
take C (Carbon) for example, the (or a) standard Fe (Iron) and Al (Aluminium). In principle, these three
channels cover the secondary slit frame well (one short wavelength, one medium and one long). If you have
no experience of this, avoid channels S (Sulphur), P (Phosphorus) and Pb (Lead) which are difficult to
measure. If you do not have a Fe base, request advice from the service engineer who installs your instrument.
A homogeneous profiling sample should be selected. It should contain a sufficient concentration of element
to be profiled, so that the maximum profile response on the readout multimeter is at least at 80% of a full
scale. You can change the scale's sensitivity among four choices by moving the sliding knob of the vacuum
and profile board. Keep in mind the bar has 6 positions, two of them are for vacuum reading and
measurement.
1
(vacuum)
2 _
3
4 profile
5 sensitivity
6 +
Figure 4.7
It is preferable to always use the same sample. It is not necessary to use a certified standard, nor a standardi-
sation sample. It just has to be relatively homogeneous, contain enough of the elements to be profiled and its
surface preparation must be correct.
The software will request the source conditions (of the sparks); use a condition specially created for the
direct profile taking and always keep to the same one.

Note: If such a condition still does not exist, you must create it. Name it PROFILE for example, and
copy the parameters of another standard condition, but change the integration time; you should
enter a sufficient large time in order to let you to take the profile, for example 150 seconds. See our
example, later on figure 4.9.
The profile position must be taken quickly, but nevertheless care must be taken to perform this important
task properly. The source operates permanently and it is not advisable to overheat the sample too much, nor
to form a crater in it. With practice you will only need a maximum of thirty seconds to find the profile
position of an element (some elements are volatile in the sample and you will have to be faster).
The analogue deviation of the direct profile watched on the multimeter is not always very stable and this
is quite normal. This is where your experience and your judgement take on their importance.

4.8.1.2 Direct Profile Taking
There are three monitoring modes for the direct profile:

Physical galvanometer on the instrument
Virtual galvanometer displayed by the software
Chart display
An example with the virtual galvanometer and chart display is given in the Running Direct Profile section of
the Instrument Status and Profile chapter of the WinOE Operator Manual.
The procedure described below is one of several that are valid, it uses the physical galvanometer of the in-
strument. If necessary, ask the service engineer who does the installation to give you a demonstration.
From the menu choose Initialisation, click on the Direct Profile icon.
Figure 4.8

The next dialogue box is displayed
Figure 4.9
Choose an analytical condition valid for the direct profile (our example FEGEN), then a channel to pro-
file (our example: Fe4N).
If necessary change the integration time by entering the maximum (150 seconds).

Click on the Options button, the following dialogue box is displayed.
Figure 4.10
Be sure the Use Instrument Galvanometer check box is checked. If it is the case click on Cancel. If it is
not the case, check it and click on Save as Defaults, and then on OK. You are returned to previous
dialogue box (figure 4.9).
Put the profile sample on the analysis table, and close the stand door.
Click with the mouse on the Start button. The analysis starts.
Note: The analysis will start only if the parameter Automatic Start is Enabled (default value). If the
Automatic Start is Disabled, it will additionally be necessary to press the green START
button on the stand in order to start really the analysis. For selecting the Automatic Start, see
your WinOE Software Configuration Manual.

The dialogue box becomes partially greyed. The Select Channel list box and the Stop button (which now
substitutes the Start button) remain available, as you can see below:
Figure 4.11
At the end of the pre-integration phase (our example 8 seconds) the software put the chosen channel in di-
rect profile mode. You should then see a deviation of the needle of the multimeter. If necessary, change
the scale's sensitivity by changing the position of the bar switch on the vacuum and profile board (see
figure 4.7).

By moving (slightly) the position of the scanning screw forwards and backwards, you can ensure that you
are approximately on the profile average of the element, corresponding to the peak response of the needle.
The ideal is that corresponds to at least 80% of the chosen scale.
Max. > 80%
Figure 4.12
Turn the disk counter clockwise for around 20 divisions.
Figure 4.13

