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ATOMIC SPECTROSCOPY

PINAACLE 900 SERIES

Customer Hardware and


Service Guide
PinAAcle 900 Series

Customer Hardware and Service Guide


Release Information
Part Number Release Publication Date
09931201 A January 2015
Any comments about the documentation for this product should be addressed to:

User Assistance
PerkinElmer
710 Bridgeport Avenue
Shelton, CT 06484-4794
U.S.A.

Or emailed to: info@perkinelmer.com

Manufacturer:
PerkinElmer Singapore Pte Ltd
28, Ayer Rajah Crescent,
#04-01/08,
Singapore 139959

Notices
The information contained in this document is subject to change without notice.
Except as specifically set forth in its terms and conditions of sale, PerkinElmer makes no warranty of any kind with
regard to this document, including, but not limited to, the implied warranties of merchantability and fitness for a partic-
ular purpose.
PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in connection with fur-
nishing, performance or use of this material.

Copyright Information
This document contains proprietary information that is protected by copyright.
All rights are reserved. No part of this publication may be reproduced in any form whatsoever or translated into any
language without the prior, written permission of PerkinElmer, Inc.

Copyright © 2015 PerkinElmer, Inc.

Trademarks
Registered names, trademarks, etc. used in this document, even when not specifically marked as such, are protected by
law.

PerkinElmer is a registered trademark of PerkinElmer, Inc.


Windows is a trademark and Microsoft is a registered trademark of Microsoft Corporation.
Customer Service .............................................................................. xiii
Safety and Regulatory Information ................................................... xiv
How this Guide is Organized ........................................................... xvii

Chapter 1. Safety Practices .................................................... 1


Overview ...............................................................................................1
Precautions ............................................................................................2
Environmental Conditions ....................................................................3
Electrical Safety ....................................................................................4
Fuses .....................................................................................................6
Warning Labels on the Instrument ........................................................6
Safe Handling of Chemicals ...............................................................13
Waste Disposal ..................................................................................15
UV Radiation ......................................................................................17
Magnetic Field ....................................................................................17
High Temperatures .............................................................................18
Handling Compressed Gases ..............................................................19
Safe Handling of Gas Cylinders .........................................................21
Safety Practices for Flame Atomization .............................................23
Safety Practices for Electrothermal Atomization ...............................29
Safety Practices for FIAS and Mercury Hydride Systems ..................31
Decontamination and Cleaning ...........................................................33
WEEE Instructions for PerkinElmer Products ...................................34
References for Laboratory Safety Practice .........................................35

Chapter 2. Preparing Your Laboratory ............................. 37


Introduction .........................................................................................37
Environmental Requirements .............................................................37
Lab Space Requirements ....................................................................38
Fume Ventilation ................................................................................41
Magnetic Field (PinAAcle 900T and 900Z Only) ..............................46
Line Power Requirements ...................................................................47
Gas Requirements ...............................................................................52
Furnace Gas Requirements .................................................................55
Flame Gas Requirements ....................................................................56
Atomic Absorption Source Lamps .....................................................64
Drain Vessels ......................................................................................65
Cooling Requirements ........................................................................66
PC Configuration and Printer .............................................................67
Installation Preparation .......................................................................67
Product Line Experience .....................................................................68

Chapter 3. Principles of Operation ..................................... 69


The PinAAcle 900 Series Spectrometer System .................................69
Intended Use .......................................................................................69
Concept ...............................................................................................69
Principle of Operation of an Atomic Absorption Spectrometer .........70
The Electrical Connectors and Switches ............................................79
The Gas and Cooling Connectors .......................................................82
Burner Assembly System ....................................................................83
Specifications ......................................................................................92
Chapter 4. Installation ........................................................101
Introduction .......................................................................................101
Unpacking Instructions .....................................................................103
Before You Install the Spectrometer ................................................105
If You Must Move and Reinstall the Spectrometer ..........................106
Connecting the Gases ........................................................................111
Connecting the Computer and Printer ..............................................119
Electrical Connections ......................................................................121
Installing the Cooling System ...........................................................126
Connecting the Drain System to the Burner .....................................130
Nebulizer Installation ........................................................................135
Installing AS 900 Furnace Autosampler ...........................................135
Installing the Sample Capillary .........................................................146
Installing S10 Autosampler ..............................................................160
Lamps ................................................................................................160
Replacement Parts .............................................................................160
Shipping List for the PinAAcle 900F ...............................................161
Shipping List for the PinAAcle 900H ...............................................162
Shipping List for the PinAAcle 900T ...............................................164
Shipping List for the PinAAcle 900Z ...............................................167

Chapter 5. Preparing the System .......................................169


Switching on the System ...................................................................169
Installing the Lamps ..........................................................................172
Installing Sample Trays ....................................................................177
Setting up the System for Analyses Using the Flame Technique .....180
Setting up the System for Analyses Using the Furnace
Technique For the PinAAcle 900 T/Z ..............................................186
Setting up the System for Analyses Using the Furnace
Technique For the PinAAcle 900 H .................................................189
Setting up the AS 900 Autosampler .................................................195
Shutting Down the System ...............................................................196

Chapter 6. Maintenance ......................................................199


Introduction .......................................................................................199
Calibration of the Instrument ............................................................200
General Maintenance Checklist ........................................................200
Instrument Maintenance Checklist ...................................................201
Cleaning the Instrument ....................................................................202
Checks ...............................................................................................202
Burner Maintenance Checklist ..........................................................203
Spectrometer Maintenance Checklists ..............................................206
Changing the Air Filter .....................................................................207
Changing the Vent Filter ...................................................................210
Changing the Fuses ...........................................................................211
Cleaning the Burner Chamber ..........................................................212
Cleaning the Burner System .............................................................217
Cleaning the Burner Head .................................................................218
Pre-Conditioning a New Burner or Drain Tube ................................220
Removing the Burner Assembly From the Instrument .....................221
Removing the Burner Head ..............................................................224
Disassembling the Burner Chamber .................................................224
Reassembling the Burner System .....................................................226
To Install the Burner in the Spectrometer .........................................226
To Install the Burner Head ................................................................229
Drain System Maintenance ...............................................................229
Organic Drain Assembly ..................................................................235
Nebulizer Removal and Reinstallation .............................................235
PinAAcle 900 Metal Body Nebulizer ...............................................238
Metal Body Nebulizer with Organic Solvent Resistant O-Rings .....247
High Sensitivity Plastic Nebulizer ....................................................257
High Sensitivity Plastic Nebulizer with Chemical Resistant
O-Rings .............................................................................................269
Removing and Replacing the Nebulizer's Impact Bead ....................277
Reassembling the Nebulizer .............................................................279
Replacing Parts of Wear ...................................................................282
Maintaining the Acetylene Supply ...................................................284
Lamp Maintenance and Cleaning .....................................................285
Replacing the Lamps ........................................................................285
Removing and Replacing the Deuterium Arc Background
Corrector Lamp .................................................................................287
Graphite Furnace Maintenance for the PinAAcle 900T/900Z ..........295
Graphite Furnace Maintenance for the PinAAcle 900H ...................331
S10 Autosampler Maintenance .........................................................357
AS 900 Furnace Autosampler Maintenance .....................................357
Replacement Parts .............................................................................362
Replacement Parts for the PinAAcle 900 .........................................363

Chapter 7. Troubleshooting ............................................... 377


Overview ...........................................................................................377
Introduction ......................................................................................377
Performance Problems ......................................................................378
Customer Service xiii

Customer Service
Company Name and Address:

PerkinElmer
710 Bridgeport Avenue
Shelton, Connecticut 06484-4794 USA
Tel: (800) 762-4000 or (203) 762-4000

Every day you count on PerkinElmer to provide you with solutions that deliver
reliable performance, control operating costs and maximize operational time. Our
complete portfolio of consumables, parts, supplies, training and service helps you
meet both routine and demanding measurement challenges. We invest heavily in
testing and validating our products to ensure you receive guaranteed compatibility
and performance-on-time, every time, for every instrument in your laboratory.

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


PerkinElmer, using the part numbers quoted in the guides provided with the
instrument. For the service and maintenance of the instrument, you should contact
your local PerkinElmer Sales or Service offices, or visit our website:

http://perkinelmer.com

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

To place an order for supplies and many replacement parts, request a free catalog,
or ask for information:

If you are located within the U.S., call toll free 1-800-762-4002, 8 a.m. to

8 p.m. EST. Your order will be shipped promptly, usually within 24 hours.

If you are located outside of the U.S., call your local PerkinElmer sales or service
office.
xiv

Safety and Regulatory Information

Safety Information in the Manual


Safety information is contained in Chapter 1 of this manual. Before setting up and
operating this instrument, carefully read the safety precautions described in
this chapter and observe them at all times.

Caution The protection provided by this equipment may be impaired if


the equipment is used in a manner not specified by PerkinElmer.

This manual contains important information regarding potential hazards that may
arise during the operation of the instrument. It is essential that this information is
read and thoroughly understood by all potential users of the instrument.

The instrument should be used according to the instructions provided in this


manual. If used otherwise, the protection provided by the instrument may be
impaired.

In this manual, the following graphic symbols and special text formats are used to
set apart important safety information.
Any of the following safety conventions can be used throughout this guide:

A warning indicates an operation that could cause personal injury if


! precautions are not followed.
Warning

This symbol alerts you to the risk of electric shock that could result in personal
injury to yourself or other persons.
Details about these circumstances are in a box like this one.
Safety and Regulatory Information xv

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

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

This symbol alerts you to the risk of strong magnetic fields that could cause
injury to persons wearing a heart pacemaker or having metallic implants.
Details about these circumstances are in a box like this one.

Caution A caution indicates an operation that could cause instrument damage


if precautions are not followed.
xvi

Regulatory Information

Safety compliance
Safety information is located in the European Union Declaration of Conformity.

Electrical protection
Insulation
Class I as defined in EN 61010-1.

Installation category
This instrument is able to withstand transient overvoltage according to
Installation Category II as defined in EN 61010-1 and IEC 664.

Pollution degree
This equipment will operate safely in environments that contain nonconductive
foreign matter and condensation up to Pollution Degree 2 as defined in
IEC 1010-1 and IEC 664.

Electromagnetic compatibility (EMC)

European Union (EMC Directives)


All information concerning EMC standards is in European Union Declaration
of Conformity and these standards may change as the European Union adds new
requirements.

United States (FCC)


This instrument is classified as a digital device used exclusively as industrial,
commercial, or medical equipment. It is exempt from the technical standards
specified in Part 15 of FCC Rules and Regulations, based on Section 15.103 (c).
How this Guide is Organized xvii

How this Guide is Organized


Thoroughly read the Safety chapter before using the instrument. Consult the
appropriate reference materials listed at the end of the Safety chapter.

Read Chapter... To find out about...

1 Introduction This chapter contains a brief


introduction on the instrument, the
conventions and warnings used in the
manual.
2 Safety Practices Important safety information is
provided in this chapter.
3 Preparing Your Laboratory The preparation of your laboratory
needed for the PinAAcle 900 Series.
Laboratory requirements for the
instrument are reviewed in this chapter.
4 Principles of Operation This chapter contains information on
the components of the instrument, how
it works and instrument specifications.
5 Installation Information on moving and reinstalling
your instrument is provided.
6 Preparing the System for Information on preparing your
Analysis instrument for analysis is provided.
7 Maintenance Maintenance and cleaning procedures
for the various components of your
instrument are provided.
8 Troubleshooting Performance checks, troubleshooting
information and software.
xviii

Using the Index


Use the index to look up information on the different hardware components. If you
need to find information on cleaning the nebulizer, for example, look up
“nebulizer” in the index. Also, use the index to look up information on the
following topics:
• installation
• maintenance
• troubleshooting

A Word on Troubleshooting
We recommend that you consult the troubleshooting information included in this
manual before you call a PerkinElmer service engineer. The Troubleshooting
chapter contains suggestions to help you determine systematically whether
instrument problems are due to improper analytical techniques, improper selection
of instrument parameters, or malfunction of the instrument.

Conventions Used in this Manual


Normal text is used to provide information and instructions.

Bold text refers to text that is displayed on the screen.

UPPERCASE text, for example ENTER or ALT, refers to keys on the PC


keyboard. '+' is used to show that you have to press two keys at the same time, for
example, ALT+F.

All eight digit numbers are PerkinElmer part numbers unless stated otherwise.

Software Help
This manual contains hardware information for PinAAcle 900 Series instruments.
For information on the software for the PinAAcle 900 Series, see the following
help file.

• This software help file can be accessed by opening the software application
and selecting Help > Contents and Index from the menu bar.
Safety Practices 1
Overview
This chapter describes the general safety practices and precautions that must be
observed when operating the PinAAcle 900 Series.

This advice is intended to supplement, not supersede, the normal safety codes in
the user's country. It is also a supplement to the PerkinElmer standard Safety and
Health Policy. The information provided does not cover every safety procedure
that should be practiced. Ultimately, maintenance of a safe laboratory environment
is the responsibility of the analyst and the analyst's organization.

Please consult all manuals supplied with the PinAAcle Series and accessories
before you start working with the instrument. Carefully read the safety information
in this chapter and in the other manuals supplied. When setting up the instrument
or performing analyses or maintenance procedures, strictly follow the instructions
provided.

Note This equipment requires no specified inspection or preventive


maintenance to ensure the continuous functioning of its safety features.
2 Safety Practices

Precautions

Be sure to read and understand the precautions listed below. It is also


! recommended to post a copy of the precautions near or on the instrument
shelf.
Warning

Caution The protection provided by this equipment may be impaired if the


equipment is used in a manner not specified by PerkinElmer.

The laboratory manager is responsible for warning operators of this


! instrument about biohazardous materials that are processed in this
instrument and about waste that results from the operation of this
Warning instrument.

Warning: Explosive Atmosphere


! This instrument is not designed for operation in an explosive atmosphere.
Warning

The following precautions must be observed when using the PinAAcle Series:

• Be sure that the voltage of the PinAAcle Series corresponds to the voltage
used in your laboratory.

• Never remove the side panels of the PinAAcle Series without shutting
down the instrument and disconnecting the instrument power cord from
line power.

• Only high quality purge gases should be used with the PinAAcle Series.
Minimum purity of 99.9% is recommended. A high quality filter-dryer
Environmental Conditions 3

accessory is recommended for the removal of any moisture from the purge
gases.

• Before the instrument is installed, the area around, under and behind the
instrument's planned location is to be cleared of any dirt and dust to
prevent their entry into the instrument's interior which could cause a
negative effect on performance.

• Do not position the instrument so that it is difficult to disconnect the mains


power switch on the rear panel.

• Keep the work area scrupulously clean to avoid contaminating your


samples and to maintain a safe working environment. Clean up spilled
chemicals immediately and dispose of them properly.

• Do not allow smoking in the work area. Smoking is a source of significant


contamination and also a potential route for ingesting harmful chemicals.

• Do not store, handle, or consume food in the work area.

• When you remove the instrument from storage and before you put it into
operation, allow it to stand for at least a day under the approved operating
conditions.

Environmental Conditions
The instrument will operate correctly under the following conditions:

• Indoors.

• Ambient temperature +10 °C to +35 °C (+50 °F to +95 °F), with a


maximum change not exceeding 2.8 °C (5 °F) per hour.
• Safe temperature range: +5 °C to +40 °C (+41 °F to +104 °F).

• Ambient relative humidity: 20% to 80%, without condensation.

• Altitude: in the range -400 m to 2 000 m (-1300 to 6500 feet).

• The location must be free of dust, smoke, and corrosive fumes.


4 Safety Practices

• Mains fluctuations not exceeding ± 10% of the nominal voltage.

You can store the instrument safely under the following conditions:
• Ambient temperature: -20 °C to +60 °C (-4 °F to +140 °F).
• Ambient relative humidity: 20% to 80%, without condensation.
• Altitude: in the range -400 m to 12 000 m (-1300 to 39 000 feet).

When you remove the instrument from storage and before you put it into operation,
allow it to stand for at least a day under the approved operating conditions.

Electrical Safety

Lethal voltages are present at certain areas within the instrument.


Installation and internal maintenance of the instrument should only
be performed by a PerkinElmer service engineer or similarly
Warning authorized and trained person.

When the instrument is connected to line power, opening the instrument


covers is likely to expose live parts. Even when the power switch is off,
high voltages can still be present. Power supplies inside the instrument
may still be charged even if the instrument has been disconnected from
all voltage sources.

Grounding circuit continuity is vital for safe operation of the


equipment. Never operate equipment with grounding conductor
disconnected.
Warning
Electrical Safety 5

Connect the instrument to an AC line power outlet that has a


protective ground connection. To ensure satisfactory and safe operation
of the instrument, it is essential that the protective ground conductor (the
Warning green/yellow lead) of the line power cord is connected to true electrical
ground. Any interruption of the protective ground conductor, inside or
outside the instrument, or disconnection of the protective ground terminal
may impair the protection provided by the instrument.

Grounding circuit continuity is vital for safe operation of the


equipment. Grounding is accomplished by use of an IEC60309
instrument power plug furnished by the factory and not removed during
Warning or after installation.

The instrument must be correctly connected to a suitable electrical supply. The


supply must have a correctly installed protective conductor (earth ground) and
must be installed or checked by a qualified electrician before connecting the
instrument.

Any interruption of the protective conductor (earth ground) inside or


! outside the instrument or disconnection of the protective conductor
terminal is likely to make the instrument dangerous. Intentional
Warning interruption is prohibited.

Do not operate the instrument with any covers or parts removed.


! Disconnect the power cord from the AC line power wherever the cover is
removed.
Warning

When working with the instrument:


6 Safety Practices

• Connect the instrument to a correctly installed line power outlet that has a
protective conductor connection (earth ground).
• Do not operate the instrument with any covers or internal parts removed unless
required to do so.
• Never leave the instrument unattended with the cover off and connected
to AC power!
• Do not attempt to make internal adjustments or replacements except as
directed in the manuals.
• Disconnect the instrument from all voltage sources before opening it for any
adjustment, replacement, maintenance, or repair. If afterwards, the opened
instrument must be operated for further adjustment, maintenance, or repair,
this must only be done by a qualified person who is aware of the hazards
involved.
• Whenever it is possible that the instrument is no longer electrically safe for use,
make the instrument inoperative and secure it against any unauthorized or
unintentional operation. The electrical safety of the instrument is likely to be
impaired if, for example, the instrument shows visible damage; has been
subjected to prolonged storage under unfavorable conditions; or has been
subjected to severe stress during transportation.

Fuses
Use only fuses with the required current rating and of the specified type for
replacement.

Do not use makeshift fuses or short-circuit the fuse holders.

Warning Labels on the Instrument


Any of the following symbols can be used on the instrument:

This symbol indicates that there is a potential hazard and that the user must look
in the guide for an explanation of the hazard and how to avoid it.
Warning Labels on the Instrument 7

This symbol indicates the risk of electric shock.

This symbol indicates the risk of hot surfaces.

This symbol indicates that there is a potential hazard due to a strong magnetic
field and that persons wearing heart pacemakers should remain at least 0.6 m
away from the furnace.

This symbol indicates the risk of laser radiation.

This symbol indicates the off position of the main power switch or circuit
breaker. With the switch in this position, the instrument is disconnected entirely
from the line power supply.

This symbol indicates the on position of the main power switch or circuit breaker.
With the switch in this position, the instrument is connected to the line power
supply but is not necessarily switched on and operational.

This symbol indicates the operational on/off switch.

This symbol indicates alternating current.

! When this label is attached to an instrument it means refer to the manual.


8 Safety Practices

Warning Labels at the Front of the Instrument

Graphite Furnace Labels


1
3

Item Description Item Description


1 Warning - No Pacemakers. See Magnetic Field 3 Warning-Hot Surface
on page 17
2 Warning-Strong Magnetic Field

Item Description
1 Warning-Hot Surface (the PinAAcle 900H)
Warning Labels on the Instrument 9

Burner Locking Mechanism Label

Item Description
1 Press To Lock And Unlock The Latch
10 Safety Practices

Flame Door Labels

1
2

Item Description
1 Warning-Hot Surface
2 Warning-UV Light Hazard. Avoid looking directly at flame
3 Warning-Not to open the door-Chemical Hazard
Warning Labels on the Instrument 11

Warning Labels at the Rear of the Instrument

4
1

2
3

Item Description
1 Warning-To reduce the chance of electric shock do not remove covers that
require tool access. No user serviceable parts are inside. Refer servicing to
qualified service personnel.
2 Warning-Ground circuit continuity is vital for safe operation of this
instrument. Grounding is accomplished by use of an IEC 60309 instrument
power plug furnished by the factory. The plug is not to be removed during
or after installation.
3 Warning-For protection against fire hazard, replace with only same type
and rating of fuse.
4 Warning-Furnace gases minimum and maximum pressures.
12 Safety Practices

Warning Labels at the Sides of the Instrument


Right Side of Instrument

Item Description
1 Caution-Do not restrict air intake or exhaust
Safe Handling of Chemicals 13

Left Side of Instrument

Item Description
1 Caution-Do not restrict air intake or exhaust
Do not use an air filter. This is an air exhaust.

Safe Handling of Chemicals


The responsible body must take the necessary precautions to ensure that the
surrounding workplace is safe and that the instrument operators are not exposed to
hazardous levels of toxic substances (chemical or biological) as defined in
applicable national, state and local health and safety regulations and laws. Venting
for fumes and disposal of wastes must be in accordance with all national, state and
local health and safety regulations and laws.
14 Safety Practices

When using organic solvents, wear safety goggles. It is recommended


! that a sink or the equipment for washing eyes be installed nearby in case
the organic solvent in use comes into contact with the eye(s) or skin.
Warning

Some chemicals used with this PinAAcle 900 Series instrument may be
! hazardous or may become hazardous after completion of an analysis. The
responsible body (for example, the Lab Manager) must take the necessary
Warning precautions to insure that the instrument operators and the surrounding
workspace are not exposed to hazardous levels of toxic substances
(chemical and biological) as defined in the applicable Material Safety
Data Sheets (MSDS) or OSHA or ACGIH or COSHH documents.
Venting for fumes and disposal of waste must be accordance with all
national, state and local health and safety regulations and laws.

Definitions in Warning for Hazardous Chemicals

Responsible body Individual or group responsible for the use and maintenance of equipment, and
for ensuring that operators are adequately trained. [per IEC 61010-1].
Operator Person operating equipment for its intended purpose [per IEC 61010-1]
OSHA Occupational Safety and Health Administration (United States)
ACGIH American Conference of Governmental Industrial Hygienists
COSHH Control of Substances Hazardous to Health (United Kingdom)

• Use, store and dispose of chemicals in accordance with the manufacturer's


recommendation and the applicable national, state, and/or local
regulations.
• Wear appropriate eye protection at all times while handling chemicals.
Depending on the types of chemicals you are handling, wear safety glasses
with the side shields, or goggles, or a full-face shield.
Waste Disposal 15

• Wear suitable protective clothing, including gloves if necessary, resistant


to the chemicals you are handling.
• When preparing chemical solutions, always work in a fume hood that is
suitable for the chemicals you are using.
• Perform sample preparations away from the instrument to minimize
corrosion and contamination.
• Clean up spills immediately using the appropriate equipment and supplies,
such as spill cleanup kits.
• Do not put open containers of solvent near the instrument.
• Store solvents in an approved cabinet (with the appropriate ventilation)
away from the instrument.

Pollution Degree
This product will operate safely in environments that contain nonconductive
foreign matter up to Pollution Degree 2 in EN/IEC 61010-1.

Waste Disposal

Contents of Waste Containers


The materials that you collect in waste containers may include small amounts of
the substances that were analyzed and other chemicals used in the analyses.

Organic solvent waste and aqueous (Inorganic) waste must be separated, in


separate containers for disposal.

If these materials are toxic, corrosive, or contain organics you may have to treat the
collected effluent as hazardous waste. Refer to your local safety regulations for
proper disposal procedures.

Disposing of Defective Lamps


Hollow cathode lamps and electrodeless discharge lamps contain small quantities
of the lamp element in a very pure form. If a lamp containing toxic elements
becomes defective or otherwise unusable, you must treat it as hazardous waste and
16 Safety Practices

dispose of it accordingly. A licensed company in the chemical waste disposal


business can provide lamp disposal in accordance with environmental regulatory
requirements. Please note that PerkinElmer does take back defective lamps for
disposal.

In addition, hollow cathode lamps and deuterium lamps are maintained under
reduced pressure. Handle and dispose of them correctly to minimize the implosion
risk.

For information, the quantities of analyte material contained in the cathodes of


hollow cathode lamps are listed in the table below:

Table 1-1. Quantities of analyte material contained in the


cathodes of hollow cathode lamps

Quantity of material Single-element hollow Multi-element hollow


in the cathode cathode lamps cathode lamps

less than 5 g As, Au, B, Ba, Be, Ca, Na-K, Pt-Ru


Dy, Er, Eu, Ga, Gd, Ge,
Hf, Ho, In, Ir, K, La, Li,
Mg, Na, Nd, Pd, Pr, Pt.
Re, Rh, Ru, Sc, Se, Sm,
Sn, Ta, Tb, Tm, Yb, Y
5-10 g Ag, Al, Bi, Cd, Co, Cr, Ca-Mg, Ca-Zn, Ag-Au,
Mn, Mo, Ni, Sb, Si, Sr, Sn-Te, Ca-Mg-Zn, Ca-
Te, V, W, Zn, Zr Mg-Al
10-15 g Cu, Fe, Hg, Nb, P, Pb, Ti, all other multi-element
Tl HCLs

For EDLs, the quantity of analyte material used is much less than the quantities
used in HCLs. Typically, only several milligrams of material are placed in the EDL
bulb. No PerkinElmer EDLs (System 1 or 2) contain more than 0.05 g of analyte
material.
UV Radiation 17

UV Radiation
You should be aware of the health hazard presented by UV radiation.
• When the instrument is on, do not remove any covers unless specifically
instructed to do so in the guide or you may be exposed to potentially hazardous
UV radiation.
• Always wear UV-absorbing eye protection when viewing any of these sources:
• The flame, especially the nitrous oxide/acetylene flame.
• The graphite furnace when it is heated to incandescence.
• Hollow cathode or electrodeless discharge lamps.
• The deuterium background correction lamp.

Magnetic Field

Zeeman Graphite Furnace Systems (PinAAcle 900T and PinAAcle


900Z)
The electromagnet generates a strong magnetic field inside the furnace during
measurement cycles.
There is a weak, accessible, stray magnetic field around the graphite furnace. This
stray magnetic field can affect heart pacemakers and metallic implants up to 0.6
meter from the furnace in all directions. This stray field can also affect other
instruments, watches, and magnetic storage devices.

Warning - No Pacemakers
There is a potential hazard due to a strong magnetic field and persons
wearing heart pacemakers or other metallic implants should remain at
Warning least 0.6 m away from the furnace.
18 Safety Practices

Figure 1-1. Magnetic fields

High Temperatures

Burner System
The flame can generate temperatures of up to 2800 °C.
• Do not touch the burner head until it has cooled to room temperature.

Graphite Furnace
The THGA graphite furnace can generate temperatures of up to 2600 °C.
Handling Compressed Gases 19

The HGA graphite furnace can generate temperatures of up to 2700 °C.


• Do not touch any part of the graphite furnace until it has cooled to room
temperature.

• Do not attempt to inject a sample into the graphite tube when the furnace is hot.
You may be subjected to fumes from the sudden vaporization of the sample,
and may damage the pipette.

Quartz Tube Atomizer Cell


The quartz tube atomizer cell (QTA-cell) used for the hydride-generation
technique (option) can reach temperatures of up to 1000 °C.

• Do not touch any part of the heating mantle (electrically heated systems), or
the cell holder (flame-heated systems), or the QTA-cell until they have cooled
to room temperature.

Handling Compressed Gases

Note The responsible body must ensure that the type of connector used at the
outlet side of the gas-pressure regulator conforms to applicable national
requirements.

Note The responsible body is responsible for the correct collection and disposal
of waste materials. This includes the necessity for a suitably sized waste
container of appropriately resistant material for the collection of organic
solvent waste and provision for the removal into an appropriate exhaust
system of any gases or vapors which may be produced in hazardous
concentrations.

Note The responsible body must carry out appropriate leakage tests necessary
for safety on those gas and liquid connections which the operator is
directed to assemble during installation, normal use, or maintenance.
20 Safety Practices

Note The permanent installation of gas supplies is the responsibility of the user
and should conform to local safety and building regulations.

Summary of Gas Hazards


Hazards associated with the different gases used in atomic absorption spectrometry
are presented in the table below:

Table 1-2. Gas Hazards

Spontaneous Decomposition
Gas Suffocation Explosion
or Combustion

Air - - -
Argon x - -
Nitrogen x - -
Acetylene (ethyne, C2H2) x x x

Nitrous Oxide (dinitrogen x - x


monoxide, N2O)

Contact the gas supplier for a material safety data sheet (MSDS) containing
detailed information on the potential hazards associated with the gas.

Warning: Compressed Gases

! High pressure gas cylinders can be dangerous if mishandled or misused.


Always handle gas cylinders with caution and observe your local
Warning regulations for the safe handling of gas cylinders.
Safe Handling of Gas Cylinders 21

Identifying Cylinders
• Legibly mark cylinders to clearly identify the contents and status (full, empty,
etc.). Use the chemical name or commercially accepted name for the gas.

Safe Handling of Gas Cylinders


Gas commonly used with the PinAAcle 900 Series include acetylene, compressed
air, nitrous oxide, nitrogen and argon. The major hazard associated with these
gases is suffocation. This can occur if the gas is allowed to escape in an enclosed
area and displaces the oxygen in the air. These gases are neither explosive nor
combustible.

Combustion products may vary with the analysis of each sample. Acetylene (less
than 1 liter) is released during the bleeding of the gas box prior to shutdown. An
exhaust venting system is always required to remove those gases which are
generated during the normal operation of the instrument.

Contact the gas supplier for a material safety data sheet (MSDS)
containing detailed information on the potential hazards associated
! with the gas. Carefully use, store, and handle compressed gases in
cylinders. Gas cylinders can be hazardous if they are mishandled.
Warning

Note The permanent installation of gas supplies is the responsibility of the user
and should conform to local safety and building codes.

Listed below are some general safety practices for the proper identification,
storage, and handling of gas cylinders. Consult the following references for more
detailed information and additional guidelines.

• Compressed Gas Association (USA), “Safe Handling of Compressed


Gases in Containers,” pamphlet no. P 1, 2008.

• Compressed Gas Association (USA), “The Inert Gases - Argon, Nitrogen


and Helium,” pamphlet no. P-9, 2008.
22 Safety Practices

Identification of Gas Cylinders


• Legibly mark cylinders to identify their contents. Use the chemical name or
commercially accepted name for the gas.

Storing Cylinders
Review the following precautions with the customer to ensure the safe use and
storage of gas cylinders.
• Cylinders should be stored in accordance with the regulations and standards
applicable to the customers locality, state, and country.

• Flammable gases must be stored separately from the non-flammable gases and
oxidizing gases stored separately from the non-oxidizing gases.
• When cylinders are stored indoors in storage rooms, the storage room should
be well ventilated and dry. Ensure that the ventilation is adequate to prevent
the formation of dangerous accumulations of gas. This is particularly important
in small or confined areas.
• Do not store cylinders near elevators, gangways, or in locations where heavy
moving objects may strike or fall against them.
• Use and store cylinders away from exits and exit routes.
• Locate cylinders away from heat sources, including heat lamps. Compressed
gas cylinders should not be subjected to temperatures above 52 °C (126 °F).
• Do not allow ignition sources in the storage area and keep cylinders away from
readily ignitable substances such as gasoline or waste, or combustibles in bulk,
including oil.
• Store cylinders standing upright, fastened securely to an immovable bulkhead
or permanent wall.
• When storing cylinders outdoors, they should be stored above ground on a
suitable floor and protected against temperature extremes (including the direct
rays of the sun).
• Mark gas cylinders clearly to identify the contents and status (full, empty, etc.).
• Do not attempt to refill gas cylinders.
Safety Practices for Flame Atomization 23

Handling Cylinders
Review the following precautions to ensure the safe use and handling of gas
cylinders.
• If it becomes necessary to move cylinders, do so with a suitable hand truck
after insuring that the container cap is secured and the cylinder is properly
fastened to the hand truck.
• Use only regulators, tubing and hose connectors approved by an appropriate
regulatory agency.
• Arrange gas hoses where they will not be damaged or stepped on and where
objects will not be dropped on them.
• Do not refill cylinders.
• Check the condition of pipes, hoses and connectors regularly. Perform gas leak
tests at all joints and seals of the gas system regularly, using an approved gas
leak detection system.
• When the equipment is turned off, close all gas cylinder valves tightly at the
cylinder. Bleed the remainder of the line before turning the exhaust vent off.

Safety Practices for Flame Atomization

Safety Interlocks
PerkinElmer provides a number of safety interlocks on the burner system to
monitor gas pressure and check for the proper setup of the burner head, nebulizer,
and drain system. In addition a flame sensor checks that the flame is burning.

• Do not attempt to defeat these interlocks; you may compromise your own,
or someone else's, safety.

Safe Use of Burner Gases


The seepage of fuel gas or fuel gas mixture from the burner system, the drain
system, the gas control system, or the gas connections constitutes a serious fire
hazard.
• Make sure that there are no breaks or leaks in any of these systems and that
all the seals are correctly installed and in good condition.
24 Safety Practices

• Regularly check for leaks at joints and seals using an approved leak test
solution.
• When you perform any maintenance or installation procedures, follow the
instructions in the guide exactly.
• Do not attempt to service the gas control system yourself. A PerkinElmer
service engineer, or similarly authorized and trained person, must perform
the work.
• When you shut down the instrument, for example at the end of the working
day, shut all the gas lines at the cylinder or regulator valves. Bleed the lines
between the regulator and instrument to atmosphere before switching off
the ventilation system.

Air Supply
An air compressor is recommended for the air supply to the burner system.
Cylinders of compressed air should only be used as an emergency or short-term
solution.
• If you use cylinder air, make sure that it is compressed air and not oxygen-
enriched air (e.g. breathing air); the use of oxygen-enriched air can cause
a flashback of the flame.
• Never use oxygen as the oxidant since this can cause an explosion.

Nitrous Oxide (dinitrogen monoxide, N2O)


• Tubing and fittings carrying nitrous oxide must be free of all oil, grease,
and organic materials. Spontaneous combustion may occur if nitrous oxide
comes into contact with these materials.
• Use a double-stage or heated regulator for nitrous oxide to prevent freezing
of the diaphragm and a loss of pressure regulation.
• Do not store nitrous oxide in close proximity to flammable gases, such as
acetylene or hydrogen.
Safety Practices for Flame Atomization 25

Acetylene
• Always use “Atomic Absorption Grade” acetylene (ethyne) dissolved in
acetone (propane-2-one). This is satisfactory for all PerkinElmer AA
spectrometers.
• Do not store acetylene in close proximity to oxidizing gases, such as
nitrous oxide.
• Use approved tubing and fittings for acetylene. Never use copper fittings
since acetylene forms an explosive compound with copper.
• Prevent acetylene from coming into contact with copper, silver, mercury
or gaseous chlorine.
• Periodically check for the presence of acetylene in the laboratory
atmosphere, especially near the ceiling.
• For acetylene, set an outlet gauge pressure of between 90 kPa and 100 kPa
(0.9-1.0 bar, 13-14.5 psig). Never allow the outlet gauge pressure to
exceed 103 kPa (1.03 bar, 15 psig); acetylene can explode spontaneously
above this pressure.
• Solvent Carryover:
If the acetylene cylinder pressure falls to below 600 kPa / 6.0 bar / 87 psig
(at 20 °C), some of the solvent used to stabilize the acetylene (such as
acetone) may be carried over into the burner. This could influence the
characteristics of the burner with a resulting influence on the analytical
results.
Change to a new acetylene cylinder when the cylinder pressure falls to
below this value.

Safe Operation of the Flame


Before you ignite the flame make sure that:
• The laboratory fume ventilation system is operating;
• The burner head is installed correctly;
• The burner end cap is secured firmly;
• The fuel and oxidant tubing fittings are properly connected;
• The burner unit contains the necessary solvent-resistant components if you
intend to analyze samples containing organic solvents;
26 Safety Practices

• The atomizer compartment door is closed;


• The pH of the liquid in the drain vessel is greater than pH 10 if you intend
to aspirate cyanide solutions.

• Do not leave the flame unattended. Always make sure that there is a fire
extinguisher near the instrument.

• Never change the gas pressure or shut a gas valve while the flame is
burning.

• Make sure that the drain tubing is attached.

• Do not allow the burner head slot to become blocked. This can cause a
flashback of the flame.

• Do not place open containers of flammable liquids and solvents near the
flame. Be especially careful with samples that contain highly volatile
solvents.

• When you have analyzed samples containing organic solvents, flush all
traces of solvent from the burner system.

Warning: Do not open the flame door during flame operation. When
the flame is ON, do not open or remove the burner door. The burner
! door is there to protect the operator from the hot flame and UV radiation
while running the flame atomization.
Warning
Safety Practices for Flame Atomization 27

The Drain System

Explosion Risk!
! The waste bottle must be placed out in the open, where there is no
possibility of a build-up of potentially hazardous gases.
Warning

It cannot be placed inside a cabinet, or on a shelf with an obstructed


view. The drain bottle must be in full view at all times so it can be seen if
the bottle is full or near full, and the condition of the drain tubing is
readily apparent.

• Always place the drain (waste) vessel in a well ventilated place underneath
the spectrometer, in full view while you are working with the
spectrometer. This prevents the build-up of potentially hazardous gases,
and allows you to see the liquid level.

• Never use a glass drain (waste) vessel.

• Do not kink, fold, or loop the drain tube.

• Never place the drain tube directly into a laboratory sink.

• Empty the drain vessel frequently; especially do not allow the drain vessel to
fill with organic solvent (Burner Drain Assembly for Organic Solutions Part
No. N3150232).

• Thoroughly flush the drain system, as described in the guide, when you shut
down the system.

• Check the condition of the drain tube regularly, especially if you use organic
solvents. Replace the drain tube when it first shows signs of cracking or
discoloration.

Flashbacks
A flashback is an explosion of the premixed gases in the spray chamber. The safety
interlocks normally prevent conditions that could cause a flashback, but if a
flashback should ever occur:
28 Safety Practices

• Check that the burner head slot is clean.


• Make sure that you are using compressed air and not oxygen-enriched air.
• Check the flow spoiler or impact bead for damage, and replace any damaged
parts.
• Carefully check and tighten all connections to, and seals on, the burner unit,
and check the gas flow settings before you attempt to ignite the flame. Seepage
of fuel and oxidant from the spray chamber may cause a flashback.
• Check that the burner head is seated correctly.

Hazards with Flame Atomization

Toxic Combustion Products


Toxic combustion products can be generated by the system, depending on the type
of analyses being performed.

• You must provide an efficient laboratory ventilation system to remove toxic


products generated during instrument operation.

High Temperatures
The flame can generate temperatures of up to 2800 °C.

• To avoid serious burns, never touch the burner head until it has cooled to room
temperature.

UV Radiation
The flame, especially the nitrous oxide/acetylene flame, emits ultraviolet radiation.

• Keep the atomizer compartment door closed when the flame is burning and
never directly view the flame unless you are wearing UV-absorbing glasses.

Acetylides
If you have aspirated high concentrations of copper, silver, or mercury solutions
into an acetylene flame, unstable acetylides may have formed in the spray chamber.
If permitted to dry, these compounds may explode.
Safety Practices for Electrothermal Atomization 29

• Aspirate solution continuously to prevent residues from drying.


• Thoroughly flush the spray chamber and drain system with water immediately
after such an analysis.

Cyanide Solutions
If you intend to aspirate cyanide solutions, make sure that the pH of the liquid in
the drain vessel is greater than pH 10; toxic hydrogen cyanide gas is formed when
cyanides contact acidic solutions.

• Never allow solutions containing cyanides to mix with acidic solutions.

Safety Practices for Electrothermal Atomization

Safety Interlocks
PerkinElmer provides a number of safety interlocks on the graphite furnace
(electrothermal atomization) system that monitor the gas pressure and the
temperature of certain system components.

• Do not attempt to defeat these interlocks; you may compromise your own, or
someone else's, safety.

Inert Gas
The graphite furnace requires a supply of inert gas. PerkinElmer recommends
argon.

Although nitrogen can be used, it is not recommended for the inert gas supply. At
furnace temperatures above 2300 °C, nitrogen reacts with graphite to form toxic
cyanogen gas (CN)2.

Safety Checks
Before you start an analysis, make sure that:
• The laboratory fume ventilation system is operating;
• The inert gas supply is connected and set to the correct pressure;
30 Safety Practices

• The cooling water supply is turned on;


• The autosampler waste bottle is empty.

Hazards with Electrothermal Atomization

Toxic Products
Toxic metal vapors, ozone, etc., can be generated by the system, depending on the
type of analyses being performed.
• You must provide an efficient laboratory ventilation system to remove toxic
products generated during instrument operation.
• If you use nitrogen as the inert gas, toxic cyanogen gas (CN)2 will be produced
when the furnace temperature is above 2300 °C.