Turn the disk slowly back clockwise until you obtain a deviation on the multimeter of around 70% of the
maximal value that you obtained when you were practically on the maximum of the profile's peak. Use a
graduated position on the multimeter as a reference mark. Read the position on the scanning dial corre-
sponding to this graduated position and note it down on paper. You should read the dial position to the
nearest quarter of a division.
0.6 97
Figure 4.14
Continue turning the scanning screw in the same direction (clockwise) and you will pass the profile maxi-
mum peak and then the deviation on the multimeter will decrease. Stop at the same position on the mul-
timeter (the one you already used for the previous measurement). Read this new position of the scanning
dial and note it on paper.
0.6 110.5
Figure 4.15

The profile position of the element you have just measured (our example: Fe4N) corresponds to the
arithmetic mean of the two positions of the scanning dial.
I
1.0
0.8
1/3
0.6
0.4 = =
2/3
0.2
97 103.75 110.5
97 + 110.5
= 103.75
2
Figure 4.16
To take the direct profile of another channel, click another channel from the Select Channel list box (see
figure 4.11), the signal shown on the galvanometer is now from the new channel.
Note: If you like so, for example for changing the sample position or changing the sample, you can
also stop the procedure (and consequently the sparking on the sample) by clicking the Stop
button. Even then there, you can change the channel, but you will need to start again by pressing
the Start button, and then wait for the end of the pre-integration phase in order to profile this
new channel.
Check by the same way the profile of this new channel, and if needed the other channels to be profiled.
Once all selected channels are profiled, click on the Stop button (figure 4.11). The dialogue box appears
now again as on the figure 4.9.
To get out the Direct Profile routine, click on Exit. This sends you back to the Initialisation menu
(figure 4.8) of the WinOE software.
The instrumental average profile position corresponds to the arithmetic mean of the positions determined
individually for each element (our example 103.75).

Place the scanning dial on this position, first turning the disk counter clockwise at least 20 divisions more
than the position calculated and then coming back to it clockwise (these operations are necessary so as to
compensate any possibly play in the scanning screw).
103.75
Figure 4.17
Keep the average values in a log book in order to observe the evolution. This will help you to decide if the
frequency of the profile taking can be modified.
The instrument is now profiled. Do not forget to standardise before carrying out routine analysis on un-
known samples.
4.8.2 Profile by Integration
4.8.2.1 Basic Advice
The profile by integration is more simple, but in principle longer than the direct profile. The disadvantage is
that the software does not have enough intelligence to interpret a bad measurement, or a profile curve which
can be interfered by an unwanted element. This is why some users prefer the direct profile method.
The method by integration consists of making a certain number of consecutive measurements on the same
sample, by turning regularly (and always in the same direction) the position of the scanning dial between
each measurement.
You must select a sample which contains a good concentration of the elements which you wish to check; a
"synthetic" sample, as long as it is homogeneous, can also be used. The same sample must be used for the
entire profile operation and we recommend that you always use this same sample for subsequent profiling.

4.8.2.2 Measuring the Profile by Integration
From the Main Menu choose Analysis, then Initialise Instrument, and finally Integrated Profile.
Figure 4.18
The integrated profile dialogue box is displayed, as hereunder.
Figure 4.19

Note: Dialogue boxes of this section are described in the Integrated Profile section of the
Instrument Status and Profile chapter of the WinOE Operator Manual.
Choose one analytical condition amongst the proposed ones in the top left window (our example COND1).
Select the channels you want to measure amongst the available ones. The select the ones you want display.
10 channels can be displayed at a time, but all selected channels are measured and can be used later on for
graphical display.
Take a look at the current profile dial position, write it down on paper. Take away around 10 from the profile
value and enter this value as Start Dial Position. In our example we would have read 100 as current
position, therefore we enter 90 as Start Dial Position.
For a quick profile measurement, enter 2 as Step Dial Divisions and 10 as Maximum number of steps. For
a more accurate measurement we recommend to enter 1 as Step Dial Divisions and 20 as Maximum
number of steps.
Click on the Save as Default button to record these parameters as default for a next integrated profile
measurement session.
When you are ready, click on the Start Profile button. The Run Profile dialogue box is displayed.
Figure 4.20

Put the sample on the analysis table, close the stand door.
Put the scanning dial on the position required at the bottom of the screen (our example: 90), do not forget to
compensate the play of the screw.
100 - 10 = 90
Figure 4.21
Click with the mouse on the Start next step button (figure 4.20.) The analysis starts.
Note: The analysis will start only if the parameter Automatic Start is Enabled (default value). If the
Automatic Start is Disabled, it will additionally be necessary to press the green START button
on the stand in order to start really the analysis. For selecting the Automatic Start, see your
WinOE Software Configuration Manual.