High Temperatures
The THGA graphite furnace can generate temperatures of up to 2600 °C.
The HGA graphite furnace can generate temperatures of up to 2700 °C.
• To avoid serious burns, never touch the graphite components until the furnace
has cooled to room temperature.
• Do not attempt to inject a sample into the graphite tube when the furnace is hot.
You may be subjected to fumes from the sudden vaporization of the sample,
and may damage the pipette.

UV Radiation
The graphite furnace emits ultraviolet radiation when it is heated to incandescence.

• Never directly view the graphite furnace unless you are wearing UV-absorbing
glasses.

Strong Magnetic Field


The electromagnet generates a strong magnetic field inside the THGA furnace
during measurement cycles.
• Do not operate the furnace when persons wearing electronic heart pacemakers,
or having other metallic implants, are present.
Safety Practices for FIAS and Mercury Hydride Systems 31

• Anyone wearing a heart pacemaker or having metallic implants should remain


at least 0.6 meter away from the furnace - in any direction - while the furnace
is operating.

Safety Practices for FIAS and Mercury Hydride Systems


These systems are offered as options for the spectrometer.

Safety Checks
Before you start an analysis, make sure that:
• The laboratory fume ventilation system is operating;
• The tubing in the fluid system is not constricted since this could lead to a
pressure build-up in the system;
• The drain tubing is inserted in the waste container and that this container
is empty.

• If you are using a flame to heat the QTA-cell or if you intend to perform
flame-FIAS analyses, refer to the information under Safety Practices for
Flame Atomization before you ignite the flame.

Hazards with FIAS and Mercury Hydride Systems

Toxic Products
• Toxic metal vapors, etc., can be generated by the system, depending on the
type of analyses being performed.
• You must provide an efficient laboratory ventilation system to remove
toxic products generated during instrument operation.

High Temperatures
The QTA-cell used for the hydride-generation technique can reach temperatures of
up to 1000 °C.

• Do not touch any part of the heating mantle (electrically heated systems),
or the cell holder (flame-heated systems), or the QTA-cell until they have
cooled to room temperature.
32 Safety Practices

Hazardous Chemicals
Some of the chemicals required for analyses are corrosive and/or toxic.

• Refer to the information under Safe Handling of Chemicals and to the


specific warnings in the documentation provided with the system before
you start an analysis.
Decontamination and Cleaning 33

Decontamination and Cleaning


Before using any cleaning or decontamination methods except those specified by
PerkinElmer, users should check with PerkinElmer that the proposed method will
not damage the equipment.

Note The responsible body has the responsibility for usage of decontamination
or cleaning agents that could cause a hazard as a result of a reaction with
parts of the equipment or with materials contained in it.

Decontamination
Customers wishing to return instrumentation and/or associated materials to
PerkinElmer for repair, maintenance, warranty or trade-in purposes are
advised that all returned goods must be certified as clean and free from
contamination.
The customer's responsible body is required to follow the “Equipment
Decontamination Procedure” and complete the “Certificate of Decontamination”.
These documents are available on the PerkinElmer public website:
Procedure:
http://www.perkinelmer.com/Content/technicalinfo/dts_instrumentdeconprocedure.pdf
Certificate form:
http://www.perkinelmer.com/Content/technicalinfo/dts_perkinelmercertificationofdecontaminationform.pdf

If you do not have access to the internet and are located in the U.S., call toll free at
1-800-762-4000 or (+1) 203-925-4602, 8:30 a.m. - 7 p.m. EST and speak to
Customer Support.
In Canada, call toll free 800-561-4646 and speak to Customer Support.
If you are located outside of the United States or Canada, please call your local
PerkinElmer sales office for more information.

Cleaning the Instrument


Exterior surfaces may be cleaned with a soft cloth, dampened with a mild detergent
and water solution. Do not use abrasive cleaners or solvents.
34 Safety Practices

WEEE Instructions for PerkinElmer Products

A label with a crossed-out wheeled bin symbol and a rectangular bar indicates that
the product is covered by the Waste Electrical and Electronic Equipment (WEEE)
Directive and is not to be disposed of as unsorted municipal waste. Any products
marked with this symbol must be collected separately, according to the regulatory
guidelines in your area.
The objectives of this program are to preserve, protect and improve the quality of
the environment, protect human health, and utilize natural resources prudently and
rationally. Specific treatment of WEEE is indispensable in order to avoid the
dispersion of pollutants into the recycled material or waste stream. Such treatment
is the most effective means of protecting the customer's environment.
Requirements for waste collection, reuse, recycling, and recovery programs vary
by regulatory authority at your location. Contact your local responsible body (e.g.,
your laboratory manager) or authorized representative for information regarding
applicable disposal regulations. Contact PerkinElmer at the web site listed below
for information specific to PerkinElmer products.
Web address:
http://www.perkinelmer.com/pages/010/onesource/environmental-health-and-
safety/environmental-directives-compliance.xhtml
For Customer Care telephone numbers select “Contact us” on the web page.
Products from other manufacturers may also form a part of your PerkinElmer
system. These other producers are directly responsible for the collection and
processing of their own waste products under the terms of the WEEE Directive.
Please contact these producers directly before discarding any of their products.

Consult the PerkinElmer web site (above) for producer names and web addresses.
References for Laboratory Safety Practice 35

References for Laboratory Safety Practice


• Bretherik, L., Bretherik's Handbook of Reactive Chemical Hazards, 7th ed.,
Butterworth & Co. Ltd., London, UK, 2006.

• Safe Practices in Chemical Laboratories, Royal Society of Chemistry, London,


UK, 1989.

• Hazards in the Chemical Laboratory, 5th edition, Luxon, S.G., ed., Royal
Society of Chemistry, London, UK, 1993.

• CRC Handbook of Laboratory Safety, 5th edition, Furr, K., ed., The Chemical
Rubber Co. Press, Florida, USA, 2000.

• Prudent Practices for Handling Hazardous Chemicals in Laboratories and


Prudent Practices for Disposal of Chemicals from Laboratories, 2nd edition,
National Research Council, National Academic Press, Washington D.C., USA,
2010.

• Sax's Dangerous Properties of Industrial Materials, 11th edition, Sax, N.I. and
Lewis, R.J., eds., Wiley, New York, USA, 2004.

• Pohanish, R.P., HazMat Data, 2nd edition, Barnes & Noble, New York, USA,
2004.

• Compressed Gas Association, Inc., Arlington, VA 22202, USA, various


publications.

• Data Sheets provided by chemical manufacturers, e.g.:


• USA, Material Safety Data Sheets (MSDS),
• FRG, DIN-Sicherheitsblätter,
• UK, Hazard Data Sheets.
36 Safety Practices
Preparing Your
Laboratory 2
Introduction
The PinAAcle 900 Series spectrometer has some special requirements that you
must consider when setting up the laboratory. The laboratory must fulfill these
requirements, described in this chapter, before you can operate the spectrometer
correctly.

Environmental Requirements
The location where the PinAAcle 900 Series is to be installed must fulfill the
criteria listed below:
• Indoors
• Free from vibrations
• Free from dust, smoke and corrosive fumes.
• Out of direct sunlight.
• Away from radiators and heaters.
• Have a suitable fume ventilation system.
• Room temperature between +15 °C to + 35 °C (59-95 °F), with a maximum
change rate of 3 °C (5.4 °F) per hour.
• Relative humidity between 20 and 80%, non-condensing.
38 Preparing Your Laboratory

Lab Space Requirements


The work bench must be sufficiently sturdy to carry the weight of the PinAAcle
900 Series, computer with monitor, keyboard, mouse and printer. The weight of the
optical accessories must also be taken into account. The maximum load imposed
by the instrument is 0.5kN/m2. Check that the floor can withstand this load.

At least 25 cm (10 in) free space must be available behind the instrument for
ventilation purposes and servicing. Do not block the fans operating on both sides
of the instrument.

In addition, an area of at least 69 cm (27 in) should be available. If this is not


possible, the bench on which the instrument is installed must be on wheels that can
be locked.

Make sure that there is enough room on the work bench. The monitor can usually
be placed on top of the PC unit in order to save working space. Some clearance
between the instruments should be provided to ensure sufficient air circulation.

If a printer is included in the delivery, additional space must be provided. Do not


forget the space required for a mouse and mouse pad.

Optional Accessories (e.g., AutoPrep 50) require additional space. It is


recommended to install these accessories on the sample tray or on a sample cart in
front of the instrument.
Lab Space Requirements 39

Dimensions and Weights

Figure 2-1. Instrument dimenstions


40 Preparing Your Laboratory

Note Instrument dimensions are in millimeter units of measure.

Table 2-1. PinAAcle Instruments Dimensions and Weights

Weight
Instrument Width Depth Height
(Mass)

PinAAcle 900T 950 mm 680 mm 730 mm 133kg


(37.3 in) (26.7 in) (28.7 in) (293 lb.)
with AS 900 1038 mm
(40.9 in)
PinAAcle 900Z 950 mm 680 mm 730 mm 118kg
(37.3 in) (26.7 in) (28.7 in) (260 lb.)
with AS 900 1038 mm
(40.9 in)
PinAAcle 900H 950 mm 680 mm 730 mm 107kg
(37.3 in) (26.7 in) (28.7 in) (235 lb.)
with AS 900 1038 mm
(40.9 in)
PinAAcle 900F (No 950 mm 680 mm 730 mm 87kg
AS 900) (37.3 in) (26.7 in) (28.7 in) (191 lb.)
1038 mm
(40.9 in)
AS 900 280 mm 299 mm 344 mm 7.2 kg
(11.0 in) (11.7 in) (13.5 in) (15.8 lb.)
Cooling System 200 mm 500 mm 375 mm 18.0 kg
(7.9 in) (19.7 in) (14.8 in) (39.6 lb.)

PC and printer dimensions and weight will vary by model.


Fume Ventilation 41

Fume Ventilation

Note Local electrical codes do not permit PerkinElmer Service Engineers to


install the blower and vent assembly.

A ventilation system is required to remove fumes emitted from the flame or


graphite furnace during operation. The exhaust hood should be 950 mm (37 in)
above the bench and provide a flow rate of approximately 5700 L/min. A
minimum flow rate of 5,700 L/min. (200 cubic feet/min) is required for an air-
acetylene flame, and furnace operation. A flow rate of approximately 7,000-
8,500 L/min (250-300 cubic feet/min) is required for nitrous oxide-acetylene
flame operation.

For the high temperatures of the nitrous oxide-acetylene flame, the fume hood and
ducting should be made of stainless steel.
PerkinElmer offers an accessory, Blower and Vent Kit (Part No. 03030406), which
will fulfill the exhaust requirements for all AA instruments (see Figure 1). Included
in the kit are a rotary blower with capacitor and hardware, a vent to be located
above the instrument, and an adapter to permit connection of the blower
and vent with suitable metal tubing. The adapter and vent are made of stainless
steel sheets.
The metal tubing required to connect the vent to the blower and to provide suitable
exhaust from the blower is not included in the Blower and Vent Kit. Flexible
stainless steel tubing is recommended for this purpose and can be obtained from
the companies listed in the following table and from various other firms. In some
instances, this type of flexible metal tubing is sold only in minimum lengths of 3
meters (10 feet).

Note Local electrical codes do not permit PerkinElmer Service Engineers to


install the blower and vent assembly.
42 Preparing Your Laboratory

Table 2-2. U.S. Suppliers of Flexible Metal Duct Tubing.

Flexaust Co. Potomac Rubber Co.


11 Chestnut St. 9011 Hampton Overlook
Amesbury, Ma 01913 Capital Heights, MD 20743
(508) 388-9700 (301) 336-7400
Triplex Inc. Fox Manufacturing Inc.
1142 Kress Street P.O. Box 1047
Houston, TX 77020 Clarkdale, AZ 86324
(713) 672-7521 (602) 634-5897

For the names of suppliers in other areas, contact your PerkinElmer representative.

The capacity of the blower depends on the duct length and the number of elbows
or bends used to install the system. If an excessively long duct system or a system
with many bends is used, a stronger blower may be necessary to provide sufficient
exhaust volume. Alternatively, smooth stainless steel tubing may be used instead
of flexible stainless steel tubing where flexibility is not required to reduce system
friction loss or "drag." A length of smooth stainless steel ducting has 20-30% less
friction loss than a comparable length of flexible ducting. When smooth stainless
steel tubing is used, elbows must be used to turn corners. These elbows should turn
at a center line radius of 45 degrees to reduce friction losses, and the number of
elbows should be minimized.

If a rigid tubing system is used, it is strongly recommended that flexible tubing be


used from the vent hood to the ceiling to facilitate hood alignment and service
access to the instrument.

When installing a venting system, all connections should be made with metal
screws or rivets. Solder must not be used. The blower should be located at least 4
meters (12 feet) and not more than 6.5 meters (20 feet) from the flame or the
graphite furnace and should exhaust to the atmosphere or into a considerably wider
exhaust duct. Under these conditions, the following temperatures have been
measured during operation of a nitrous oxide-acetylene flame: 310 °C at the vent
intake; 160 °C at 2.4 meters (8 feet) from the vent intake; 105 °C at the blower
intake; and 50 °C at the blower motor housing near the front bearing. Instructions
Fume Ventilation 43

for installation (Part No. 09936775) are provided with the Blower and Vent
assembly. The blower provided in the

PerkinElmer accessory kit requires a line voltage of 115 V or 230 V.

Additional recommendations on the venting system include:


• Make sure the duct casing is installed using fireproof construction. Route
ducts away from sprinkler heads.
• Locate the discharge outlet as close to the blower as possible. All joints on
the discharge side should be airtight, especially if toxic vapors are being
carried.
• Equip the outlet end of the system with a back draft damper and take the
necessary precautions to keep the exhaust outlet away from open windows
or inlet vents and to extend it above the roof of the building for proper
dispersal of the exhaust.
• Equip the exhaust end of the system with an exhaust stack to improve the
overall efficiency of the system.
• Make sure the length of the duct that enters into the blower is a straight
length at least ten times the duct diameter. An elbow entrance into the
blower inlet causes a loss in efficiency.
• Design local exhaust ventilation systems individually for each specific AA
instrument. Also, the opening of the exhaust vent should be large enough
to cover the graphite furnace or flame area completely.
• Provide make-up air in the same quantity as is exhausted by the system. An
"airtight" lab will cause an efficiency loss in the exhaust system.
• Ensure that the system is drawing properly by releasing smoke into the
mouth of the collector hood (vent). A synthetic "smoke" can be generated
by placing open bottles of hydrochloric acid and ammonium hydroxide in
proximity under the hood.
• Equip the blower with a pilot light located near the instrument to indicate
to the operator when the blower is on.
44 Preparing Your Laboratory

Warning: Toxic Gases - Fume Ventilation System


! Without adequate ventilation, potentially toxic vapors can build up in the
Warning laboratorym.

Your laboratory must have a reliable fume ventilation system before


you use this instrument

Exhaust venting is important for the following reasons:


• It will protect laboratory personnel and the instrument from toxic vapors,
which may be produced by some samples.
• It will minimize the effects of room drafts and the laboratory atmosphere
on flame stability.
• It will help to protect the instrument from corrosive vapors which may
originate from the samples.
• It will remove dissipated heat produced by the flame or furnace.

We strongly recommend that you do not place the spectrometer in a chemical


hood. If a chemical hood must be used, make arrangements to prevent
contamination due to corrosive vapors and back drafts from other hoods.

Do not perform sample preparation in the same hood as the spectrometer.

Vent Hood Dimensions


Approximately 58 cm (23 in) from back of Instrument to center of Atomizer,
approximately 68 cm (27 in) from right side of Instrument to center of atomizer, 27
cm (10.5 in) from left side of Instrument to center of atomizer and 95 cm (37.5 in)
from the bench top the instrument rests on to the bottom of the exhaust vent. There
should be 22 cm (8.5 in) of clearance from the top of the burner shield (732 mm)
to the bottom flange of the exhaust vent. The clearance from the top of the
instrument (641 mm) to the bottom of the exhaust shield approximately 30 cm (12
in).
Fume Ventilation 45

Figure 2-2. Instrument dimenstions


Item Description
A Length
B Height to top of cover
C Depth
D Distance from the center of the atomizer compartment to the right
hand edge of instrument
E Protuberance of sample tray in front of the instrument
F Height of flame shield above top of the instrument cover
46 Preparing Your Laboratory

Item Description
G 10 cm (4 inches) in all cases
H 30 cm (12 inches) in all cases
J 15 cm (6 inches) in all cases

Magnetic Field (PinAAcle 900T and 900Z Only)


The THGA furnace generates and uses a strong magnetic field during measurement
cycles.

The magnetic field affects an area radius 0.6 m (24 in) around the graphite furnace.
The affected area extends all around the furnace, including above and below the
furnace. In addition to posting a health hazard for persons wearing heart
pacemakers, the magnetic field can also affect other instruments, watches and
magnetic storage devices (disks, credit cards, etc.).

Warning - No Pacemakers
There is a potential hazard due to a strong magnetic field and persons
wearing heart pacemakers or other metallic implants should remain at
Warning least 0.6 m away from the furnace.
Line Power Requirements 47

Figure 2-3. Magnetic field

Line Power Requirements


The line power supply must conform to the local safety regulations and be checked
by a qualified electrician before the instrument is connected.

The PinAAcle Series 900T/H/Z/F models require a stable, 50 or 60 Hz power


supply at the correct voltage, and must have a correctly wired protective conductor
terminal (earth, ground). The supply must be free from line transients in excess of
50 V peak.
48 Preparing Your Laboratory

It is essential to avoid ground loops.

Power Consumption
10100 VA for the PinAAcle 900T and the PinAAcle 900Z

10100 VA for the PinAAcle 900H

800 VA for the PinAAcle 900F

140 VA for the Cooling System

Power Specification PinAAcle 900T and PinAAcle 900Z


230 VAC ±10%, 50 or 60 Hz ± 0.3 Hz, single phase alternating current.

The PinAAcle 900T and 900Z will ship standard an IEC 60309 32A power
connector.

Operating range of 207 - 253 VAC/60 Hz, 30 A


(2 pole- 3 wire-grounding), and a dedicated circuit.
fuse 30 A slow blow, must be able to hold a 3x surge current for 3 seconds.

The mains line house wiring must have a minimum wire cross section of 6 mm²
(8 gauge) or 10 mm² (6 gauge) for distances > 10 m.

Power Specification PinAAcle 900H


230 VAC ±10%, 50 or 60 Hz ± 0.3 Hz, single phase alternating current.

The PinAAcle 900H will ship standard an IEC 60309 16/20 A power connector.

Operating range of 207 - 253 VAC/60 Hz, 20 A


('2 pole- 3 wire-grounding), and a dedicated circuit.
fuse 20 A slow blow, must be able to hold a 3x surge current for 3 seconds.

The mains line house wiring must have a minimum wire cross section of 4 mm²
(10 gauge) or 6 mm² (8 gauge) for distances > 10 m.
Line Power Requirements 49

Power Specification PinAAcle 900F


100 - 230 VAC +10/-15%, 50 or 60 Hz ± 3 Hz, single phase alternating current.

Operating Range
90-253 VAC, 4A - 8A, 47 - 63 Hz

Operating voltage range must be maintained both at nominal and under load of
maximum power. For the PinAAcle 900H, PinAAcle 900T and the PinAAcle 900Z
it is recommended to install a Buck Boost transformer if the line drops below 208
volts at maximum power during atomization. If the line sags to 208 volts or lower,
excessive current draw will occur to provide the power needed, which will lead to
excessive heat dissipation. This excessive heat dissipation and current draw will
stress the furnace power supply, cause overheating failures, and shorten the life of
the supply.

Power that does not meet these minimum specifications will need the installation
of a Buck-Boost transformer, or a PowerVar Line Conditioner with built in boost
capabilities. Please refer to SDB # 4200041B.STS for more information on
whether the uses of a Buck-Boost transformer in necessary. If the voltage drops
below 208 VAC during atomization peak power, it is highly recommended that a
Buck-Boost or Line-Conditioner with boost be installed at Installation. Large
voltage drops (>16v) during atomization, or abnormally low nominal "no-load"
voltage (< 200 VAC) are an indication that the wiring requirements are not to our
required Preparing Your Laboratory or Site Readiness specifications.

Note The PinAAcle 900H, 900T and 900Z standard IEC 60309 should not be
replaced will an L6-30R twist lock plug, or any other Non-IEC 60309 type
plug or receptacle. The PinAAcle 900T and 900Z Series Instruments
require the IEC 60309 PLUG to prevent the inherent high leakage current
from shocking the user. Removing the IEC 60309 plug and replacing it
with a Non-IEC 60309 type plug violates all safety labels and approvals for
the PinAAcle.

Power Specification For The Cooling System


207 - 253 VAC, 50/60 Hz, 4A Max
50 Preparing Your Laboratory

Noise Specifications
The electrical noise levels of the incoming power to the customer's lab should be
checked to insure safe and reliable operation of our instrumentation and relative
electronics used for analysis. The electrical noise levels should be within the
following specifications:

Common Mode Noise: Neutral to ground noise should be ≤ 0.5 volts peak-to-
peak

Normal Mode Noise: Hot to neutral noise should be ≤ 10 volts peak-to-peak

Line Conditioners
PowerVar makes a series of line conditioner units that are suitable for all PinAAcle
900 Series model Instruments we sell. Line conditioner units are strongly
recommended where the customer's lab does not meet our minimum noise
specification requirements for both common and normal mode allowable line noise
levels. Please see the table below for the line conditioner models that are suitable
for each PinAAcle Instrument model we sell:
Line Power Requirements 51

Table 2-3. Line Conditioners

Instrument
Instrument
Model Description Output Frequency Part No. Description Frequency Part No.
Voltage
PinAAcle 5.8 KVA Line 208/240 60 Hz N9307760 10 KVA 50/60 Hz N9306757
900T/Z Conditioner True On-Line
Power
Conditioned
UPS
PinAAcle 6.0 KVA Line 220 50 Hz N9307523 10 KVA 50/60 Hz N9306757
900T/Z Conditioner True On-Line
Power
Conditioned
UPS
PinAAcle 720 VA Line 120 60 Hz N9307515* 800 VA 60 Hz N0777681
900F Conditioner Power
Conditioned
UPS
PinAAcle 750 VA Line 220 50 Hz N9307521 800 VA 50 Hz N0777689
900F Conditioner Power
Conditioned
UPS
PinAAcle 5.8 KVA Line 208/240 60 Hz N9307760 10 KVA 50/60 Hz N9306757
900H Conditioner True On-Line
Power
Conditioned
UPS
PinAAcle 6.0 KVA Line 220 50 Hz N9307523 10 KVA 50/60 Hz N9306757
900H Conditioner True On-Line
Power
Conditioned
UPS

Note *The installation of an Isolation Ground Outlet Receptacle can help


improve electrical noise for 120 VAC power configurations, which can
eliminate the need of a Line Conditioner in some instances. The part
number of the Isolation Ground Outlet receptacle is: N3151390.
52 Preparing Your Laboratory

UPS Systems
The PowerVar 10.0 KVA On-Line Conditioned UPS 50/60Hz unit is currently
available for the THGA PinAAcle models (900H/T/Z). It meets the minimum
surge current handling rating of 90 A for about 3 seconds during Atomization stage
peak power. The PerkinElmer part number for the 10.0 KVA UPS is N9306757.

The PowerVar 800 VA On-Line Conditioned UPS 50/60Hz unit is currently


available for the PinAAcle 900F Flame Only model. The PerkinElmer part number
for the 800 VA UPS is N0777681.

Power Outlets
In addition to the above, the following are required:
• For connection of the Cooling System, a 230 VAC socket is provided at
the rear of the PinAAcle Series 900 T/H/Z models.
• For the PC, monitor, printer, and addition accessories, e.g., FIAS or Auto
Prep 50, suitable outlets must be provided. Protecting earth and ground
must be the same as for the PinAAcle Series 900 T/H/Z models (avoid
ground loops).

Gas Requirements

Note Standards for cylinder dimensions, regulator connections, gas fittings, etc.
vary from country to country. The information provided here is for the
U.S. Contact your PerkinElmer representative for information on the
specific requirements of your area.

Gas Line Connections


PerkinElmer AA instruments include the hoses necessary for connection to gas
lines. It is the responsibility of the user to provide the appropriate gas lines,
regulators, connectors and valves to which the hoses are connected.
Gas Requirements 53

Safety of Gas Cylinders and Gas Delivery Lines

Note The permanent installation of gas supplies is the responsibility of the user
and should conform to local safety and building codes.

While the installation and operation of all gas supplies is the responsibility of the
user, the following safety information concerning the handling of gas cylinders is
included for your reference:
• Flammable gas cylinders (such as acetylene) should not be stored with
oxygen, or nitrous oxide cylinders, or adjacent to oxygen charging
facilities.
• Fasten all gas cylinders securely to an immovable bulkhead or a permanent
wall.
• When gas cylinders are stored in confined areas, such as a room,
ventilation should be adequate to prevent toxic or explosive
accumulations. Move or store gas cylinders only in a vertical position with
the valve cap in place.
• Locate gas cylinders away from heat or ignition sources, including heat
lamps. Cylinders have a pressure-relief device that will release the
contents of the cylinder if the temperature exceeds 52 °C (125 °F).
• When storing cylinders external to a building, the cylinders should be
stored so that they are protected against temperature extremes (including
the direct rays of the sun) and should be stored above ground on a suitable
floor.
• Mark gas cylinders clearly to identify the contents and status (full, empty,
etc.).
• Do not attempt to refill gas cylinders.
• Use only approved regulators and hose connectors. Left-hand thread
fittings are used for fuel gas tank connections, whereas right-hand fittings
are used for oxidant and support gas connections.
• Use galvanized iron tubing, steel, wrought iron or other tubing that will not
react chemically with acetylene. Never use copper tubing with acetylene.
Joints may be welded or made up of threaded or flanged fittings, typically
stainless steel, aluminum or brass composed of less than 65% copper.
54 Preparing Your Laboratory

Rolled, forged or cast steel or malleable iron fittings may also be used. Cast
iron fittings cannot be used safely for acetylene lines.
• Arrange gas hoses where they will not be damaged or stepped on and
where things will not be dropped on them.
• Never run acetylene at a pressure higher than 100 kPa (15 psig). At
pressures above this level, acetylene may spontaneously explode.
• Perform periodic gas leak tests by applying a soap solution to all joints and
seals.

Contact between acetylene gas and copper or silver (or high


! concentrations of silver salts), liquid mercury or gaseous chlorine can
produce potentially unstable acetylides. Always clean the burner
Warning thoroughly after analyzing solutions with high silver or mercury
concentrations, and aspirate solution continuously during the analysis to
prevent any residues from drying.

• Periodically check for the presence of acetylene in the laboratory


atmosphere, especially near the ceiling.
• When the equipment is turned off (for example, at the end of the working
day), close all gas cylinder valves tightly at the tank. Bleed the remainder
of the line to the atmosphere before the exhaust fan (vent) is turned off.
• When using premix burners with cyanide solutions, check the pH of the
liquid trap and drain vessel. The pH of the liquid should be greater than 10.
If the liquid is even slightly acidic, highly toxic hydrogen cyanide gas may
be released.
• Take suitable precautions when using volatile organic solvents. A
potentially flammable organic vapor "cloud" can form around the opening
of the sample vessel. Feeding the capillary tubing through a small hole in
a covered sample container is one way of reducing the possibility for
ignition.
• Never view the flame, hollow cathode lamps (HCLs), electrodeless
discharge lamps (EDLs) or deuterium background corrector lamps directly
without protective eye wear. Potentially hazardous ultraviolet radiation
may be emitted. Ordinary safety glasses will in general provide sufficient
protection, but additional side shields will ensure a further margin of
safety. Safety glasses will also provide mechanical protection for the eyes.
Furnace Gas Requirements 55

• Never leave the flame unattended.


• Zeeman background-corrected AA instruments generate a strong magnetic
field. People with cardiac pacemakers are advised not to operate or
frequent the vicinity of Zeeman background-corrected instruments while
they are in operation.

Gas Specifications
Air: Please refer to the Flame Gas Requirements below.

Furnace Gas Requirements

Gas Specifications:

Normal Gas
Usually argon is used to prevent the tube and the atoms from being oxidized when
the tubeis heated. If you cannot obtain argon, you can use nitrogen, but nitrogen
does not provide such efficient protection as argon at temperatures above 2000 °C.
Nitrogen may react with samples and the tube at typical atomization temperatures.

Warning: Toxic Gases


! If nitrogen is used as a normal gas, toxic cyanogen gas (CN)2 will be
Warning
produced when the furnace temperature is above 2300 °C.

Make sure that the main laboratory fume ventilation system removes
all gases and fumes emitted by the furnace.

Special Gas
For some applications a special gas, for example, a gas mixture containing oxygen,
could be useful for the pre-treatment of organic samples.
56 Preparing Your Laboratory

Table 2-4. Specifications and Requirements for the Furnace


Gases

Fitting Specification Furnace Gases


For connecting the furnace gases two ¼ inch Swagelock fittings (nut, front ferrule,
back ferrule and hose insert as single parts) are supplied in the instrument accessory
kit. The customer must supply the respective wall outlets or pressure regulator
outlets.

Flame Gas Requirements

Gas Specification
Air: Compressed air is required as oxidant for flame operation.

Warning: Risk of Flashback


! Never use oxygen or synthetic air instead of compressed air. Risk of
flashback, caused by the higher amount of oxygen.
Warning

For flame operation, the air supply should provide a minimum of 28 liters/min (1
cubic foot/min) at a minimum pressure of 350 kPa (50 psig). The pneumatics of the
PinAAcle 900H and PinAAcle 900T systems require a minimum air pressure of
350 kPa (50-58 psig).
Flame Gas Requirements 57

It is desirable to have a water and oil trap or filter between the compressor and the
instrument gas control system. The use of an Air Filter Accessory (Part No.
00470652) or an Air/Acetylene Filter Accessory (Part No. N9301398) is strongly
recommended to remove entrained water, oil, water aerosols and solid particles
from compressed air lines.

When using an air or air/acetylene accessory, never exceed 1050 kPa


! (150 psig).
Warning

If there is any doubt regarding the usability of a central air supply (insufficient
volume or pressure or excessive oil or water contamination), the quality of the
supply should be checked prior to the arrival of the instrument. A small, oil-less air
compressor meeting the stated requirements is available from PerkinElmer (Part
No. 03030313 for 115 volts, 60 Hz or Part No. 03030314 for 230 volts, 50 Hz
service).

Air compressors are generally uncomfortably noisy to have in the immediate


vicinity of the instrument. Whenever possible, it is advisable to locate them at some
distance from laboratory workers in an area providing suitable ventilation.

Cylinders of compressed air can also be used but are recommended only as an
emergency or short-term solution for the following reasons:
• A standard #1 size air cylinder contains about 6200 liters (220 cubic feet)
of air at standard temperature and pressure (STP). A premix burner-
nebulizer system uses about 20 liters/min (0.7 cubic feet/min), and,
therefore, a cylinder will last only about five hours. Unless an instrument
is used only a few hours per day, changing cylinders becomes a nuisance
as well as being expensive.
• Occasionally, cylinder air may be obtained from a liquefaction process
during which the oxygen-to-nitrogen ratio can change. Therefore, it is not
uncommon to find other than 20% oxygen in air cylinders. This can cause
erratic burner operation and non-reproducible analytical results and, in
extreme cases, may provide a potential safety hazard. In general, if
cylinder air is to be used, it is important to specify compressed air rather
than breathing air (i.e. medical grade) or an unspecified form.
58 Preparing Your Laboratory

For safe operation, oxygen must NEVER be used with PerkinElmer


! premix burner systems.
Warning

The use of air cylinders requires the use of a suitable dual-stage regulator. A
regulator for cylinders with a CGA 590 connection is available from PerkinElmer
(Part No. 03030264)

Acetylene:

Acetylene is used as fuel for flame operation.

For the overwhelming majority of analyses, acetylene is the preferred fuel gas with
AA spectrometers. Air/acetylene is the preferred flame for the determination of
about 35 elements by AA. The temperature of the air/acetylene flame is
approximately 2300 °C. For most air/acetylene flames, the acetylene flow used is
about 4 liters/min or 0.14 cubic feet/min. Using a heat-combustion value of 1,450
BTU per cubic foot, the heat given off would be approximately 12,300 BTU per
hour (3,600 W). An air/acetylene flame can be used with all PerkinElmer burner
heads but is most commonly used with the supplied 10-cm (4-inch) burner head.

It is recommended that special higher purity "atomic absorption" grade acetylene


(minimum 99.9% purity) be used instead of the welding-grade acetylene. If this is
not available, a welding-grade acetylene that has a minimum purity specification
of 99.6% may be used. In this case, an acetylene-specific filter (such as N930-1399,
or N930-1398)must be installed for the gas supply before it enters the instrument.

Regardless, it is still a good practice to install this filter even if the "atomic
absorption" grade acetylene is used.

A size 1A acetylene cylinder contains about 8,500 liters (300 cubic feet) of
acetylene and usually lasts about 30 hours of burning time with an air/acetylene
flame. The cylinder requires an acetylene pressure regulator, which can be
obtained from the supplier of the gas or from PerkinElmer (Part No. 03030106).
Flame Gas Requirements 59

Acetylene may react with copper, silver or mercury to form a


! potentially explosive compound. Never use copper tubings or fittings
for acetylene gas connections. the use of stainless steel tubings and
Warning fittings is recommended.

The PerkinElmer Acetylene Regulator Assembly includes an adapter so that the


pressure regulator can be connected to cylinders requiring either CGA 300 or CGA
510 fittings as well as a connector for attaching the fuel hose assembly supplied
with the instrument. The fuel hose assembly is constructed of red neoprene,
reinforced with high tensile-strength rayon cord, and provides a rated working
pressure of about 1700 kPa (250 psig). The connectors are permanently mounted
at each end of the hose assembly for connection to the pressure regulator and
instrument gas controls, and use left-hand threads as per accepted practice for fuel
gas connections. (See Section 5 for more details.)

It may be desirable to have an acetylene filter between the acetylene tank and the
instrument gas control system to remove particulates and acetone droplets from
acetylene, protecting the gas controls and AA burner system from contamination
and corrosion. An Acetylene Filter (Part No. N9301398) and an Air/Acetylene
Filter Accessory (Part No. N9301398) are available from PerkinElmer. Some
countries also require the use of a flashback arrestor, such as PerkinElmer Part No.
N9307506 in the acetylene fuel line.

Acetylene is normally supplied dissolved in acetone, and a small amount of


acetone carryover with the acetylene is normal. However, as tank pressure falls, the
relative amount of acetone entering the gas stream increases and can give erratic
results, particularly for elements such as calcium, tin, chromium, molybdenum and
others whose sensitivity is highly dependent on the fuel/ oxidant ratio. For this
reason, acetylene tanks should be replaced when the cylinder pressure drops to
about 600 kPa (85 psig).

Caution Failure to change the acetylene cylinder before the cylinder pressure drops
below 600 kPa (85 psig) may cause damage to valves or tubing within the
burner gas control system due to high acetone carryover. Such damage
from acetone is not covered by instrument warranties.
60 Preparing Your Laboratory

Usually acetylene is dissolved in acetone, thus the tanks must be operated in the
upright position in order to prevent acetone from entering the tubing and hoses. At
low acetylene tank pressure the amount of acetone in the gas increases and may
produce an unstable flame. Therefore exchange the acetylene tank when the
cylinder pressure falls below 600 kPa (6 bar, 85 psig).

New tanks should be positioned vertically for at least 8 hours prior to use. The
practice of "cracking the valve" of an acetylene tank (that is, opening the valve
slightly fora very short period prior to attaching the regulator) is not recommended.
While such an action will clear the valve opening of dust or dirt particles and may
remove acetone from the cylinder valve, it is a potentially hazardous practice and
one which should never be attempted in the presence of an open flame, sparks or
other possible sources of ignition.

Warning: Explosive
! Danger Acetylene line pressure from the tank to the instrument
Warning should never exceed 103 kPa (1.03 bar, 15 psig). At the higher
pressures, acetylene can spontaneously decompose or explode.

PerkinElmer recommends that a maximum acetylene line pressure of


80-95 kPa (12-14 psig) be used to provide a reasonable margin of
safety.

A flashback arrestor is required at the outlet of the pressure


regulator.

Both fuel and oxidant gas lines should be relieved of pressure at the end of the
working day or if the instrument is to remain unused for an extended period.
Cylinder valves should be closed to avoid the possibility of pressure regulators
failing and gas lines being subjected to the full cylinder pressure.
Flame Gas Requirements 61

Nitrous Oxide:

The nitrous oxide flame requires high flow rates of up to 30 L/min.


! Simple pressure regulators may freeze and cause malfunction. The
two-step or heated pressure regulator is highly recommended.
Warning

For higher temperatures, nitrous oxide is used as an oxidant.


The nitrous oxide/acetylene flame has a maximum temperature of approximately
2800 °C and is used for the determination of elements that form refractory oxides.
It is also used to overcome chemical interferences that may occur in flames of
lower temperatures. For the nitrous oxide/acetylene flame, the acetylene flow is
about 14 liters/min or 0.5 cubic feet per min. Using a heat of combustion value of
1,450 BTU per cubic foot, the heat given off would be approximately 43,000 BTU
per hour (12,500 W).
The use of air cylinders requires the use of a suitable dual-stage regulator. A
regulator for cylinders with a CGA 590 connection is available from PerkinElmer
(Part No. 03030264).
The use of nitrous oxide requires a number of accessories and precautions. A size
1A cylinder of nitrous oxide contains about 14,800 liters (520 cubic feet) and will
typically last for 10 to 12 hours of burning time. Cylinders of nitrous oxide (99.0%
minimum purity) are available from local suppliers. A dual-stage regulator is
recommended (and is mandatory in some countries).
Nitrous oxide is supplied in the liquid state, initially at a pressure of about 5000 kPa
(750 psig). Since the nitrous oxide is in liquid form, the pressure gauge does not
give a true indication of how much nitrous oxide remains in the cylinder until the
pressure starts to fall rapidly as the residual gas is drawn off.
When nitrous oxide is rapidly removed from the cylinder, the expanding gas causes
cooling of the cylinder pressure regulator and the regulator diaphragm sometimes
freezes. This can create erratic flame conditions or, in the most extreme case, a
flashback. It is therefore advisable to heat the regulator using either a built-in heater
or an externally supplied heat source, such as an electrical resistance heating tape.
62 Preparing Your Laboratory

Caution All lines carrying nitrous oxide should be free of grease, oil or other
organic material, as it is possible for spontaneous combustion to occur.
Cylinders of nitrous oxide should be considered high-pressure cylinders
and should be handled with care at all times.

A dual-stage heated nitrous oxide pressure regulator for use with gas cylinders with
a CGA 326 connection is available from PerkinElmer [Part No. 03030204 (115
volts) or 03030349 (230 volts)]. These regulators provide pressure control from
350-520 kPa (50-75 psig) and contain an integral thermostatted heater to prevent
freezing of the regulator diaphragm. A color-coded hose with suitable connectors
at each end is supplied with the regulators to provide connection to the instrument
gas controls.
Flame Gas Requirements 63

Argon:

Argon is required for external and internal gas streams through the THGA or HGA
graphite furnace or as a carrier gas with mercury/hydride systems such as the FIAS
or FIMS flow injections systems or the MHS-15. The quality criteria listed in the
following table for argon are suitable for these applications. Normally, for graphite
furnace operation, gaseous argon is used, although either liquid or gaseous argon
can be used. The choice of liquid argon or gaseous argon tanks is determined
primarily by the availability of each and the usage rate. Liquid argon is usually less
expensive per unit volume to purchase, but cannot be stored for extended periods.
If liquid argon is used, the tank should be fitted with an over-pressure regulator
which will vent the tank as necessary in order to keep the liquid argon cool enough
to remain in the liquid state. Gaseous argon tanks do not require venting and
consequently can be stored for extended periods without loss.

A dual-stage cylinder regulator that can be used with either gaseous argon or
nitrogen is available from PerkinElmer (Part No. 03030284). The regulator has a
CGA 580 fitting, and includes a color-coded hose with 1/4-inch Swagelok®
fittings to permit direct connection to the regulator and to the instrument gas
controls.

Table 2-5. Specifications for the Flame Gases


64 Preparing Your Laboratory

Table 2-6. Specifications for the Purge Gases

Fitting Specification Flame Gases


The customer must supply the respective wall outlets or pressure regulator outlets.

Table 2-7. Fitting Specification Flame Gases

Atomic Absorption Source Lamps


AA spectrometers require different source lamps, depending on the elements to be
determined and the instrument to be used. Multielement lamps are available for
some elements, but most lamps are constructed using a single element to avoid
potential spectral interferences and reduced performance, especially when using a
graphite furnace.
Drain Vessels 65

PerkinElmer manufactures all of its hollow cathode and electrodeless discharge


lamps. The Lumina™ series of hollow cathode lamps are especially noted for
spectral purity, brightness, stability and long life.

Hollow cathode lamps (HCLs) are excellent for most elements; however, there are
a number of "difficult" elements for which an improved light source is desirable.
PerkinElmer electrodeless discharge lamps (EDLs) provide improved performance
in most instances. EDLs are more intense than their corresponding HCLs. Most
also provide better lamp life and stability as well as better sensitivity. EDLs do not
require a separate power supply as it is built-in the PinAAcle systems.

A lamp mount or turret is supplied with all PerkinElmer AA instruments and will
accommodate all PerkinElmer HCLs or EDLs. Users who may have lamps with
1.5-inch diameters rather than the standard PerkinElmer 2-inch diameter can adapt
those lamps for use in PerkinElmer lamp mounts with the Small Diameter Lamp
Adapter Kit, (Part No. 03030870).

The PinAAcle Series 900T/H/Z/F operates correctly with PerkinElmer Standard


2" Lumina. Hollow Cathode Lamps (HCLs). PerkinElmer Coded Electrodeless
Discharge Lamps (EDL s) can also be used.

Drain Vessels
A specially-configured drain vessel is supplied with all PerkinElmer AA
instruments with burner systems. That vessel must be used to gather the effluent
from the AA burner drain.

The drain vessel should NOT be stored in an enclosed storage area. Rather, the
drain vessel should be stored in plain sight of the operator, usually on the floor in
front of the instrument or on an open shelf underneath the instrument table.

The drain system should be checked regularly and replaced when necessary.
Follow the directions in the instrument manuals regarding the proper placement of
the drain tube in the drain vessel and the proper liquid level in the drain vessel.
66 Preparing Your Laboratory

Cooling Requirements

Furnace Cooling
The graphite furnace uses water cooling to allow the graphite tube to return to its
equilibrium temperature (approximately ambient) quickly between measurements.

Furnace Power Supply Cooling


Cooling coils are incorporated in the furnace power supply to maintain the
components at a comfortable working temperature.

Cooling System
A water recirculating system and a cooling water system are also offered as options
for the PinAAcle 900H, PinAAcle 900T and PinAAcle 900Z systems. These water
systems provide coolant at a constant temperature and flow to allow the most
reproducible analytical conditions. They also make the system independent of
external water supplies and saves water.

External Cooling
If you intend to run the spectrometer system without the PerkinElmer cooling
system, you must connect another suitable source of cooling. The main water
system supply to the lab can be used if it meets the specifications defined in the
charts below. Laboratory water cooling systems can also be used if they meet our
specifications of the recirculating system we offer.
PC Configuration and Printer 67

Table 2-8. External Cooling Specifications

Water Temperature 20-40 °C


Water Pressure min. 350 kPa (3.5 bar, 50.8 psig)
max. 400 kPa (4.0 bar, 58 psig)
Water Flow Rate 2.5 L/min
pH of the Water Between 6.5 and 7.5
Hardness of the Water Not greater than 6 °d or 2.5mmol/L(100 mg/L
(ppm) Ca(CO3)2)

Caution If the water is too cold or flowing too fast, moisture may condense on the
graphite contacts, on the furnace windows or inside the water cooled
furnace power supply resulting in malfunction and severe damage.
Moisture on the contacts causes rapid attrition of the graphite surface,
while moisture on the furnace windows leads to attenuation of the energy.

PC Configuration and Printer


Only the currently shipping PerkinElmer supplied PCs will be installed free of
charge. Only for these PCs is operation guaranteed. There will be no support for
any other PC, as no compliance testing has been done to operate our software
efficiently. For details on computer requirements see Data System on page 96.

Installation Preparation

Check for Damage


• The customer must check the shipping box for damage. If any is found, the
carrier must be notified immediately.
Unpacking
• The spectrometer must be unpacked and brought into the laboratory at least
one day prior to installation to allow acclimation. The customer must be
68 Preparing Your Laboratory

warned about the weight of the instrument and informed that at least three and
preferably four adults are necessary to lift the instrument.
• The PC, printer and all other accessories should not be unpacked but be
available in their boxes at the installation location.
• If the PC is going to be networked, the customer should have an IT Specialist
available during the installation.

Product Line Experience

PC Skills
• The customer should have a basic working knowledge of Windows and how to
operate the software.
The customer should have a fundamental knowledge of atomic absorption
spectroscopy.
Principles of Operation 3
The PinAAcle 900 Series Spectrometer System

Concept
The PinAAcle 900 series spectrometer from PerkinElmer is a compact, high
performance atomic absorption spectrometer incorporating a burner system for
flame atomization and a graphite furnace for electrothermal atomization. The
spectrometer is capable of fully automatic single-element and sequential multi-
element analyses. The complete system is operated from the associated computer
using the software.
70 Principles of Operation

Principle of Operation of an Atomic Absorption Spectrometer


An Atomic Absorption Spectrometer consists of five basic components; light
source, a sample introduction system (atomizer of flame or graphite furnace), the
spectrometer (monochromater), the light detector and a system controller
(computer and software assembly).

The sample is measured for its elemental contents in solution and it is aspirated in
the sample introduction system, where their atoms absorb the light emitted from
the light source at its characteristic wavelength. This light at the characteristic
wavelength is aligned to the light detector. Based on the amount of light absorbed
and reaching the light detector, the concentration of the elements in the sample can
be determined. This is done with reference to a known concentration of the
elements to be measured at its characteristic wavelength.
Principle of Operation of an Atomic Absorption Spectrometer 71

Features of the PinAAcle 900 Series System


Table 3-1. PinAAcle Instrument Configurations and Models

Part Number Model Configuration Nebulizer Recirculator


N3200080 PinAAcle 900T THGA + Flame Stainless Steel With
Recirculator
N3200081 PinAAcle 900T THGA + Flame Stainless Steel Optional
Recirculator
N3200082 PinAAcle 900T THGA + Flame High With
Sensitivity Recirculator
Plastic
N3200083 PinAAcle 900T THGA + Flame High Optional
Sensitivity Recirculator
Plastic
N3200070 PinAAcle 900H HGA + Flame Stainless Steel With
Recirculator
N3200071 PinAAcle 900H HGA + Flame Stainless Steel Optional
Recirculator
N3200072 PinAAcle 900H HGA + Flame High With
Sensitivity Recirculator
Plastic
N3200073 PinAAcle 900H HGA + Flame High Optional
Sensitivity Recirculator
Plastic
N3200060 PinAAcle 900Z THGA N/A With
Recirculator
72 Principles of Operation

Part Number Model Configuration Nebulizer Recirculator


N3200061 PinAAcle 900Z THGA N/A Optional
Recirculator
N3200050 PinAAcle 900F Flame Only Stainless Steel N/A
N3200051 PinAAcle 900F Flame Only High N/A
Sensitivity
Plastic

• The PinAAcle models H and T has a stacked design with the graphite furnace
located on the bottom of the stack.

• When the flame atomizer is in operation, the furnace atomizer is protected by


a furnace head cover. When the furnace atomizer is in operation, the flame
burner assembly has to be removed, with the furnace head cover flipped up.

• Transversely-heated graphite furnace featuring full Stabilized Temperature


Platform Furnace (STPF) technology.

• Longitudinal Zeeman-effect background correction for the PinAAcle 900Z


and 900T and D2 background correction for the PinAAcle 900 for the
electrothermal atomization.

• Deuterium background correction for flame atomization.

• Automated self-optimization of the burner system.

• High capacity furnace autosampler.

• Intuitive, easy-to-use software with which you control the spectrometer


system. The software also incorporates a range of powerful quality control
functions.

System Components
The PinAAcle 900 is a compact bench top spectrometer. The major components of
the system are:
Principle of Operation of an Atomic Absorption Spectrometer 73

• The spectrometer, containing the optical system, the electronics, and the
atomizer compartment.

• The burner system can be driven into and out of the atomizer compartment by
software command.

• The furnace autosampler, mounted on a swing arm in front of the atomizer


compartment.

• The furnace cooling system.

• The computer and the associated software.

• The printer; this is optional but strongly recommended.

System Control
To control the spectrometer and perform your analyses, you use the software for
AA application program, which runs under the Microsoft Windows operating
system. The computer keyboard, the screen, and the mouse form the user interface.

When you switch on the spectrometer system it performs an initialization


procedure to check the instrument. While the spectrometer is operating, the control
system continually monitors many instrument functions. It generates appropriate
messages when a problem occurs and prevents potentially hazardous situations
from arising.

You can obtain more information about the application program from the help by
selecting F1 on the computer keyboard.

Accessories
PerkinElmer offers autosamplers for operation with the burner system, flow
injection systems, Autoprep, and much more. Please contact your local
PerkinElmer office to obtain detailed information.

The Optical System


A common feature of the PinAAcle 900 series compared to previous atomic
absorption models is the change from free path optics to fiber optics. This change
74 Principles of Operation

reduces the number of optical components, decreases the size of the instrument as
well as reduces stray light and scattering losses. All glass fibers have been
optimized to provide high transmission for the whole wavelength range of interest.

Four different types of instruments are available, PinAAcle 900F, 900H, 900T and
900Z. But two parts of the optical layout are common to all versions, the lamp
compartment and the monochromator:

The lamp compartment has positions for up to eight spectral sources: HCL and/or
EDLs. The radiation from the requested source lamp is collected by a movable
mirror and coupled into the source fiber.

At the other end of the optical path the fiber bundle coming from the sample
compartment is coupled onto the Litttrow-configuration monochromator. This
contains of a parabolic mirror and a large area reflecting grating blazed at two
wavelengths; 236 nm for operation in the UV spectral range and 597 nm for
operation in the visible spectral range. Various slit widths are available to adjust
the signal throughput and resolution to the requirements of each measurement.

The PinAAcle 900T and PinAAcle 900H can both be used for flame and furnace
atomization. They use a double-beam configuration as depicted in the following
schematics beginning on page 75. In addition to the HCL and EDL source both
models are equipped with a deuterium lamp for background correction. The light
from the source and the deuterium lamps are guided to a fiber coupler, which splits
the light into separate sample and reference beams. Thus each channel, sample and
reference, contains a certain percentage of the source and deuterium lamp. Both
beams pass through the sample compartment before they are coupled into another
pair of fibers by a set of ellipsoidal mirrors and guided to the monochromator and
detector.

The deuterium and source light is split into two beams---one that passes through
the upper part of the sample compartment, and one that passes through the lower
part of the sample compartment. In the flame mode, the upper beam is the the
"sample" beam and the lower beam (which passes through the graphite furnace) is
the "reference" beam. In the furnace mode, only the lower beam (that passes
through the graphite furnace) is used.

The main difference between the PinAAcle 900T and 900H lies in the type of
furnace atomizer. The PinAAcle 900H uses a HGA atomizer. The PinAAcle 900T
is equipped with a THGA atomizer using Zeeman background correction.
Principle of Operation of an Atomic Absorption Spectrometer 75

The PinAAcle 900F flame system is similar to the 900T model as it uses a double-
beam configuration and a deuterium lamp for background correction. However
instead of passing through the sample compartment, the reference beam is directly
guided from the fiber coupler to the monochromator.

The PinAAcle 900Z is a Zeeman-THGA furnace only system and uses a single
fiber to transmit the source light to graphite furnace and then to the monochromator
and detector.

Optical System Schematics for the PinAAcle 900 Series

Figure 3-1. Optical System for the PinAAcle 900F


76 Principles of Operation

Figure 3-2. Optical System for the PinAAcle 900H


Principle of Operation of an Atomic Absorption Spectrometer 77

Figure 3-3. Optical System for the PinAAcle 900T


78 Principles of Operation

Figure 3-4. Optical System for the PinAAcle 900Z


The Electrical Connectors and Switches 79

The Electrical Connectors and Switches

Operational On/Off Switches

Figure 3-5. On/Off switch on the instrument


Item Description
1 On/Off switch

Spectrometer
You normally switch the system on and off with the operational on/off switch on
the front panel of the spectrometer.
80 Principles of Operation

Cooling System
The cooling system requires a 230 V line power supply, which is supplied and
controlled from the spectrometer. A special line power cord is provided for this
purpose. Do not connect the cooling system to an external power source.

You can leave the on/off switch on the cooling system in the "on'" position since
the system is controlled from the spectrometer.
The Electrical Connectors and Switches 81

Connectors and Controls on the Rear Panel

1
3 4
8
2 6
5

Figure 3-6. Gas, cooling and electrical connectors on the rear panel
Item Description
1 Power circuit breaker 5 230 v power receptacle
2 Main power cord 6 Water hose in
3 Argon (or Nitrogen) gas line 7 Water hose out
4 Special gas line 8 Purge gas connection
82 Principles of Operation

The Gas and Cooling Connectors

Furnace Cooling

Item Designation Function

1 In Fitting for connection of the cooling water inlet hose to the


spectrometer.
2 Out Fitting for connection of the cooling water outlet hose from the
spectrometer.

Furnace Gases

Item Designation Function

3 Ar/N2 Connector for the connection of the normal gas supply to the
Normal furnace (argon or nitrogen).

4 Special Gas Connector for the connection of the special gas supply to the
furnace. If you are not using a special gas, you must also
connect the normal gas to this connector.
Burner Assembly System 83

Burner Gases

Item Designation Function

5 Air Fitting for connection of the air supply to the spectrometer.


The air supply is required for the burner and also for the
pneumatic system in the spectrometer.
6 N2O Fitting for connection of the nitrous oxide supply to the burner.

7 C2H2 Fitting for connection of the acetylene supply to the burner.

Burner Assembly System


The burner system used in the spectrometer system is of the premix design. The
measurement solution is sprayed by a pneumatic nebulizer into the burner chamber
in the form of an aerosol. This aerosol is thoroughly premixed with the burner fuel
and oxidant gases in the burner chamber. This gas mixture then passes through the
burner slot into the flame.

The burner system comprises the following major components:

• Nebulizer

• Burner chamber

• End cap

• Burner head

• Drain system

• Gas control system (incorporated in the spectrometer)


84 Principles of Operation

2 1

3
5
4

Figure 3-7. Major components of the burner system


Item Description Item Description
1 Burner head 5 Stainless steel nebulizer (is shown
here but you can also have a high
sensitivity plastic nebulizer
attached here)
2 Burner head adjustment tool 6 End cap assembly
3 Spray chamber 7 Retaining ring
4 Flow spoiler 8 Burner head o-ring
Burner Assembly System 85

How the Burner System Works


The basic instrument includes a burner system for flame sampling operation. A
system block diagram is shown in the next figure. The heat produced by the flame
converts sample aerosol into free atoms that can absorb the light from the source
lamp specific for the element to be determined.

A sample solution is aspirated through the nebulizer and sprayed as a fine aerosol
mist into the burner chamber. Here, the sample mist is thoroughly mixed with the
fuel and either air or nitrous oxide gases. Fuel gas enters the chamber through the
fuel inlet hose while the oxidant enters through the inlet built into the burner
chamber body.

To prevent incomplete sample atomization, a plastic flow spoiler is placed inside


the chamber directly in front of the nebulizer. The high sensitivity plastic nebulizer
has a ceramic, one-piece, impact-bead structure which improves nebulization
efficiency. Larger sample droplets not carried around the flow spoiler by the gas
flow are forced by the spoiler to the bottom of the chamber. This, in turn, allows
only the finer sample droplets to be carried into the chamber. The flow spoiler
improves precision but reduces sensitivity. The larger droplets are removed
through the drain. Stainless steel nebulizer used on the PinAAcle 900 Series does
not have an impact bead.

Once the sample aerosol is thoroughly mixed in the chamber, it then advances to
the burner head where atomization occurs.

The gas control system monitors and controls fuel and oxidant flows. Burner
operation, including flame ignition, flame shutoff and gas flow settings, is
controlled through the software.

The next figure shows a "block diagram" of how the burner system flows, from the
gas supplies, to the gas box, to the burner hardware itself and out to the drain vessel.
86 Principles of Operation

Figure 3-8. Block diagram of the burner system


Burner Assembly System 87

Burner Head Options


All the burner heads are made from titanium. The 10 cm, air-acetylene burner head
is standard with the PinAAcle 900 Series instruments. All the available burner
heads are listed next in numerical order.

• N0400100: 5 cm, single-slot burner head (for nitrous oxide-acetylene


operation only).

• N0400101: 5 cm, single-slot burner head (for air-acetylene operation). It


features a wider slot than the nitrous oxide burner head. Used to extend
linear and working range.

• N0400102: 10 cm, single-slot burner head (for air-acetylene operation -


Standard for all PinAAcle instruments.).

• N0400103: 10 cm, three-slot burner head (for analysis of high dissolved


solids content solutions with air-acetylene flames).

• N3161240: burner head adjustment tool. Insert the adjustment tool into the
burner head and adjust the angle to extend the linear range. This tool
allows you to do adjustments while the burner is hot.
88 Principles of Operation

2 3
1 4

5
6

Figure 3-9. The four burner heads available and adjustment tool.
Item Description Part Number
1 5-cm, single-slot burner head (for N0400100
Nitrous oxide-acetylene flame)
2 5-cm, single-slot burner head (for air- N0400101
acetylene flame)
3 10-cm, single-slot burner head N0400102
4 10-cm, three-slot burner head N0400103
5 Burner head adjustment tool N3161240
6 Burner head adjustment hole for -
adjustment tool

The Burner Mount


The quick change burner mount provides horizontal, vertical, and rotational
adjustment. The quick-disconnect release lever simplifies removal of the burner
assembly.
Burner Assembly System 89

The Ignitor Assembly


The ignitor assembly includes the glow plug, the ignitor solenoid and ignitor arm,
the burner head interface circuit, and the flame detect circuit. When the ignitor is
activated (automatically), the glow plug is energized and heats up. The ignitor
solenoid, which is also energized, swings the ignitor arm into place. The ignitor
arm is a gas-capture tube through which the gases flow from the burner to the glow
plug. The gases in the tube are ignited by the heat of the glow plug, which, in turn,
ignite the flame at the burner head slot.

The Gas Controls


The gas controls provide control of the flow rates of the fuel gas (acetylene) and
the oxidant (air or nitrous oxide). You select the gas flow rates and optimize the
flame via software. The gas control system is incorporated in the spectrometer. The
system includes safety interlocks for the flame. If the fuel or oxidant pressure falls
below a minimum value for safe operation the flame is shut down in a safe
sequence. The system also includes automatic sequencing of the gases when the
nitrous oxide-acetylene flame is ignited or extinguished.

The burner will be shut down in a safe sequence in the event of a power failure.

The Drain System


During flame operation, measurement solution that condenses out in the spray
chamber runs to waste through the siphon interlock drain trap and is collected in
the drain vessel.

The siphon interlock drain trap is integral with the burner end cap and includes an
internal trap to make certain that back pressure is applied to the burner chamber.
This ensures that a fuel/oxidant mixture cannot enter the drain vessel. There is a
magnetic float in the drain trap that shuts down the flame if the drain system is not
functioning properly. If the liquid level in the trap is too low, the switch is activated
and the flame is shut down.
90 Principles of Operation

Figure 3-10. The burner drain system and its parts


Item Description
1 Drain Interlock
2 Drain hose
3 Drain cap
4 Drain bottle
Burner Assembly System 91

Burner Installation
The burner is shipped in place so it does not need to be installed in the instrument.
For information on burner installation after maintenance procedures refer to
Chapter 6, Maintenance, in this hardware guide. See Chapter 4, Installation, in this
hardware guide, for information on connecting the burner gases.

Burner System Maintenance


Refer to Chapter 6, Maintenance, in this hardware guide for extensive burner
system maintenance information.

Burner System Troubleshooting


We recommend that you consult the troubleshooting information included in this
hardware guide before you call a PerkinElmer service engineer. Refer to Chapter
7, Troubleshooting, in this hardware guide, for your burner system troubleshooting
information. Included are suggestions to help you determine systematically
whether instrument problems are due to improper analytical techniques, improper
selection of instrument parameters, or a malfunction of the instrument.

Burner Spare Parts and Accessories


Refer to the end of Chapter 6, Maintenance, in this hardware guide for burner
system spare parts information.
92 Principles of Operation

Specifications

System Design:

Instrument Description

PinAAcle 900T and PinAAcle 900T and PinAAcle 900H are fully-integrated bench
PinAAcle 900H: top design atomic absorption spectrometers, incorporating all
spectrometer, flame atomizer and graphite furnace atomizer
components in a single instrument.
PinAAcle 900Z: PinAAcle 900Z is fully-integrated bench top design atomic
absorption spectrometer that incorporates a single-beam
spectrometer system and graphite furnace atomizer in a single
instrument.
PinAAcle 900F: PinAAcle 900F is a fully-integrated bench top design atomic
absorption spectrometers, incorporating the spectrometer, and
flame components in a single instrument.
Optical System Photometer: Real-time double-beam optical system. Front-surfaced,
reflecting optics with protective coating. Optical system sealed
within protective cover.
Monochromator: Littrow design with motorized drive for automatic wavelength
selection and peaking.
Wavelength range: 184 - 900 nm.
Diffraction grating: 1800 lines/mm blazed at 236 nm and 597
nm.
Grating area:64 x 72 mm
Reciprocal linear dispersion: 1.6nm/mm (nominal)
Focal length: 267 mm
Spectral bandwidths: Slits available are 0.2, 0.7 and 2.0 nm.
Detector: Wide-range segmented solid-state detector, including a built-in
low-noise CMOS charge amplifier array.
Specifications 93

Instrument Description

Automatic Lamp Selection: 8-lamp holder with built-in power supplies for hollow cathode
and electrodeless discharge lamps. Computer-controlled lamp
selection and alignment via software. Lamp elements and
recommended operating currents are automatically recognized
and set when using PerkinElmer Lumina™ hollow cathode
lamps.

Background Correction

Background Correction Description

Deuterium arc lamp: PinAAcle 900H and PinAAcle 900F Auto Built-in continuum
source double-beam background correction using a high-
intensity deuterium arc lamp.
PinAAcle 900Z and PinAAcle 900T use Longitudinal AC
Zeeman-effect background correction using a modulated 0.8
Tesla magnetic field oriented longitudinal to the optical path.
The magnet is automatically switched on during the
atomization step only. Also built-in is continuum source
double-beam background correction for uses with flame
operation.

Flame Atomizer

Flame Atomizer Description

Gas Controls: Fully computer-controlled with oxidant and fuel monitoring.


Acetylene flow is automatically adjusted prior to the oxidant
change when switching to or from nitrous oxide-acetylene
operation.
94 Principles of Operation

Flame Atomizer Description

Safety Functions: Interlocks prevent ignition if the proper burner head, the
nebulizer/end cap, or the burner drain system is not correctly
installed; the liquid level in the drain vessel is incorrect; or gas
pressures are too low. Interlocks also will automatically shut
down burner gases if a flame is not detected, or if any of the
other interlock functions are activated. Provision is included
for safe shutdown from all operating modes in the event of a
power failure.
Burner System: This system has a stacked design, with flame unit on the top,
and graphite furnace at the bottom. The burner is equipped
with a high-strength inert mixing chamber, angled to ensure
proper drainage. Depending on the type of analysis you can
use either the high sensitivity corrosion-resistant plastic
nebulizer and stainless steel nebulizer. There are separate part
numbers for the plastic or stainless steel nebulizers.

Graphite Furnace Atomizer

Graphite Furnace Atomizer Description

PinAAcle 900H Built-in fully computer-controlled Heated Graphite Atomizer


(HGA™).
PinAAcle 900T and Built-in fully computer-controlled Transversely Heated
PinAAcle 900Z Graphite Atomizer (THGA™). The graphite tube is
transversely heated providing a uniform temperature profile
over the entire tube.
Specifications 95

Graphite Furnace Atomizer Description

PinAAcle 900H, PinAAcle An external protective gas stream around the graphite tube
900T and PinAAcle 900Z prevents the entrance of outside air to maximize tube life. An
internal purge gas goes through the graphite tube to remove the
volatilized matrix vapors during drying and thermal
pretreatment. The two gas streams are computer-controlled
independently. Pneumatic opening and closing of the furnace
for easy tube change.
Common Furnace Features: Program Flexibility: Analytical programs with up to 12 steps
can be set up. Each step can be programmed with the following
parameters:
Temperature: Ambient up to 2600 °C (up to 2700 °C with HGA) in steps of
10 °C.
Ramp Time: 0 to 99 s in steps of 1 s.
Hold Time: 0 to 99 s in steps of 1 s.
Internal Gas Flow: 0 mL/min (gas stop), 50 mL/min (mini-flow), 250 mL/min
(full flow); can be switched over to another type of gas
(Alternate Gas).
Furnace Opening and Pneumatically-operated by software command.
Closing:
Required Inert Gas: Argon. Inlet pressure 300 kPa (3 bar) minimum. Maximum gas
consumption is 700 mL/min with the PinAAcle 900T and
PinAAcle 900Z. Maximum gas consumption is 1220 mL/min.
Water Coolant: There are separate part numbers for the main instrument with
and without the water circulatory system.
It is recommended to use the re-circulatory system for the
graphite furnace analyses. When operating the PinAAcle 900
Series without the circulatory cooling system, cooling water
meeting the following specification should be used: Sediment-
free drinking water; 20-40 C; flow rate not less than 2 L/min;
pressure between 2.5 and 4.5 bar; pH not harder than 6 dH or
100 mg/L (ppm) of Ca(CO3)2.
96 Principles of Operation

Furnace Autosampler

Furnace Autosampler Description

Furnace Autosampler: Sampler Table: Installed in front of the furnace unit.


Removable sample tray with 88 and 148 sampling positions
for sample and reference solutions and 1 overflow container
for pipette washing. Minimum sample requirement: ca. 0.1
mL.
Dispensable Volume: Sample and Reagent: 1...99 uL, selectable in increments of 1
uL. Max. dispensable vol. 99 uL (sample volume + reagent
volume). Flushing volume 1.3 mL, fixed.
Electronics: The autosampler is powered from the spectrometer and is
software-controlled.

Data System

Data System Description

Computer: Lenovo ThinkCentre M83 Windows® 7 (64-bit), Tower USA.


Product Family M83
Machine Type 10AGS01A00
Processor Intel Core i5-4670 Processor (3.4GHz, 6M Cache)
HDD 1TB 7200RPM
Form Factor Tower
Graphics Intel HD Integrated Graphics
Memory 4GB X 2 DIMM 1600MHz
UDIMM DDR3
Specifications 97

Data System Description

2nd Serial Port Yes


Optical DVD Recordable
Wireless WiFi 6235
Operating System Win 7 Ultimate 64-bit
Warranty 3 year Onsite
Recovery DVD Yes
Mouse: USB optical mouse with scroll
Keyboard: USB Keyboard

Includes Operating System and its power cord;

Physical Data - Instruments

Specifications Descriptions

Dimensions: PinAAcle 900T: 95 cm wide x 73 cm high x 68 cm deep (104 cm deep


with furnace autosampler)
PinAAcle 900Z: 95 cm wide x 73 cm high x 68 cm deep (104 cm deep
with furnace autosampler)
PinAAcle 900H: 95 cm wide x 73 cm high x 68 cm deep (104 cm deep
with furnace autosampler)
PinAAcle 900F: 95 cm wide x 73 cm high x 68 cm deep.
Weight: PinAAcle 900T: 133 kg (instrument only).
PinAAcle 900Z: 118 kg (instrument only).
PinAAcle 900H: 107 kg (instrument only).
PinAAcle 900F: 87 kg (instrument only).
Electronics: The autosampler is powered from the spectrometer and is software-
controlled.
98 Principles of Operation

Specifications Descriptions

System Power requirements 230V (± 10%), 50/60 Hz (± 1%)


Electrical Protection: Insulation class I; pollution degree 2.
Certification: Designed and tested to be in compliance with the legal requirements
for laboratory instruments. The instrument is developed and produced
in compliance with ISO 9001. The software provides required control
parameters for GLP and instrument performance validation.
Environmental Requirements: Ambient temperature: +10 C to +35 C. Relative humidity: 20 to 80%
non-condensing.

Physical Data - Cooling System

Specifications Description

Cooling System: Self-priming recalculating system with fan-assisted heat


exchanger for constant cooling of the graphite furnace. Water
temperature during operation approximately 36 C; water flow
2.5 L/min
Power requirements: 230V (± 10%), 50/60 Hz (± 1%); approx. 140 VA maximum
power consumption.
Electronics: The autosampler is powered from the spectrometer and is
software-controlled.
Dimensions: 20 cm wide x 375 cm high x 50 cm deep.
Weight: 18 kg with coolant.
Certification: Designed and tested to be in compliance with the legal
requirements for cooling systems.
Specifications 99

Technical Performance for the Flame AA

High Sensitivity Nebulizer


Standard Solution Stainless Steel Nebulizer
without spacer

2 mg/L Copper (Cu) ≥ 0.11 Absorbance unit ≥ 0.35 Absorbance unit


standard solution
Precision,% RSD ≤ 0.5 ≤ 0.5

Under the standard and/or optimized operating conditions.

Technical Performance for the Graphite Furnace AA

Heated Graphite Transversely-Heated Graphite


Standard Solution
Atomizer (HGA) Tube Atomizer (THGA) Tube

20 μL of 25 μL Copper (Cu) - ≥ 0.13 A.s (Characteristic Mass, Mo


standard solution = 17pg)
20 μL of 25 μL Copper (Cu) ≥ 0.11 A.s (Characteristic -
standard solution
Mass, Mo = 4pg)

Under the default and/or optimized operating conditions. A variation of ± 20% is


possible and acceptable.
100 Principles of Operation
Installation 4
Introduction
This chapter describes how to install the PinAAcle Series instruments. In
conjunction with this material, be sure to consult the Safety Practices chapter and
Preparing Your Laboratory chapter in this manual. The following sections are
included in this chapter:

• Unpacking Instructions on page 103

• Before You Install the Spectrometer on page 105

• If You Must Move and Reinstall the Spectrometer on page 106

• Connecting the Gases on page 111

• Connecting the Computer and Printer on page 119

• Electrical Connections on page 121

• Installing the Cooling System on page 126

• Connecting the Drain System to the Burner on page 130

• Nebulizer Installation on page 134

• Installing AS 900 Furnace Autosampler on page 135

• Installing the Sample Capillary on page 146


102 Installation

• Installing S10 Autosampler on page 160

• Lamps on page 160

• Replacement Parts on page 160

• Shipping List for the PinAAcle 900F on page 161

• Shipping List for the PinAAcle 900H on page 162

• Shipping List for the PinAAcle 900T on page 164

• Shipping List for the PinAAcle 900Z on page 167


Unpacking Instructions 103

Unpacking Instructions
Carefully read these instructions before unpacking the PinAAcle Series to avoid
damage to the instrument. The PinAAcle Series is packed in a cardboard box that
has been designed to safely move and unload the instrument. The bottom of the
crate is a shipping platform designed for use with a forklift.

The shipping platform used to pack the instrument is returnable for reuse within the
U.S.A. only.

Inspecting the Shipment


Upon receipt of the instrument, the exterior of all the shipping cartons should be
inspected. All cartons should arrive unopened and undamaged. If the examination
reveals that damage has occurred in shipment, notify the carrier and PerkinElmer
immediately. A representative of the shipping carrier must be present for insurance
purposes.

Unpacking the PinAAcle 900 Series Spectrometer


The instrument is shipped in one carton. Two cardboard boxes containing the
accessories are shipped separately.

Tools Needed

• Snipers for banding and tie wraps

Banding on the Box

Wear safety glasses when cutting the steel banding to prevent injury.
!
Warning

1. Check the shock watch and the two tip-and-tell indicators. Record the status of
the indicators on the waybill if they have been tripped.
2. Record any visible damage on the waybill before accepting the shipment.
Notify your local PerkinElmer customer support engineer immediately.
104 Installation

How to Unpack the Instrument


1. Place the instrument carton on the floor in front of the bench on to which the
instrument will be placed.
2. Cut the bands that hold the carton together, lift off the top of the shipping
carton.

3. Pull out all the foam pieces that secure the instrument in the box.

4. The two cardboard boxes containing the accessories are shipped separately.

5. Lift up and remove the carton sleeve.

6. Remove the polyethylene bag covering the instrument.

7. Prepare to lift the instrument out of the carton. You will need four people to
do this. The bench should be nearby and if the bench has wheels make sure that
the wheels are locked.

The instrument can weigh at least 87 kg (191 lbs, for a PinAAcle


! 900F; 900T weighs 133 Kg/293 lbs). Use proper lifting posture when
lifting the instrument out of the carton. Be aware that most of the weight
Warning is located at the right side of the instrument. It will want to tip forward
when it is lifted out of the carton, so be prepared to support that corner.

8. Along the underside of the instrument are hidden handles. Locate these handles
and position two people on each where these handles are located.

9. Squat down and place both hands underneath the instrument handles. Spread
your hands as far apart as possible while grasping the underside of the
instrument.

10. With knees bent, simultaneously lift the instrument up as you end up in a
standing position. Carefully place the instrument on the bench.

11. Remove any adhesive tape on instrument.


Before You Install the Spectrometer 105

Recycling the Instrument Box


If the customer plans on moving your PinAAcle Series Spectrometer they may
want to keep the cardboard box that the instrument was shipped in. If the customer
needs to dispose of the cardboard box please have them do so in accordance with
their local environmental regulations

Before You Install the Spectrometer

When the spectrometer arrives


• Check the exterior of the shipping crate for obvious signs of damage. If the
crate has been damaged, file a claim with the authorized carrier immediately
and inform your nearest PerkinElmer office.

• Contact your local PerkinElmer office to arrange for the installation.

Before the service engineer arrives


• You must prepare a suitable site for the spectrometer and any accessories. See
Chapter 2, Preparing Your Laboratory on page 37 and the guides for any
accessories.

• You must make sure that the fume ventilation system and the necessary gas
supply lines and regulators are installed.

• Although you should not perform the initial installation yourself, we


recommend that you read the installation instructions to learn about the
spectrometer and its requirements before you start using it.

These instructions are also provided in case you need to alter any of the
connections or move the instrument, autosampler or accessories in your
laboratory.

When the service engineer arrives


• The service engineer will remove the spectrometer from the crate and check
that all parts have been delivered. If anything is missing or damaged, the
service engineer will make sure that the respective parts are supplied.
106 Installation

• The service engineer will remove the shipping locks, perform pre-installation
checks, install the spectrometer, and make sure that everything functions
correctly.

If You Must Move and Reinstall the Spectrometer


We recommend that only a PerkinElmer service engineer or a PerkinElmer trained
and authorized person moves and reinstalls the spectrometer.

If the customer should attempt to do this themselves, PerkinElmer cannot be held


responsible for any damage or malfunctioning of the spectrometer.

The instructions here are primarily intended for occasions where the customer may
want to move the spectrometer short distances to a new location within the
laboratory.

Have the customer read the instructions carefully and be sure they understand them
thoroughly before they attempt to move the spectrometer. Have the customer read
the detailed information given in the relevant sections of this chapter before they
reinstall the spectrometer.

If the customer intends to transport the spectrometer over a longer distance, have
them contact their local PerkinElmer office since internal shipping locks must be
set via the service software, inside the spectrometer.

Preparing the Spectrometer to be Moved


1. Close the software application then shut down the Windows operating system.

2. Switch off the spectrometer power switch including the rear circuit breaker,
the computer, and all the accessories.

3. Disconnect all the electrical cables.

4. Remove the furnace autosampler from the spectrometer.

5. Disconnect the burner gas supplies. Bleed the flame gases if moving to another
location.
If You Must Move and Reinstall the Spectrometer 107

6. Flush with DI water for 1-2 minutes and then aspirate dry air for 1 minute if
moving to another location. This will prevent clogging and contamination of
the nebulizer.

7. Disconnect the drain system from the burner.

8. Disconnect the furnace gas and water supplies.

9. Prepare the computer and other system components for transport as described
in their own guides.

Moving the Spectrometer to Another Location


Moving the PinAAcle 900 over a short distance on a movable table is no problem,
if the following precautions are observed.

However, transporting over a larger distance (including tilting or mechanically


lifting) should only be done after securing the THGA furnace and the optical
components.

Warning: Risk of injury through lifting


The instrument can weigh at least 87 kg (191lbs for a PinAAcle 900F;
! 900T weighs 133 kg 293 lbs).
Improper lifting can cause painful and sometimes permanent back injury.
Warning Use proper lifting techniques and always use the handles to lift or
move the instrument.

Caution The spectrometer is a precision optical instrument. Move the spectrometer


very carefully and protect it from vibrations and jolts. Do not tilt the
spectrometer.
If the spectrometer must be tilted or mechanically lifted, contact your
PerkinElmer service representative before moving the spectrometer. The
shipping locks must be properly secured to prevent any damage occurring
if the spectrometer is tilted or jolted.

Carefully lift the spectrometer onto a movable table to transport it to the new
location.
108 Installation

For instructions on reinstallation see Reinstalling the Spectrometer on page 109.

Furnace Shipping Position


1. Open the flame door.

2. For PinAAcle 900T and 900Z, make sure that the furnace knob is securely
tightened all the way so that the furnace head will not move if the spectrometer
must be relocated.

Figure 4-1. Furnace locking knob


Item Description
1 Furnace locking knob
If You Must Move and Reinstall the Spectrometer 109

Reinstalling the Spectrometer

Tools Needed

• Phillips screwdriver

• Adjustable wrench

• Flat bladed screwdriver

Install the spectrometer by following exactly the procedures described in this


chapter, as summarized in the steps below.

Note The instrument ships with the nebulizer in place based on the part number
configuration ordered (a stainless steel or high sensitivity corrosion
resistant plastic nebulizer).

1. Prepare the new site for the spectrometer; see Chapter 2, Preparing Your
Laboratory on page 37.

2. Connect the burner and furnace gas supplies.

3. Connect the drain system to the burner.

4. Install the furnace autosampler.

5. Connect the cooling system for the graphite furnace.

6. Make sure that the main power switches of all the instruments are in the off
position, then connect the electrical cables.

Connecting the Burner Gases


The connectors for the burner gases are located on the rear panel of the
spectrometer.
110 Installation

What you need to provide


• Suitable supplies of acetylene, air, and nitrous oxide. The gases must conform
with the requirements listed in Chapter 2, Preparing Your Laboratory on page
37.

• Suitable pressure regulators and on/off valves near to the spectrometer for the
gas supplies.

The gas supply systems must comply with your local safety regulations. Also refer
to the information given under Gas Requirements on page 52.

Warning: Flashback Hazard


PerkinElmer burner systems are designed for use with compressed air.
! The use of oxygen can cause an explosion in the burner system, and
oxygen-enriched air can cause a flashback of the flame.
Warning
Never use oxygen or oxygen-enriched air with PerkinElmer burner
systems. Use only compressed air.

What is Provided With the Spectrometer


• Gas hose assemblies for acetylene, air, and nitrous oxide. The fittings on the
gas hose assemblies are suitable for connection to most commercially available
pressure regulators. These are R 3/8'' standard threaded fittings. The fuel
(acetylene) fitting has a left-hand thread, while the oxidant (air, nitrous oxide)
fittings have right-hand threads.
If you require an adapter for your regulator, contact the gas supplier or the
regulator manufacturer, or your local PerkinElmer office.
• The instrument ships with standard US gas line configurations. For European
gas connection adapters see the figure on page 113.
Connecting the Gases 111

Connecting the Gases


Refer to the figure on page 112, Connecting the burning gases.

Air
1. Make sure that the air supply is turned off.
2. Use the black hose assembly to connect a source of clean, dry, and filtered air
to the fitting labeled Air on the rear panel of the spectrometer. Use an
adjustable wrench to tighten the connections.

Nitrous oxide
1. Make sure that the nitrous oxide supply is turned off.
2. Use the blue N2O hose assembly to connect a source of clean, dry nitrous oxide
to the fitting labeled N2O on the rear panel of the spectrometer. Use an
adjustable wrench to tighten the connections.

Acetylene
1. Make sure that the acetylene supply is turned off.
2. Use the orange C2H2 hose assembly to connect a source of clean, dry acetylene
to the fitting labeled C2H2 on the rear panel of the spectrometer. Use an
adjustable wrench to tighten the connections.
112 Installation

3
2

Figure 4-2. Connecting the gas lines


Item Description Item Description
1 Acetylene (C2H2) 3 Air

2 Nitrous Oxide (N2O)

Converting Standard U.S. Gas Lines to European Requirements


The U.S. original gas lines are shipped with the instrument and these lines will need
to be cut and the European gas connection adapters will need to be used.
1. Cut the the original gas lines shipped with the instrument.
Connecting the Gases 113

2. Use the pinch clamp tool to secure the connection clamps (Part No. B0155661)
to the European gas connection adapters to the gas line.
3. Attach the modified gas lines to the proper gas outlets.
For European gas connection adapters see the following figure.

Figure 4-3. European gas connectors (with part numbers listed)


Item Description
1 Air/Acetylene/Nitrous Oxide (3 pieces)
2 Air/Nitrous Oxide (2 pieces)
3 Acetylene (1 piece)

As an alternative, European gas lines can be purchased for European installations.


114 Installation

Part Number Hose Description


B0154987 Air Hose
B0154990 Nitrous Oxide Hose
B0154984 Acetylene Hose

Connecting the Furnace Gases


The connectors for the furnace gases are located on the rear panel of the
spectrometer.

Note The furnace will operate correctly only if there is gas pressure at both the
Normal Gas and Special Gas inlets. If you are using only an inert gas you
must connect the gas to both inlets using the Y-connector.

What you need to provide


• A suitable supply of argon (or nitrogen) and if necessary a suitable supply of a
special gas. The gases must conform with the requirements listed in Chapter 2,
Preparing Your Laboratory on page 37.

• Suitable pressure regulators and on/off valves near to the spectrometer for the
inert and special gas supplies.

• A tube cutter for the special gas tube. This is an optional accessory; Part No.
09923183.