Once this first analysis is finished, the absolute intensities of the selected channels are displayed, and a new
position of the scanning dial is required.
Figure 4.22
Move the dial on this new position (our example: 92), by turning always in the same direction. Rotate the
sample in order to not spark it again on a previous spot.
90 + 2 = 92
Figure 4.23
Run the next measurement by clicking with the mouse on the Start next step button (figure 4.22). The
analysis starts.

Once this new analysis is finished, the absolute intensities of the selected channels are displayed, and a new
position of the scanning dial is required.
Move the dial on this new position (our example: 94), by turning always in the same direction. Rotate the
sample in order to not spark again on a previous spot.
Repeat the measurements until the Maximum Number of Steps predefined is accomplished or until the
computer enables the Calculate Average button. The Calculate Average button becomes available when at
least the profile position of two channels have been found; but we recommend to calculate the average on
more than two, possibly all selected elements, to have a better accuracy.
As soon a profile position is found for a channel, the value is displayed in the Profile Position group box
under the corresponding channel name. Once the operation has been completed (i.e. the profile position for at
least two, but preferably all selected channels, has been found), press on the Calculate Average button so
that the computer calculates the average profile position.
If for example the software has determined the average profile position at 100.6 dial divisions, set the
scanning dial on that calculated average value; do no forget to compensate the possible play in the scanning
screw.
100.6
Figure 4.24
Click on the Print Results button (figure 4.22), and keep the printout in a log binder in order to follow the
profile taking evolution. The software has more functions, for example graphical displays (Scan Graphics
button, see the WinOE Operator Manual).
Finally click on Exit. The software asks you if you want to save the session in a file. Answer either by Yes
or No. For more details refer to the Integrated Profile section of the Instrument Status and Profile chapter of
the WinOE Operator Manual.

The integrated profile dialogue box is again displayed, as hereunder.
Figure 4.25
If you want so, you can run a new batch of measurements with another sample, in order to determine profile
positions of other elements. Otherwise, you can quit the routine by clicking on the Exit button, this lead you
back to the Initialisation menu of the WinOE (figure 4.18).
The instrument is now profiled. Do not forget to standardise before carrying out routine analysis on unknown
samples.

4.9 Greasing of the Stand Door's Hinges

Once a month the stand door's hinges and the sample clamp's rod must be greased. Use bearing grease,
number AA24714.
4.10 Lens Cleaning

We recommend that you clean the lens every six months. In case of very high throughput the frequency
could be reduced to two months. When the values of the standardisation factor of the elements measured in
the ultraviolet (<200 nm, for example elements S, P, C, etc.) become high and the instrument is operating in
good conditions (vacuum OK), it probably means that the lens needs cleaning; indeed the elements with
short wavelengths will most early be affected as they will be absorbed by dirt that lay down on the lens.
4.10.1 Lens Holder Extraction

In order to correctly clean the lens, the lens holder must be removed from the stand.
The lens holder must never be dismantled. The lens useful area can easily be cleaned
without dismantling the lens holder.
Do not touch the lens fixing screw or of the heating body and never attempt to re-
move the lens from its holder! Major risks of vacuum leaks and to put optic out or
order!
Heating
supply
contacts
Lens
Figure 4.26
Note: To identify the items in the following extraction procedure, please refer to the figures of the
Stand section of the Layout and Controls chapter.
Open the stand's door, remove the protection plate, turn the manual vacuum shutter completely to the
right.
Remove the analysis table, then remove the primary optical channel taking care to not bend too much the
copper pipe attached to the channel. Remove the lens heating connector.
Slightly untighten the two knurled knobs so as to free the locking clamps. Free the lens holder by
screwing a little the extraction screw (red knurled knob).