The gas supply systems must comply with your local safety regulations. Refer also
to the information given under Gas Requirements on page 52.

What is provided with the spectrometer


• About 10 m of special gas tube, Part No. B0508264.

• A Y-connector with automatic push-fit connectors, Part No. 09920179.


Connecting the Gases 115

• Two screw connectors, R ¼'' for the gas regulator. These are not supplied with
all instrument versions.

To Connect Argon (or Nitrogen) Only


Refer to the figure on page 116 when you connect the furnace gas.

1. Make sure that the argon (or nitrogen) supply is turned off.

2. Use the special tube cutter to cut two, 10 cm lengths of tube from the special
gas tube. The ends of the tubes must be cut squarely.

3. Connect the long gas tube to the argon (or nitrogen) pressure regulator. Use the
R ¼'' screw connector provided or use a connector or adapter suitable for the
gas regulator. Make sure that all the connections are secure.

4. Pass the gas tube to the rear of the spectrometer. Make sure that it cannot be
damaged or strained.

5. Push the two short tubes and the long tube into the connectors on the Y-
connector as shown on the figure on page 116.

6. Push the free ends of the two short gas tubes into the Normal Gas and Special
Gas connectors on the manifold as shown on the figure on page 116.

Push the tubes into the connectors until the tubes butt up to the end of the
connector.

Note To disconnect the gas tube from a connector: Carefully push the black
locking ring of the connector into the connector and pull the tube out of the
connector.
116 Installation

1
2

Figure 4-4. Connecting the Argon (or Nitrogen) only


Item Description
1 Y connector
2 Argon (or Nitrogen) gas line
Connecting the Gases 117

To Connect Both Argon and a Special Gas


Refer to the figure on page page 118 when you connect the furnace gases.

1. Make sure that the gas supplies are turned off.

2. Use the special tube cutter to cut the special gas tube into two pieces for the
two gas supplies. The ends of the tubes must be cut squarely.

3. Connect the gas tubes to the argon (or nitrogen) and special gas pressure
regulators. Use the R ¼'' screw connectors provided or use a connector or
adapter suitable for the gas regulator. Make sure that all the connections are
secure.

4. Pass the gas tubes to the rear of the spectrometer. Make sure that they cannot
be damaged or strained.

5. Push the free ends of the gas supply tubes into the Normal Gas and Special Gas
connectors on the manifold as shown. Push the tubes into the connectors until
the tubes butt up to the end of the connector.

Note To disconnect the gas tube from a connector: Carefully push the black
locking ring of the connector into the connector and pull the tube out of the
connector.
118 Installation

Figure 4-5. Connecting the Argon (or Nitrogen) and a Special Gas
Item Description
1 Argon (or Nitrogen) gas line
2 Special gas line
3 230 V power receptacle
Connecting the Computer and Printer 119

Connecting the Computer and Printer


We recommend placing the computer to the right of the instrument on the
workbench. See the figure on page 120 for connection details.

1. Place the computer on the bench and position the monitor on top of the
computer.

2. Connect the monitor cord to the computer.

3. Connect the Ethernet and furnace camera USB connection from the instrument
to the back of the computer.

4. Connect the mouse and keyboard to the back of the computer.

5. Plug in the computer power cord to an external power source.

6. If a printer is used see the accompanying printer manual for instructions on


connecting the printer to the computer.
120 Installation

12

1
11

7 3
9
10
2

6
5 4

Figure 4-6. Computer connections


Item Description
1 Back of instrument
2 Ethernet instrument connection (from instrument)
3 Furnace camera USB connection (from instrument)
4 Ethernet cable from computer to Internet/Shared Network (optional).
Electrical Connections 121

Item Description
5 Ethernet instrument connection (to computer)
6 Furnace camera USB connection (to computer), view partially obstructed
7 Keyboard and mouse (one connection hidden from view)
8 Monitor connection from monitor to computer
9 Monitor connection to computer
10 Computer main power cord
11 Monitor main power cord
12 Back of monitor

Electrical Connections
Warning: Electrical Hazard
To prevent potential injury to yourself and damage to the instrument,
! switch OFF all instruments in the system and disconnect them from the
line power supply before you perform the procedures described below.
Warning

Warning: Electrical Hazard


The Circuit breaker in the rear panel disconnects the instrument for the
! line power supply.
Warning Never position the equipment so that it is difficult to operate the
circuit breaker on the rear panel.

Read the following instructions very carefully before connecting any cables.
See Chapter 2, Preparing Your Laboratory on page 37 for the specification of the
line power supply.

1. Remove the plastic bag around the main power cord.


2. Confirm that the circuit breaker on the rear panel of the spectrometer is set to
the off position.
122 Installation

3. If there is a circuit breaker on the rear of your instrument , confirm that the
power circuit breaker is in the off position. See the following figure.

Figure 4-7. Power circuit breaker on the PinAAcle 900


Item Description
1 Power circuit breaker in off position
2 Power circuit breaker in on position

This indicates the off position of the main power switch or circuit breaker.
With the switch in this position, the instrument is disconnected entirely
from the line power supply.
Electrical Connections 123

This indicates the on position of the main power switch or circuit breaker.
With the switch in this position, the instrument is connected to the line
power supply but not necessarily switched on and operational.

Note The instrument comes with a Ceekon 32 Amp power connection. A


Hubble connection is available if needed.

4. Please make sure that the computer, and all other accessories that will connect
to the instrument or computer are off. Please refer to the guides of all attached
accessories for procedures on how to use them.

5. Connect the line power cords of the spectrometer and all other accessories to
the main power supply.
124 Installation

Figure 4-8. Main instrument power cord


Item Description
1 Main power cord

6. From the front of the instrument toggle on the on/off green switch.
Electrical Connections 125

Figure 4-9. Instrument on/off switch


Item Description
1 Instrument on/off switch

7. Start up the computer to install the software.


126 Installation

Installing the Cooling System


PerkinElmer offers a recirculating cooling system as an option for the spectrometer
system. This system includes a pressure-sensitive safety switch that switches off
the pump if the internal pressure in the circulatory system increases to above a safe
value.

Caution Risk of damage to the instrument from high water pressure.


High water pressure may cause the coolant tubes on the furnace to burst.
The cooling system includes a pressure-sensitive safety device that opens
a bypass if the pressure becomes too high for any reason. The pressure in
the main laboratory water supply may be too high for safety.
Never connect the spectrometer system directly to the main
laboratory water supply.

For operating conditions see Environmental Requirements on page 37.

Locating the Cooling System


Place the cooling system in a convenient position on the floor underneath the
PinAAcle 900 Series. Do not place the cooling system on the same bench as the
PinAAcle 900 Series since vibrations can adversely influence the analytical
instrument.

Make sure that:

• You can reach the on/off switch at the rear.

• There is space at the rear and sides of the cooling system for air to circulate
freely.

• There is space to remove the stopper and fill the system.

• You can see the water level indicator.


Installing the Cooling System 127

Connecting and Disconnecting the Water Hoses


The inlet and outlet hoses are permanently attached to the cooling system. They
have automatic connectors which are marked with the direction of the water flow.
1. Pass the two hoses from the cooling system to the rear of the spectrometer.
Make sure they are not strained.

Figure 4-10. The cooling system


Item Description Item Description
1 Cooling system 4 Water hose in
2 On/Off switch 5 Water hose out
3 Power cord
128 Installation

2. Push the hose connectors onto the correct fittings on the spectrometer as shown
opposite. The connectors are spring loaded. Push them straight onto the fittings
until they click into place. Lightly tug on the water line connections on the back
of the instrument to ensure that they are secure, and will not pop off.

To disconnect the water hoses:


Note Carefully pull the knurled locking ring back slightly, to release the lock,
and pull the connector off the fitting on the spectrometer.

Figure 4-11. Connecting the cooling system


Item Description
1 Instrument
2 Water hose in
3 Water hose out
Installing the Cooling System 129

See the following procedure Filling the Cooling System on page 129 before you
plug in and start the cooling system.

Filling the Cooling System


The cooling system is self-priming; air in the system is removed automatically as
the cooling system operates. The coolant is a 1:10 solution of glycerol in water (1
part glycerol plus 9 parts water).

The cooling system contains 0.5 L glycerol when it leaves the factory
Note (do not use antifreeze).

Figure 4-12. Water level indicator


Item Description
1 Water level indicator
130 Installation

1. Remove the stopper from the top of the cooling system - twist and pull.

2. Fill the system to the Max mark with sediment-free drinking water - about 4.5
L. Do not use deionized water since this can cause corrosion.

3. Replace the stopper securely.

4. Plug the power patch cord into the receptacle on the back of the Cooling
System. Refer to the figure on page 127.

5. Plug the other end of the power patch cord into 230 V receptacle on the back
of the instrument. Refer to the figure on page 118.

6. Turn the On/Off rocker power switch on the Cooling System down to the On
position.

Connecting the Drain System to the Burner


To connect the drain system to the burner refer to the following procedure and the
following two figures.

Explosion Risk!
! The waste bottle must be placed out in the open, where there is no
possibility of a build-up of potentially hazardous gases.
Warning

It cannot be placed inside a cabinet, or on a shelf with an obstructed


view. The drain bottle must be in full view at all times so it can be seen if
the bottle is full or near full, and the condition of the drain tubing is
readily apparent.
Connecting the Drain System to the Burner 131

Figure 4-13. Instrument without drain tubing attached

1. Carefully take the drain tubing and attach it to the drain fitting.

2. Take the clamp and use a flat bladed screwdriver to secure around the drain
hose fitting.
132 Installation

3 4

Figure 4-14. Drain hose attached


Item Description
1 End cap
2 Clamp
3 Drain hose
4 Drain Interlock
Connecting the Drain System to the Burner 133

Explosion Risk!
! The waste bottle must be placed out in the open, where there is no
possibility of a build-up of potentially hazardous gases.
Warning

It cannot be placed inside a cabinet, or on a shelf with an obstructed


view. The drain bottle must be in full view at all times so it can be seen if
the bottle is full or near full, and the condition of the drain tubing is
readily apparent.

3. Take the other end of the drain hose, where the drain float assembly is located,
and secure it to the drain waste bottle (Carboy 15L).

4. Connect the drain interlock.

5. Before connecting the drain tube to the burner assembly, pour about 250 mL
of water into the free end of the drain tube to fill the drain loop and to activate
the drain float. Both the Air pressure and Drain interlocks will be activated
until the magnetic sensor is engaged. Both interlocks should clear once the
drain float is filled with water.

Note The safety interlock connection goes to the instrument. Until you
precondition the drain tube, a drain and air pressure interlock error
message will appear on the computer. See the following procedure to
satisfy the drain interlock.

Preconditioning A Drain Tube


In order for a new sample introduction system to aspirate and drain smoothly,
the internal surfaces must be preconditioned.

Note You must perform this procedure directly after installation of a new burner
system and you should repeat it if you replace the drain tube or any of the
sample introduction component.
134 Installation

• Aspirate for 5 minutes a 1+1 solution of methanol in water.

Adding Water to the Drain Trap


The drain vessel includes an internal trap to make certain that burner gases cannot
escape into the drain vessel. Enough water must be present in the drain system to
fill the drain loop and to activate the drain float. If not, carry out the following
procedure:
1. Open the compartment door.
2. Remove the clamp around the drain tube or take off the burner head. If the
clamp around the drain tube is taken off, it has to be secured after the water is
added. Otherwise, severe consequences would occur if there is leakage of
flammable acetylene gas during operation, and flash back can occur when
there is a spark.
3. Disconnect the drain tube from end cap.
4. Pour about 250 mL deionized water slowly through the drain tube to fill the
drain trap and activate the drain float.
5. Reattach the drain tube to the end cap.
6. Tighten the clamp around the drain tube. If the clamp around the drain tube is
taken off, it has to be secured after the water is added. Otherwise, severe
consequences would occur if there is leakage of flammable acetylene gas
during operation, and flash back can occur when there is a spark.
7. Reinstall the burner head.
8. Close the compartment door.

Nebulizer Installation
The instrument is shipped with the nebulizer already installed. Depending on the
instrument model ordered, it will be shipped with either a standard stainless steel
or a high sensitivity plastic nebulizer.

For information on removing and reinstalling the stainless steel or high sensitivity
plastic nebulizer see Nebulizer Removal and Reinstallation on page 235.
Installing AS 900 Furnace Autosampler 135

Installing AS 900 Furnace Autosampler

Note The figures shown in this section are of a PinAAcle 900T but the
installation of a AS 900 Furnace Autosampler is the same for the PinAAcle
900H and 900Z.

The AS 900 autosampler can be installed on the PinAAcle 900H, 900T and 900Z.

This autosampler will initially be installed by your PerkinElmer Service engineer


but these instructions are also provided in case you need to alter any of the
connections or move the autosampler in your laboratory.
136 Installation

Tools Needed
• T10 Torx driver

Caution Do not lift the autosampler by the motor, the autosampler arm or any of
the plastic components. This can cause irreparable damage.

The autosampler is packed in a separate box. Carefully unpack the autosampler and
set it up near the instrument.

1. Pull out the autosampler mounting arm from the instrument.


Installing AS 900 Furnace Autosampler 137

Figure 4-15. Autosampler mounting arm


Item Description
1 Front of instrument
2 Autosampler mounting arm
3 Boom receptacle
138 Installation

Note .When attaching the metal boom to the mounting arm make sure not to lose
the metal boom pin because it can easily get loose. The guide pin is a stop
which prevents the arm and boom from moving past the mechanical stop
point on the mounting arm assembly.

2. Attach the metal boom to the mounting arm and make sure that the metal boom
guide pin goes behind the mounting arm.

2 3

Figure 4-16. Autosampler guide pin


Item Description
1 Metal boom
2 Metal boom guide pin
3 Autosampler mounting arm

1. Connect the autosampler connection cable (Part No. B3002201) to the RS 232
connection port underneath the autosampler.
Installing AS 900 Furnace Autosampler 139

2. Feed the other end of the connector through the back of the boom mount
assembly.

Figure 4-17. Attaching the metal boom


Item Description
1-2 Location of 2 screws on the metal boom
3 T10 torx driver
140 Installation

3. Attach the autosampler to the metal boom, and from the underside of the metal
boom, fasten the Auto sampler to the boom with the four T10 Torx screws
located on the bottom of the Autosampler. Refer to the figure of page 139 for
details.

4. Connect the cable to the RS 232 connection port in the front of the instrument.

5. To lock the autosampler in place, tighten the right locking knob first and then
tighten the left locking knob.

4
2 3

Figure 4-18. Location of locking knobs


Item Description
1 AS 900 furnace autosampler in place
2 Left locking knob
3 Right locking knob
4 RS 232 connection port
Installing AS 900 Furnace Autosampler 141

Installing the Drain Tube and the Waste Bottle


The basic waste bottle provided with the instrument is made from polyethylene
(PE). PE is resistant to most rinsing solutions that are commonly used. A PTFE
waste bottle is offered as an option. If you are using an aggressive rinsing solution,
use the PTFE waste bottle.

Note New plastic components may be contaminated with copper as a result of


the production process. We recommend that you rinse all the new
components in dilute nitric acid and then in deionized water before you use
them.

You may have to change the drain tube more often if you use an aggressive rinsing
solution.

You will require:

• a rinse bottle and the cap with a small hole

• the rinse feed assembly, consisting of a flexible PTFE tube with two screw
fittings and a rigid FEP tube complementary screw thread
1. Push one end of the drain tube into the drain nipple on the rinsing port.
2. Slip the rinsing port onto the guides on the left side of the trough for the sample
tray.
142 Installation

1
2

Figure 4-19. AS 900 trough location


Item Description
1 AS 900 furnace autosampler tray in place
2 Trough

3. Slide the waste bottle into the left-hand bracket on the boom.
4. Place the end of the drain tube into the mouth of the waste bottle. If necessary,
shorten the drain tube so that it protrudes only about 30 mm into the waste
bottle. Do not put a cap on the bottle. The drain tube must hang straight down,
without any loops, and the end must never be immersed in the liquid in the
bottle.

Note You may use a 1.2 mL sample cup inserted into the rinse position of the
rinse port. This minimizes the volume of the overflow rinse container.
Installing AS 900 Furnace Autosampler 143

Figure 4-20. Location of rinse port and drain tube


Item Description
1 Rinse port
2 Drain tube
3 AS 900 sample tray

5. Slide the rinse bottle into the right hand bracket on the boom.
144 Installation

6. Connect the other end of the flexible tube to the inlet fitting of the rinse pump.
You may have to shorten the flexible tube,

Figure 4-21. Sample and rinse bottle detail

Installing Sample Tray and Cover


Two sample trays are provided with the autosampler, one tray has 88 locations
while the other tray has 148 locations. Select the type of sample tray you are going
to use in the Instrument tab click on the Devices icon and in the Devices window
select the option Tray size 88 Locations.

To install the sample tray and cover:

1. Grip the hub of the sample tray and lower it onto the drive spindle.

2. Rotate the tray gently until the key on the hub engages into the keyway on the
drive spindle. There is a notch in the outer ring of the sample locations to mark
the position of the key.
Installing AS 900 Furnace Autosampler 145

3. Place the sample tray cover over the hub and line it up so that the lugs on the
sample tray trough engage in the notches in the cover. the ports in the cover are
to the left.

Note Always place the cover on the sample tray to protect the samples from
contamination and to reduce the rate of evaporation of the solvent. You can
reduce the rate of evaporation further by pouring a small volume of water
into the trough; the water level in the trough must always be below the top
of the central ring around the drive spindle.

1 2

Figure 4-22. Location of rinse port and drain tube


Item Description Item Description
1 Notch 2 Hub
146 Installation

Table 4-2. Sample cups and reagent containers

Cup or container 88-location tray 148-location tray


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

• Polypropylene are translucent containers preferred for most solvents


• Polyethylene are translucent low-density containers recommended for use
with most aqueous and organic solutions
• Polystyrene are clear containers recommended for use with most aqueous
solutions
• Teflon® is recommended for use with the most concentrated acids
including HF, and for analysis where the lowest detection levels are
required.

Installing the Sample Capillary


To avoid any damage to the sample capillary during shipment, the sample capillary
will have to be removed from the pipette arm assembly.

To install the sample capillary:

1. Carefully remove any tape used for holding the capillary during transportation.
Installing the Sample Capillary 147

2. Push the metal mount of the sample capillary into the clip at the end of the
pipette arm. Make sure that the sharp side of the metal mount goes first.

3. Pass the sample tube through the hooks on the pipette arm such that it forms a
smooth loop from the metal mount.

4. Pass the sample tube around the hooks on the sample table, leaving a
sufficiently large loop so that the pipette arm can move freely.

Filling and Flushing the Rinsing System


The quality of the rinsing and sample delivery system of the AS 900 autosampler
is most important to achieve good analytical results. Flushing is necessary after all
alterations to the system (e.g. new sample capillary). after changing the sample
capillary flushing the system will remove air from the system. Flush the system
when you complete an analysis in order to prevent future contamination..

1. Make sure that the rinsing system components are correctly installed, are in
good condition, and suitable for the rinsing fluid you will use.

2. Clean the system:


If new components have been installed-
Hold the rise feed tube in a bottle of 50% nitric acid (50% water with 50%
HN03). From the Instrument tab click on the Furnace Control icon. In the
Furnace Control window, click on Flush Sampler. This activates a special
rinse cycle. Repeat this as often as required until all the tubes are completely
filled with the acid mixture. Wait about five minutes. Start 4 more rinse cycles.
Hold the rise feed tube into a bottle of deionized water. In the Furnace Control
window, click on Flush Sampler. This activates a special rinse cycle. Repeat
this as often as required until all the tubes are completely filled with water.
Start four more rinse cycles.
Regular cleaning-
Hold the rise feed tube in a bottle of isopropanol. In the Furnace Control
window, click on Flush Sampler. This activates a special rinse cycle. Repeat
this as often as required until all the tubes are completely filled with
isopropanol. Start four more rinse cycles.

3. Fill the rinse bottle with clean, filtered and degassed rinsing fluid. To reduce
surface tension you may add 0.1% of Triton X-100. If there are particles in the
rinsing fluid they can clog the valves, causing leaks and non-reproducible
results.
148 Installation

4. Flush the system:


From the Instrument tab click on the Furnace Control icon. In the Furnace
Control window, click on Flush Sampler. This activates a special rinse cycle.
Repeat this as often as required until all the tubes are completely filled with
rinsing fluid (and the isopropanol completely flushed out).

Note Make certain there are no air bubbles in the rinsing system. Air bubbles
lead to non-reproducible results.

Note If you want to use a different rinsing fluid to that already in the rinsing
system, rinse all traces of the previous fluid out of the rinsing system. Use
a rinsing fluid that is miscible with both the new and the old rinsing fluids.
You may have to use intermediate rinsing fluids. For example, if you are
changing from an acidic fluid to an organic solvent, you could use:
1. Deionized water.
2. Ethanol or another water-miscible solvent.
3. An organic solvent.

To Align the Autosampler Tip in the Graphite Tube

Caution Risk of damage to the autosampler.


Check that the flame door is fully opened.
Before running the furnace, make sure that the flame door is in the fully open
position. Otherwise, the door may interfere with the movement of the furnace
autosampler arm, potentially damaging the autosampler probe.

Unless you are absolutely sure that the pipette tip is already well aligned, always
perform the Align Autosampler Tip in the graphite tube command from the Align
Autosampler Tip wizard. You use this command to make sure that the tip will not
strike the sides or the inside of the tube.
Installing the Sample Capillary 149

Caution Risk of damage to the autosampler.


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

Refer to Figure 4-23 for the alignment controls.

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


• From the Instrument tab click on the Furnace Control icon. In the
Furnace Control window, click on Align Tip.
The Align Autosampler Tip Wizard appears.
150 Installation

• From the Align Autosampler Tip wizard select Align the autosampler
tip in the graphite tube. The autosampler arm is unlocked and the pipette
tip moves to a position directly above the graphite tube.
Installing the Sample Capillary 151

2. Using the depth control wheel, very carefully lower the pipette tip to just
above the graphite contact.
Do not allow the pipette tip to touch any part of the furnace.
3. Continue lowering the tip and adjusting the left/right and forward/backward
controls on the autosampler until the pipette tip is positioned just inside the
dosing hole of the graphite tube.
152 Installation

Figure 4-23. Alignment controls on the autosampler


Item Description
1 Depth control wheel
2 Left/right alignment control
3 Forward/backward alignment control
Installing the Sample Capillary 153

Warning: UV Radiation – Risk of Eye Damage


! The lamps may emit UV radiation which can damage your eyes.
Always wear UV-absorbing safety glasses when aligning the
Warning autosampler.

4. Use the TubeView window that is currently open on the workspace to see the
tip in the tube.
5. Use the Depth Knob to set the depth of the autosampler tip in the tube so that
it is 1-2 mm above the platform; view the alignment within the TubeView
window. Only adjust in the down direction. If you adjust too low, click on the
< Back button and try again. Do not lower the pipette tip so far that it could
strike the platform. Frequent striking the platform may break it off from the
tube.
Refer to the following figure for an example of a well aligned tip.

Figure 4-24. Alignment tip in the TubeView camera


Item Description
1 Tip
154 Installation

6. When you are done click Finish to save the position.


Reopen the Align Autosampler Tip Wizard and select the option: Check
autosampler tip alignment in the graphite tube to make any fine
adjustments.

To check and make fine-adjustments to the penetration depth of the


pipette tip in the graphite tube

The steps described in this section describe how to make sure the tip is properly
aligned in the tube. If it is not properly aligned, click < Back and select Check
autosampler tip alignment tip in the graphite tube.

Warning: UV Radiation – Risk of Eye Damage


! The lamps may emit UV radiation which can damage your eyes.
Always wear UV-absorbing safety glasses when aligning the
Warning autosampler.

Caution
Risk of damage to the pipette tip
The pipette tip enters the graphite tube when you issue the In Tube command.
The pipette tip can strike the edge of the injection hole if the autosampler arm
has not been aligned.
Make sure that the autosampler arm has been aligned before you issue the In
Tube command.
Installing the Sample Capillary 155

Before you perform the steps outlined in this procedure, make sure you have
aligned the autosampler arm as described in To align the autosampler tip in the
graphite tube.

1. From the Furnace Control window select Align Tip > Check autosampler tip
alignment in the graphite tube.
The autosampler arm is unlocked and the pipette tip enters the graphite tube.
Make sure that the tip is centered in the hole in the tube. Do not allow the tip
to touch any part of the furnace.

2. Using the TubeView window that is currently open make sure that the tip is
1-2 mm above the platform. If not, click on< Back and try again to adjust its
position.
156 Installation

Figure 4-25. Penetration depth of pipette tip in the graphite tube, as viewed from
the Furnace Camera Window on the screen.

3. If you make any additional adjustments in the depth (down only), click on
Finish to save the revised position for use in performing analyses.

4. If the position is not correct, click < Back and perform the Align Tip procedure
again.

To check the depth of the autosampler tip in the sampling cup


The steps described in this section describe how to check that the autosampler tip
depth is properly set.

1. Make a preliminary adjustment as described in the section titled To set the


depth of the autosampler tip in the sampling cup.

2. Put a sample cup in location 1 of the sample tray.

3. From the Furnace Control window click Align Tip.


The Align Autosampler Tip wizard appears.

4. Select Check depth of autosampler tip in the sampling cup.

5. Adjust the depth control wheel so that the pipette tip is at the depth where you
want it to withdraw samples.

6. If you make any additional adjustments to the depth, click on Finish to save
the revised depth for use when performing analyses.
Installing the Sample Capillary 157

Checking the solution droplet delivery


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

Warning: UV Radiation – Risk of Eye Damage


! The lamps may emit UV radiation which can damage your eyes.
Always wear UV-absorbing safety glasses when aligning the
Warning autosampler.

1. Create a furnace program comprising drying, pyrolysis, atomization, and


clean-out.
Enter the total volume of solution that you will use in the subsequent analyses.
Refer to the help by selecting F1 on the computer keyboard on how to create a
method.

2. Place a sample cup containing blank solution in location 1 in the autosampler.


Use an identical blank solution to the one that you will use for the subsequent
analyses.

3. In the Analysis window, on the automated page, in the Locations column,


enter the autosampler location of the blank solution.

4. Start the method:


In the Analysis window, on the automated page, click on the Analyze All
button. The Analysis Warning screen will appear click on OK.

5. Look in the TubeView camera window and watch the delivery of the solution
droplet onto the platform.

6. If the solution droplet delivery was unsatisfactory, make the appropriate small
adjustments to the penetration depth of the pipette tip. See To check and make
fine-adjustments to the penetration depth of the pipette tip in the graphite tube
on page 154.

7. Repeat step 4 through step 6 to dispense further aliquots of blank solution until
you are satisfied with the delivery.
158 Installation

Note If the pipette tip is too far above the platform and the droplet does not
contact the graphite surface, the liquid may remain in the tip, leading to
pipetting errors.
If the pipette tip is too close to the platform, the liquid may hang up on the
tip, leading to pipetting errors.

8. The pipette tip is at the correct height when the solution droplet contacts the
graphite surface just before leaving the tip.
Installing the Sample Capillary 159

Figure 4-26. Checking the solution droplet delivery, as viewed from the Furnace
Camera Window on the screen
Item Description
1 Wrong: Tip too far above the platform
2 Wrong: Tip too near the platform
3 Correct
160 Installation

Installing S10 Autosampler


The S10 autosampler can be installed on the PinAAcle 900H, 900T and 900F. For
complete installation instruction see the S10 Autosampler User's Guide (Part No.
09936788).

Lamps
The spectrometer has an eight position motor controlled lamp selector, and is
designed to hold eight PerkinElmer Lumina hollow cathode lamps (HCLs) or two
electrodeless discharge lamps (EDLs) and six PerkinElmer Lumina hollow cathode
lamps (HCLs). This spectrometer also comes with a background corrector
deuterium lamp (D2). The deuterium arc lamp has a finite life and it is a
consumable part.
For information on adding or replacing see Replacing the Lamps on page 285.

Replacement Parts
Every day you count on PerkinElmer to provide you with solutions that deliver
reliable performance, control operating costs and maximize operational time. Our
complete portfolio of consumables, parts, supplies, training and service helps you
meet both routine and demanding measurement challenges. We invest heavily in
testing and validating our products to ensure you receive guaranteed compatibility
and performance-on-time, every time, for every instrument in your laboratory.
Supplies, replacement parts, and accessories can be ordered directly from
PerkinElmer, using the part numbers quoted in the guides provided with the
instrument.
See our website:
http://perkinelmer.com
PerkinElmer's catalog service offers a full selection of high-quality supplies.
To place an order for supplies and many replacement parts, request a free catalog,
or ask for information:
If you are located within the U.S., call toll free 1-800-762-4002, 8 a.m. to
8 p.m. EST. Your order will be shipped promptly, usually within 24 hours.
If you are located outside of the U.S., call your local PerkinElmer sales or service
office.
Shipping List for the PinAAcle 900F 161

Shipping List for the PinAAcle 900F

Table 1: Shipping Kit Part No. N3160990


Part No. Description Quantity
N3160182 Stainless Steel Flame Burner Assembly 1
or Nebulizer

N3160179 High Sensitivity Plastic Nebulizer Flame 1


Burner Assembly

N3160920 Burner Door Assembly 1

N3161120 Sample Tray 1

N3160941 Accessories Kit 1

Table 2: Accessories Kit Part No. N3160941

Part No. Description Quantity


09904991 Wide Mouth 15L Natural Bottle 1

N0400058 Drain Assembly Louie Burner 1

03031573 N2O Burner Head Cleaner 1

09902219 Viton Burner Head O-Ring Kit 1


B0147498 Insert For Plastic Hose 2
B0190413 Organic Solvent Agent Card 1
N3161240 Burner Head Handle 1
B0501696 Air and Vent Filter (Felt) 1
09903004 Hose Clamp 7/32-5/8 SST 1
162 Installation

Shipping List for the PinAAcle 900H


Table 3: Shipping Carton Part No. N3160992
Part No. Description Quantity
N3160182 Stainless Steel Flame Burner Assembly 1
or Nebulizer

N3160179 High Sensitivity Plastic Nebulizer Flame 1


Burner Assembly

N3160920 Burner Door Assembly 1

N3161120 Sample Tray 1

N3160942 Accessories Kit 1

09904991 Wide Mouth 15L Natural Bottle 1

N0400058 Drain Assembly Louie Burner 1

B0198072 Cooling System 4100 1

N3160090 AS 900 Tested 1

N3160283 AS900 HGA Carrier 1

Table 4: Accessories Kit Part No. N3160942


Part No. Description Quantity
03031573 N2O Burner Head Cleaner 1

09902219 Viton Burner Head O-Ring Kit 1


B0147498 Insert For Plastic Hose 2
B0190413 Organic Solvent Agent Card 1
N3161240 Burner Head Handle 1
Shipping List for the PinAAcle 900H 163

B0501696 Air and Vent Filter (Felt) 1


09903004 Hose Clamp 7/32-5/8 SST 1

09290587 Cable - USB Extension 1.8 Meters 1

09920179 Fitting- Push-In Metric "Y" 6 OD TBG 1


BRS

09920583 Nut- Metric- HEX 6MM TBG OD BRS 2

09923472 Ferrule- Metric- Back 6MM BRS 2

09923473 Ferrule- Metric- Front 6MM BRS 2

B0080112 Tube Adjustment Aid 1

B0080259 Mirror-Instrument (Plastic) 1

B0114851 O-Ring 47.29 ID X 2.62 CS VITON 1


DURO 7

B0128495 CC-Graphite Pieces Packaged 1

B0156272 Hose 0-58 X 0-19 1

B0505368 Cleaning Tips PK/10 1

B0508264 FLEXO-55 Tube 6X4 10

B3001262 Graphite Tube With Platform 1

B3121301 Contact Changing Tool 1


164 Installation

Shipping List for the PinAAcle 900T

Table 5: Shipping Kit Part No. N3160993


Part No. Description Quantity
N3160090 AS 900 Assembly 1

N3160923 AS 900 Carrier 1

N3160182 Stainless Steel Flame Burner Assembly 1


or Nebulizer

N3160179 High Sensitivity Plastic Nebulizer Flame 1


Burner Assembly

B0198072 Cooling System 1

N3160920 Burner Door Assembly 1

N3161120 Sample Tray 1

N3160913 Accessories Kit 1


Shipping List for the PinAAcle 900T 165

Table 6: Accessories Kit (Part No. N3160913)


Part No. Description Quantity
N0400058 Drain Assembly Louie Burner 1

09904991 Wide Mouth 15L Natural Bottle 1

09290587 USB Extension Cable 1

03031573 N2O Burner Head Cleaner 1

09210225 T-Handle HEX Screwdriver 6.0 X 200 1

09210335 T-Handle HEX Screwdriver 5.0 X 200 1

B0508264 FLEXO-55 Tube 6X4 10

09290602 USB LED Light Source 1

09902219 Viton Burner Head O-Ring Kit 1

09907925 Cuvette-Wood 8 MM Clamp 1

09920179 Push-In Fitting Metric "Y" 6 OD Tubing 1


Brass

09920583 HEX Nut Metric 6MM TBG OD Brass 2

09923472 Ferrule - Metric- Back 6MM Brass 2

09923473 Ferrule - Metric- Front 6MM Brass 2

09935220 Recommended Conditions for THGA 1


Furnaces

B0147498 Insert For Plastic Hose 2

B0190413 Organic Solvent Agent Card 1


166 Installation

B0500748 O-Ring 16 X 1.75 VITON 1

B0500999 Safety Information Zeeman-AAS 1

B0504035 1 Piece Contact IP-Long/Short Set 1

B0505339 Cord Nut Key 1

B0505368 Cleaning Tips 1 Package


of 10

B0851900 ZL Furnace Mirror 1

B0856585 TORX Screwdriver T20X100 1

B3000641 THGA Graphite Tubes Standard 5 Pack

N9307832 THGA Advanced Platform Graphite Pack of 5


Tubes with End Caps

B3120410 Press-In Gage THGA 1

B3120416 Press-In Sleeve 1

B3120420 Press-Out Tool 1

N3161240 Burner Head Handle 1

09903004 Hose Clamp 7/32-5/8 Stainless Steel 1

B0501696 Air and Vent Filter (Felt) 1

09903004 Hose Clamp 7/32-5/8 SST 1

B0859760 T-Handle HEX Screwdriver 5.0 X 200


Shipping List for the PinAAcle 900Z 167

Shipping List for the PinAAcle 900Z


Table 7: Shipping Kit Part No. N3160991
Part No. Description Quantity
N3160090 AS 900 Assembly 1

N3160923 AS 900 Carrier 1

B0198072 Cooling System 1

N3160940 Accessories Kit 1

Table 8: Accessories Kit (Part No. N3160940)


Part No. Description Quantity
09210225 T-Handle HEX Screwdriver 6.0 X 200 1

09210335 T-Handle HEX Screwdriver 5.0 X 200 1

B0508264 FLEXO-55 Tube 6X4 10

09290602 USB LED Light Source 1

09907925 Cuvette- Wood 8 MM Clamp 1

09920179 Push-In Fitting Metric "Y" 6 OD Tubing 1


Brass

09920583 HEX Nut Metric 6 MM Tubing OD Brass 2

09923472 Ferrule-Metric- Back 6 MM Brass 2

09923473 Ferrule-Metric- Front 6 MM Brass 2

09935220 Recommended Conditions for THGA 1


Furnaces
168 Installation

B0500999 Zeeman Safety Information - AAS 1

B0504035 1 Piece Contact IP-Long/Short Set 1

B0505339 Cord Nut Key 1

B0505368 Cleaning Tips 1 Package


of 10

B0851900 ZL Furnace Mirror 1

B0856585 TORX Screwdriver T20X100 1

B3000641 THGA Graphite Tubes Standard 5 Pack

N9307832 THGA Advanced Platform Graphite Pack of 5


Tubes with End Caps

B3120410 Press-In Gage THGA 1

B3120416 Press-In Sleeve 1

B3120420 Press-Out Tool 1

B0501696 Air and Vent Filter (Felt) 1

09290587 USB Extension Cable 1

N0400058 Drain Assembly Louie Burner 1

09904991 Wide Mouth 15L Natural Bottle 1


Preparing the System 5
Switching on the System
1. Read the safety information at the front of this guide before you operate the
system.

2. Make sure that the spectrometer system and other ancillary instruments are
correctly installed and connected to their power supplies. Make sure that the
coolant hoses are connected correctly to the spectrometer. Where applicable,
make sure that the cooling system is filled to the Max mark (see Filling the
Cooling System on page 129).

3. Switch on the fume ventilation system for the work area.

4. Turn on the burner gases and adjust the outlet gauge pressures to the
recommended values. See Table 5-1 Required Pressures for the Burner Gases
on page 171.

5. Turn on the inert (and special) gas for the furnace and adjust the outlet gauge
pressures to the recommended values. See Table 5-2 Required Pressures for
the Furnace Gases on page 172 .

Note You must always turn on the air supply since air pressure is required for
the internal pneumatic system. If you intend to work with only one
atomizer, you only need to additionally turn on the gas supplies for that
atomizer.
170 Preparing the System

6. Turn on the cooling water to the system: Switch on the circulatory cooling
system by pressing the power switch located on the rear panel.

7. You can leave this switch permanently in the on position since power is
supplied by the spectrometer. Switch the circuit breaker on the rear panel of the
spectrometer to the on position (marked I).

You can leave this switch permanently in the on position during routine
operation; you switch the spectrometer system on and off via the operational
on/off switch located on the front panel.

8. Switch on the computer. If your computer has a power management system,


switch this off.

9. Switch on the spectrometer system with the operational on/off switch located
on the front panel.

10. If you need the diluter, autosampler, or flow injection system, switch on the
respective systems.

11. If you have changed the configuration of the system, such as installed a
different autosampler or added or removed any accessories, use the
Reconfigure utility to reconfigure the software (see the help by selecting F1 on
the computer keyboard).

12. Start the software.

13. Set up the various parts of the system:

• Install any further lamps that you require for the analyses. See Installing
the Lamps on page 172.

• Set up the burner system. See Setting up the System for Analyses Using the
Flame Technique on page 180.

• Set up the graphite furnace system. See Setting up the System for Analyses
Using the Furnace Technique For the PinAAcle 900 T/Z on page 186.

Procedures for shutting down the system are described see Shutting Down the
System on page 196.
Switching on the System 171

In an emergency, you can shut down the system as described in Emergency


Shutdown on page 197

Table 5-1. Required Pressures for the Burner Gases

• Set the outlet gauge pressure for each gas to a value just below the
maximum value (see Pmax column).

• Always set the same outlet gauge pressure for air and nitrous oxide.

• Never set the outlet gauge pressure to a value exceeding the maximum
pressure (see Pmax column).

• Always turn on the air supply since air pressure is required for the
spectrometer's pneumatic system.

Warning: Acetylene - Explosion Hazard


Acetylene can decompose explosively at pressures higher than 103 kPa/
! 1.03 bar/15 psig.
Always make sure that the acetylene outlet gauge pressure is below this
Warning value.

Warning: Flashback Hazard


Never set up the nebulizer using a nitrous oxide-acetylene flame.
! • Set up the nebulizer using an air-acetylene flame only, and make small
adjustments slowly.
Warning
172 Preparing the System

Table 5-2. Required Pressures for the Furnace Gases

• Set the outlet gauge pressure for each gas to a value just below the
maximum value (see Pmax column).

• Never set the outlet gauge pressure to a value exceeding the maximum
pressure (see Pmax column).

Warning: Toxic Gases


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

Installing the Lamps


The spectrometer has an eight position motor controlled lamp selector, and is
designed to hold eight PerkinElmer Lumina hollow cathode lamps (HCLs) or two
electrodeless discharge lamps (EDLs) and six PerkinElmer Lumina hollow cathode
lamps (HCLs). With the exception of the PinAAcle 900Z model, the spectrometer
also comes with a background corrector deuterium lamp (D2).

For information on lamp maintenance and cleaning see Nebulizer Removal and
Reinstallation on page 235.
Installing the Lamps 173

Lamp Compartment
The lamp compartment is located behind the door on the right-hand side at the front
of the spectrometer.

Figure 5-1. Lamp compartment


Item Description
1 Right side of instrument
2 Cu lamp installed (lamp door open)
174 Preparing the System

Installing and Connecting HCLs


You can use both single-element and multi-element hollow cathode lamps.

Note Single element lamps are recommended for furnace.

1. Open the lamp door.


2. Slide the Lumina lamp into the lamp holder and make sure that the integrated
4-pin socket fully slides over the receptacle on the lamp holder for proper
connection.
3. Close the lamp door.

Electrodeless Discharge Lamps (EDL)


While hollow cathode lamps are an ideal source for determining most elements by
atomic absorption, for volatile elements, an electrodeless discharge lamp (EDL) is
recommended instead. EDLs provide greater light output for improved detection
limits and precision, along with increased sensitivity and working curve linearity.
EDLs also have a longer life than corresponding hollow cathode lamps. For certain
elements (such as arsenic and selenium), EDLs will also provide improved
sensitivity.

An EDL consists of a quartz bulb under an inert gas atmosphere, containing the
element or a salt of the element for which the lamp is to be used. When an RF field
is applied to the bulb, the inert gas is ionized and the coupled energy excites the
vaporized analyte atoms inside the bulb, causing them to emit their characteristic
spectrum. The emission spectra produced is typically much more intense than that
from hollow cathode lamps, frequently tenfold larger or more.