Once the lens holder is free, turn it about one eighth of a turn so that the two notches are facing to the
clamps. Then take out the lens holder by pulling it towards you.
Unscrew the red knurled knob so that the extraction screw does not protrude past the lens holder on the
side which will rest against the stand's flange. This is important later when the lens holder will need to be
set back correctly to its working position.
Note: The lens must be warm, if not contact the local Thermo Electron after-sales office.
Proceed to the lens cleaning.
4.10.2 Cleaning
If the lens is not too dirty, cleaning with alcohol can be sufficient. If it is very dirty, proceed as follows: use
iron oxide that is mixed with some alcohol to make a paste, then rinse with alcohol. It is preferable to use a
piece of clean rag or paper (optic paper for example) which does not leave any particles. In order to eliminate
particles that remain on the surface, you can blow with argon (never use compressed air that always contains
a small quantity of greasy matter).
Attention!
The instruments equipped for VUV analysis (nitrogen, oxygen) have a special
lens. Iron oxide (or another oxide) cannot be used for the cleaning the lens
would be destroyed! This special lens can however be cleaned with isopropyl
alcohol (without any other additive). Kindly refer to the manual for the op-
tional VUV lines for more details concerning the handling and the cleaning of
the stand's components.
Once the lens is clean, do not touch the surface with the fingers any more.
When the lens is dry, put it back by doing the operations in the reverse order.
Note: If, after the lens has been cleaned, the values of the standardisation factor for elements
measured in the ultraviolet have not reduced considerably, the two following conclusions
must be considered:
The lens was very dirty and the cleaning has not been efficient enough; it is imperative to
clean it again with iron oxide.
The lens was clean and the cause of the great factors must be looked for elsewhere.

4.11 Changing or Cleaning of the Dust Filters

At least once a month the dust filters situated at the rear of the instrument should be cleaned. If your environ-
ment is very dusty, the filters should be cleaned more often.
For access to the filter, the outside plastic frame must be removed. If you have difficulties to remove the
plastic frame, use a screwdriver as shown on the figure below.
Figure 4.27
In principle, a filter is cleaned with the vacuum cleaner, but it is also possible to wash it in slightly soapy wa-
ter (in this case, only re-install the filter once it is completely dry).
We recommend you to replace the filters by new ones at least once a year, but more frequently if your envi-
ronment is dusty. This exchange is automatically done during a service maintenance visit.
Note: The operation of cleaning the filters should not be neglected. A dirty filter becomes too airtight and
leads to a temperature rise in the cabinet. This can cause a stability loss in the electronic compo-
nents, which affects the results. In addition, the most sensitive components can start having discon-
tinued operation (intermittent breakdown), or complete breakdown.

4.12 Check of the Cabinet Fans

The control electronics is ventilated from the back by two large fans, one in each bay. The proper operation
of these fans must be regularly checked, at least once a week.
To check them, just remove the two front panels of the instrument and observe the operation of the fans. If
one is not rotating, contact immediately your local Thermo Electron service office.
4.13 Analytical Checks

The analytical factor is developed in the Operator Manual. Each case is particular, and there are various
theories to reach the same goal. If in the past we use to standardise systematically at regular intervals, today
the trend is to standardise only when it is necessary.
The use of Control Sample(s), regularly or controlled by computer, helps to determine if it is necessary or
not to standardise (partially or totally) the instrument.
4.13.1 Control Sample

The use of Control Sample(s) is optional, but it helps for an efficient use of standardisation. It can be
controlled by statistical tools (WinOE option) such as the SPC (Statistical Process Control), but it can also be
used manually (regularly or randomly).
If this operation is not controlled by the software, we recommend to run at least once a day the Control
Sample(s).
The tolerance limits entered in the software (or otherwise the inspection of result deviancy) will determine
the need or not to standardise.
4.13.2 Standardisation
When Control Sample(s) does not control the standardisation, we recommend to standardise the instrument
at least once a week (at beginning once a day).
The standardisation theory is explained in the Operator Manual.
4.14 Backup
The backup procedure is explained in an appendix of the WinOE Configuration Manual.
Backup should be performed at least once a week.

4.15 Accessories
4.15.1 Sircal Argon Purifier

In order to keep its efficiency, the molecular sieve must be regularly regenerated. Frequency and procedure
are given in the manual supplied with the purifier.
Important:
Before proceeding to the molecular sieve regeneration it is mandatory to remove the

argon inlet of the instrument by opening the circuit at the purifier outlet. This is needed in
order to avoid impurities and moisture evacuated during the regeneration to enter and
pollute the instrument stand.
However, because it is necessary to have an argon flow during the regeneration, you must
ensure the purifier argon outlet is not closed by the swaglock fitting, if needed add
another fitting with a piece of pipe opened to ambient air.