Installing and Connecting EDLs


If necessary, assemble the lamp by sliding the lamp driver into the lamp sleeve for
the required element. Depress the locking pin as the sleeve slides into place and
make sure that the locking pin extends through the locating hole in the sleeve.

EDL
1. Open the lamp door.
Installing the Lamps 175

2. Insert the coding plug over the receptacle on the lamp holder.
3. Slide the lamp carefully into the lamp holder. Do not push in until the
mechanical stop since this will push in the lamp too far to function properly.
Do not cover the venting slots of the lamp driver or overheating, drift and/or
event shutoff will occur. See the following figure for the proper lamp postion.

Figure 5-2. EDL lamp


Item Description
1 EDL 1 cable connection
2 EDL Lamp in position (lamp door open)
3 Venting slots
176 Preparing the System

4. Connect the lamp cable to an EDL cable connection (see the previous figure)
to the EDL driver power supply connection. From the Instrument tab click
on the Lamp Setup icon. Use the Lamp Setup window in software to
automatically align the lamp.

Note EDLs may only be installed in positions 1 and 2 of the lamp housing.
Refer to the figure on page 173 for the assigned lamp numbers on the turret
(mount). For example, if the EDL lamp is installed in position 1 of the
turret, connect the EDL cable to the EDL 1 cable connection on the EDL
driver power supply connection.

Removing lamps
Do not unplug and remove lamps while they are switched on.

1. From the Instrument tab click on the Lamp Setup icon. The Lamp Setup
window appears.

2. Make sure that the lamps you want to remove are switched off: The On buttons
must not be green. If necessary, click on the respective On buttons.

3. Close the Lamp Setup window.

4. Unplug and remove the lamps. For EDLs, remove the coding plugs as well.

Tips for installing lamps

Danger HOT LAMP


! Make sure that the lamp is completely cooled down when you remove
Na, Li and K lamps, since the cathode will be in the molten form when it
Warning is in use and will be very hot and could cause a burn.

• We recommend the use of PerkinElmer lamps. You can use both hollow
cathode and electrodeless discharge lamps.
Installing Sample Trays 177

• Do not touch the front window of the lamp; perspiration or other


contamination can reduce the intensity of the radiation.

• If you install more than one lamp containing a particular element, for example,
a single-element copper lamp and a multi-element lamp containing copper, the
system will use the lamp in the holder with the lower number when you
perform determinations of that element. Make sure that you place the preferred
lamp in the holder with the lower number.

• With EDLs, connect each lamp plug to the socket that has the same number as
the holder of the lamp.

• With EDLs, make sure that you use the correct coding plug and connect it to
the receptacle on the lamp holder containing the EDL.

• If you use the wrong coding plug or connect the coding plug to the wrong
receptacle, you will cause the spectrometer to malfunction and may cause
irreparable damage to the lamp.

Installing Sample Trays


The sample tray can be inserted at the front of the instrument. You cannot install
the tray if the furnace autosampler is installed. If the furnace autosampler is
swiveled to the standby position you can then install a sample tray. There are two
positions for the flame sample tray, one at the top position, which is the normal
position, and another at the lower position.

1. Take the sample tray, place the drain hose in the notched area of the tray.

2. Slide the tray into place on the tray supports.


178 Preparing the System

Figure 5-3. Sliding sample tray into place


Item Description
1 Sample tray
2 Tray supports
3 Drain hose
Installing Sample Trays 179

3. Secure the sample tray in place. Make sure that the instrument is not pushed so
far back on the bench that the drain tube bends when the tray is installed.

Figure 5-4. Sample tray in place


Item Description
1 Drain hose
2 Sample tray
180 Preparing the System

To remove the tray


Gently lift the tray at the front and then pull it back to slide it out of the guides.

Setting up the System for Analyses Using the Flame Technique

Summary of the procedure


1. Switch on the system (see Switching on the System on page 169).

2. If you need to change techniques from furnace technique to the flame


technique, you need to run the Reconfigure utility. Click on Start > All
Programs > PerkinElmer Syngistix for AA > Reconfigure.

3. Create or open a method (see the help by selecting F1 on the computer


keyboard).

4. If you intend to make emission measurements, in the Method Editor on the


Spectrometer tab, for Signal Type, select Emission.

5. If you intent to make absorption measurements, install the lamps that you
require (see Installing the Lamps on page 172).

6. Set up the burner system (see Setting Up the Burner System on page 180)

7. Perform the safety checks (see Safety Checks for the Flame Technique on page
181).

8. Ignite the flame (see Igniting the Flame on page 182)

You should now set up the nebulizer, then optimize the burner and nebulizer before
checking the sensitivity. Refer to the help by selecting F1 on the computer
keyboard.

Setting Up the Burner System


Summary of the procedure

1. Make sure that the correct nebulizer is installed – the stainless steel nebulizer
or a high sensitivity plastic nebulizer (see Nebulizer Installation on page 134).
Setting up the System for Analyses Using the Flame Technique 181

2. Perform the safety checks (see Safety Checks for the Flame Technique on page
181).

3. Ignite the flame (see Igniting the Flame on page 182).

For the correct procedure to extinguish the flame see Extinguishing the Flame on
page 184.

Safety Checks for the Flame Technique


Before igniting the flame, always make sure that:

• The fume ventilation system for the laboratory is switched on.

• The burner head is correctly installed and the end cap is secured.

• The correct nebulizer is fitted and that it is correctly secured.

• The fuel and oxidant hoses are correctly fitted to the (back of the) instrument.

• The drain system is installed and operating correctly.

• The compartment door is in the closed position.

• All safety interlocks are correctly closed.

Explosion Risk!
! The waste bottle must be placed out in the open, where there is no
possibility of a build-up of potentially hazardous gases.
Warning

It cannot be placed inside a cabinet, or on a shelf with an obstructed


view. The drain bottle must be in full view at all times so it can be seen if
the bottle is full or near full, and the condition of the drain tubing is
readily apparent.

If software indicates an interlock error, one or more of the following may be the
cause:
182 Preparing the System

• The burner head, the nebulizer, or the drain system is not correctly
installed.

• The acetylene or oxidant pressure is too low.

• The liquid level in the drain trap is too low or there is no liquid in the drain
trap.

• The liquid level in the drain vessel is too high.

Igniting the Flame

Explosion Risk!
! The waste bottle must be placed out in the open, where there is no
possibility of a build-up of potentially hazardous gases.
Warning

It cannot be placed inside a cabinet, or on a shelf with an obstructed


view. The drain bottle must be in full view at all times so it can be seen if
the bottle is full or near full, and the condition of the drain tubing is
readily apparent.

Warning: Flammable Gases – Fire and Explosion Hazard


! Before you ignite the flame, set up your spectrometer and burner correctly
and observe all the safety precautions described in Safety Checks for the
Warning Flame Technique on page 181.

Note In an emergency, switch off the spectrometer using the operational on/off
switch on the front panel.
The flame is automatically extinguished and the gases shut down in a safe
sequence. See Emergency Shutdown on page 197 for the procedure to
follow after an emergency shutdown.
Setting up the System for Analyses Using the Flame Technique 183

To ignite the flame:

1. Switch on and set up the spectrometer system (see Setting up the System for
Analyses Using the Flame Technique on page 180).

2. Perform the safety checks (see Safety Checks for the Flame Technique on page
181).

3. Adjust the outlet gauge pressures of the burner gases to the recommended
values (see Table 5-1 on Required Pressures for the Burner Gases on page
171).

4. On the Instrument tab, click on Flame icon. The Flame Control window
appears.

5. Select the oxidant: In the Flame Control window, click on Air or N2O.

6. Ignite the flame: In the Flame Control window, click on Flame On/Off icon.

Warning: UV Radiation – Risk of Eye Damage


! The flame, especially the nitrous oxide-acetylene flame, may emit UV
radiation which can damage your eyes.
Warning • Keep the door closed when the flame is burning, unless you need to
adjust the burner as described in the user documentation.
• Always wear UV-absorbing safety glasses when looking at the flame.

Select an air-acetylene flame:


• – If you are setting up the burner system.

• – If you have installed a different nebulizer, cleaned the nebulizer, or if the


settings on the nebulizer have been altered since it was last used.

• – If you are using the flame to heat the quartz-cell.


184 Preparing the System

Warning: Acetylene - Explosion Hazard


Acetylene can decompose explosively at pressures higher than 103 kPa/
! 1.03 bar/15 psig.
Always make sure that the acetylene outlet gauge pressure is below this
Warning value.

Warning: Flashback Hazard


Never set up the nebulizer using a nitrous oxide-acetylene flame.
! • Set up the nebulizer using an air-acetylene flame only, and make small
adjustments slowly.
Warning

For the correct procedure to extinguish the flame see Extinguishing the Flame on
page 184.

Extinguishing the Flame


Before you extinguish the flame or begin maintenance or disassembly procedures,
you must rinse the burner system. After you extinguish the flame, allow the burner
head to cool.

To rinse the system:

The procedure for rinsing the burner system depends on the type of samples that
you have analyzed.

Recommendations:

• If the sample solutions contained organic solvents, use a multi-rinse procedure


to remove all traces of the solvents from the system.

• If the sample solutions contained toxic substances, you must rinse all traces of
these substances out of the system.

• If the sample solutions contained high concentrations of copper, silver or


mercury salts, which can form unstable acetylides, you must rinse all traces of
these substances out of the system.
Setting up the System for Analyses Using the Flame Technique 185

Procedure:

• If you used only aqueous solutions during the analyses:

1. Aspirate deionized water for five minutes.

• If you used organic solvents during the analyses:

2. Aspirate for five minutes an organic solvent that is miscible with the samples
that have just been aspirated.

3. Aspirate for five minutes methanol or another solvent that is miscible both with
water and the solvent used previously.

4. Aspirate 1% (v/v) nitric acid solution for five minutes.

5. Aspirate deionized water for five minutes.

To extinguish the flame:


1. With the flame still burning, aspirate the correct rinsing solutions to rinse the
burner system. Either aspirate the solutions manually or use the flame
autosampler.
2. In the Flame Control window, click on the Flame icon.
3. Select the Off side of the Flame On/Off switch. The indicator in the switch
goes off.

The system uses a predetermined shutdown sequence to extinguish the flame


safely.
4. Shut down the gases to the spectrometer at source.
5. Touch the Bleed Gases button to depressurize the gas lines.
186 Preparing the System

Setting up the System for Analyses Using the Furnace Technique


For the PinAAcle 900 T/Z

Locking the Furnace Cover in Place


The furnace cover is shipped in place and protect the furnace head from accidental
spillage from the flame analysis operation. This cover must remain in place when
running flame analysis. When running furnace analysis tilt up the furnace cover
and lock it into place.

Figure 5-5. Furnace covers in place (for the PinAAcle 900T and 900Z)
Item Description
1 Furnace cover down in flame position
2 Furnace stage cover (remains in place and is not removed)
Setting up the System for Analyses Using the Furnace Technique For the 187

1. For the PinAAcle 900T, with one hand on each side of the furnace cover, tilt
the cover up and back.

2. Gently snap the cover into place. It is now secured for furnace analysis.

Note The furnace cover must be locked in the up position when running furnace
analysis. The cover should remain in place down while running the flame
analysis to protect the furnace from corrosion and contamination from
accidental acid and sample spills.

Caution Check that the flame door is fully opened.

Before running the furnace, make sure that the flame door is in the fully
open position. Otherwise, the door may interfere with the movement of the
furnace auotsampler arm, potentially damaging the autosampler probe. .
188 Preparing the System

Figure 5-6. Furnace cover in the locked furnace analysis position


Item Description
1 Furnace cover in locked up position for furnace analysis

Setting up the Analysis


1. Switch on the system (see Switching on the System on page 169).

2. If you need to change techniques from furnace technique to the furmace


technique, you need to run the Reconfigure utility. Click on Start > All
Programs > PerkinElmer Syngistix for AA > Reconfigure.
Setting up the System for Analyses Using the Furnace Technique For the 189

3. Carefully swivel the AS 900 autosampler in front of the graphite furnace and
secure it with the large securing knobs.
4. Create or open a method (see the help by selecting F1 on the computer
keyboard).
5. Install the lamps that you require (see the procedure, Installing the Lamps on
page 172).
6. If required, install or change and condition a graphite tube (see Changing the
Contact Cylinders on page 305 and Conditioning the Graphite Tube on page
326).
7. Set up the furnace autosampler. Refer to the help by selecting F1 on the
computer keyboard.
You should now optimize the analytical conditions. Refer to the help by selecting
F1 on the computer keyboard.

Setting up the System for Analyses Using the Furnace Technique


For the PinAAcle 900 H

To use the furnace


1. If the flame is burning, extinguish it, shut down the gases, and bleed the gas
supply lines (see "Extinguishing the flame" in the help by selecting F1 on the
computer keyboard).
2. Remove the burner assembly from the spectrometer (see Removing the Burner
Head on page 224).
3. Lift the furnace cover up.

Caution Check that the flame door is fully opened.

Before running the furnace, make sure that the flame door is in the fully
open position. Otherwise, the door may interfere with the movement of the
furnace auotsampler arm, potentially damaging the autosampler probe. .
190 Preparing the System

Figure 5-7. Removing the burner assembly


Item Description
1 Remove the burner assembly
2 Lift up this furnace cover
3 Burner assembly removed and furnace cover up
Setting up the System for Analyses Using the Furnace Technique For the 191

4. Move into place the autosampler. Lock the autosampler in position with the
knobs.

Warning: High Temperatures – Risk of Burns


The graphite furnace can generate very high temperatures. Do not touch
! any parts of the furnace, especially the graphite components, until they
have cooled to room temperature.
Warning

Warning: High Temperatures UV Radiation – Risk of Burns and Eye


! Damage
Warning The graphite furnace can generate very high temperatures, and can emit
UV radiation which can damage your eyes, when it is heated to
incandescence.
The furnace is exposed when it is in the standby position, thus increasing
these risks..
Never heat the furnace when it is in the standby position. Always
move it into the atomizer compartment before you heat it.

Aligning the Graphite Furnace


The graphite furnace must be correctly aligned in the radiation beam. Once you
have aligned the furnace, it remains aligned during routine operation. Nevertheless,
always check alignment of the furnace:

• If you change from a graphite tube without an integrated platform to a


graphite tube with an integrated platform, check the alignment.

Refer to following figure for the alignment controls.


192 Preparing the System

2
3

Figure 5-8. Alignment controls on the furnace


Item Description
1 Vertical (up-down) alignment control
2 Horizontal (forward-backward) alignment control
3 Locking lever (locks horizontal movement of the furnace)
4 Move lever left to unlock
5 Move lever right to lock

1. Check that a lamp for the element you intend to determine is installed in the
spectrometer and aligned.

2. Where applicable, switch off the deuterium lamp background corrector.


Setting up the System for Analyses Using the Furnace Technique For the 193

3. Check that the graphite tube you intend to use for your analyses is installed in
the furnace.

4. Remove both window assemblies from the furnace (see Checking and
Cleaning the Furnace Windows on page 328).

5. Autozero the spectrometer:


1. In the Instrument tab menu, click on Continuous Graphics icon. The
Continuous Graphics window appears.
2. Click on Autozero graph button.
3. Align the furnace as described in the next step

6. Align the furnace:


1. Move the locking lever to the left to release horizontal (forward
backward) movement of the furnace.
2. Rotate the horizontal (forward-backward) control in small increments to
find the position that gives minimum absorbance reading on the display.
3. Remove the vertical alignment cover. Rotate the vertical (up-down)
alignment control in small increments to find the position that gives
minimum absorbance reading on the display.
4. Repeat the horizontal and vertical adjustments until you have obtained
the minimum absorbance reading.
5. Move the locking lever to the right to lock the furnace.
6. Reinstall the vertical alignment cover.
194 Preparing the System

Figure 5-9. Cover


Item Description
1 Cover

7. When you have completed furnace alignment, autozero the spectrometer:

8. Refit both window assemblies (see To refit the windows: on page 355).The
absorbance reading after replacing the windows should be about 0.06-0.09
when measured at the Cu line at 324.8 nm using the AA mode. The absorbance
increases toward shorter wavelengths.
Setting up the AS 900 Autosampler 195

Setting up the AS 900 Autosampler


Perform these steps before the start of every analysis run

1. Fill and flush the rinsing system (see Filling and Flushing the Rinsing System
on page 147).

2. Align the autosampler arm (see To Align the Autosampler Tip in the Graphite
Tube on page 148).

3. Adjust the penetration depth of the pipet tip in the graphite tube (see the
procedure, To check and make fine-adjustments to the penetration depth of the
pipette tip in the graphite tube on page 154).

4. Adjust the immersion depth of the pipet tip in the sample cup (see the
procedure, To check the depth of the autosampler tip in the sampling cup on
page 156).

5. Check delivery of the solution droplet (see the procedure, Checking the
solution droplet delivery on page 157).
196 Preparing the System

Shutting Down the System

Note In an emergency, switch off the spectrometer using the operational on/off
switch on the front panel.
The flame is automatically extinguished and the gases shut down in a safe
sequence. See Emergency Shutdown on page 197 for the procedure to
follow after an emergency shutdown.

To shut down the flame system


1. With the flame still burning, aspirate the correct rinsing solutions to rinse the
burner system (see Extinguishing the Flame on page 184). Either aspirate the
solutions manually or use the flame autosampler.

2. Extinguish the flame and bleed the gas lines:

• From the Instrument tab click on the Flame Control icon. The system
uses a predetermined shutdown sequence to extinguish the flame safely.

• Shut down the gases to the spectrometer at source.

• In the Flame Control window, click on Bleed Gases button to


depressurize the gas lines.

To shut down the furnace system


1. Flush the furnace autosampler rinsing system (see AS 900 Furnace
Autosampler Maintenance on page 357).

2. Shut down the furnace gases to the spectrometer at source.

To shut down the spectrometer


1. Exit the software.

2. Switch off the spectrometer at the operational on/off switch on the front panel.

3. Switch off any accessories.


Shutting Down the System 197

4. If you do not want to use the computer for other tasks, shut down the computer
and printer as described in their user's guides.

5. Empty the burner drain vessel (see Emptying the Drain System on page 232).

6. Empty the furnace autosampler waste bottle.

Note Dispose of hazardous or corrosive solutions properly and refer to your


local safety regulations for proper disposal procedures.

Emergency Shutdown
If a situation arises where you have to shut down the system quickly and you can
use the on/off switch on the front panel of the instrument.
198 Preparing the System

Figure 5-10. Location of instrument on/off switch


Item Description
1 Instrument On/Off switch
Maintenance 6
Introduction
This chapter describes the routine maintenance procedures required to keep your
instrument in proper working condition and to ensure the highest possible level of
performance. It includes maintenance checks that should be done on a daily basis
and maintenance procedures that should be done periodically depending on
instrument use. This chapter is divided into several sections, each section covering
maintenance procedures for a particular component of the system..

Caution Before using any cleaning or decontamination methods except


those specified by PerkinElmer, the responsible bodies should
check with PerkinElmer that the proposed method will not damage
the equipment.

Note The responsible body has the responsibility for carrying out appropriate
decontamination if hazardous material is spilled on or inside the
equipment.
200 Maintenance

Decontamination
Note If the instrument or an accessory requires decontamination before
repair, maintenance, warranty or trade-in purposes at PerkinElmer, the
responsible body should read the procedure and complete the certificate which is
available on the PerkinElmer public website:

http://las.perkinelmer.com/OneSource/decontamination.htm

Follow the “Decontamination of Instrumentation and Associated Sub-


assemblies” procedure and complete the “Certificate of Decontamination.” The
certificate is used to certify the decontamination process was completed before
equipment can be returned to PerkinElmer.

Note This equipment requires no specified inspection or preventive


maintenance to ensure the continuous functioning of its safety features.

Calibration of the Instrument


Service engineers need to be contacted for calibration of the instrument. You
should contact your local PerkinElmer Sales and Service office

General Maintenance Checklist


The following checklist describes general maintenance procedures.

• For safety reasons, and to avoid contaminating new samples, you should
ensure that the work area is kept absolutely clean. This is especially
important when working with toxic substances and when measuring trace
amounts of any elements.

• Clean up spills immediately, using a spill clean-up kit approved by your


organization.
Instrument Maintenance Checklist 201

In accordance with safe laboratory practices, spilled material should be


cleaned up and disposed of promptly and properly, taking into
! consideration the following:
location and size of the spill;
Warning
chemical and physical properties of the material;
hazardous properties of the material; and
types of personal protective equipment that might be needed.

Instrument Maintenance Checklist

Caution Flame should be turned off while performing the instrument


maintenance checklist.

To properly maintain the spectrometer instrument, do the following as required:


• Clean the exterior of the instrument.
• Inspect and clean any fans and filters.
• Monitor tank pressures
• Inspect the burner assembly (see checklist later in this chapter).
• Inspect the drain system.
• Inspect the cooling system for proper operation.
• If the intensity of the deuterium arc background corrector source is too low,
refer to the troubleshooting information in the Troubleshooting chapter of this
manual. The background corrector source lamp may need to be realigned or
replaced.
• Normally, the spectrometer optics will require little or no maintenance.
However, low energy lamp readings, or noisy or erratic results may indicate
that the optics require cleaning or re-calibration of the wavelengths, if all the
elements have low energies. This should only be done by a PerkinElmer
service engineer.
• The windows in the burner sample compartment need to be inspected and
cleaned as necessary with a mild detergent or isopropanol.
202 Maintenance

Caution If optic surfaces become dirty (e.g., from exposure to


laboratory vapors), cleaning should be done only by a
PerkinElmer service engineer.

Caution Never touch or clean the grating surfaces. Fingerprints or


scratches will adversely affect the dispersion characteristics of the
grating and impair the operation of the instrument.

Cleaning the Instrument


Exterior surfaces may be cleaned with a soft cloth, dampened with a mild detergent
and water solution. Do not use abrasive cleaners or solvents. Use the same
technique to clean the sample compartment windows, too.

Checks

Periodic Checks
The frequency of maintenance required will be determined by the amount of use
the system receives, the cleanliness of the environment, and the number and nature
of the samples being analyzed.

Instrument parts that require periodic checks:

• Nebulizer: Check the wear and tear of the o-rings on the end caps and on the
burner head. To replace the o-rings, see Disassembling the Burner Chamber
later in this chapter.

• Drain System Maintenance: Check for wear and/or chemical attack. The drain
tubing should be clear with as few bends as possible. The drain system should
be replaced if it has deteriorated. See Drain System Maintenance later in this
chapter.
Burner Maintenance Checklist 203

• Burner System: Check for uneven flame and deposits build up along the burner
slot.

• Air Filters: Should be replaced yearly or as needed in a dusty environment.

Burner Maintenance Checklist


Maintenance checklists for the burner system are presented below.

Burner system, maintenance checklist

If you analyze samples that have 'dirty' matrices, such as blood, sugar or oil, you
will probably have to clean the components more often than if you were analyzing
'clean' samples, such as drinking water.

Part Maintenance

Burner system Always rinse the burner system correctly before extinguishing the flame.
If you are analyzing samples with high solids content: Clean the burner
chamber at least once daily.

If you are using organic solvents: Clean the burner chamber before you switch
to aqueous solutions. Empty the drain vessel and dispose of hazardous
solutions properly.

If you are analyzing samples containing high concentrations of copper, silver,


or mercury: Thoroughly flush the burner chamber and drain tube immediately
after completing such analyses. Empty the drain vessel and dispose of
hazardous solutions properly.
Burner head Inspect the burner head for deposits before igniting the flame. The burner should
provide an even flame over the length of the burner slot. An uneven flame may
indicate that the slot needs cleaning. See the section on cleaning procedures later
in this chapter.

Check the width of the burner slot periodically.


204 Maintenance

Part Maintenance

Nebulizer If there is an obstruction in the nebulizer, clear it using a copper cleaning wire.
Drain system Flush the drain system thoroughly at the end of each working day by pouring
water down the neck of the burner chamber. Make sure to remove the flow
spoiler from the burner chamber so that all the water drains out.
Drain vessel This is not a waste storage, but it is a waste collection device for the daily
operation, so empty the drain vessel regularly. Do not allow it to fill with
corrosive, toxic, or organic solutions. Dispose of hazardous solutions properly.
Drain trap Periodically remove the drain trap and clean.
Drain tube Inspect the drain tube regularly for wear and/or chemical attack. Replace it if it
has kinked and also deteriorated.
O-rings Check the condition of the o-rings regularly: burner end cap o-ring; o-ring in
neck of burner chamber; there are four o-rings on the metal body nebulizer, and
five o-rings on the high sensitivity plastic nebulizer. Either of these nebulizers
can be used on the (different) end-cap of the burner assembly.
Gas hoses Check the gas hoses regularly for leaks, particularly at the fittings, using a
proprietary leak testing fluid. Call a PerkinElmer service engineer if a leak is
detected.
Acetylene cylinder If the cylinder pressure falls to below 600 kPa (6 bar; 85 psig) some of the
solvent used to stabilize the acetylene (e.g. acetone) may be carried over into
the burner. This could influence the characteristics of the burner and could
eventually cause irreversible damage to the gas box. Always change to a new
acetylene cylinder when the cylinder pressure falls to below this value.

Warning: Unauthorized Adjustments and Servicing


Only a PerkinElmer service engineer or similarly trained and authorized
! person should be permitted to service the instrument.
Warning
Burner Maintenance Checklist 205

If the spectrometer system does not function correctly…


• Switch off the spectrometer system and make sure that it cannot be operated.

• Contact your local PerkinElmer office.

• You should only perform the maintenance procedures described in this guide.

For any other maintenance or service contact your local PerkinElmer office to
arrange for a service engineer to visit. In particular you should only allow a
PerkinElmer service engineer or similarly trained and authorized person to perform
any work on:

1. Electrical components inside the instrument (excluding the electrical/


electronic components)

2. The gas connections and gas system pneumatics

3. The monochromator and all other optical system components

Before the service engineer arrives

• Make sure that the instrument and work area are clean.

• Empty corrosive solutions from the burner drain vessel.

• Then add water to the drain trap to activate the function.


206 Maintenance

Spectrometer Maintenance Checklists


Maintenance checklists for the spectrometer system are presented below.
General Preventative Maintenance Procedures

Part Maintenance

Instrument and work For safety reasons, and to avoid contaminating new samples, you should make
area sure that the instrument and the work area are always absolutely clean. This is
especially important when you are working with toxic substances and when
you are measuring trace amounts of any elements. Wipe up spills immediately
before they can cause further contamination or damage. Before you leave the
instrument standing idle for any period of time, make sure that all the
components are clean.
Fume ventilation Make sure that the main exhaust ventilation system functions correctly. Always
switch it on when you are using the instrument.
Environmental Make sure that the environmental conditions are as described in Chapter 2
conditions

Spectrometer Maintenance Checklist

Part Maintenance

External Surfaces Wipe over the surfaces with a lint-free cloth moistened with a dilute solution of
laboratory detergent. The surfaces are resistant to dilute acids and alkalis, and
to a lesser extent to strong acids and alkalis and organic solvents.
Air filters Replace filter yearly or more often in a dusty environment.
Changing the Air Filter 207

Changing the Air Filter


1. To make sure that the electrical components in the spectrometer are properly
cooled, the air filters must allow sufficient air into the instrument. Check the
filters regularly and change it if it is dirty.

You should not need to change the filters more than once every year if the
environmental conditions are as described in the Spectrometer Maintenance
Checklist located in this chapter.

Replacement filters (Part No. B0501696) are available; see Replacement Parts
on page 362, for the part number.

2. Locate the air filter on the right side of the instrument.


208 Maintenance

4
3

Figure 6-11. Location of air filters on the right side of the instrument
Item Description Item Description
1 Air filter cover tab 3 Air filter cover
2 Air filter location 4 Air filter

3. Depress the tab and lift out the air filter cover that holds the air filter in place.
4. Replace the air filter (Part No. B0501696) and then put the air filter cover back
into place.
Changing the Air Filter 209

5. The vents located on the left side of the instrument are for the furnace power
supply. Hot air is blown out of these vents and no air filters are needed. Do
not restrict the air flow exhaust from these vents.

Figure 6-12. Location of Furnace Power Supply vents


Item Description
1 Furnace Power Supply vents
210 Maintenance

Changing the Vent Filter


For the PinAAcle 900H, 900T and 900Z models have a vent filter located at the
rear of the instrument. Periodically this filter (Part No. B0501696) will have to be
changed.

1. Pull off the frame around the filter.

2. Take the filter out from the frame and replace with a new filter.

3. Snap the frame with the new filter back into place.

Figure 6-13. Location of vent filter


Item Description
1 Vent filter
Changing the Fuses 211

Changing the Fuses


Do not use makeshift fuses or short-circuit the fuse holders.

Caution Use only fuses with the required current rating and of the specified type for
replacement.

1. Switch off the spectrometer and all other instruments in the system
2. Switch the circuit breaker on the rear panel of the spectrometer to the off
position.

1 2

Figure 6-14. Location of fuses


Item Description
1 Fuse for the cooling system power outlet; 4A Slow-Blow (T)
2 Fuse for the cooling system power outlet; 4A Slow-Blow (T)
212 Maintenance

3. Disconnect the spectrometer's line power cord from the line power supply.

4. Disconnect all the line power cords from the sockets at the rear of the
spectrometer.

5. To change the fuses numbered F1, F2:

a). Insert the tip of a suitable screwdriver in the slit of the fuse holder and
unscrew the fuse holder.

b). Remove the blown fuse, and then insert a new one of the correct type and
rating. The correct rating is shown on the label of the fuse on the rear panel
of the spectrometer.

c). Screw the fuse holder into the correct socket.

6. Reconnect the line power cords correctly.

Cleaning the Burner Chamber


It is very important to clean the burner chamber with a soft wireless brush and a
mild laboratory detergent solution on a regular basis. This regular cleaning will
prevent the buildup of solids on the burner chamber.

Note Do not scrape the plastic components with metal tools. Do not soak the
burner chamber in acid or use an abrasive cleaner.

1. Remove the burner chamber from the atomizer compartment by disengaging


the latch on the right side of the burner by pushing the latch back.
Cleaning the Burner Chamber 213

Figure 6-15. Location of end cap


Item Description
1 Latch
2 End cap

2. The end cap must be removed to access the inside of the burner chamber.

3. The end cap is secured to the burner chamber by the latches located on each
side. Pull both latches back to remove the end cap from the burner chamber.
214 Maintenance

1 2

3 4

Figure 6-16. Lever positions


Item Description
1-2 Latches closed position
3-4 Latches open position
Cleaning the Burner Chamber 215

4. Clean the burner chamber and flow spoiler with a soft brush and a mild
laboratory detergent solution.

5. Clean the inside of the burner end cap with a soft wireless brush and a mild
laboratory detergent solution.

Note If the solid deposits cannot be removed with a soft brush and a mild
laboratory detergent solution, the internal cavity of the chamber may be
soaked overnight with the 0.5% Triton X-100 + 5% HNO3 acid when the
opening for the burner head is closed. Thoroughly rinse the internal cavity
with de-ionized water before use. If solid deposits still remain, you will
need to replace the spray chamber.

6. After cleaning, rinse thoroughly with deionized water.

7. Reassemble the burner system.

Cleaning the Burner Chamber After Use With Organic Solvents


If you aspirate aqueous samples immediately after organic samples (e.g. oils or
MIBK extracts), the absorption signals can be noisy and erratic. After aspirating
organic samples, perform the procedure below to prevent contamination of
subsequent aqueous samples.

1. Aspirate for 5 minutes an organic solvent that is miscible with the samples that
have just been aspirated.

2. Aspirate methanol or another solvent miscible with both the organic solvent
and water, for 5 minutes.

3. Aspirate 1% nitric acid solution for five minutes.

4. Flush the drain tube thoroughly with water. Empty the collection vessel and
refill with water. Dispose of hazardous or corrosive solutions properly and
observe local codes concerning the effect of the waste on the environment.
216 Maintenance

Note Dispose of hazardous or corrosive solutions properly and refer to your


local safety regulations for proper disposal procedures.

Cleaning the Burner Chamber After Aspirating Solutions Containing


Cu, Ag, or Hg
If you have aspirated high concentrations of copper, silver, or mercury solutions
into an acetylene flame, unstable acetylides may have formed in the burner
chamber. If permitted to dry, these compounds may explode.

1. Aspirate dilute acid (1% (v/v) HCl solution) for 5 minutes before turning off
the flame.

2. Extinguish the flame and allow the burner head to cool.

3. Remove the burner head.

4. Flush the drain system see Cleaning (or Flushing) the Drain System on page
231.

5. Reinstall the burner head.

6. Empty the drain vessel.

Note Dispose of hazardous or corrosive solutions properly and refer to your


local safety regulations for proper disposal procedures.
Cleaning the Burner System 217

Cleaning the Burner System


The nature of the samples aspirated determines how frequently you need to clean
the burner system.

• The burner should provide an even flame over the length of the burner slot. An
uneven flame may indicate that the slot needs cleaning. A badly clogged slot
may cause a flashback of the flame.

• Aspirating samples with high solids content may cause deposits to build up
along the burner slot

• Prolonged operation of the nitrous oxide-acetylene flame may cause deposits


of pyrolytic carbon to build up along the burner slot. This is especially so if the
fuel-oxidant ratio is not set correctly

Unstable acetylides, which are likely to explode when dry, may be


! formed when aspirating high concentrations of silver, copper, or mercury
salts into an acetylene flame.
Warning

Warning: Hydrochloric and Nitric Acids - Risk of Burns


Hydrochloric (HCl) and nitric (HNO3) acids are corrosive and can cause
! severe burns.
Warning

Caution If high concentrations of Cu, Ag, or Hg have been aspirated into an


acetylene flame, clean the burner chamber immediately after use by
following the procedures in this section called Cleaning the Burner After
Aspirating Cu, Ag, or Hg sample.
218 Maintenance

Flashbacks
A flashback is an explosion of the premixed gases in the burner chamber. The
safety interlocks normally prevent conditions that could cause a flashback, but if a
flashback should ever occur:

• Check that the burner head slot is clean.

• Check that the burner head is seated correctly.

• Check the flow spoiler or impact bead for damage, and replace any damaged
parts.

• Check the inside of the end cap for any cracks.

• Make sure that you are using compressed air and not oxygen enriched air.

• Carefully check and tighten all connections to, and seals on, the burner unit,
and check the gas flow settings before you attempt to ignite the flame. Any
seepage of fuel and oxidant from the burner chamber may cause a flashback.

Cleaning the Burner Head

Quick Cleaning Procedure


1. Extinguish the flame, allow the burner head to cool, shut down the gases at
source, and bleed the gas supply lines.

2. Open the atomizer compartment door.

3. Remove the burner head up and out by pushing the latch located on the left side
of the burner head to the rear. Refer to the figure on page 222.

4. Carefully work along and through the burner head slot with the cleaning tool
provided. Do not nick the edges of the slot.

Note The cleaning tool resembles a strip of thin metal sheet. Do not use other
tools to clean inside the burner slot since they may have burrs that could
nick the slot.
Cleaning the Burner Head 219

5. Rinse the burner head well with deionized water and make sure that all
scrapings are removed from inside and outside the burner head.

Wear safety glasses when blowing the burner head with clean
! compressed air.
Warning

6. Blow the burner head dry with clean compressed air.

7. Reinstall the burner head.

8. Close the atomizer compartment door.

Complete Cleaning Procedure


If the quick cleaning procedure, above, fails to remove deposits or if you wish to
clean the burner head more thoroughly, see Changing the Fuses on page 211.
Checking the Slot Width
Over time, the burner slot becomes wider due to abrasion. The level of abrasion
depends on the types of solutions you are aspirating. A burner slot that is too wide
causes unstable flame conditions and, in the worst case, may cause a flashback of
the flame. For this reason you should check the width of the burner slot at regular
intervals.
A set of feeler gauges is required to check the slot width. The table below specifies
the correct slot width and the feeler gauge required for checking.

Table 6-1. Slot Width and Feeler Gauge

Feeler Gauge
Burner Head Slot Width Tolerance
for check

air-acetylene 0.65 mm + 0.075/-0.025 mm 0.7 mm


(0.026 inch) (± 0.003/-0.001 inch) (0.030 inch)
220 Maintenance

Table 6-1. Slot Width and Feeler Gauge

Feeler Gauge
Burner Head Slot Width Tolerance
for check

N2O-acetylene 0.5 mm ± 0.025 mm 0.5 mm


(0.020 inch) (± 0.001 inch) (0.020 inch)

To check the slot width:


1. Carefully slide the specified feeler gauge through the length of the burner slot.
2. The gauge must fit tightly in the slot.
3. The slot is too wide if the gauge is loose along the slot. If the slot is too wide,
replace the burner head with a new one.

Burner head surface


The condition of the top surface of the burner head along the slot influences the
stability of the signals. Discard the burner head if the top surface is corroded.

Pre-Conditioning a New Burner or Drain Tube

Note This important procedure MUST be performed when a new burner or


drain tubing is installed.

This procedure should be done directly after installation of a new burner and
repeated if the drain tube or any of the sample introduction system components are
replaced.

In order for a new sample introduction system to aspirate sample and drain
smoothly, all the internal surfaces need to be prepared. This is easily accomplished
by aspirating a 0.1% Triton X-100 solution for approximately five minutes.
Removing the Burner Assembly From the Instrument 221

Removing the Burner Assembly From the Instrument


1. Extinguish the flame, turn off the gases, and switch off the instrument. Let the
burner head cool. Open the burner door.

2. Disconnect the drain tube, unplug the drain interlock connector.

3. Locate and press the locking pin down, and push the locking lever backward
to disengage the whole burner assembly. The burner assembly will be pushed
forward, and can now be removed. See the following figure.
222 Maintenance

1
2

3
4

Figure 6-17. Remove the burner head from the burner chamber
Item Description Item Description
1 Safety latch 3 Pressing the safety latch
2 Burner lever 4 Pushing the burner lever
Removing the Burner Assembly From the Instrument 223

4. The burner assembly is now accessible for maintenance. Remove the burner
assembly.

Figure 6-18. Location of the furnace locking pin


Item Description
1 Burner assembly mount
2 Furnace assembly
3 Furnace locking screw

5. Place the burner assembly on a bench for routine maintenance and cleaning.
224 Maintenance

Removing the Burner Head


To remove the burner head, press the tab on the safety latch found on the left side
of the ignitor assembly with one hand, and gently pull and twist the burner head in
an upward direction with the other hand until it comes off the chamber.

Depending on the type of analysis you need to do, you may need to change the
burner head, see Burner Head Options on page 87.

Disassembling the Burner Chamber


This procedures assumes that you have removed the burner assembly from the
instrument and placed it on a workbench. Next you will disassemble it.

1. The burner head should also be removed by following the procedure Removing
the Burner Assembly From the Instrument on page 221
Disassembling the Burner Chamber 225

2. Unscrew the retaining ring (see figure below) and pull out the burner o-ring.

3 1
5
4

Figure 6-19. Exploded view of the burner chamber assembly


Item Description Item Description
1 Burner head 5 Metal body nebulizer (is shown
here but you can also have a high
sensitivity plastic nebulizer
attached here)
2 Burner head adjustment tool 6 End cap assembly
3 Spray chamber 7 Retaining ring
4 Flow spoiler 8 Burner head o-ring
226 Maintenance

3. Remove the nebulizer from the end cap assembly. Refer to Removing the Metal
Body Nebulizer on page 238. Refer to Removing the High Sensitivity Plastic
Nebulizer on page 257.

4. Clean the chamber. Place the parts in a detergent solution until they are
completely clean. See Cleaning the Burner Chamber on page 212 for details.

5. Remove and rinse with deionized water. Allow time for complete drying.

Reassembling the Burner System


After you have completed maintenance procedures, reassemble the burner system
as given below.

To reassemble the burner chamber

1. Before you reassemble the burner system, verify that the o-rings are in good
condition. If an o-ring appears damaged, replace it.

2. Connect the drain tube and clamp.

3. Carefully slide the nebulizer into the end cap and lock into place with the
nebulizer clamp.

4. Place the burner o-ring into the burner chamber and screw on the retaining ring.

5. Press the safety latch on the ignitor box while gently pushing and twisting the
burner head onto the chamber.

To Install the Burner in the Spectrometer


1. Guide the burner assembly into the tracks of the Burner Assembly mount.

2. Push the burner assembly in so that the rear gas fittings line up with the gas
connectors at the back of the Burner Assembly mount. Push the burner
assembly fully in until it clicks into place. Press the locking pin down, pull the
locking level forward until it locks the burner assembly in place. The locking
pin is locked.
To Install the Burner in the Spectrometer 227

3. Locate the drain vessel. The drain tube and interlock cable will be attached to
the drain vessel retainer cap.

4. Place the drain vessel in full view on the floor in front of the instrument. Never
place the drain vessel inside a cabinet.

5. Before connecting the drain tube to the burner assembly, if necessary pour
about 250 mL of water into the free end of the drain tube to fill the drain loop
and to activate the drain float.

6. Place the hose clamp over the free end of the drain tubing.

Caution When installing the free end of the drain tubing over the drain outlet, take
care not to damage the inner Teflon lining of the drain tube.

7. Carefully install the free end of the drain tubing over the drain outlet, making
sure that the inner Teflon lining of the drain tube does not get damaged.

8. Use a flat-blade screwdriver to tighten the hose clamp.

9. Plug the white drain interlock connector into the drain interlock plug on the
burner assembly as shown in the figure below.
228 Maintenance

2
3

Figure 6-20. Drain hose attached


Item Description
1 Clamp
2 Drain hose
3 Drain Interlock
To Install the Burner Head 229

To Install the Burner Head


Depending on the type of analysis you need to do, you may need to change the
burner head, see Burner Head Options on page 87.

1. Put the burner head back onto the burner chamber while pressing the safety
latch tab.

2. Position the magnetic strip on the burner head ring around the back of the
assembly - it should face the ignitor box. Release the safety latch. Be sure the
burner head is fully seated on the chamber. A gentle twisting and pushing may
be necessary. You will know that the burner head is fully seated because the
ignitor will swing over the burner.

3. Put the burner assembly back into the instrument.

4. Check the burner alignment. You should readjust the burner any time the
burner is aligned.

Drain System Maintenance


Drain system maintenance includes cleaning (or flushing) the drain system,
replacing the drain tubing and emptying the drain vessel when it is filled with waste
solutions. (The drain vessel should never be used as a long-term waste storage
container.) Replacing the drain trap and assembly must be done by trained service
personnel only. The figure below shows all the parts of the PinAAcle 900 Series
drain system.
230 Maintenance

2
1

Figure 6-21. Drain bottle attached


Item Description
1 Drain Interlock
2 Drain hose
3 Drain bottle
Drain System Maintenance 231

The drain hose and vessel must be checked periodically for wear and/or chemical
attack. The drain tubing should be clear with as few bends as possible. The drain
system should be replaced if it has deteriorated.

Cleaning (or Flushing) the Drain System


It is recommended that the drain system be flushed thoroughly with water at the
end of each working day to remove caustic, corrosive, or organic waste materials
that could otherwise damage the burner chamber or drain tubing.

1. Remove the clamp around the drain tube.

2. Disconnect the drain tube from end cap.

3. Pour about 250 mL deionized water slowly through the drain tube to
completely flush the chamber and the drain system.

4. Allow the water to drain into the drain vessel.

5. Reattach the drain tube to the end cap.

6. Tighten the clamp around the drain tube.


232 Maintenance

Emptying the Drain System

Figure 6-22. Drain bottle attached


Item Description
1 Retainer cap
2 Drain trap assembly
3 Drain bottle

1. Extinguish the flame, allow the burner head to cool, shut down the gases at
source, and bleed the gas supply lines.

2. Switch off the spectrometer.

3. Flush the drain system. See Cleaning (or Flushing) the Drain System on page
231.
Drain System Maintenance 233

4. Unscrew the retainer cap from the drain bottle.


5. Carefully lift out the drain trap assembly. Do not disconnect the electrical lead.
6. Place the drain trap assembly into a suitably large bucket or container so that
it is vertical. If the drain trap assembly is laid on its side, liquid can run out onto
the floor.
7. Rinse the outside of the assembly well with water.
8. Empty the drain bottle.

Note Dispose of hazardous or corrosive solutions properly and refer to your


local safety regulations for proper disposal procedures.

9. Place the drain trap assembly back into the drain bottle and screw on the
retainer cap.

Replacing the Drain Tubing


If the drain tubing (Part No.02507987) is damaged or extremely dirty and needs to
be replaced, refer to the next figure and proceed as described next.

Dispose of drain vessel waste in accordance with the regulations


! applicable to your locality, state, and/or country.
Warning

1. Turn off the instrument power switch.


2. Empty the drain vessel.
3. Unplug the drain interlock connector from the burner (see the previous figure).
4. Remove the spiral wrap from the drain tubing by unwrapping it. This will
release the drain interlock cable.
5. Disconnect the drain tubing from both the drain vessel and the drain outlet on
the burner end cap by loosening the clamps on each end of the tubing. Once the
clamps are loosened, the tubing should easily pull out.
6. Place the new piece of drain tubing (Part No. 02507987) next to the drain
interlock cable and carefully rewrap the spiral wrap around them both.
234 Maintenance

7. Place the drain clamp on the upper end of the new drain tubing. Then attach the
tubing to the drain outlet on the burner end cap. Tighten the clamp securely.
8. Place the other drain clamp on the lower end of the drain tubing. Then attach
the tubing to the drain trap switch assembly. Tighten the clamp securely.
9. Plug the drain interlock connector into the receptacle under the burner. Make
sure the interlock connector is plugged in all the way.
10. Go to Preparing the New Drain Tubing for Use on page 234.

Preparing the New Drain Tubing for Use

Note This important procedure MUST be performed at this point of the drain
tube replacement process.

In order for the sample introduction system to drain smoothly, the internal surface
of the new drain tube needs to be prepared. This is easily accomplished when you:
1. Aspirate a 50/50 solution of water and methanol for approximately 5 minutes.
2. Replacement and preparation is now complete.

Adding Water to the Drain Float Assembly


Enough water must be present in the drain system to fill the drain loop and to
activate the drain float assembly. If not, carry out the following procedure:
1. Loosen the drain clamp and remove the drain tubing from the drain outlet on
the burner end cap.
2. Pour about 250 mL of water into the drain tubing.
3. Carefully reconnect the drain tubing to the burner end cap. Replace the drain
clamp and tighten securely.
4. Installation of the burner drain is complete.
Organic Drain Assembly 235

Organic Drain Assembly


The organic drain vessel assembly (Part No. N3150232) has a smaller capacity
volume vessel (10 liters) and needs to be emptied after every use.
The interlock mechanism in the organic drain vessel has been tested to withstand
degradation by commonly used solvents.
Although the organic drain vessel can be used to collect solvent waste, the organic
drain vessel can also be used to collect acid waste as long as you following this
warning:

Acid and organic solvent wastes should never be combined in the


! same bottle.
Warning

The same procedure should be followed for conditioning and maintaining the
organic drain assembly as outlined earlier in Drain System Maintenance on page
229. Except instead of using water to fill up the drain loop, the drain loop should
be filled up with the organic solvent, such as kerosene or xylene which is
commonly used in the organic solvent-based analysis.
Aqueous acidic wastes must never be mixed with the organic solvent-based
wastes. You should always use appropriate drain assembly for your analysis.

Nebulizer Removal and Reinstallation


The instrument is shipped with the nebulizer already installed. Depending on the
instrument model ordered, it will be shipped with either a metal body or a high
sensitivity plastic nebulizer and its corresponding nebulizer.

Options are available for other nebulizers using Kalrez O-rings and Tantalum
needle valve that are resistant to aqua regia, corrosive chemicals and organic
solvents commonly used in the elemental analysis. They should be maintained in a
similar manner as described below.
236 Maintenance

Table 6-2. Nebulizer Configurations


Model and Part No. Configuration Nebulizer
PinAAcle 900T- THGA + Flame Metal
N3200080 or N3200081
PinAAcle 900T- THGA + Flame High Sensitivity Plastic
N3200082 or N3200083
PinAAcle 900H- HGA + Flame Metal
N3200070 or N3200071
PinAAcle 900H- HGA + Flame High Sensitivity Plastic
N3160072 or N3160073
PinAAcle 900Z- THGA Only N/A
N3200060 or N3200061
PinAAcle 900F- Flame Only Metal
N3200050
PinAAcle 900F- Flame Only High Sensitivity Plastic
N3200051

Table 6-3. Nebulizer Assemblies and Spares


Replacement
Complete End Cap
O-Ring Needle
Description Type Needle Assembly Assembly
Type Assembly
P/N P/N
P/N

Stainless Steel Aqueous Stainless Viton N3160143 N3160102 03030354


(standard)
Plastic High Aqueous Platinum/ Viton N3160144 N3160111 B3150525
Sensitivity Iridium
(standard)
Plastic High Aqueous Platinum/ Kalrez N3160159 N3160189 N3160154
Sensitivity or Iridium
Organics
Nebulizer Removal and Reinstallation 237

Replacement
Complete End Cap
O-Ring Needle
Description Type Needle Assembly Assembly
Type Assembly
P/N P/N
P/N

Plastic High Aqueous Tantalum Kalrez N3160152 N3160189 N3160146


Sensitivity or
(suitable for Organics
aqua regia in
addition to
organics)
Stainless Steel Aqueous Stainless Kalrez N3160158 N3160188 N3160153
or
Organics
Stainless Steel Aqueous Plastic Viton N/A N3160102 03030402
Stainless Steel Aqueous Platinum Viton N/A N3160102 03033124
Alloy

Warning: Flammable Gases - Fire and Explosion Hazard


! If you do not use a PinAAcle nebulizer for your burner system, there be
a seepage of fuel gas which is a serious fire hazard.
Warning Use only a PinAAcle nebulizer for your burner system.
238 Maintenance

PinAAcle 900 Metal Body Nebulizer


The nebulizer is an adjustable pneumatic device that is used to draw the sample into
the capillary tubing and spray it as a fine aerosol into the spray chamber. The
oxidant gas is routed through the oxidant tubing into the nebulizer through a
connecting passage in the burner assembly (spray chamber). The sample uptake
rate/sensitivity is optimized by adjusting the nebulizer.

The metal body nebulizer can be used for most solutions containing < 5 % acid. It
has excellent performance (precision and signal-to-noise ratio) and it is less prone
to clogging. The needle assembly and venturi can be changed to produce a
Platinum alloy and corrosion resistant version.
Removing the Metal Body Nebulizer
Remove the nebulizer using the following procedure:

1. Open up the Sample Introduction Compartment door to the burner chamber.

2. Pull out the nebulizer locking clamp back and carefully but firmly, rotate the
metal side arm upwards 90 degrees to the unlock position.
PinAAcle 900 Metal Body Nebulizer 239

3
4

Figure 6-23. Metal body nebulizer


Item Description Item Description
1 Nebulizer in locked position 4 Nebulizer metal arm in up position
2 Nebulizer metal arm in locked 5 Nebulizer Interlock sensor
position

3 Nebulizer in unlock position

3. Pull the nebulizer out from the nebulizer assembly end cap.
240 Maintenance

2 7 10
3 8
5

1 4 6 9 11

Figure 6-24. Exploded view of the metal body nebulizer


Item Description Item Description
1 Fine adjustment nut 7 Nebulizer body o-rings (2) ((P/N
(P/N 0301460) 09902015)
2 Sample capillary (P/N 09908265) 8 Venturi O-ring (P/N 09902005)
3 Teflon® washer (P/N 03031802) 9 Venturi (P/N 03031810)

4 Needle valve (P/N 03030354) 10 Cap (P/N N3161057)


5 Spring (P/N 03031806) 11 O-ring (P/N 09902239) that seals the
nebulizer to the end cap
6 Nebulizer body (P/N N3160133)

Note Use Apiezon®-L grease. Make sure that no grease gets onto the tip of the capillary.
Use only the Apiezon grease supplied with the nebulizer. It is metal-free.

4. Inspect the all the o-rings. Replace any cracked or damaged o-rings. Apply a
small amount of Apiezon-L grease (Part No. 0300405) onto the o-rings (Part
No. 09902015). The nebulizer will then slide easily into the end cap.
5. Inspect the needle valve and replace if needed.
PinAAcle 900 Metal Body Nebulizer 241

6. For information on cleaning the nebulizer, see Cleaning the Metal Body
Nebulizer on page 243.
Reinstalling the Metal Body Nebulizer
1. Carefully reinstall the needle assembly by taking the beveled edge of the
needle valve and insert it into the nebulizer in the 1 o’clock position to align
with the nebulizer gas port in the end cap. See the following figure.

1
2

4 3

Figure 6-25. Needle valve


Item Description Item Description
1 Needle valve assembly 3 Metal body nebulizer body
2 Beveled edge of the hypodermic needle 4 Needle valve in 1 o’clock position
in the middle needle valve assembly
242 Maintenance

2. Apply a small amount of Apiezon grease (Part No. 03030405) onto the o-rings
(Part No. 09902015) on the nebulizer body. The nebulizer will then slide easily
into the end cap.

3. Insert the re-assembled nebulizer into the end cap in the unlocked position.

4. Rotate the arm 90 degrees clockwise into the locked position.

5. Push the locking clamp all the way in to lock the nebulizer in place.

Note When the nebulizer is securely in place, the nebulizer interlock will be
depressed and you will be able to run the instrument. If the nebulizer
interlock is not depressed, the software will indicate that the safety
interlock is not satisfied. A checked off green box in the software will
indicate that the safety locks are engaged and the instrument will allow an
analysis to occur.

The metal body nebulizer reinstallation is complete.

Cleaning the Capillary Assembly


Clean the capillary assembly whenever you notice degradation in absorbance
values due to a blockage in the capillary. There are two ways to clean the capillary
assembly:

• The first (simplified) way should be used if the nebulizer capillary assembly is
not difficult to clear. This method involves simply passing one of the cleaning
wires, supplied, through the capillary assembly.

• The second (complete) procedure requires shutting down the spectrometer,


removing the nebulizer from the end cap, removing the capillary tubing,
cleaning the capillary assembly and replacing the capillary tubing. This
procedure must be performed if you have no success with the first method.
PinAAcle 900 Metal Body Nebulizer 243

Cleaning the Metal Body Nebulizer


A low or erratic absorbance reading may indicate that the burner head, burner
chamber, or the nebulizer and capillary tubing require cleaning. If you find that the
burner chamber and burner head is clean, the problem is probably due to an
obstruction in the nebulizer or capillary tubing.

To clear an obstruction in the nebulizer

1. Aspirate pure solvent with the flame on until the absorbance reading is
satisfactory for a standard.

2. If you cannot obtain a satisfactory absorbance, try to clear the obstruction by


pushing the copper cleaning wire through the capillary and into the nebulizer.
Move the wire in and out to dislodge any solid particles

Caution Use only the copper cleaning wire provided with the nebulizer to clean the
capillary. Other wire may be burred and can damage the nebulizer.

3. If deposits cannot be removed using these measures, remove the nebulizer so


you can disassemble and clean it.

Cleaning the Nebulizer


To clean a stubborn blockage from the nebulizer, perform the procedure below.

Wear protective gloves when you remove the nebulizer from the end cap
! if you were analyzing toxic samples.
Warning

1. Turn off the spectrometer and turn off all gas supplies.

2. Lift the end-cap spring clamp and gently pull the nebulizer out of the burner
end cap.

3. After you have taken the nebulizer apart, clean the components as follows:
244 Maintenance

4. Clean the capillary assembly using a mild laboratory detergent solution, or a


solvent such as isopropanol, preferably in an ultrasonic bath.

5. Clean the nebulizer body and any other parts that appear dirty in a mild
laboratory detergent solution, or a solvent such as isopropanol, preferably in an
ultrasonic bath.

6. Rinse all the cleaned components thoroughly with deionized water. If the
venturi or the tip of the needle assembly looks worn, than that part should be
replaced.

7. Inspect the all o-rings on the nebulizer body and clean them if necessary in
mild laboratory detergent solution, followed by a thorough rinsing with
deionized water. If they look damaged, replace them.

After you have cleaned the components, reassemble the nebulizer.

Adjusting the PinAAcle Metal Body Nebulizer for Maximum


Absorbance
Adjust the nebulizer to achieve maximum absorbance as follows:

1. Ignite the flame. Refer to the procedure for igniting the flame in Igniting the
Flame on page 182.

2. Set up the spectrometer for the determination of copper, magnesium, or


another element which has an absorbing wavelength above 250 nm and whose
sensitivity is not dependent on the fuel/oxidant ratio. Do not select an element
requiring a nitrous oxide-acetylene flame, as the nebulizer should never be
adjusted when a nitrous oxide-acetylene flame is lit. The height for the air-
acetylene flame is not as critical as in the nitrous oxide-acetylene flame where
the sensitivity can vary a lot.

3. Use the Align Burner Wizard in the Flame Control Window to optimize the
burner position. After the flame is turned on, autozero on a blank. Then aspirate
a standard and make sure the solution is being aspirated by the nebulizer so
there will be an absorbance with which the horizontal and rotational positions
can be optimized. If necessary, adjust the burner height.

4. While aspirating the standard, turn the nebulizer locking ring clockwise until
it is free of the nebulizer adjustment nut.
PinAAcle 900 Metal Body Nebulizer 245

5. Slowly turn the nebulizer adjustment nut counterclockwise until bubbles begin
to appear at the end of the needle assembly tube in the sample solution.

6. Slowly turn the nebulizer adjustment nut clockwise until the absorbance goes
to a maximum and then begins to decrease. Go back to the maximum
position.

7. Lock the nebulizer adjustment nut in its current (optimum) position by turning
the nebulizer locking ring counter-clockwise while carefully holding the
nebulizer adjustment nut.

8. Check the characteristic concentration as instructed in your spectrometer


manuals. This characteristic concentration should normally be within ±20% of
the value listed in the Analytical Methods for AA Spectroscopy (Part No.
03030152).

Using Organic Solvents


It is often beneficial to lower the nebulizer uptake rate when aspirating organic
solvents. The normal nebulizer update rate for aqueous solutions is typically 6-8
mL/min.

Caution When an organic solvent is aspirated, the flame will become richer. The
uptake rate should be reduced to obtain a moderately lean flame. The
organic solvent is a fuel and it will act as a fuel. If needed, the fuel flow
can also be reduced while the solvent is being aspirated. The fuel flow
must be increased before the sample capillary is removed from the solvent
for any length of time, or the flame will be too lean, which will cause a
flashback.

Depending on the type of organic solvent aspirated, reducing the uptake rate to 1-
3 mL/min, will minimize how rich the flame will become. This leaner flame
typically provides improved precision, particularly when aspirating a commonly
used solvent such as xylene.

The organic solvent is also a fuel and can act as a fuel just as acetylene.
246 Maintenance

To adjust the nebulizer uptake rate, unlock the nebulizer locking nut and rotate the
nebulizer adjustment nut until you locate a position which provides reduced sample
uptake. Then lock the nebulizer locking nut.

Note The uptake rate is easily measured by using a graduated cylinder.

All uptake rate adjustments should be performed while running an air/acetylene


flame. The nebulizer should never be adjusted while running a nitrous oxide/
acetylene flame.

Maintaining Optimum Metal Body Nebulizer Performance


To maintain optimum nebulizer performance, you must periodically clean the
nebulizer parts, and occasionally replace the capillary (sample) tubing. A pinhole
can develop in the capillary tubing which will greatly reduce the sample uptake
rate. See the figure on Figure 6-24. on page 240 for an exploded view of the
nebulizer. Since the needle assembly and the venturi come in direct contact with
the sample, these parts will need to be replaced over time.

Also, the nebulizer is only a part of the overall burner system.

For optimum burner-system performance, it is important to also periodically clean


the burner chamber, burner head, and the end cap. All o-rings must be checked on
a regular basis and replaced if sticky, flat, cut, or damaged in any way.

When aspirating concentrated samples with complex matrices, it is especially


important to keep the burner chamber and nebulizer free of sample deposits. In
addition to regular cleaning, it is beneficial to periodically aspirate a dilute
surfactant solution, such as 0.1% Triton X-100, for several minutes to keep the
system clean.

The surfactant solution will encourage constant drainage, which is required for
obtaining optimum burner system performance.
Metal Body Nebulizer with Organic Solvent Resistant O-Rings 247

Metal Body Nebulizer with Organic Solvent Resistant O-Rings


The nebulizer is an adjustable pneumatic device that is used to draw the sample into
the capillary tubing and spray it as a fine aerosol into the spray chamber. The
oxidant gas is routed through the oxidant tubing into the nebulizer through a
connecting passage in the burner assembly (spray chamber). The sample uptake
rate/sensitivity is optimized by adjusting the nebulizer.

The metal body nebulizer can be used for most solutions containing < 5 % acid. It
has excellent performance (precision and signal-to-noise ratio) and it is less prone
to clogging. The needle assembly and venturi can be changed to produce a
Platinum alloy and corrosion resistant version.

Removing the Metal Body Nebulizer


Remove the nebulizer using the following procedure:
1. Open up the Sample Introduction Compartment door to the burner chamber.

2. Pull out the nebulizer locking clamp back and carefully but firmly, rotate the
metal body side arm upwards 90 degrees to the unlock position.
248 Maintenance

Figure 6-26. Metal body nebulizer


Item Description
1 Nebulizer in locked position
2 Nebulizer metal body arm in locked position
3 Nebulizer in unlock position
4 Nebulizer metal body arm in up position
5 Nebulizer Interlock sensor
Metal Body Nebulizer with Organic Solvent Resistant O-Rings 249

3. Pull the nebulizer out from the nebulizer assembly end cap.

1 7
3 4 5 6 8 9 11
2

10

Figure 6-27. Exploded metal body nebulizer


Item Description Item Description
1 Fine adjustment nut 7 Nebulizer body (P/N N3160133)
(P/N 0301460)
2 Sample capillary (P/N 09908265) 8 Nebulizer body organic solvent resistant O-rings
(2) (P/N 09200276)
3 Teflon® washer (P/N 03031802) 9 Organic solvent resistant O-ring (P/N 09200273)

4 Needle valve (P/N N3160153) 10 Venturi (P/N 03031810)


5 Spring (P/N 03031806) 11 Cap (P/N N3161057)
6 Organic solvent resistant O-ring (P/
N 09200273)

The o-ring (Part No. 09200274) that is not in this figure seals the nebulizer to the
end cap.

Note Use Apiezon®-L grease. Make sure that no grease gets onto the tip of the
capillary. Use only the Apiezon grease supplied with the nebulizer. It is
metal-free.
250 Maintenance

4. Inspect all the o-rings. Replace any cracked or damaged o-rings. Apply a small
amount of Apiezon grease (Part No. 0300405) onto the o-rings (Part No.
09902015). The nebulizer will then slide easily into the end cap.

5. Inspect the needle valve and replace if needed.

6. For information on cleaning the nebulizer see Cleaning the Metal Body
Nebulizer with Organic Solvent Resistant O-Rings on page 252.

Reinstalling the PinAAcle 900 Metal Body Nebulizer with Organic


Solvent Resistant O-Rings
Install the PinAAcle metal body nebulizer using the following procedure:

1. Carefully reinstall the needle assembly by taking the beveled edge of the
needle assembly and insert it into the nebulizer in the 1 o'clock position to align
with the nebulizer gas port in the end cap. See the following figure.
Metal Body Nebulizer with Organic Solvent Resistant O-Rings 251

4
3

Figure 6-28. Close Up of the Needle Assembly


Item Description Item Description
1 Needle valve 3 Nebulizer body
2 Beveled edge of the hypodermic 4 Needle valve in 1 o’clock position
needle in the needle assembly

2. Apply a small amount of Apiezon grease (Part No. 0300405) onto the o-rings.
The nebulizer will then slide easily into the end cap and seal better.

3. Insert the re-assembled nebulizer into the end cap in the unlocked position.
252 Maintenance

4. Rotate the arm 90 degrees clockwise into the locked position.

5. Push the locking clamp all the way in to lock the nebulizer in place.

Note When the nebulizer is securely in place, the nebulizer interlock will be
depressed and you will be able to run the instrument. If the nebulizer
interlock is not depressed, the software will indicate that the safety
interlock is not satisfied. A checked off green box in the software will
indicate that the safety locks are engaged and the instrument will allow an
analysis to occur.

The metal body nebulizer reinstallation is complete.

Cleaning the Capillary Assembly


Clean the capillary assembly whenever you notice degradation in absorbance
values due to a blockage in the capillary. There are two ways to clean the capillary
assembly:

• The first (simplified) way should be used if the nebulizer capillary


assembly is not difficult to clear. This method involves simply passing one
of the cleaning wires, supplied, through the capillary assembly.

• The second (complete) procedure requires shutting down the spectrometer,


removing the nebulizer from the end cap, removing the capillary tubing,
cleaning the capillary assembly and replacing the capillary tubing. This
procedure must be performed if you have no success with the first method.

Cleaning the Metal Body Nebulizer with Organic Solvent Resistant O-


Rings
A low or erratic absorbance reading may indicate that the burner head, burner
chamber, or the nebulizer and capillary tubing require cleaning. If you find that the
burner chamber and burner head is clean, the problem is probably due to an
obstruction in the nebulizer or capillary tubing.

To clear an obstruction in the nebulizer:


Metal Body Nebulizer with Organic Solvent Resistant O-Rings 253

1. Aspirate pure solvent with the flame on until the absorbance reading is
satisfactory for a standard.

2. If you cannot obtain a satisfactory absorbance, try to clear the obstruction by


pushing the copper cleaning wire through the capillary and into the nebulizer.
Move the wire in and out to dislodge any solid particles.

Caution Use only the copper cleaning wire provided with the nebulizer to clean the
capillary. Other wire may be burred and can damage the nebulizer.

3. If deposits cannot be removed using these measures, remove the nebulizer so


you can disassemble and clean it.

Cleaning the Nebulizer with Organic Solvent Resistant O-Rings


To clean a stubborn blockage from the nebulizer, perform the procedure below.

Wear protective gloves when you remove the nebulizer from the end cap
! if you were analyzing toxic samples.
Warning

1. Turn off the spectrometer and turn off all gas supplies.

2. Push the end-cap spring clamp and rotate the nebulizer counter clockwise to
unlock and gently pull the nebulizer out of the burner end cap.

3. After you have taken the nebulizer apart, clean the components as follows:

4. Clean the capillary assembly using a mild laboratory detergent solution, or a


solvent such as isopropanol, preferably in an ultrasonic bath.

5. Clean the nebulizer body and any other parts that appear dirty in a mild
laboratory detergent solution, or a solvent such as isopropanol, preferably in an
ultrasonic bath.
254 Maintenance

6. Rinse all the cleaned components thoroughly with deionized water. If the
venturi or the tip of the needle assembly looks worn, then that part should be
replaced.

7. Inspect the all o-rings on the nebulizer body and clean them if necessary in
mild laboratory detergent solution, followed by a thorough rinsing with
deionized water followed by isopropanol and dry. If they look damaged,
replace them.

After you have cleaned the components, reassemble the nebulizer.

Adjusting the PinAAcle 900 Metal Body Nebulizer for Maximum


Absorbance
Adjust the nebulizer to achieve maximum absorbance as follows:

1. Ignite the flame. Refer to the procedure for igniting the flame in Igniting the
Flame on page 182.

2. Set up the spectrometer for the determination of copper, magnesium, or


another element which has an absorbing wavelength above 250 nm and whose
sensitivity is not dependent on the fuel/oxidant ratio. Do not select an element
requiring a nitrous oxide-acetylene flame, as the nebulizer should never be
adjusted when a nitrous oxide-acetylene flame is lit.

3. Use the Align Burner Wizard in the Flame Control Window to optimize the
burner position. After the flame is turned on, autozero on a blank. Then aspirate
a standard and make sure the solution is being aspirated by the nebulizer so
there will be an absorbance with which the horizontal and rotational positions
can be optimized. If necessary, adjust the burner height.

4. The height for the air-acetylene flame is not as critical as in the nitrous oxide-
acetylene flame where the sensitivity can vary a lot.

5. While aspirating the standard, turn the nebulizer locking ring clockwise until
it is free of the nebulizer adjustment nut.

6. Slowly turn the nebulizer adjustment nut counterclockwise until bubbles begin
to appear at the end of the needle assembly tube in the sample solution.
Metal Body Nebulizer with Organic Solvent Resistant O-Rings 255

7. Slowly turn the nebulizer adjustment nut clockwise until the absorbance goes
to a maximum and then begins to decrease. Go back to the maximum position.

8. Lock the nebulizer adjustment nut in its current (optimum) position by turning
the nebulizer locking ring counter-clockwise while carefully holding the
nebulizer adjustment nut.

9. Check the characteristic concentration as instructed in your spectrometer


manuals. This characteristic concentration should normally be within ±20% of
the value listed in the Analytical Methods for AA Spectroscopy (P/N
03030152).

Using Organic Solvents


It is often beneficial to lower the nebulizer uptake rate when aspirating organic
solvents. The normal nebulizer update rate for aqueous solutions is typically 6-8
mL/min.

Caution When an organic solvent is aspirated, the flame will become richer. The
uptake rate should be reduced to obtain a moderately lean flame. The
organic solvent is a fuel and it will act as a fuel. If needed, the fuel flow
can also be reduced while the solvent is being aspirated. The fuel flow
must be increased before the sample capillary is removed from the solvent
for any length of time, or the flame will be too lean, which will cause a
flashback.

Depending on the type of organic solvent aspirated, reducing the uptake rate to 1-
3 mL/min, will minimize how rich the flame will become. This leaner flame
typically provides improved precision, particularly when aspirating a commonly
used solvent such as xylene.

The organic solvent is also a fuel and can act as a fuel just as acetylene.

To adjust the nebulizer uptake rate, unlock the nebulizer locking nut and rotate the
nebulizer adjustment nut until you locate a position which provides reduced sample
uptake. Then lock the nebulizer locking nut.
256 Maintenance

Note The uptake rate is easily measured by using a graduated cylinder.

All uptake rate adjustments should be performed while running an air/acetylene


flame. The nebulizer should never be adjusted while running a nitrous oxide/
acetylene flame.

Maintaining Optimum PinAAcle 900 Metal Body Nebulizer


Performance
To maintain optimum nebulizer performance, you must periodically clean the
nebulizer parts, and occasionally replace the capillary (sample) tubing. A pinhole
can develop in the capillary tubing which will greatly reduce the sample uptake
rate. See Figure 6-27. on page 249 for an exploded view of the nebulizer. Since the
needle assembly and the venturi come in direct contact with the sample, these parts
will need to be replaced over time.

Also, the nebulizer is only a part of the overall burner system. For optimum burner-
system performance, it is important to also periodically clean the burner chamber,
burner head, and the end cap. All o-rings must be checked on a regular basis and
replaced if sticky, flat, cut, or damaged in any way.

When aspirating concentrated samples with complex matrices, it is especially


important to keep the burner chamber and nebulizer free of sample deposits. In
addition to regular cleaning, it is beneficial to periodically aspirate a dilute
surfactant solution, such as 0.1% Triton X-100, for several minutes to keep the
system clean.

The surfactant solution will encourage constant drainage, which is required for
obtaining optimum burner system performance.
High Sensitivity Plastic Nebulizer 257

High Sensitivity Plastic Nebulizer


The high sensitivity plastic nebulizer (Part No. N3160112) is an adjustable
pneumatic device that is used to draw the sample into the needle assembly tubing
and spray it as a fine aerosol into the spray chamber. The oxidant gas is routed
through the oxidant tubing into the nebulizer through a connecting passage in the
burner assembly (spray chamber). The sample uptake rate/sensitivity is optimized
by adjusting the nebulizer.

The plastic high sensitivity plastic nebulizer provides exceptional sensitivity,


precision and corrosion resistance and can be used to aspirate almost all solutions,
even those solutions containing a high percentage of acids.

Note If you are running an aqua regia solution, you will need to use a tantalum
needle assembly kit (Part No. N3160136) with this nebulizer.

Removing the High Sensitivity Plastic Nebulizer


Remove the nebulizer using the following procedure:
1. Open up the Sample Introduction Compartment door to the burner chamber.
2. Pull back the locking clamp and rotate the plastic arm to the unlock position.
3. Grasp the plastic arm from the locked position and firmly rotate it up (the arm
will be tightly in place).
258 Maintenance

2 1

3
4

6
7
5
8
9

Figure 6-29. Plastic nebulizer


Item Description Item Description
1 Nebulizer in locked position 5 Nebulizer in unlocked position
2 Nebulizer assembly end cap 6 Nebulizer plastic arm in up (unlocked)
position
3 Nebulizer plastic arm in lock position 7 Nebulizer interlock sensor
4 Locking clamp 8-9 Latch

4. Wiggle the nebulizer out from the nebulizer assembly end cap.
High Sensitivity Plastic Nebulizer 259

5. The nebulizer assembly end cap is secured to the burner chamber by the levers
located on each side. Pull both levers back to remove the nebulizer assembly
end cap from the burner chamber.
6. Inspect the o-rings in the nebulizer assembly end cap. Replace any cracked or
damaged o-rings.

1
2 4
5
3

Figure 6-30. Plastic nebulizer assembly end cap 0-rings


Item Description Item Description
1 Nebulizer assembly end cap 2-6 O-rings

7. Take apart the nebulizer.


260 Maintenance

7 4
6 5

8 3 2

Figure 6-31. Exploded plastic nebulizer


Item Description Item Description
1 Nebulizer Assembly End Cap 6 Needle Assembly(P/N B3150525) with spring
(P/N N316 0111)
2 Impact Bead (P/N B3150457) 7 Knurled Needle assembly Adjustment Nut (P/N
B3150462)
3 Spacer (P/N B3150531) 8 Sample Tubing (P/N B3150458)
4 Nebulizer Body (P/N B3161049) 9 Apiezon Grease (P/N 03030405)
5 Locking Ring (P/N B3161205)
High Sensitivity Plastic Nebulizer 261

Note Use Apiezon®-L grease. Make sure that no grease gets onto the tip of the
capillary. Use only the Apiezon grease supplied with the nebulizer. It is
metal-free.

Note Located on the spring are two o-rings, one larger and one very small one.
The small o-ring can be lost very easily if the Apiezon®-L grease is not
applied on the needle valve.

8. Inspect all the o-rings. Replace any cracked or damaged o-rings. Apply a small
amount of Apiezon grease (Part No. 0300405) onto the o-rings (Part No.
09902015). The nebulizer will then slide easily into the end cap.

9. Inspect the needle valve and replace if needed.

10. For information on cleaning the nebulizer see Cleaning the High Sensitivity
Plastic Nebulizer on page 262.

Reinstalling the High Sensitivity Plastic Nebulizer

Note If not already done, inspect the tiny o-ring on the capillary assembly for
damage and replace them if necessary. Lightly lubricate the surface of the
o-rings with a minimum of Apiezon grease. Make sure that no grease gets
onto the tip of the capillary.

1. Slide the spring back onto the needle assembly (if it was removed).

2. Slide the assembled needle assembly into the nebulizer body.

3. Line up the alignment key with the keyway in the nebulizer body.

4. Push the needle assembly in until it bottoms out in the nebulizer body.
262 Maintenance

5. If you inserted the needle assembly correctly, it should move freely in and out
of the nebulizer body. If it does not, remove and reinstall, paying particular
attention to the alignment key.

6. Screw the adjusting nut onto the nebulizer body.

7. Refit the spacer (if applicable) and the fragile impact bead onto the plastic
nebulizer.

8. Reattach the nebulizer sample tube to the nebulizer by screwing the connector
into the nebulizer body.

9. Reinstall the nebulizer in the end cap

Note When the nebulizer is securely in place, the nebulizer interlock will be
depressed and you will be able to run the instrument. If the nebulizer
interlock is not depressed, the software will indicate that the safety lock is
not satisfied.
A checked off green box in the software will indicate that the safety locks
are engaged and the instrument can be run.

The high sensitivity plastic nebulizer reinstallation is complete.

Cleaning the High Sensitivity Plastic Nebulizer

Cleaning the Needle Assembly


Clean the needle assembly whenever you notice degradation in absorbance values
due to blockage of the needle assembly. There are two ways to clean the needle
assembly holder:

• The first (simplified) way should be used if the blockage is not difficult to
clear. This method involves simply passing one of the cleaning wires,
supplied, through the sample capillary tubing and the needle assembly,
while they are still attached to the nebulizer body.

• The second procedure requires removing the needle assembly from the
nebulizer body before inserting the cleaning wire. This procedure must be
performed if you have no success with the first method.
High Sensitivity Plastic Nebulizer 263

Simplified Cleaning Procedure for the PinAAcle 900 Series High


Sensitivity Plastic Nebulizer
For a simplified (light) cleaning of a standard the nebulizer needle assembly
holder, see the following procedure:

1. Remove the impact bead.

Note It may take several attempts to pass the wire through the nebulizer.

2. Take one of the cleaning wires supplied, and then push it through the needle
assembly holder from its wider (open) end.

3. Repeat step 2 several times. Then replace the impact bead and sample tubing.

4. Run several standards to determine if the needle assembly holder had been
cleared. If it has been cleared, proceed with normal spectrometer operation:
otherwise, see the next procedure.

Complete Cleaning Procedure of High Sensitivity Plastic Nebulizer


To clean a stubborn blockage from the nebulizer, perform the procedure below.

Wear protective gloves when you remove the nebulizer from the end cap
! if you were analyzing toxic samples.
Warning

Removal and Disassembly

Caution Make sure that the flame is turned off before proceeding.

1. Pull back the locking ring that secures the nebulizer in place.

2. Rotate the nebulizer body counter clockwise so the locking arms are not in the
locked position. Gently pull the nebulizer out of the burner end cap.
264 Maintenance

3. Remove the impact bead and if using the impact bead spacer, remove the
spacer as well. Handle with care. (See the instructions on Removing and
Replacing the Nebulizer's Impact Bead on page 264.)

4. Unscrew the sample tubing.

5. Refer to Figure 6-31. on page 260. Loosen and remove the adjustment nut.

6. Remove the needle assembly from the nebulizer body assembly.

Cleaning

Note It may take several attempts to pass the wire through the nebulizer.

1. While holding the needle assembly in one hand, take one of the cleaning wires
supplied.

2. Push it through the needle assembly from its wider (open) end.

3. If needed, the needle assembly can be cleaned with a detergent solution or mild
solvent. An ultrasonic bath can also be used.

Removing and Replacing the Nebulizer's Impact Bead


The PinAAcle 900 Series high sensitivity plastic nebulizer utilizes a ceramic, one-
piece, impact-bead structure which improves the nebulization efficiency. The
nebulizer should never be used without the impact bead. The bead itself is held by
two fragile support arms.

The bead structure mounts directly on the nebulizer's body assembly, see the
following figure.
High Sensitivity Plastic Nebulizer 265

1 3

Figure 6-32. Installing Spacer onto the Nebulizer


Item Description Item Description
1 Locking Ring 4 Spacer
2 Locking Arm 5 Impact Bead
3 Nebulizer Body

To Install Impact Bead


1. Hold the impact bead by its base and carefully push it onto the body of the
nebulizer in front of the venturi.

2. Then rotate it, holding only the base, approximately 1/8 turn until it reaches a
stop.
266 Maintenance

To Remove Impact Bead


1. Hold the impact bead by its base only.

2. Rotate it approximately 1/8 turn counterclockwise before carefully lifting it


from the nebulizer's body assembly.

Installing the Spacer


The addition of the spacer reduces the amount of sample delivered to the flame.

The high sensitivity plastic nebulizer assembly can be used with or without the
spacer when using the 10-cm burner head. Maximum sensitivity for Air-Acetylene
elements can be achieved without the use of the spacer.

The spacer is recommended for all nitrous oxide/acetylene elements, and for air/
acetylene elements that are flame sensitive, such as calcium, and chromium. When
analyzing some complex sample matrices, it may be desirable to add the spacer to
reduce chemical interferences. This nebulizer's sensitivity and linearity will be
similar to the metal body nebulizer when the spacer is installed.

To Install the Spacer


1. Hold the impact bead by its base only.

2. Carefully remove the impact bead by rotating it 1/8 turn and then pull the
impact bead off.

3. Place the spacer onto the back of the nebulizer and replace the impact bead.

4. Rotate the bead 1/8 turn to "lock" the bead in place.


High Sensitivity Plastic Nebulizer 267

Adjusting the PinAAcle 900 Series High Sensitivity Plastic Nebulizer


for Maximum Absorbance
Adjust the nebulizer to achieve maximum absorbance as follows:

1. Ignite the flame. Refer to the procedure for igniting the flame in Igniting the
Flame on page 182.

2. Set up the spectrometer for the determination of copper, magnesium, or


another element which has an absorbing wavelength above 250 nm and whose
sensitivity is not dependent on the fuel/oxidant ratio. Do not select an element
requiring a nitrous oxide-acetylene flame, as the nebulizer should never be
adjusted when a nitrous oxide-acetylene flame is lit.

3. Use the Align Burner Wizard in the Flame Control Window to optimize the
burner position. After the flame is turned on, autozero on a blank. Then aspirate
a standard and make sure the solution is being aspirated by the nebulizer so
there will be an absorbance with which the horizontal and rotational positions
can be optimized. If necessary, adjust the burner height.

4. The height for the air-acetylene flame is not as critical as in the nitrous oxide-
acetylene flame where the sensitivity can vary a lot.

5. While aspirating the standard, turn the nebulizer locking ring clockwise until
it is free of the nebulizer adjustment nut.

6. Slowly turn the nebulizer adjustment nut counterclockwise until bubbles begin
to appear at the end of the needle assembly tube in the sample solution.

7. Slowly turn the nebulizer adjustment nut clockwise until the absorbance goes
to a maximum and then begins to decrease. Go back to the maximum position.

8. Lock the nebulizer adjustment nut in its current (optimum) position by turning
the nebulizer locking ring counter-clockwise while carefully holding the
nebulizer adjustment nut.

9. Check the characteristic concentration as instructed in your spectrometer


manuals. This characteristic concentration should normally be within ±20% of
the value listed in the Analytical Methods for AA Spectroscopy (Part No.
03030152).
268 Maintenance

Using Organic Solvents


It is often beneficial to lower the nebulizer uptake rate when aspirating organic
solvents. The normal nebulizer update rate for aqueous solutions is typically 6-10
mL/min. The metal body nebulizer has the lowest uptake rate, followed by high
sensitivity plastic nebulizer with the spacer, and high sensitivity plastic nebulizer
without the spacer.