A
SAMPLE PREPARATION
Sample Preparation Appendix A
A. SAMPLE PREPARATION
A suitable sample taking and a careful surface preparation are absolutely essential. Indeed, it is necessary to
have a sample as homogeneous as possible without inclusions on one hand, and on the other hand a clean
and flat surface is needed in order to insure reliable and reproducible measurements.
For the sample taking, several kinds of moulds can be bought or machined. As well for sample surface prepa-
ration, several kinds of machines that are suitable exist on the market.
Your local representative will gladly advise you about the type and model that will fit at best for your own
application. We remember hereunder only general aspects of the various sample preparation machine types
and their main applications.
The section Sample Taking - Moulds points out a few mould types for the sample taking.
The section Surface Preparation - Sample Preparation Machines points out a few machine types for the
sample's analysis surface preparation.
AA83321 Reference Manual - ARL 3460 A-1

Appendix A Sample Preparation
A.1 Sample Taking - Moulds

The sample taking for spectroscopy analysis is a fundamental step. Several spectroscopy books explain that
stage and advise suitably about the mould's choice for a given application. ISO and ASTM standards also
provide specifications and information about that subject.
Usually:
The sample cooling must be quick so that a fine grain metallic structure is kept.
The mould will be in copper and maintained clean.
The mould in stand-by of use must be turned upside down (or covered) in order to avoid dirties or other
material to be introduced into it.
Here are some examples of moulds that are suitable for casting good quality samples and adapted for optical
emission spectroscopy analysis. A probe for direct sample taking is also shown.
A.1.1 Non Ferrous Metals

The mushroom form sample taking is the most used for non ferrous metals. There are however segregation
risks, and the mould diameter must be adapted.
cut
here
useful surface
for analysis
Figure A.1
A.1.2 Fe, Ni, Co Bases

Here is a very simple mould, frequently used for alloys of Fe, Ni and Co bases. (More specifically for cast
irons and traces, see hereunder sections Cast Irons and Traces)
useful surface
for analysis
Figure A.2
A-2 Reference Manual - ARL 3460 AA83321

A.1.3 Cast Irons

The kind of mould hereunder is specifically adapted for casting cast irons in general, and pig iron in particu-
lar. The cooling speed is very high.
cut
here
useful surface
for analysis
Figure A.3
A.1.4 Traces
The ring mould type, as shown hereunder, is advisable for casting pure metals (traces' analysis), or metals
that will have low tendency to segregation. The ring is of stainless steel or ceramic, so that the sample will be
mostly cooled by the bottom copper plate. The sample is homogeneous on its surface, but only on some
few millimetres in depth!
useful surface
for analysis
Figure A.4

A.1.5 SPEMIS Probe

For steels, the sample taking can be greatly simplified with a SPEMIS probe that can take liquid metal di-
rectly from the casting. The sample obtained has the following form:
cut
here
useful surface
for analysis
Figure A.5

A.2 Surface Preparation - Sample Preparation Machines

It is essential to use an appropriate machine in order to obtain a clean and flat surface. We recommend the
use of one of the following sample preparation machine types:
A.2.1 Disk Sander

This is a sander with a rotary abrasive disk.
Some machines have two disks; that is convenient if a coarse grain is used for preliminary surface
preparation, and a fine grain for final preparation.
abrasive
disk
Figure A.6
This surface preparation method is the quickest way to prepare iron, nickel and cobalt samples (as well as
some few coppers). Sample must be thick enough so that they can be hold with fingers without the risk to in-
jury themselves.
The abrasive paper may always distort the result of some analyses, especially for elements in low
concentration in the sample. The choice of the paper depends on which elements must be determined or not.
The abrasive paper disk based with aluminium and silicon oxide mixed with resin (Al/Si = 1.47) is usually
suitable. A grain of "80" or "60" is recommended. If this paper seems to distort the result on some elements,
try another one that does not content the distorted elements. In case of doubt consult our local service for
advice.
Note: The metals like copper, aluminium, lead, zinc, magnesium, etc., pure or even very low alloyed, and
generally all soft material, cannot be properly prepared on abrasive paper disks.