Caution When an organic solvent is aspirated, the flame will become richer. The
uptake rate should be reduced to obtain a moderately lean flame. If
needed, the fuel flow can also be reduced while the solvent is being
aspirated. The fuel flow must be increased before the sample tubing is
removed from the solvent for any length of time, or the flame will be too
lean, which will cause a flashback.

Depending on the type of organic solvent aspirated, reducing the uptake rate to 1-
3 mL/min, will minimize how rich the flame will become. This leaner flame
typically provides improved precision, particularly when aspirating a commonly
used solvent such as xylene.

To adjust the nebulizer uptake rate, unlock the nebulizer locking ring and rotate the
nebulizer adjustment nut until you locate a position which provides reduced sample
uptake. Then lock the nebulizer locking ring.

Note The uptake rate is easily measured by using a graduated cylinder.

All uptake rate adjustments should be performed while running an air/acetylene


flame. The nebulizer should never be adjusted while running a nitrous oxide/
acetylene flame.
High Sensitivity Plastic Nebulizer with Chemical Resistant O-Rings 269

Maintaining Optimum High Sensitivity Plastic Nebulizer Performance


To maintain optimum nebulizer performance, you must periodically clean the
needle assembly, and occasionally replace the needle assembly sample tubing. See
Figure 6-31. on page 260 for an exploded view of the nebulizer.

Also, the nebulizer is only a part of the overall burner system. For optimum burner-
system performance, it is important to periodically clean the nebulizer, burner
chamber, burner hed, and the end cap.

When aspirating concentrated samples with complex matrices, it is especially


important to keep the burner chamber and nebulizer free of sample deposits. In
addition to regular cleaning, it is beneficial to periodically aspirate a dilute
surfactant solution, such as 0.1% Triton X-100, for several minutes to keep the
system clean.

The surfactant solution will encourage constant drainage, which is required for
obtaining optimum burner system performance.

When using the PinAAcle 900 Series high sensitivity plastic nebulizer, the impact
bead may have to be replaced. Also, to avoid damage to the impact bead, the bead
should be removed when cleaning the needle assembly. Steps for removing and
replacing the bead are included in this instruction document.

High Sensitivity Plastic Nebulizer with Chemical Resistant O-


Rings
The high sensitivity plastic nebulizer (Part No. N3160187) is an adjustable
pneumatic device that is used to draw the sample into the needle assembly tubing
and spray it as a fine aerosol into the spray chamber. The oxidant gas is routed
through the oxidant tubing into the nebulizer through a connecting passage in the
burner assembly (spray chamber). The sample uptake rate/sensitivity is optimized
by adjusting the nebulizer.

The high sensitivity plastic nebulizer provides exceptional sensitivity, precision


and corrosion resistance and can be used to aspirate almost all solutions, even those
solutions containing a high percentage of acids.
270 Maintenance

Note If you are running an aqua regia solution, you will need to use a tantalum
needle assembly kit (Part No. N3160137) with this nebulizer.

Removing the High Sensitivity Plastic Nebulizer with Chemical


Resistant O-Rings
Remove the nebulizer using the following procedure:
1. Open up the Sample Introduction Compartment door to the burner chamber.
2. Pull back the locking clamp and rotate the plastic arm to the unlock position.
3. Grasp the plastic arm from the locked position and firmly rotate it up (the arm
will be tightly in place).
High Sensitivity Plastic Nebulizer with Chemical Resistant O-Rings 271

2 1

3
4

6
7
5 8
9

Figure 6-33. Plastic nebulizer


Item Description Item Description
1 Nebulizer in locked position 5 Nebulizer in unlocked position
2 Nebulizer assembly end cap 6 Nebulizer plastic arm in up (unlocked)
position
3 Nebulizer plastic arm in lock position 7 Nebulizer interlock sensor
4 Locking clamp 8-9 Latch

4. Wiggle the nebulizer out from the nebulizer assembly end cap.
272 Maintenance

5. The nebulizer assembly end cap is secured to the burner chamber by the levers
located on each side. Pull both levers back to remove the nebulizer assembly
end cap from the burner chamber.
6. Inspect the o-rings in the nebulizer assembly end cap. Replace any cracked or
damaged o-rings.

1
2 4
5
3

Figure 6-34. Plastic nebulizer assembly end cap 0-rings


Item Description Item Description
1 Nebulizer assembly end cap 2-6 O-rings
High Sensitivity Plastic Nebulizer with Chemical Resistant O-Rings 273

7. Take apart the nebulizer.

6
9

7
5
3
1

Figure 6-35. Exploded View of the Nebulizer


Item Description Item Description
1 Nebulizer Assembly End Cap (P/N 6 Needle Assembly
N3160189) (P/N N3160154) with spring
-comes with 4x Chemical Resistance O-Ring
(P/N 09200275) and 1X Chemical
Resistance O-Ring (P/N 09200277)
2 Impact Bead (P/N B3150457) 7 Knurled Needle assembly
Adjustment Nut
(P/N B3150462)
274 Maintenance

Item Description Item Description


3 Spacer (P/N B3150531) 8 Sample Tubing
(P/N B3150458)
4 Nebulizer Body (P/N N3161049) 9 Apiezon Grease
(P/N 03030405)
5 Locking Ring (P/N N3151205)

Note Use Apiezon®-L grease. Make sure that no grease gets onto the tip of the
needle assembly. Use only the Apiezon grease supplied with the nebulizer.
It is metal-free.

1. Apply a small amount of Apiezon grease onto the o-rings. The nebulizer will
then slide easily into the end cap when you perform steps 2 and 3, below.

2. Insert the nebulizer into the end cap in the unlocked position.

Caution Use care installing the nebulizer as the impact bead is quite fragile.

3. Rotate the arm 90 degrees clockwise into the locked position.

4. Push the locking clamp all the way in to lock the nebulizer in place.

Note When the nebulizer is securely in place, the nebulizer interlock will be
depressed and you will be able to run the instrument. If the nebulizer
interlock is not depressed, the software will indicate that the safety
interlock is not satisfied. A checked off green box in the software will
indicate that the safety locks are engaged and the instrument will allow an
analysis to occur.

The nebulizer installation is complete.


High Sensitivity Plastic Nebulizer with Chemical Resistant O-Rings 275

Cleaning the High Sensitivity Plastic Nebulizer with Chemical


Resistant O-Rings

Cleaning the Needle Assembly


Clean the needle assembly whenever you notice degradation in absorbance values
due to blockage of the needle assembly. There are two ways to clean the needle
assembly holder:

• The first (simplified) way should be used if the blockage is not difficult to
clear. This method involves simply passing one of the cleaning wires,
supplied, through the sample capillary tubing and the needle assembly,
while they are still attached to the nebulizer body.

• The second procedure requires removing the needle assembly from the
nebulizer body before inserting the cleaning wire. This procedure must be
performed if you have no success with the first method.

Simplified Cleaning Procedure for the PinAAcle 900 Series High


Sensitivity Plastic Nebulizer with Chemical Resistant O-Rings
For a simplified (light) cleaning of a standard the nebulizer needle assembly
holder, see the following procedure:

1. Remove the impact bead.

Note It may take several attempts to pass the wire through the nebulizer.

2. Take one of the cleaning wires supplied, and then push it through the needle
assembly holder from its wider (open) end.

3. Repeat step 2 several times. Then replace the impact bead and sample tubing.

4. Run several standards to determine if the needle assembly holder had been
cleared. If it has been cleared, proceed with normal spectrometer operation:
otherwise, see the next procedure.
276 Maintenance

Complete Cleaning Procedure of PinAAcle 900 Series High Sensitivity


Plastic Nebulizer with Chemical Resistant O-Rings
To clean a stubborn blockage from the nebulizer, perform the procedure below.

Wear protective gloves when you remove the nebulizer from the end cap
! if you were analyzing toxic samples.
Warning

Removal and Disassembly

Caution Make sure that the flame is turned off before proceeding.

1. Pull back the locking ring that secures the nebulizer in place.
2. Rotate the nebulizer body counter clockwise so the locking arms are not in the
locked position. Gently pull the nebulizer out of the burner end cap.
3. Remove the impact bead and if using the impact bead spacer, remove the
spacer as well. Handle with care. (See the instructions on Removing and
Replacing the Nebulizer's Impact Bead on page 277.)
4. Unscrew the sample tubing.
5. Refer to Figure 6-35. on page 273. Loosen and remove the adjustment nut.
6. Remove the needle assembly from the nebulizer body assembly.

Cleaning

Note It may take several attempts to pass the wire through the nebulizer.

1. While holding the needle assembly in one hand, take one of the cleaning wires
supplied.
2. Push it through the needle assembly from its wider (open) end.

3. If needed, the needle assembly can be cleaned with a detergent solution or mild
solvent. An ultrasonic bath can also be used
Removing and Replacing the Nebulizer's Impact Bead 277

Removing and Replacing the Nebulizer's Impact Bead


The PinAAcle 900 Series high sensitivity plastic nebulizer utilizes a ceramic, one-
piece, impact-bead structure which improves the nebulization efficiency. The
nebulizer should never be used without the impact bead. The bead itself is held by
two fragile support arms.

The bead structure mounts directly on the nebulizer's body assembly, see the
following figure.

1
3
4

5
2

Figure 6-36. Installing Spacer onto the Nebulizer


Item Description Item Description
1 Locking Ring 4 Spacer
2 Locking Arm 5 Impact Bead
3 Nebulizer Body

To Install Impact Bead


1. Hold the impact bead by its base and carefully push it onto the body of the
nebulizer in front of the venturi.
278 Maintenance

2. Then rotate it, holding only the base, approximately 1/8 turn until it reaches a
stop.

To Remove Impact Bead


1. Hold the impact bead by its base only.

2. Rotate it approximately 1/8 turn counterclockwise before carefully lifting it


from the nebulizer's body assembly.

Installing the Spacer


The addition of the spacer reduces the amount of sample delivered to the flame.

The high sensitivity plastic nebulizer assembly can be used with or without the
spacer when using the 10-cm burner head. Maximum sensitivity for Air-Acetylene
elements can be achieved without the use of the spacer.

The spacer is recommended for all nitrous oxide/acetylene elements, and for air/
acetylene elements that are flame sensitive, such as calcium, and chromium. When
analyzing some complex sample matrices, it may be desirable to add the spacer to
reduce chemical interferences. This nebulizer's sensitivity and linearity will be
similar to the metal body nebulizer when the spacer is installed.

To Install the Spacer


1. Hold the impact bead by its base only.

2. Carefully remove the impact bead by rotating it 1/8 turn and then pull the
impact bead off.

3. Place the spacer onto the back of the nebulizer and replace the impact bead.

4. Rotate the bead 1/8 turn to "lock" the bead in place.


Reassembling the Nebulizer 279

Reassembling the Nebulizer

Note If not already done, inspect all the o-rings on the needle assembly and the
body of the nebulizer for damage and replace them if necessary. Lightly
lubricate the surface of the o-rings with a minimum of supplied Apiezon®-
L grease. Do not use Apiezon grease of unknown source and quality as it
may contain trace metals. Make sure that no grease gets onto the tip of the
needle assembly.

1. Slide the spring back onto the needle assembly (if it was removed).

2. Slide the assembled needle assembly into the nebulizer body.

3. Line up the alignment key with the keyway in the nebulizer body.

4. Push the needle assembly in until it bottoms out in the nebulizer body.

5. If you inserted the needle assembly correctly, it should move freely in and out
of the nebulizer body. If it does not, remove and reinstall, paying particular
attention to the alignment key.

6. Screw the adjusting nut onto the nebulizer body.

7. Refit the spacer (if applicable) and the fragile impact bead onto the plastic
nebulizer.

8. Reattach the nebulizer sample tube to the nebulizer by screwing the connector
into the nebulizer body.

9. Reinstall the nebulizer in the end cap

Note When the nebulizer is securely in place, the nebulizer interlock will be
depressed and you will be able to run the instrument. If the nebulizer
interlock is not depressed, the software will indicate that the safety lock is
not satisfied.

A checked off the green box in the software will indicate that the safety locks are
engaged and the instrument can be run.
280 Maintenance

Adjusting the PinAAcle 900 Series High Sensitivity Plastic Nebulizer


with Chemical Resistant O-Rings for Maximum Absorbance
Adjust the nebulizer to achieve maximum absorbance as follows:

1. Ignite the flame. Refer to the procedure for igniting the flame in Igniting the
Flame on page 182.

2. Set up the spectrometer for the determination of copper, magnesium, or


another element which has an absorbing wavelength above 250 nm and whose
sensitivity is not dependent on the fuel/oxidant ratio. Do not select an element
requiring a nitrous oxide-acetylene flame, as the nebulizer should never be
adjusted when a nitrous oxide-acetylene flame is lit. The height for the air-
acetylene flame is not as critical as in the nitrous oxide-acetylene flame where
the sensitivity can vary a lot.

3. Use the Align Burner wizard in the Flame Control window to optimize the
burner position. After the flame is turned on, autozero on a blank. Then aspirate
a standard and make sure the solution is being aspirated by the nebulizer so
there will be an absorbance with which the horizontal and rotational positions
can be optimized. If necessary, adjust the burner height.

4. The height for the air-acetylene flame is not as critical as in the nitrous oxide-
acetylene flame where the sensitivity can vary a lot.

5. While aspirating the standard, turn the nebulizer locking ring clockwise until
it is free of the nebulizer adjustment nut.

6. Slowly turn the nebulizer adjustment nut counterclockwise until bubbles begin
to appear at the end of the needle assembly tube in the sample solution.

7. Slowly turn the nebulizer adjustment nut clockwise until the absorbance goes
to a maximum and then begins to decrease. Go back to the maximum position.

8. Lock the nebulizer adjustment nut in its current (optimum) position by turning
the nebulizer locking ring counter-clockwise while carefully holding the
nebulizer adjustment nut.

9. Check the characteristic concentration as instructed in your spectrometer


manuals. This characteristic concentration should normally be within ±20% of
the value listed in the Analytical Methods for AA Spectroscopy (Part No.
03030152).
Reassembling the Nebulizer 281

Using Organic Solvents


It is often beneficial to lower the nebulizer uptake rate when aspirating organic
solvents. The normal nebulizer update rate for aqueous solutions is typically 6-10
mL/min. The metal body nebulizer has the lowest uptake rate, followed by high
sensitivity plastic nebulizer with the spacer, and high sensitivity plastic nebulizer
without the spacer.

Caution When an organic solvent is aspirated, the flame will become richer. The
uptake rate should be reduced to obtain a moderately lean flame. If
needed, the fuel flow can also be reduced while the solvent is being
aspirated. The fuel flow must be increased before the sample tubing is
removed from the solvent for any length of time, or the flame will be too
lean, which will cause a flashback.

Depending on the type of organic solvent aspirated, reducing the uptake rate to 1-
3 mL/min, will minimize how rich the flame will become. This leaner flame
typically provides improved precision, particularly when aspirating a commonly
used solvent such as xylene.

To adjust the nebulizer uptake rate, unlock the nebulizer locking ring and rotate the
nebulizer adjustment nut until you locate a position which provides reduced sample
uptake. Then lock the nebulizer locking ring.

Note The uptake rate is easily measured by using a graduated cylinder.

All uptake rate adjustments should be performed while running an air/acetylene


flame. The nebulizer should never be adjusted while running a nitrous oxide/
acetylene flame.
282 Maintenance

Maintaining Optimum High Sensitivity Plastic Nebulizer with Chemical


Resistant O-Rings Performance
To maintain optimum nebulizer performance, you must periodically clean the
needle assembly, and occasionally replace the needle assembly sample tubing. See
Figure 6-35. on page 273 for an exploded view of the nebulizer.

Also, the nebulizer is only a part of the overall burner system. For optimum burner-
system performance, it is important to periodically clean the nebulizer, burner
chamber, burner head, and the end cap.

When aspirating concentrated samples with complex matrices, it is especially


important to keep the burner chamber and nebulizer free of sample deposits. In
addition to regular cleaning, it is beneficial to periodically aspirate a dilute
surfactant solution, such as 0.1% Triton X-100, for several minutes to keep the
system clean.

The surfactant solution will encourage constant drainage, which is required for
obtaining optimum burner system performance.

When using the PinAAcle 900 Series high sensitivity plastic nebulizer, the impact
bead may have to be replaced. Also, to avoid damage to the impact bead, the bead
should be removed when cleaning the needle assembly. Steps for removing and
replacing the bead are included in this instruction document.

Replacing Parts of Wear

Burner System O-Rings


Check the large o-ring in the neck of the burner chamber, the four small o-rings and
one large o-ring in the end cap. You must check the condition of these o-rings at
regular intervals and replace them if they are damaged or show signs of
deterioration.
Replacing Parts of Wear 283

Warning: Flammable Gases - Fire and Explosion Hazard


! If the o-rings in the burner system are damaged or have deteriorated, they
may no longer form a proper seal. This may result in a gas leak which is
Warning a serious fire hazard.
Check the condition of the o-rings regularly and replace them if they are
damaged or show signs of deterioration.

1. Take the burner system apart.

2. Inspect the large o-ring located in the neck of the burner chamber. Carefully
lever the o-ring out of the neck of the burner chamber using a plastic pipette tip
or the like.

Note Never use sharp or pointed tools to remove the o-ring. Examine the o-ring.
If it is damaged, replace it.

3. Place the large o-ring back into the neck of the burner chamber and press it
down with your finger.

4. Inspect the four smaller o-rings and the large o-ring located in the burner end
cap. Very carefully pry them out and inspect the o-rings for nicks, cuts and
deterioration . Replace the o-rings as needed.

5. Examine the o-rings. If they are damaged, replace them.

6. Gently place the o-rings back into the end cap and then press them into place
with your finger.

7. Reassemble the burner system.


284 Maintenance

Nebulizer O-Rings
There are o-rings on the nebulizer. Always carefully check the condition of these
o-rings whenever you take the nebulizer apart.

Maintaining the Acetylene Supply

Warning: Acetylene - Explosion Hazard


! Acetylene can decompose explosively at pressures higher than 103 kPa /
1.03 bar / 15 psig. Always make sure that the acetylene outlet gauge
Warning pressure is below this value.

• Depressurize both the fuel and oxidant gas hoses at the end of the working day
or if you are not going to use the instrument for an extended period. Close the
cylinder valves to avoid the possibility of gas hoses being subjected to the full
cylinder pressure in the event that a pressure regulator should fail.

• Acetylene is supplied dissolved in a solvent such as acetone, and a small


amount of solvent carryover with the acetylene is normal. However, as tank
pressure falls, the relative amount of solvent entering the gas stream increases
and can give erratic results, particularly for elements such as calcium, tin,
chromium, molybdenum and others whose sensitivity is highly dependent on
the fuel: oxidant ratio. The pressure drop is not linear with gas removal since
the acetylene is dissolved in a solvent, and a pressure of 600 kPa (6 bar; 85
psig) at ambient temperature indicates that the cylinder is nearly empty. For
this reason, replace acetylene cylinders when the cylinder pressure drops to
about 600 kPa (6 bar, 85 psig).

• Always store and use acetylene cylinders vertically, rather than horizontally,
to prevent liquid acetone from reaching the cylinder valve.

• The practice of "cracking the valve" of an acetylene tank (that is, opening the
valve slightly for a very short period previous to attaching the regulator) is not
recommended. While such an action will clear the valve opening of dust or dirt
particles and may remove acetone from the cylinder valve, it is a potentially
hazardous practice and one which should never be attempted in the presence of
an open flame, sparks or other possible sources of ignition.
Lamp Maintenance and Cleaning 285

Lamp Maintenance and Cleaning


There are really no maintenance procedures for any of the PerkinElmer lamps. If
you notice fingerprints on the "window" of your lamp, wipe them off with a soft,
dry, lint free cloth. Do not use chemicals or water. See the section below regarding
lamp life and when to replace them.

Lamp Life
Both hollow cathode and electrodeless discharge lamps have a finite lifetime.
Electrodeless discharge lamps typically last longer than hollow cathode lamps for
the same element. If, while aligning a lamp, you are not able to obtain a satisfactory
energy value, this may indicate that the lamp is starting to deteriorate. As a hollow
cathode lamp reaches the end of its useful life, the current on the lamp may be
increased up to the maximum current recommended on the label. Once the
intensity of a lamp begins to deteriorate, it should be replaced. The Lumina lamps
comes with an electronic means of monitoring its usage, also in mA-Hours, with
an in-built EEPROM, that can be addressed and read from the PinAAcle AA.
PerkinElmer lamps have a warranty for 5000 mA-hour or six months whichever
comes earlier.

Lamp Troubleshooting
Refer to Chapter 8, Troubleshooting, in this manual for lamp troubleshooting
information.

Caution To avoid damages to the instrument optics, do not insert uncoded non-
Lumina lamps, such as Intensitron lamps, too far into the lamp holder.

Replacing the Lamps

Always wear UV-absorbing safety glasses when installing, replacing or


! aligning hollow cathode lamps or electodeless discharge lamps.
The ultraviolet radiation emitted by these lamps can harm your eyes.
Warning
286 Maintenance

Lamp Compartment Location


The next figure shows where the lamp compartment is located on the instrument.
Access to the lamp compartment is front of the instrument. This allows for easy
lamp replacement. If you swing open the lamp compartment cover, the lamp
compartment can be seen inside.

Figure 6-37. Accessing the lamp compartment


Item Description
1 Lamp compartment cover
Removing and Replacing the Deuterium Arc Background Corrector Lamp 287

Removing lamps
Danger HOT SURFACE
The lamp is hot when it is in operation..
! Make sure that the lamp is completely cooled down when you remove
Na, Li and K lamps, since the cathode will be in the molten form when it
Warning is in use and will be hot and could cause a burn.

1. Do not unplug and remove lamps while they are switched on.

2. On the Instrument tab click on the Lamp Setup icon to display the Lamp
Setup page.

3. In the Lamp Setup window, go to the On/Off column and click on each green
button to turn the lamp off. The button will change color from green to dark
gray.

4. Make sure that the lamp is switched off before you remove it.

5. Swing open the lamp compartment cover to access the lamp.

6. Unplug and remove the lamp. For EDLs, remove the coding plug as well.

Removing and Replacing the Deuterium Arc Background


Corrector Lamp
Tools Needed

• deuterium arc lamp - Part No. N3160231

• ultraviolet-absorbing safety glasses

• phillips head screwdriver

Removing the Deuterium Lamp Assembly


1. Turn OFF the power switch and unplug the power cord.
288 Maintenance

2. The access to the D2 lamp compartment cover is located on the right side of the
instrument. Use a Phillips screwdriver to remove the screw that holds the cover
in place. Remove the cover.

2
1

Figure 6-38. Accessing the D2 lamp compartment cover

Item Description
1 D2 lamp compartment cover

2 Phillips screw

3. Locate the deuterium lamp assembly in the instrument. Loosen the


thumbscrew that holds the assembly in the instrument.

Caution As you slide out the D2 lamp assembly take care not to damage the cable.
Removing and Replacing the Deuterium Arc Background Corrector Lamp 289

4. Carefully slide the D2 lamp assembly away from the instrument.

3
2

Figure 6-39. Deuterium lamp assembly


Item Description
1 Thumbscrew
2 D2 Lamp

3 Bracket
290 Maintenance

Replacing the Deuterium Lamp


Use great care when handling the deuterium lamp, it is fragile.

Caution Wear contaminant-free gloves when handling the new lamp to prevent
getting fingerprints on the viewing area of the lamp, as this will decrease
the UV performance and damage the lamp.

1. Loosen the thumbscrew that holds the D2 lamp in place.

2. Unscrew the bracket thumbscrew.

3. Unplug the back connector.

4. Slide the bracket and bulb up to remove it from the assembly.

5. Replace the assembly with a new bracket/ bulb set by sliding the cutout on the
metal bracket over the alignment pin on the instrument.
Removing and Replacing the Deuterium Arc Background Corrector Lamp 291

1 2

Figure 6-40. Accessing the D2 lamp compartment

Item Description
1 D2 lamp

2 Cutout
3 Alignment pin

6. Plug in the lamp.


292 Maintenance

7. Tighten the D2 lamp thumbscrew on the bracket assembly.

8. You have completed replacing the deuterium lamp.

Reassembling the Deuterium Lamp Assembly


Next put the deuterium lamp assembly back into the instrument.

1. Plug in the lamp cable.

2. Carefully slide the deuterium lamp assembly down on to the alignment pin on
the D2 lamp housing.

3. Tighten the assembly thumbscrew.

4. Return the screw to the D2 lamp compartment cover and tighten down the
cover.

Reassembly is complete. Next you may have to align the deuterium lamp.

Aligning Deuterium Lamp


1. To align the lamp, see Removing the Deuterium Lamp Assembly on page 287
for instructions access the deuterium lamp.

2. Set up the standard conditions for copper (including slit).

3. Turn on the lamp and let it warm up.

4. In the Lamp Setup window for Cu and select Background Corrector button.
Removing and Replacing the Deuterium Arc Background Corrector Lamp 293

5. While watching the computer screen, use a 2 mm Allen key to adjust the
vertical and horizontal alignment screws located on the rear of the deuterium
lamp compartment, until you achieve the maximum energy counts. See the
following figure.
294 Maintenance

Figure 6-41. Location of the alignment screws of the deuterium lamp


Item Description
1 Horizontal alignment
2 Vertical alignment

The alignment procedure is now complete.


Graphite Furnace Maintenance for the PinAAcle 900T/900Z 295

Resetting the D2 Hours

After aligning the deuterium lamp you need to reset the hours.

1. Select Instrument tab> Diagnostics icon> Spectrometer tab.

2. Click the Advanced button.


The Advanced Tools window appears. The Advanced Tools window is used
to run diagnostic tests, perform maintenance on log files, and reset D2 hours.

3. Click Reset D2 Hours to reset D2 hours.

Graphite Furnace Maintenance for the PinAAcle 900T/900Z

Removing the Graphite Tube


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

1. Make sure that the furnace is cool.

2. Release the pressure holding the furnace heads closed.

3. In the Furnace Control window, click on Open/Close.

4. Swing the support lever to the left side. Tilt the front contact housing
downward. See the following figure.
296 Maintenance

2
1

Figure 6-42. Front Contact Housing


Item Description
1 Support lever
2 Front contact housing

5. The graphite tube is now visible in the rear contact. Use the insertion/removal
tool provided to remove the graphite tube. Do not touch the tube with bare
fingers.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 297

Figure 6-43. Insertion/removal tools


Item Description
1 Graphite tube holder (insertion/removal tool)
298 Maintenance

Inserting the Graphite Tube

Note Do not touch the graphite tube or contacts with your fingers. Wear
contaminant-free gloves when changing the contact cylinders and graphite
tube.

2
1

Figure 6-44. Using insertion/removal tools


Item Description
1 Graphite tube
2 Graphite tube holder

1. When you insert the graphite tube, make sure that:

• The sample injection hole is uppermost.

• The side of the tube to which the platform is attached faces the left of the
furnace. The platform is then higher toward the rear.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 299

Figure 6-45. Graphite tube


Item Description
1 Radiation Beams
2 Rear contact
3 Sample Injection hole

2. Use the insertion/removal tool provided to insert the graphite tube into the rear
contact.
300 Maintenance

Figure 6-46. Insertion/removal tools


Item Description
1 Graphite tube holder (insertion/removal tool)

3. Carefully tilt the front contact housing up into the closed position (1).

4. Swing the support lever underneath the front contact housing (2).
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 301

2 1

Figure 6-47. Front Contact Housing


Item Description
1 Front contact housing
2 Support lever

5. Activate the pressure that holds the furnace closed:


In the Furnace Control window, click on Open/Close.

6. Carefully swivel the furnace autosampler back into place and secure it with the
large securing knobs.

7. If you have installed a new graphite tube, perform the procedure on


Conditioning the Graphite Tube on page 326.
If you are reusing a previously conditioned graphite tube, heat manually at
2500 °C for 5 seconds to remove surface contamination (see Manually Heating
the Graphite Tube on page 327).
302 Maintenance

Cleaning the Graphite Tube and Contacts


Good, reproducible analytical results depend on good electrical contact between
the graphite contacts and the graphite tube. The contact surfaces of the graphite
tube and the contacts must be smooth and clean to allow good electrical contact.
After prolonged use, the contacts may become contaminated with remnants of
samples and small particles of graphite. Even quite small particles can spoil the
contact and cause poor analytical results.
Every time that you open the furnace, clean the contacts.

Note Do not touch the graphite tube or contacts with your fingers. Wear
contaminant-free gloves when changing the contact cylinders and graphite
tube.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 303

1
4

4
3

Figure 6-48. Graphite components


Item Description
1 Rear contact
2 Graphite tube
3 Front contact
4 Optical path
304 Maintenance

Heating The Graphite Tube to Remove Contamination

Warning: UV Radiation – Risk of Eye Damage


! When the graphite furnace is heated to incandescence (approximate
Warning temperature, such as higher than 800 °C.), e.g. during the pyrolysis and
atomization steps, the furnace can emit UV radiation which can damage
your eyes.
Always wear UV-absorbing safety glasses when looking at the
furnace.

You can sometimes remove contamination from the graphite tube by heating the
tube. Heat the graphite tube manually at 2500 °C for approximately 5 seconds
(see Manually Heating the Graphite Tube on page 327).
You may need several cycles to remove this element. Discard the tube for this
element, as this element is the contaminant. This tube may still be clean for other
elements and could still be used for other elements. But if there are stubborn
deposits in the tube that you cannot remove, discard the tube and use a new one.

Cleaning the Contact Surfaces of the Graphite Tube and Contacts

Warning: High Temperatures – Risk of Burns


The graphite furnace can generate very high temperatures. Do not touch
! any parts of the furnace, especially the graphite components, until they
have cooled to room temperature.
Warning

1. Open the furnace and remove the graphite tube (see Removing the Graphite
Tube on page 295).

2. Use a dry, clean swab to clean the inside of the contacts, especially around the
apertures where the radiation beam enters and exits.
Remove any particles from inside the contacts using clean, dry compressed
air.
Be careful not to scratch the inner surfaces of the contacts.
If the surfaces of the contacts are pitted or cracked, remove the contacts and
install new ones (see Changing the Contact Cylinders on page 305).
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 305

3. Heat out the graphite tube to remove contamination (see Manually Heating the
Graphite Tube on page 327).

Changing the Contact Cylinders


Change the graphite contacts when one or both contacts are badly contaminated
or show visible pits and small cracks. Always change both contacts at the same
time.
Used contact cylinders should not be used again, as the contact may not be
optimal, and the performance may be impaired.

Warning: High Temperatures – Risk of Burns


The graphite furnace can generate very high temperatures. Do not touch
! any parts of the furnace, especially the graphite components, until they
have cooled to room temperature.
Warning

Note It is recommended that you visually inspect the contact cylinders for wear
and tear and also for corrosion on the surfaces of the cylinders. If there is
visible wear and corrosion on the surfaces, then the contacts should be
replaced, since this can impact the quality of the analytical results.
Unexplainable spikes on the peak profile of the analysis are also an
indication that the contact cylinder is wearing off and may need to be
replaced. The precision of the analysis degrades once these components
start to show signs of wear and tear.

Note If the graphite tube breaks inside the contact cylinder, you must clean the
contact cylinder/furnace housing thoroughly and may have to replace the
contact cylinder.
306 Maintenance

To Open the Furnace For Contact Changes


1. Make sure that the furnace is cool.

2. In the Furnace Control window click Open/Close and remove the graphite
tube using the tube insertion/removal tool, and then tilt the furnace forward .

3. Switch off the spectrometer at the operational on/off switch at the front of the
instrument.

Tilting the Graphite Furnace Forward


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

Caution Risk of damage to instrument.


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

You must open the furnace to install or change the graphite tube, and also to clean
inside the graphite contacts.

1. Extinguish the flame, turn off the gases, and switch off the instrument. Let the
burner head cool. Open the Sample Introduction compartment door.

2. Loosen the furnace locking screw all the way. See the figure Tilting the
Graphite Furnace Back Into Position on page 331.

3. Grasp the graphite furnace with both hands and carefully tilt it forward.
Support its weight until it reaches the end stop. Never allow the graphite
furnace to swing down with force. This will damage the furnace assembly and
the base of the instrument.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 307

Figure 6-49. Graphite furnace positions


Item Description
1 Furnace in tilted back position
2 Furnace locking screw
3 Furnace in tilted forward position

The graphite furnace is now accessible to perform maintenance procedures .


308 Maintenance

To Remove the Front Contact

Note This procedure is easier to do if the furnace is in the forward position. See
Tilting the Graphite Furnace Forward on page 306.

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

Figure 6-50. Contact removal tool

2. Loosen the two socket-head screws that secure the pressure cylinder to the
front contact housing.

3. Carefully pull the pressure cylinder out of the front contact housing. Make sure
that you do not damage the O-ring. Put the pressure cylinder and screws in a
safe place.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 309

Figure 6-51. Front contact housing


Item Description
1 Pressure cylinder
2 Screws

4. Attach the removal tool to the front contact housing with the two captive
screws on the tool.
310 Maintenance

Figure 6-52. Removal tool


Item Description
1 Removal tool
2 Bolt

5. Use the hex-driver to screw the bolt on the removal tool into the tool to push
out the contact.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 311

Figure 6-53. Front contact housing


Item Description
1 Front contact housing
2 Bolt

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

To Remove the Rear Contact


1. Tilt the furnace forward. See Tilting the Graphite Furnace Forward on page
306.

2. From the tools provided, you require the contact removal tool, the short
posidriver (P2 size), and the Torx driver (star-shaped cross-section T20 size).
312 Maintenance

Figure 6-54. Contact removal tool

Note Make sure that you do not bend or twist the temperature sensor connector.
Also, do not damage the insulating washers.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 313

1
4

3 5

Figure 6-55. Location of optical and temperature sensor


Item Description
1 Graphite furnace
2 Optical sensor
3 Temperature sensor
4 Optical sensor screws
5 Temperature sensor screw
314 Maintenance

3. Using the Torx driver, unscrew the two captive socket-head screws that secure
the optical sensor to the rear contact housing.

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

5. Use the posidrive to remove the screw that hold the temperature sensor in
place.

6. Attach the removal tool to the rear contact housing with the two captive screws
on the tool.

Figure 6-56. Furnace removal tool


Item Description
1 Furnace removal tool
2 Rear contact housing
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 315

7. Use the hex-driver to screw the bolt on the removal tool into the tool to push
out the contact.

Figure 6-57. Furnace removal tool


Item Description
1 Bolt
2 Rear Contact Housing
3 Contact

8. Unscrew the two screws that secure the tool to the contact housing and remove
the tool.
316 Maintenance

To Insert the Front Contact

Note Do not scratch the new contact and do not touch it directly. Wear
contaminant-free gloves when changing the contact cylinders and graphite
tube. Perspiration can contaminate the contact and cause poor analytical
results

Tilt the furnace forward. See Tilting the Graphite Furnace Forward on page 306.

1. Make sure that the contact housing is completely clean and free from particles.
If necessary, blow out any graphite particles from the contact housing with
clean, dry compressed air. Wear safety glasses when doing this.

2. From the tools provided, you require:

• the hex-driver and the Torx driver (star-shaped cross-section).

• the long bolt, front contact guide, and threaded cylinder as shown below.

3. Move the swing arm, located below the furnace, out of the way. Carefully tilt
the graphite furnace forward and support it with one hand.

4. Slide the guide and the front contact onto the long bolt as shown.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 317

4
1
2
3

Figure 6-58. Guide and Front Contact


Item Description
1 Bolt
2 Guide
3 Front contact
4 Threaded cylinder

5. Slid the bolt into the front contact housing such that the new contact sits in the
opening of the housing. Screw the threaded cylinder on to the bolt

6. Put the threaded cylinder into the opposite end of the contact housing and
screw the bolt into the cylinder until the contact is pressed up against the
housing.
318 Maintenance

Figure 6-59. Threaded cylinder and bolt


Item Description
1 Bolt
2 Threaded cylinder

7. Tilt the graphite furnace back into its original position. Use the hex-driver to
screw the bolt into the threaded cylinder and push the contact into the contact
housing. Screw in the bolt until the rim of the contact is flush with the contact
housing.

Note There must be no gap between the rim of the contact and the housing.
Do not use excessive force to push the contact into the housing, otherwise
the contact may shatter.
If there is substantial resistance, check that the parts are aligned correctly.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 319

Figure 6-60. Hex driver


Item Description
1 Hex driver

8. Screw the bolt out of the threaded cylinder and carefully remove the tools. Do
not scratch the contact when you remove the tools.

9. Blow out any graphite particles from the contact housing with clean, dry
compressed air. Wear safety glasses when doing this.

10. Check the O-ring on the pressure cylinder; if it is damaged, fit a new one. See
Replacement Parts on page 362.

11. Push the pressure cylinder carefully into the front contact housing. Make sure
that you do not damage the O-ring.

12. Tighten the two screws to secure the pressure cylinder to the front contact
housing.
320 Maintenance

Figure 6-61. Pressure cylinder


Item Description
1 Pressure cylinder
2 Screws

To Insert the Rear Contact

Note Do not scratch the new contact and do not touch it directly. Wear
contaminant-free gloves when changing the contact cylinders and graphite
tube. Perspiration can contaminate the contact and cause poor analytical
results

1. Make sure that the contact housing is completely clean and free from particles.
If necessary, blow out any graphite particles from the contact housing with
clean, dry compressed air.
Wear safety glasses when doing this.

2. From the tools provided, you require:


Graphite Furnace Maintenance for the PinAAcle 900T/900Z 321

• the hex-driver and the Torx driver (star-shaped cross-section).

• the long bolt, rear contact guide, and threaded cylinder as shown below.

3. Move the swing arm, located below the furnace, out of the way. Carefully tilt
the graphite furnace forward and support it with one hand.

4. Slid the bolt into the rear contact housing such that the new contact sits in the
opening of the housing. Screw the threaded cylinder on to the bolt

2
3 4

Figure 6-62. Rear contact on to guide


Item Description
1 Threaded cylinder
2 Contact
3 Guide
4 Bolt

5. Make sure that the graphite contact is correctly orientated, with the sample
injection hole at the top.

6. Put the threaded cylinder into the opposite end of the contact housing and
screw the bolt into the cylinder until the contact is pressed up against the
housing.
322 Maintenance

1
2
4

Figure 6-63. Rear contact on furnace


Item Description
1 Threaded cylinder
2 Contact
3 Guide
4 Bolt

7. Tilt the graphite furnace back into its original position. Use the hex-driver to
screw the bolt into the threaded cylinder and push the contact into the contact
housing.
Screw in the bolt until the contact is flush with the contact housing.

Note There must be no gap between the contact and the housing.
Do not use excessive force to push the contact into the housing, otherwise
the contact may shatter.
If there is substantial resistance, check that the parts are screwed in straight
and not at an angle.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 323

Figure 6-64. Hex driver


Item Description
1 Hex driver

8. Screw the long bolt out of the threaded cylinder and carefully remove the tools.

Note Do not scratch the new contact when you remove the tools.

9. Blow out any graphite particles from the contact housing with clean, dry
compressed air. Wear safety glasses when doing this.

10. Check the O-ring on the optical sensor; if it is damaged, fit a new one. See
Replacement Parts on page 362.

11. Push the optical sensor into the rear contact housing. Make sure that you do not
damage the O-ring.
324 Maintenance

Figure 6-65. Optical Sensor


Item Description
1 Optical sensor

12. Tighten the two screws to secure the optical sensor to the rear contact housing.

13. Reattach the Temperature sensor.

To Close the Furnace After Contact Change


1. Tilt the furnace back into its original position and tighten the furnace locking
screw to lock the furnace into place (see Tilting the Graphite Furnace Back
Into Position on page 331).

2. Insert a graphite tube into the furnace, close the front contact housing, and
swing the support lever under the contact housing (see Inserting the Graphite
Tube on page 298).
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 325

3. Switch on the spectrometer at the operational on/off switch located at the front
of the instrument.

4. If you have installed a new graphite tube, see Conditioning the Graphite Tube
on page 326).

If you are reusing a previously conditioned graphite tube, heat manually at


2500 °C for 5 seconds to remove contamination (see Manually Heating the
Graphite Tube on page 327).

Note Every time you open the furnace, subsequently always heat it out manually
at 2500 °C for approximately 5 seconds.

Resetting Cycles for Tubes and Contacts


Every time a furnace program containing a read command runs to the end, the
system increments two counters; one for the graphite tube and one for the graphite
contacts.

Note It is recommended that you visually inspect the graphite tube and the
contact cylinders for wear and tear and also for corrosion on the surfaces
of the tube and cylinders. If there is visible wear and corrosion on the
surfaces, then the contacts and/or tube should be replaced, since this can
impact the quality of the analytical results. Unexplainable spikes on the
peak profile of the analysis is also an indication that the graphite tube or
the contact cylinder is wearing off and may need to be replaced. The
precision of the analysis degrades once these components start to show
signs of wear and tear.

Note If the graphite tube breaks inside the contact cylinder, you must clean the
contact cylinder/furnace housing thoroughly in addition to replacing the
contact cylinder.
326 Maintenance

Contact Cycles
Use this value to show the number of times that the furnace has been used since the
contacts were changed.

Click on Reset to reset the value to zero when you install new graphite contacts.