A.2.2 Surface Grinder

Rotating surface grinders with multiple grindstones fixed on a rotating arm are recommended, as on the
example shown hereunder:
magnetic grindstone
table
Figure A.7
This method is suitable for all sample kinds of steels and cast irons, as well as for nickel and cobalt alloys.
No cooling liquid must be used.
The magnetic samples will be kept still by the magnetic table. The non-magnetic samples must be fixed on a
magnetic vice.
The grindstones must be regularly sharpened, otherwise the risk of surface overheat and deterioration of the
sample is high. This can be the cause of bad sparking spots.
A.2.3 Milling Machine or Lathe

Such a machine should be equipped with a milling cutter or chisel of tungsten carbide.
The milling machine is the ideal machine for preparing all aluminium alloys, as well as pure coppers and
other soft metals. The milling is also the recommended method for the sample preparation of steel analysis
with nitrogen and carbon at lower than the 10 ppm level, or inclusions analysis on the ARL 4460.
For the analysis of oxygen, milling is mandatory to limit surface contamination (CNOPS option on the ARL
4460).

The milling machine is more suitable than a lathe for sample with complex shapes, for example melted or
machined pieces. Moreover, the cutting speed is constant with the milling machine, that insures a regular ma-
chined surface.
The surface preparation is normally done without coolant (i.e. dry). However for aluminium samples a
little of isopropyl alcohol can be used. Oil or any other coolant must be prohibited. The head and the table of
the milling machine, the milling cutter, the vice for holding the sample, must be cleaned before the use for
sample surface preparation if the machine is used for other means that requires oil, water, or another coolant.
As for example, some steel springs can be analysed if prepared like the following picture represents it
(surface preparation by milling or polishing):
screw and nut for

squeezing the spring
useful flat
surface for analysis
Figure A.8
A.2.4 Press Machine

For soft wire sample, one can flatten them with a pressure among 20 to 40 tons with a press.
Figure A.9
If the useful surface to be analysed is smaller than the 15 mm standard hole of the carbide tungsten disk, one
should use another disk, that is equipped with a smaller hole.
A.2.5 Inductive Furnace

Metallic chips can be re-melted in a fusion furnace. This furnace provides solid samples that can be used for
spectroscopy analysis.

B
PLACING THE SAMPLE ON THE

ANALYTICAL TABLE
Placing the Sample on the Analytical Table Appendix B
B. PLACING THE SAMPLE ON THE ANALYTICAL

TABLE
B.1 Putting the Sample

The surface to be analysed should no longer be touched with the fingers after the sample's surface
preparation. This is also valid for the analysis table.
One must avoid doing the analysis on the centre of the sample. It is a known fact the homogeneity is better in
the area near to the edge of the sample. The sample will therefore be placed so that it hides the hole of the
analysis table by about 3 mm on the table's area.
RIGHT WRONG
Figure B.1
AA83321 Reference Manual - ARL 3460 B-1

Appendix B Placing the Sample on the Analytical Table
B.2 Multiple Measurements

Usually in routine analysis, 2 or 3 measurements are carried out on each sample. Sparking spot's overlap
must be avoided. Black halos around the sparking area can however be superposed, except in the case of
oxygen analysis, where the spots must absolutely not crossover.
RIGHT WRONG
Figure B.2
Remark: The analytical table can be damaged, or the hard metal disk can be broken, if the sample
edge is too abruptly set down before covering the hole. If the disk is broken usually the next
analysis will be recognised by a characteristic whistle from the sparking. If the table is
slightly damaged, it is sometimes possible to "repair" such a damaged table with an oilstone.
However if the disk is cracked or broken the table must be exchanged.
B-2 Reference Manual - ARL 3460 AA83321

Placing the Sample on the Analytical Table Appendix B
B.3 Sample Stop

The use of the sample stop is optional. Its function is a stop guide jig for positioning the sample.
The sample stop can be used on its two faces. When you put the sample stop on the table you must be sure
the two little rubbers down the stop lay on the hard metal disk.
The next figure shows one sample positioning example using the sample clamp on each both faces.
Figure B.3
AA83321 Reference Manual - ARL 3460 B-3

C
SPECIAL PROCEDURES
Special Procedures Appendix C
C.SPECIAL PROCEDURES
This appendix brings together the particular routine maintenance procedures required for the analysis of
some alloys, in relation to the ordinary routine maintenance procedures described in the Routine
Maintenance chapter of this manual.
This concerns:
Magnesium Alloy Matrix
For all matter not explicitly described in this appendix, refer to the procedures described in the Routine
Maintenance chapter.
AA83321 Reference Manual - ARL 3460 C-1

Appendix C Special Procedures
C.1 Magnesium Alloy Matrix
C.1.1 General Consideration

The analysis of magnesium samples by sparking produces inevitably magnesium powder.
This magnesium powder has a chemical property to catch fire or at least to make sparkles
when oxidising (in contact with the air). In an airtight environment a sudden air entrance
may even generate a small explosion. If the oxidation is slow, these effects are greatly
reduced.
It is thus necessary to act with prudence with the maintenance of the parts likely to store
magnesium.
C.1.2 Working Constraints

A special argon filtering device must be used on the exhaust. In the case of a multi bases instrument with the
Mg base, a commutation valve is inserted in order to reroute the argon exhaust either on the special Mg filter
kit or to the traditional argon filtering system. Waiting time constraints tied to the commutation between the
devices are to be considered too. The Mg Filter Kit manual relating safety instructions, and the maintenance
of the filtering device is supplied with the instrument and must imperatively be read. The procedures inside
this manual must be applied in order to ensure the safety of the personal.
The use of single tip electrode, to prevent from mounting it in the inverse direction, and consequently to pre-
vent from confining an eventual magnesium deposit into the cavity under the electrode holder cylinder.
C.1.3 Particular Equipment and Tools

The use of acid being recommended for the cleaning of some hardware, the availability of a chemistry labo-
ratory or at least a working place under a ventilated vault is necessary.
Because of the risk of catching fire, the operator must wear fire-resistant gloves, safety glasses and a visor to
carry out the maintenance of the stand and argon exhaust filter.
In no case Thermo Electron can be held responsible if the instructions are not respected.
The following material is also necessary:

A vacuum cleaner with a water circuit for the aspiration and neutralisation of the dust produced by the
sparking of the samples.
Beakers and watch glasses for the cleaning with acid of the stand parts
Hydrochloric acid at 5% (vol.).
Demineralised water
Ethyl alcohol
Paper tissue
C-2 Reference Manual - ARL 3460 AA83321

Special Procedures Appendix C
C.1.4 Particular Procedures
C.1.4.1 Stand and Special Filtering Device Maintenance
The maintenance of the stand components and of the special filtering device is fully described in the
Operation chapter of the Mg Filter Kit manual. You must strictly follow the directions written of this
manual.
When the instrument is a multi bases one, a dual argon exhaust system with a commutation valve is installed.
Concerning the maintenance of the traditional filter (standard or VUV) used for the other bases than the Mg
base, refer to the procedure described in the Argon Outlet Filter section of the Routine Maintenance chapter
of the present manual.
For the cleaning of the stand components (table, hard metal disk, insulator, electrode, cylinder), refer to the
Cleaning of Stand Components section below.
C.1.4.2 Cleaning of Stand Components
The cleaning directions given in this manual (sections Cleaning of the Large Electrode and Cleaning of the
Stand and the Sparking Chamber of the Routine Maintenance chapter) can be followed. However the use of
acid for the cleaning of the analytical hardware is efficient in order to limit contamination sources. But the
products to be used are toxic and present a real potential risk of burns by acid.
The maintenance with acid described in this section can be executed only if you have the availability of a
chemistry laboratory or at least a working place under a ventilated vault. The use of concentrated acid im-
plies that this maintenance must be done by qualified personal only, under the supervision of a chemist or a
metallurgist.
Only trained and qualified personnel must handle the acids.
In no case Thermo Electron can be held responsible in the event of accident due to
handling of the chemicals products used.
If you do not have the equipment nor the competences, forget this solution.
The acid that must be used for the cleaning of the hardware used with the Mg base is the Hydrochloric acid
(HCl) at 5% (vol.).
The analysis table and the bottom of the sparking chamber cannot be cleaned with acid! The cleaning
must be done as following:
Clean the bottom of the sparking chamber with paper tissue if necessary slightly moisten with ethyl
alcohol if the part is dirty. Let well dry.
Clean conscientiously the analytical table with a vacuum cleaner and then with paper tissue slightly
moisten with ethyl alcohol, because the table cannot be cleaned with acid.
The electrode and the insulator can be cleaned with acid according to the following directions:
Electrode cleaning
Plunge the electrode tip for 3 cm in HCl acid 5% (vol.) during approximately 1 minute (until the bubbles
stop), rinse with demineralised water and wipe with paper tissue.
AA83321 Reference Manual - ARL 3460 C-3

Appendix C Special Procedures
Insulator cleaning
Usually a simple cleaning with paper tissue is enough. But when the cleaning with paper tissue leaves
blackish tracks, plunge the part for some seconds in HCl acid 5% (vol.), rinse with demineralised water and
wipe with paper tissue.
C.1.4.3 Other Subjects
For all the other parts concerning the Mg filter kit, refer to the special Mg Filter Kit manual.
For all the other maintenance subjects not explicitly described in the special Mg Filter Kit manual or this
appendix, refer to the Routine Maintenance chapter and its Summary Table section.
C-4 Reference Manual - ARL 3460 AA83321

Thermo Electron Corporation
81 Wyman Street
P.O.Box 9046
Waltham, Massachussets 02454-9046
Thermo Electron SA
United States CH-1024 Ecublens
is ISO 9001 certified
www.thermo.com

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ARL 3460

Date April 2005

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REVISION CONTROL SHEET

Date Modification Description

1. INTRODUCTION ........................................................................... 1-1

1.1 CONFORMITY TO STANDARDS ................................................. 1-2

1.2 SAFETY......................................................................................... 1-3

1.3 DOCUMENTATION....................................................................... 1-5

2. SIMPLIFIED TECHNICAL DESCRIPTION ................................... 2-1

2.1 FUNCTION PRINCIPLE ................................................................ 2-1

2.2 STRUCTURE OF THE INSTRUMENT.......................................... 2-3

2.3 ANALYTICAL PROGRAM AND OPTICAL LAYOUT..................... 2-4

2.4 THE EXCITATION......................................................................... 2-5

2.5 THE SPECTROMETER ................................................................ 2-7

2.6 THE ELECTRONIC RACK ............................................................ 2-9

2.7 THE COMPUTER........................................................................ 2-11

2.8 THE INTERCONNECTIONS ....................................................... 2-13

3. LAYOUT AND CONTROLS .......................................................... 3-1

3.1 CABINET, GENERAL VIEW.......................................................... 3-2

3.2 UNIT AND SUB-ASSEMBLIES ..................................................... 3-4

AA83321 Reference Manual - ARL 3460 I

3.3 STAND .......................................................................................... 3-9

3.4 HI-REP SOURCE ........................................................................ 3-14

3.5 POWER DISTRIBUTION RACK.................................................. 3-16

3.6 ELECTRONIC RACK .................................................................. 3-18

3.7 VACUUM PUMPING LINE .......................................................... 3-21

3.8 WATER COOLER ....................................................................... 3-25

3.9 ARGON CIRCUIT........................................................................ 3-26

3.10 OVEN AND SPECTROMETER ................................................... 3-28

4. ROUTINE MAINTENANCE ........................................................... 4-1

4.1 FOREWORDS............................................................................... 4-1

4.2 APPLICATION DOMAINS OF PROCEDURES............................. 4-2

4.3 SUMMARY TABLE........................................................................ 4-3

4.4 ANALYSIS ELECTRODE .............................................................. 4-4

4.5 CLEANING OF THE STAND AND THE SPARKING CHAMBER.. 4-6

4.6 ARGON OUTLET FILTER............................................................. 4-9

II Reference Manual - ARL 3460 AA83321

4.6.2 VUV OPTION SYSTEM .................................................................................4-10

4.7 VACUUM PUMPING LINE .......................................................... 4-11

4.8 PROFILE CHECK........................................................................ 4-13

4.9 GREASING OF THE STAND DOOR'S HINGES......................... 4-30

4.10 LENS CLEANING........................................................................ 4-30

4.11 CHANGING OR CLEANING OF THE DUST FILTERS ............... 4-32

4.12 CHECK OF THE CABINET FANS............................................... 4-33

4.13 ANALYTICAL CHECKS............................................................... 4-33

4.14 BACKUP...................................................................................... 4-33

4.15 ACCESSORIES........................................................................... 4-34

A. SAMPLE PREPARATION ............................................................A-1

A.1 SAMPLE TAKING - MOULDS ....................................................... A-2

AA83321 Reference Manual - ARL 3460 III

A.1.5 SPEMIS PROBE............................................................................................. A-4

A.2 SURFACE PREPARATION - SAMPLE PREPARATION

B. PLACING THE SAMPLE ON THE ANALYTICAL TABLE ...........B-1

B.1 PUTTING THE SAMPLE ............................................................... B-1

B.2 MULTIPLE MEASUREMENTS...................................................... B-2

B.3 SAMPLE STOP ............................................................................. B-3

C.1 MAGNESIUM ALLOY MATRIX .....................................................C-2

IV Reference Manual - ARL 3460 AA83321