Check the Display warning message when cycles exceed check box to have a
warning message displayed when an analysis is started and the contact cycles have
exceeded a user specified number. The warning message will not prohibit a user
from performing an analysis, but rather serves as a reminder to the user that the
contacts should be inspected and, if necessary, replaced.

Conditioning the Graphite Tube


We recommend that you run the graphite tube conditioning program every time
that you change the graphite tube or platform. The conditioning procedure
removes adsorbed gases and surface contamination from the graphite, and
ensures reproducible performance.
After conditioning, it is good practice to verify that the tube and/or platform are
sufficiently clean for the element you wish to determine.
In order to do this, run your method for this element, but do not inject a sample.
Perform a ‘dry fire’ instead. Evaluate the results obtained. If the absorbance
value is too high for this element, heat the tube manually at 2500 °C for 10
seconds (see Manually Heating the Graphite Tube on page 327) and then repeat
the "dry fire".
You may need to repeat this a few cycles to remove the contaminants
completely. Otherwise, change to a new tube.

1. On the Instrument tab, click on Furnace Control icon.

2. In the Furnace Control window, click on Condition Tube button


The system uses a special furnace program to heat the tube to successively
higher temperatures.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 327

Warning: High Temperatures – Risk of Burns


The graphite furnace can generate very high temperatures. Do not touch
! any parts of the furnace, especially the graphite components, until they
have cooled to room temperature.
Warning

Warning: UV Radiation – Risk of Eye Damage


! When the graphite furnace is heated to incandescence (approximate
Warning temperature, such as higher than 800 °C.), e.g. during the pyrolysis and
atomization steps, the furnace can emit UV radiation which can damage
your eyes.
Always wear UV-absorbing safety glasses when looking at the
furnace.

Warning: Toxic Gases


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

Manually Heating the Graphite Tube

Note Do not heat the graphite furnace for longer than about 10 s when the
temperature exceeds 2000 °C. Heating for longer periods will markedly
reduce the lifetime of the graphite tube.

To enter the temperature manually and heat the furnace:

1. On the Instrument tab, click on Furnace Control icon.

2. In the Furnace Control window, click on the Cleanout Temp. entry field and
type the required temperature (e.g. 2500 °C).
328 Maintenance

3. Click on Start to heat the furnace.


The furnace is heated to the selected temperature and continues to heat until
you stop it.

4. After about 10 seconds, click on Start again to stop furnace heating.

Checking and Cleaning the Furnace Windows


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

To Remove the Windows


Risk of damage to the furnace windows
Caution • The quartz windows are precision optical components; handle them
carefully to prevent scratches, fingerprints or other contamination.

1. Make sure that the furnace is cool.

2. Carefully swivel the furnace autosampler out of the way.

3. Tilt the furnace forward (see Tilting the Graphite Furnace Back Into Position
on page 331).

4. Use the key provided to unscrew the left-hand and the right-hand windows
from the furnace.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 329

Figure 6-66. Window key


Item Description
1 Window key
330 Maintenance

To Clean the Windows


1. Remove the windows from the furnace.

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

1 2 3

Figure 6-67. Window assembly


Item Description
1 Seal
2 Window
3 Mount

3. Blow any dust or particles off the surface of the window with clean dry air
before you start.

4. Clean the windows carefully with a tuft of cotton moistened with a dilute
solution of mild laboratory detergent.
Rinse the windows several times with deionized water.
If the windows are not clean after this procedure, clean them with a soft lint
free cloth moistened with spectroscopic grade alcohol.

Note To avoid scratching the windows, rub the surfaces of the windows as little
as possible. Discard scratched windows.
Graphite Furnace Maintenance for the PinAAcle 900H 331

5. Reassemble the windows. New seals and windows are available.

6. Screw the windows in the furnace.

To Refit the Windows


1. Screw each window carefully into the ends of the furnace; make sure that the
threads are properly engaged.

The windows are designed to be slightly offset from the vertical.

2. Tilt the furnace back into its original position and tighten the furnace locking
screw to lock the furnace into place (see Tilting the Graphite Furnace Back
Into Position on page 331).

Tilting the Graphite Furnace Back Into Position


1. Once all the maintenance procedures are completed, carefully tilt the furnace
back into to its original position. See the figure Graphite furnace positions on
page 307.

2. Tighten the furnace locking screw to lock the furnace into place.

3. Close the Sample Introduction compartment door.

4. Switch on the instrument, turn on the gases and restore the flame.

Graphite Furnace Maintenance for the PinAAcle 900H

Open the Furnace and Remove the Graphite Tube


You must open the furnace to install or change the graphite tube, and also to clean
inside the graphite contacts.

Warning: High Temperatures – Risk of Burns


The graphite furnace can generate very high temperatures. Do not touch
! any parts of the furnace, especially the graphite components, until they
have cooled to room temperature.
Warning
332 Maintenance

1. Make sure that the furnace is cool.


2. Release the pressure holding the furnace closed:
3. In the Furnace Control window, click on Open/Close.
The furnace opens and the graphite tube is accessible.
4. Remove the graphite tube.
Do not touch the graphite tube with bare fingers.

Figure 6-68. Graphite furnace in the open position

1. Take a graphite tube with integrated platform and insert it into the right-hand
graphite contact, so that the sample introduction hole lines up roughly with the
sample port in the graphite contact.

Note Make sure that the side of the tube to which the integrated platform is
attached is rear of the furnace.

2. Insert the alignment tool (provided) into the sample port while carefully
moving and turning the tube so that the tip of the alignment tool goes into the
Graphite Furnace Maintenance for the PinAAcle 900H 333

sample introduction hole in the tube, and that the flat side of the alignment tool
is facing towards the left.
3. With the alignment tool still in position, activate the pressure that holds the
furnace closed:
In the Furnace Control window, click on Open/Close.
The furnace closes.
4. Remove the alignment tool.
(If the furnace closes abruptly, you can adjust the speed with the speed reducer
located behind the HGA Furnace)

Figure 6-69. Speed Reducer


Item Description
1 Speed Reducer
334 Maintenance

1
2

3 4 6
5

Figure 6-70. Graphite tube viewed from the left-hand end


Item Description Item Description
1-2 Sample introduction hole 5 Right-hand graphite contact
3 Correct 6 Tube alignment tool
4 Incorrect 7 Graphite tube
Graphite Furnace Maintenance for the PinAAcle 900H 335

5. If you have installed a new graphite tube, perform the procedure outlined in
Conditioning the graphite tube on page 340.
If you are reusing a previously conditioned graphite tube, heat manually at
2500 °C for 5 seconds to remove surface contamination.
6. Every time you open the furnace, subsequently always heat it out manually at
2500 °C for approximately 5 seconds.
7. Check alignment of the furnace (see Aligning the Graphite Furnace on page
191).
8. Check alignment of the furnace autosampler (see To Align the Autosampler
Tip in the Graphite Tube on page 148).

Cleaning the graphite tube and graphite contacts


Good, reproducible analytical results depend on good electrical contact between
the graphite contacts and the graphite tube. The contact surfaces of the graphite
tube and the graphite contacts must be smooth and clean to allow good electrical
contact.
After prolonged use the graphite contacts may become contaminated with
remnants of samples and small particles of graphite. Even quite small particles
can spoil the contact and cause poor analytical results.
Every time that you open the furnace, clean the contacts as described in
Cleaning the contact surfaces of the graphite tube and contacts on page 336.

Note Do not touch the graphite tube or contacts with your fingers. Perspiration
can affect the tube lifetime and the analytical results by contaminating and
damaging the surface of the graphite.
If a graphite tube breaks inside the furnace you must remove all the
remnants and thoroughly clean the contacts.
336 Maintenance

Heating the graphite tube to remove contamination

Warning: High Temperatures UV Radiation – Risk of Burns and Eye


! Damage
Warning The graphite furnace can generate very high temperatures, and can emit
UV radiation which can damage your eyes, when it is heated to
incandescence.
The furnace is exposed when it is in the standby position, thus increasing
these risks.
Never heat the furnace when it is in the standby position. Always move
it into the atomizer compartment before you heat it.

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

Cleaning the contact surfaces of the graphite tube and contacts


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

1. Remove the furnace windows (see To remove the windows: on page 353).
2. Open the furnace and remove the graphite tube (see Open the Furnace and
Remove the Graphite Tube on page 331).
3. Use a dry, clean swab to clean the contact surfaces of the graphite tube. If the
surfaces of the graphite tube are pitted or cracked, discard the graphite tube and
use a new one.
4. Use a dry, clean swab to clean the inside of the contacts, especially around the
apertures where the radiation beam enters and exits.
Remove any particles from inside the contacts using a small vacuum cleaner.
Be careful not to scratch the inner surfaces of the contacts.
If the surfaces of the contacts are pitted or cracked, remove the contacts and
install new ones (see Changing the graphite contacts on page 341).
Graphite Furnace Maintenance for the PinAAcle 900H 337

5. Insert the graphite tube and close the furnace (see Open the Furnace and
Remove the Graphite Tube on page 331).
6. Refit the windows (see To refit the windows: on page 355).
7. Condition the graphite tube (see Conditioning the graphite tube on page 340).
Changing the graphite tube

2 3
1

Figure 6-71. Graphite components of the furnace


Item Description Item Description
1 Left-hand graphite contact 4 Right-hand graphite contact
2 Shield ring 5 Graphite tube with integrated
platform
3 Graphite tube

Note Do not handle graphite tubes with bare fingers. Perspiration from your
fingers can attack the pyrolytic coating.
338 Maintenance

Warning: High Temperatures – Risk of Burns


The graphite furnace can generate very high temperatures. Do not touch
! any parts of the furnace, especially the graphite components, until they
have cooled to room temperature.
Warning

1. If required, open the furnace and remove the graphite tube (see Open the
Furnace and Remove the Graphite Tube on page 331).
Graphite Furnace Maintenance for the PinAAcle 900H 339

Figure 6-72. Installing the graphite shield


Item Description
1 Graphite shield ring
2 Graphite shield ring installed
340 Maintenance

2. If required, install or change the graphite shield ring.


Slide the shield ring with its large plane face toward the furnace block over the
left-hand furnace contact.

3. Insert the graphite tube and close the furnace (see Open the Furnace and
Remove the Graphite Tube on page 331).

4. If you have installed a new graphite tube, perform the procedure outlined in
Conditioning the graphite tube on page 340.
If you are reusing a previously conditioned graphite tube, heat manually at
2500 °C for 5 seconds to remove surface contamination.

Note Every time you open the furnace, subsequently always heat it out manually
at 2500 °C for approximately 5 seconds.

Note When inserting the graphite tube into the furnace, make certain that the
tube end with the horizontal grooves is at the left. Otherwise sample will
be dispensed onto the wall of the tube and not into the cavity in the
platform.
L'vov platforms can only be inserted into the special graphite tubes with
horizontal grooves. These grooves have limited mechanical stability.
Repeated insertion and removal of integrated platforms causes abrasion, so
that ultimately the platforms will not seat correctly. You must then replace
the tube.

Conditioning the graphite tube


We recommend that you run the graphite tube conditioning program every time
that you change the graphite tube or platform. The conditioning procedure
removes adsorbed gases and surface contamination from the graphite, and
ensures reproducible performance.
After conditioning, it is good practice to verify that the tube and/or platform are
sufficiently clean for the element you wish to determine.
In order to do this, run your method for this element, but do not inject a sample.
Perform a "dry fire" instead. Evaluate the results obtained. If the absorbance
Graphite Furnace Maintenance for the PinAAcle 900H 341

value is too high for this element, heat the tube manually at 2500 °C for 10
seconds and then repeat the ‘dry fire’.

Warning: High Temperatures – Risk of Burns


The graphite furnace can generate very high temperatures. Do not touch
! any parts of the furnace, especially the graphite components, until they
have cooled to room temperature.
Warning

Note Do not heat the graphite furnace for longer than about 10 seconds when the
temperature exceeds 2000 °C. Heating for longer periods will markedly
reduce the lifetime of the graphite tube.

To enter the temperature manually and heat the furnace:

1. On the Instrument tab, click on Furnace Control icon.

2. In the Furnace Control window, click on the Cleanout Temp. entry field and
type the required temperature (e.g. 2400 °C).

3. Click on Start to heat the furnace.


The furnace is heated to the selected temperature and continues to heat until
you stop it.

4. After about 10 s, click on Start again to stop furnace heating.

Changing the graphite contacts


Change the graphite contacts when one or both contacts are badly contaminated.
Contacts should be changed on a routine basis. Always change both contacts at
the same time.

Summary of the procedure


Always change the graphite contacts in the following sequence:
1. Open the furnace and remove the graphite tube (see To open the furnace for
contact change: on page 342).
342 Maintenance

2. Remove the right-hand contact (see To remove the right-hand contact: on page
344).
3. Remove the left-hand contact (see To remove the left-hand contact: on page
346).
4. Install a new left-hand contact (see To install the left-hand contact: on page
348).
5. Install a new right-hand contact (see To install the right-hand contact: on page
350).
6. Insert the graphite tube and close the furnace (see To close the furnace after
contact change: on page 352).
7. Condition the graphite tube (see Conditioning the graphite tube on page 340).
8. Align the furnace (see Aligning the Graphite Furnace on page 191).
9. Align the autosampler (see To Align the Autosampler Tip in the Graphite Tube
on page 148).
Special tools to change the contacts are provided with the furnace. These are
used in different configurations for different procedures as depicted in the
following illustrations.

Caution Risk of damage to the optical sensor


Take care not to damage the optical sensor when you remove or install the
graphite contacts.

To open the furnace for contact change:


1. Make sure that the furnace is cool.
2. Exit the software.
3. Switch off the main power switch at the operational on/off on the left-hand side
panel.
4. Remove both furnace windows (see Checking and cleaning the furnace
windows on page 353).

5. Open the furnace manually and remove the graphite tube:


1. Turn off the normal and special gas supplies.
Graphite Furnace Maintenance for the PinAAcle 900H 343

2. Disconnect the normal gas tube from the inlet manifold on the power
unit:
Carefully push the black locking ring of the connector into the connector
and pull the tube out of the connector. This releases the gas pressure.
3. Pull the right-hand furnace block by hand to the side.
The graphite tube is now accessible.
4. Remove the graphite tube.
Do not touch the graphite tube with bare fingers.

6. Very carefully, using a small screwdriver, lever the graphite shield ring from
the left-hand contact.

Figure 6-73. Contact change


Item Description
1 Graphite shield ring
344 Maintenance

To remove the right-hand contact:


1. Take the contact installation tool provided and slide the dome-shaped extractor
onto the bolt. Pass the bolt from the internal side of the furnace through the
right-hand contact and out through the window cavity. The lugs on the
extractor fit over the furnace block.

2. Screw the traction nut with its long side toward the furnace block onto the free
end of the bolt. Position the traction nut so that the flat side on the rim passes
under the optical sensor.

Note Take care not to damage the optical sensor.

3. Carefully turn the bolt clockwise with the ratchet wrench provided to draw in
the traction nut and thus push the graphite contact out of the furnace block.

4. Disassemble and remove the installation tool.

5. Now remove the left-hand contact.


Graphite Furnace Maintenance for the PinAAcle 900H 345

2
3

4
1

Figure 6-74. Remove the right-hand contact


Item Description Item Description
1 Bolt 4 Optical sensor
2 Extractor 5 Traction nut
3 Right-hand contact
346 Maintenance

To remove the left-hand contact:


1. Take the contact installation tool provided and slide the dome-shaped extractor
onto the bolt. Pass the bolt from the internal side of the furnace through the left
hand contact and out through the window cavity. The lugs on the extractor fit
over the furnace block.

2. Screw the traction nut with its long side toward the furnace block onto the free
end of the bolt.
Position the traction nut so that the flat side on the rim is facing up.

3. Carefully turn the bolt clockwise with the ratchet wrench provided to draw in
the traction nut and thus push the graphite contact out of the furnace block.

4. Disassemble and remove the installation tool.

5. Now install a new left-hand contact.


Graphite Furnace Maintenance for the PinAAcle 900H 347

2
1

4
3

Figure 6-75. Remove the left-hand contact


Item Description Item Description
1 Bolt 3 Left-hand contact
2 Extractor 4 Traction nut
348 Maintenance

To install the left-hand contact:


1. Slide the long arm of the plastic alignment gauge and the replacement left-hand
(short) contact onto the bolt, so that the contact fits in the ring in the gauge.

2. Pass the bolt from the internal side through the left-hand furnace block and out
through the window cavity.

3. Screw the traction nut with its short side toward the furnace block onto the free
end of the bolt.
Position the traction nut so that the flat side on the rim is facing up.

4. Carefully turn the bolt clockwise with the ratchet wrench provided to draw the
contact into the furnace block. Make certain that the contact is not tilted.

Note Draw the contact firmly into place, but do not apply excessive force
otherwise the contact may shatter.

5. Disassemble and remove the installation tool.


Take care not to scratch or damage the contact.

6. Now install a new right-hand contact.


Graphite Furnace Maintenance for the PinAAcle 900H 349

2 3
4
1

Figure 6-76. Installing the left-hand contact


Item Description Item Description
1 Traction nut 3 Long arm of the alignment gauge
2 Left-hand contact 4 Bolt
350 Maintenance

To install the right-hand contact:


1. Slide the short arm of the plastic alignment gauge and the replacement right-
hand (long) contact onto the bolt, so that the contact fits in the ring in the gauge
and the lug in the ring inserts into the sample introduction port of the contact.

2. Pass the bolt from the internal side through the right-hand furnace block and
out through the window cavity so that the long arm of the alignment gauge rests
against the furnace block.

3. Screw the traction nut with its short side toward the furnace block onto the free
end of the bolt. Position the traction nut so that the flat side on the rim passes
under the optical sensor.

Note Take care not to damage the optical sensor.

4. Carefully turn the bolt clockwise with the ratchet wrench to draw the contact
into the furnace block.
Make certain that the contact is not tilted.

Note Draw the contact firmly into place, but do not apply excessive force
otherwise the contact may shatter..

5. Disassemble and remove the installation tool. Take care not to scratch or
damage the contact.
Graphite Furnace Maintenance for the PinAAcle 900H 351

1 2
3

Figure 6-77. Install the right-hand contact


Item Description Item Description
1 Bolt 3 Left-hand contact
2 Short arm of the alignment gauge 4 Traction nut
352 Maintenance

6. Slide the graphite shield ring with its large flat face toward the furnace block
over the left-hand contact.

Figure 6-78. Graphite shield ring installed


Item Description
1 Graphite shield ring installed

To close the furnace after contact change:


1. Insert the graphite tube and align it with the alignment tool (see Open the
Furnace and Remove the Graphite Tube on page 331).

2. Reconnect the normal gas tube to the inlet manifold and turn on the gas
supplies for the furnace. The furnace closes.

3. Remove the alignment tool.

4. Refit the windows (see To refit the windows: on page 355).

5. Switch on the instrument power.


Graphite Furnace Maintenance for the PinAAcle 900H 353

6. Start the software.

7. Condition the graphite components (see Conditioning the graphite tube on


page 340).

8. Check alignment of the furnace (see Aligning the Graphite Furnace on page
191).

9. Check alignment of the furnace autosampler (see To Align the Autosampler Tip
in the Graphite Tube on page 148).

Checking and cleaning the furnace windows


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

To remove the windows:

Caution Risk of damage to the furnace windows or optical sensor


The quarts windows are precision optical components, handle them
carefully to prevent scratches, fingerprints or other contamination..
Take care not to damage the optical sensor when you remove or refit the
windows.

The window assemblies are retained in the furnace by bayonet mounts.

1. Make sure that the furnace is cool.


354 Maintenance

Figure 6-79. Right-hand window


Item Description
1 Optical Sensor
2 Right-hand window

2. Remove the right-hand window assembly:


1. Turn the window assembly counterclockwise to release the bayonet
lock.
2. Pull the window assembly out of the furnace.

Note Take care not to damage the optical sensor.


Graphite Furnace Maintenance for the PinAAcle 900H 355

Figure 6-80. Left-hand window


Item Description
1 Left-hand window

3. Remove the left-hand window assembly:


1. Turn the window assembly counterclockwise to release the bayonet
lock.
2. Pull the window assembly out of the furnace.

To refit the windows:


1. Refit the right-hand window assembly:
1. Insert the window assembly into the window port and carefully engage
the bayonet lock.
2. Turn the window assembly clockwise to secure the bayonet lock.

2. Refit the left-hand window assembly:


1. Insert the window assembly into the window port and carefully engage
the bayonet lock.
356 Maintenance

2. Turn the window assembly clockwise to secure the bayonet lock.

To clean the windows:


1. Remove the windows from the furnace (see To remove the windows: on page
353).

2. Dismantle the window assemblies and remove the quartz windows carefully
from the mounts as follows:
1. Carefully pull the collar out of the mount.
2. Carefully push the window out of the mount with a plastic pipet tip.

1 2
3

Figure 6-81. Window detail


Item Description
1 Mount
2 Window
2 Collar

3. Blow any dust or particles off the surface with clean dry air before you start to
clean a window.

4. Clean the windows carefully with a tuft of cotton moistened with a dilute
solution of mild laboratory detergent.
S10 Autosampler Maintenance 357

Rinse the windows several times with deionized water.


If the windows are not clean after this procedure, clean them with a soft lint
free cloth moistened with spectroscopic grade alcohol.

Note To avoid scratching the window, rub the surfaces of the windows as little
as possible. Discard scratched windows..

5. Reassemble the windows:


1. Carefully drop the window into the mount, making sure that it sits
correctly.
2. Push in the collar.
New windows are available.

6. Refit the windows in the furnace (see To refit the windows: on page 355).

S10 Autosampler Maintenance


For complete maintenance information, see the S10 Autosampler User's Guide
(Part No. 09936788) shipped with the S10 Autosampler.

AS 900 Furnace Autosampler Maintenance


For information on the AS 900 Autosampler system description see Furnace
Autosampler on page 96.

For AS 900 installation information see Installing AS 900 Furnace Autosampler


on page 135.

Table 6-4. Checklist for Regular Maintenance Tasks

Autosampler external Wipe over the surfaces with a lint-free cloth moistened with a dilute solution of
surfaces laboratory detergent.
The autosampler surfaces are resistant to dilute acids and alkalis, and to a lesser
extent to strong acids and alkalis and organic solvents.
358 Maintenance

Complete rinsing Fill and flush the rinsing system before the start of every analysis run.
system Flush the rinsing system when you have finished an analysis run.
Valves The valves must function correctly to maintain the precision of the dispensed
volumes. If the precision of the analytical results deteriorates, this can be an
indication that a valve is not functioning correctly.
If a valve seizes or leaks, for example because the pump has been idle for a long
time, or because of particles lodged in the valve, or because of worn seals, you
can remove the valves to clean or change them.
Waste bottle Empty the autosampler waste bottle regularly. Never allow it to overflow or allow
the liquid to reach the end of the drain tube.
If the bottle contains hazardous, toxic, or flammable substances, dispose of the
waste properly, according to the local safety regulations.
Rinse bottle Make sure that the rinse bottle is always filled with clean, particle-free rinsing
liquid.
All tubes Make sure that all the tubes are clean and free from kinks.
Change any tubes that may be damaged or contaminated.
Pipette tip Make sure that the pipette tip is not damaged. If the tip is damaged you may get
pipetting errors during the analyses. Repair the tip or install a new pipette
assembly if necessary.
Pump heads Make sure that the pump heads are not loose. Tighten the pump head retaining
ring if necessary. Make sure that the pump head remains vertical, with the arrow
aligned vertically.
Do not remove the pump heads from the pumps.

Caution Risk of damage to the autosampler.


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

Filling and flushing the rinsing system


1. Make sure that the rinsing system components are correctly installed, in good
condition, and suitable for the rinsing liquid you will use.

2. Fill the rinse bottle with clean, particle-free rinsing liquid.


AS 900 Furnace Autosampler Maintenance 359

3. If there are particles in the rinsing liquid they can lodge in the valves, causing
leaks and non-reproducible results.

4. Empty the waste bottle. Dispose of any hazardous waste correctly.

5. Fill and flush the system:


• In the Furnace Control window, click on Flush Sampler button. This
activates a special rinse cycle.
• Repeat substep 1 as often as required to completely fill the rinsing system
with rinsing liquid and to flush out all the air.

Note Make certain there are no air bubbles in the rinsing system. Air bubbles can
lead to non-reproducible results.

6. If you want to use a different rinsing liquid to that already in the rinsing system,
rinse all traces of the previous liquid out of the rinsing system. Use a rinsing
liquid that is miscible with both the new and the old rinsing liquids.
You may have to use intermediate rinsing liquids.
For example, if you are changing from an acidic liquid to an organic solvent,
you could use:
• Deionized water,
• Isopropanol or other water-miscible solvent,
• Final organic solvent.

Valve Maintenance
The autosampler pumps dispense microliter volumes of liquid with high precision.
To maintain this high precision it is essential that the valves function correctly. If
there is a deterioration in the precision of the analytical results, and other sources
of error can be excluded, this is an indication that a valve may not be functioning
correctly.

Only the rinse pump contains valves. The sample pump contains inserts that are a
similar shape to the rinse pump outlet valve.
360 Maintenance

Routine Maintenance
The valves require little routine maintenance except to flush them thoroughly
before and after every analysis series.

Before the start of every analysis series:

1. Flush the system well with rinsing liquid.

At the end of every analysis series:

1. Flush the system well with rinsing liquid.

2. Flush the system well with dilute nitric acid (this step is especially important
for elements with a tendency to carryover).

3. Flush the system well with isopropanol.

4. Finally flush the system well with deionized water.

Checking the Valves


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

Caution Risk of damage to the autosampler.


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

Checking the outlet valve


1. Raise the pipet tip out of the rinsing port:
In the Furnace Control window, click on Align Tip button.
The Align Autosampler Tip Wizard appears.
AS 900 Furnace Autosampler Maintenance 361

2. In this dialog, click on Set the depth of the autosampler tip in the sampling
cup. Then select Use the rinse location. The pipet tip rises to a position
directly above the rinsing port.

3. Select on Next. In the dialog that appears, click on Finish.

4. In the Furnace Control window, click on Flush Sampler button to start a


rinse cycle.

5. The rinsing pump performs three cycles. During the suction phase of each
cycle (pump plunger moves backward) a droplet of rinsing liquid hangs on the
end of the pipet tip; this droplet must remain stationary.
362 Maintenance

At the end of a rinse cycle the sample pump draws the rinsing liquid droplet
back into the pipet tip.

If a valve is leaking, replace the complete valve.

Checking the inlet valve


1. Start a rinse cycle by clicking on the Flush button.

2. Remove the rinse feed tube briefly from the rinsing liquid so that an air bubble
is drawn in and then replace the tube in the rinsing liquid.

3. Watch the meniscus of the air bubble: It must remain stationary during the
expulsion phase of each cycle (pump plunger moves forward).

4. When you have finished checking the outlet valve, in the In the Furnace
Control window, click on Align Tip button.

5. In this dialog (see the previous screen shot), click on Set the depth of the
autosampler tip in the sampling cup. Select Use the rinse location and then
select Next.

6. Adjust the depth control wheel so that the pipet tip is at the correct depth inside
the rinsing port. Then click on Finish.

Note Do not attempt to take the valves apart or repair the valves or to
change individual components inside a valve. If repeated flushing does
not remedy a leaking valve, discard the valve and install a complete, new
valve.

Replacement Parts
Every day you count on PerkinElmer to provide you with solutions that deliver
reliable performance, control operating costs and maximize operational time. Our
complete portfolio of consumables, parts, supplies, training and service helps you
meet both routine and demanding measurement challenges. We invest heavily in
testing and validating our products to ensure you receive guaranteed compatibility
and performance-on-time, every time, for every instrument in your laboratory.
Replacement Parts for the PinAAcle 900 363

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


PerkinElmer, using the part numbers quoted in the guides provided with the
instrument.
See our website:
http://perkinelmer.com
PerkinElmer's catalog service offers a full selection of high-quality supplies.
To place an order for supplies and many replacement parts, request a free catalog,
or ask for information:
If you are located within the U.S., call toll free 1-800-762-4002, 8 a.m. to
8 p.m. EST. Your order will be shipped promptly, usually within 24 hours.
If you are located outside of the U.S., call your local PerkinElmer sales or service
office.

Replacement Parts for the PinAAcle 900


The following list has the most commonly used parts and solutions. For a complete
list please visit our website.
http://perkinelmer.com

Table 6-5. Consumables and Spares for the PinAAcle 900

Part No. Description Quantity


03031573 N2O Burner Head Cleaner 1

09210225 T-Handle HEX Screwdriver 6.0 X 300 1


B0859760 T-Handle HEX Screwdriver 5.0 X 200 1
B0508264 FLEXO-55 Tube 6X4 1
09290602 USB LED Light Source 1
09902219 Viton Burner Head O-Ring Kit 1
09904991 Bottle- Wide Mouth 15L Natural 1
364 Maintenance

09907925 Cuvette- Wood 8 MM Clamp 1


09920179 Push-In Fitting Metric "Y" 6 OD TBG 1
Brass
09920583 HEX Nut Metric 6MM TBG OD Brass 1
09923472 Ferrule- Metric- Back 6MM Brass 1
09923473 Ferrule- Metric- Front 6MM Brass 1
B0147498 Insert For Plastic Hose 1
B0500748 O-Ring 16 X 1.75 VITON 1
B0504035 Set-1 Piece Contact IP-Long/Short 1
B0505339 Cord Nut Key 1
B0505368 Cleaning Tips 1 Package of 10
B0851900 ZL Furnace Mirror 1
B0856585 TORX Screwdriver T20X100 1
B3000641 Standard-THGA Graphite Tubes 5 Pack
B3120410 Press-In Gage THGA 1
B3120416 Press-In Sleeve 1
B3120420 Press-Out Tool 1
N0400058 Drain Assembly Louie Burner 1
N3161240 Burner Head Handle 1
B0501696 Air and Vent Filter (Felt) 1
09290587 USB Extension Cable 1
N3160143 Nebulizer Adjustable Metal Kit 1
Tested
N3160144 Nebulizer Adjustable Plastic Kit 1
Tested
Replacement Parts for the PinAAcle 900 365

N3160162 Electric Heated FIAS MHS Cell Kit 1


Assembly
N3160161 Zeeman Heated Cell Assembly 1
Adapter
N3160809 Burner Chamber Holder Assembly 1
N3160102 Endcap Assembly - Metal 1
N3160111 Endcap Assembly - High Sensitivity 1
Plastic
N3160106 Burner Chamber Assembly 1
N0400102 Head Assembly-Louie 4" Titanium 1
Burner
N0400101 Head Assembly-Louie 2" Titanium 1
Burner
N0400100 Head Assembly-Louie 2" Tapered 1
Burner
N0400103 Head Assembly-Louie 3 Slot Burner 1
N9300244 GFAAS Mixed Standard 1
02900540 AA Test Mix 1
B0190634 1% Mg (as nitrate) matrix modifier 1
B0190635 1% Pd (as nitrate) matrix modifier 1
N9303445 10% NH4H2PO4 matrix modifier 1

B3001262 Pyrocoated HGA tubes with 5 Pack


Integrated Platforms
B3001264 Pyrocoated HGA tubes with 20 Pack
Integrated Platforms
B0128495 HGA Contact Cylinder 1 Pair
366 Maintenance

N9307834 HGA Advanced Platform Graphite Box of 5


Tubes Pyrolytically Coated.
N9307835 HGA Advanced Platform Graphite Box of 20
Tubes Pyrolytically Coated.
B3130086 HGA Contact Cylinders 5 Pair
N3160182 Flame Burner Assembly - Metal NEB 1
Kit Tested
N3160179 Flame Burner Assembly - Plastic NEB 1
Kit Tested
09908265 Nebulizer Capillary Tubing 1
03030135 Nebulizer Cleaning Wires 1
03030405 Nebulizer Grease (Apiezon-L) 1
B3150458 High Sensitivity Nebulizer Capillary 1
Assembly
N3160143 Metal Body Nebulizer Assembly 1
N3160144 High Sensitivity Nebulizer Assembly 1

Table 6-6. Single Element Lamps

Lumina Part No. EDL Part No. Description

N3050103 Aluminum
N3050170 N3050670 Antimony
N3050105 N3050605 Arsenic
N3050115 N3050615 Cadmium
N3050114 Calcium
N3050119 Chromium
Replacement Parts for the PinAAcle 900 367

Table 6-6. Single Element Lamps

N3050121 Copper
N3050107 Gold
N3050126 Iron
N3050157 N3050657 Lead
N3050144 Magnesium
N3050145 Manganese
N3050134 N3050634 Mercury
N3050152 Nickel
N3050139 Potassium
N3050172 N3050672 Selenium
N3050148 Sodium
N3050191 N3050691 Zinc

Table 6-7. Multi-Element Lamps

Part No. Description

N3050202 Calcium, Magnesium


N3050204 Potassium, Sodium
N3050212 Copper, Iron, Manganese, Zinc, Cobalt,
Chromium, Copper, Iron
N3050217 Manganese, Nickel
N3050218 Aluminum, Calcium, Copper, Iron,
Magnesium, Silicon, Zinc
368 Maintenance

Table 6-8. Single Element Standards

125 mL 500 mL Description


Part No. Part No.
N9300184 N9300100 Aluminum
N9300180 N9300102 Antimony
N9300176 N9300107 Cadmium
N9303763 N9300108 Calcium
N9300173 N9300112 Chromium
N9300183 N9300114 Copper
N9303771 N9300126 Iron
N9300175 N9300128 Lead
N9300179 N9300131 Magnesium
N9303783 N9300132 Manganese
N9300177 N9300136 Nickel
N9303779 N9300141 Potassium
N9303785 N9300152 Sodium
N9300178 N9300168 Zinc
Replacement Parts for the PinAAcle 900 369

Table 6-9. THGA Graphite Tubes

Ultraclean Standard Standard with Description


Part No Part No. End Caps
Part No.
B3140361 B3000641 B3000653 5-Pack
B3140362 B0504033 B3000655 20-Pack
N3110147 100-Pack

Standard Description Quantity


Part No.
N9307830 THGA Advanced Platform Graphite Tubes 5-Pack
N9307831 THGA Advanced Platform Graphite Tubes 20-Pack
N9307832 THGA Advanced Platform Graphite Tubes 5-Pack
with End Caps
N9307833 THGA Advanced Platform Graphite Tubes 20-Pack
with End Caps

Table 6-10. THGA Contact Cylinder

Standard Standard with Description


Part No. End Caps
Part No.
B0504035 B3002103 1 Pair
B0504036 B3002102 5 Pairs
370 Maintenance

Table 6-11. HGA Graphite Tubes

Standard Description
Part No.
B0070699 Uncoated graphite tubes (not for use
with L’vov platforms) 50-Pack
B3001253 Uncoated graphite tubes (not for use
with L’vov platforms) 20-Pack
B3001264 Pyrocoated graphite tubes with
integrated platforms 20-Pack
B3001262 Pyrocoated graphite tubes with
integrated platforms 5-Pack
B0109322 Pyrocoated graphite tubes with grooves
for L’vov platforms 50-Pack
B3001254 Pyrocoated graphite tubes with grooves
for L’vov platforms 20-Pack
B0137111 Pyrocoated graphite tubes with grooves
for L’vov platforms
N9307834 HGA Advanced Platform Graphite
Tubes Pyrolytically Coated 5-Pack
N9307835 HGA Advanced Platform Graphite
Tubes Pyrolytically Coated 20-Pack

Table 6-12. HGA Graphite Contact

Standard Description (Left Hand


Part No. and Right Hand)
B0128495 1 Pair
Replacement Parts for the PinAAcle 900 371

Table 6-13. Nebulizers

Assembly End Caps Description


Part No. Part No.
N3160143 N3160102 Metal Body Nebulizer
N3160144 N3160111 High Sensitivity Nebulizer

Table 6-14. Nebulizer Assemblies and Spares


Replacement
Complete End Cap
O-Ring Needle
Description Type Needle Assemply Assembly
Type Assembly
P/N P/N
P/N

Stainless Steel Aqueous Stainless Viton N3160143 N3160102 03030354


(standard)
Plastic High Aqueous Platinum/ Viton N3160144 N3160111 B3150525
Sensitivity Iridium
(standard)
Plastic High Aqueous Platinum/ Kalrez N3160159 N3160189 N3160154
Sensitivity or Iridium
Organics
Plastic High Aqueous Tantalum Kalrez N3160152 N3160198 N3160146
Sensitivity or
(suitable for Organics
aqua regia in
addition to
organics)
Stainless Steel Aqueous Stainless Kalrez N3160158 N3160188 N3160153
or
Organics
Stainless Steel Aqueous Plastic Viton N/A N3160102 03030402
Stainless Steel Aqueous Platinum Viton N/A N3160102 03033124
Alloy
372 Maintenance

Table 6-15. Burner Heads

Part No. Flame Type Length Description


N3160134 Air-Acetylene 10 cm Single-slot
N3160142 Air-Acetylene 5 cm Single-slot
N3160140 Nitrous Oxide 5 cm Single-slot
Acetylene
N3160141 Air-Acetylene 10 cm Single-slot

Table 6-16. Graphite Furnace Autosampler Cups

Part No. Volume Composition Quantity


B0510397 1.2 mL Polypropylene 2,000
B3001566 2.5 mL Polypropylene 1,000
B3001567 7.0 mL Polypropylene 100
B0087056 2.0 mL Polyethylene 1,000
B0119079 2.0 mL Polystyrene 1,000
B0129303 3.5 mL Polystyrene 100
B0087600 2.0 mL Teflon® 30

Table 6-17. Matrix Modifiers

Part No. Volume Concentration Modifiers


B0190634 100 mL 1% Mg (as nitrate) Mg (NO3)2

B0190635 50 mL 1% Pd (as nitrate) Pd


Replacement Parts for the PinAAcle 900 373

Table 6-17. Matrix Modifiers

N9303445 100 mL 10% NH4H2PO4 NH4H2PO4

Table 6-18. Kalrez O-Rings for Sampling Accessories

Part Equivalent Descriptions Remarks


Number Part
(Kalrez Number
material) (Non-
Kalrez
material)
N3160157 N/A Nebulizer, End Cap, Kit-Tucson Organic
and Burner Head O- O-Rings Plastic
Ring Kit for Plastic Nebulizer
Nebulizer for
PinAAcle AA
N3160156 N/A Nebulizer, End Cap, Kit-Tucson Organic
and Burner Head O- O-Rings Stainless
Ring Kit for Stainless Steel Nebulizer
Steel Nebulizer for
PinAAcle AA
N3160192 N/A Nebulizer O-Ring Kit Kit-Tucson Organic
for Stainless Steel O-Rings Stainless
Nebulizer for Steel Nebulizer
PinAAcle AA
N3160193 N/A Nebulizer O-Ring Kit-Tucson Organic
Kit O-rings for O-Rings Plastic
Plastic Nebulizer for Nebulizer
PinAAcle AA
N3160194 N/A End Cap O-Ring Kit Kit-Tucson Organic
for PinAAcle AA O-Rings Endcap
374 Maintenance

Table 6-18. Kalrez O-Rings for Sampling Accessories

N3160158 N3160143 Metal Body Nebulizer Adjustable


Nebulizer Assembly Metal Body Tucson
on PinAAcle for Organic
Organics -tested
N3160159 N3160144 High Sensitivity Nebulizer Adjustable
Plastic Nebulizer Plastic Tested
Assembly on Organic
PinAAcle for
Organics - tested
09200276 09902015 O-ring(2) for (Metal O-Ring - Kalrez 6380
Body/Plastic) 9.25 X 1.78 MM
Nebulizer Assembly
09200271 09926083 & O-ring(1) for Metal O-Ring - Kalrez 6380
09902102 Body Nebulizer for 1.80 X 1.00 MM
PinAAcle AA
09200272 09926127 O-ring(1) for High O-Ring - Kalrez 6380
sensitivity Plastic 2.00 X 1.00 MM
Nebulizer Assembly
09200273 09902005 O-ring(2) for Metal O-Ring - Kalrez 6380
Body Nebulizer for 4.47 X 1.78 MM
PinAAcle AA
09200274 09902239 O-ring(1) for Metal O-Ring - Kalrez 6380
Body Nebulizer for 5.28 X 1.78 MM
PinAAcle AA
09200275 09200253 O-Rings(4) for O-Ring - Kalrez 6380
Endcap Assembly for 7.65 X 1.78 MM
PinAAcle AA
09200277 09902147 O-Ring(1) for Endcap O-Ring - Kalrez 6380
Assembly for 47.29 X 2.62 MM
PinAAcle AA
09200278 09200079 Burner head O-Ring O-Ring - Kalrez 6380
(1) for PinAAcle/ 24.99 X 3.53 MM
AAnalyst AA
Replacement Parts for the PinAAcle 900 375

Table 6-18. Kalrez O-Rings for Sampling Accessories

09200369 O-RING - O-rings for High O-Ring - Kalrez 6380


VITON 4.47 Sensitivity Plastic 1.42 x 1.52 mm
X 1.78 MM Nebulizer (Capillary
kit)
N/A 09200360 O-ring for Burner O-Ring - Viton 4.47
connector X 1.78 MM
376 Maintenance
Troubleshooting 7
Overview
This section describes the error messages for the system and their meaning. Where
possible, corrective actions are suggested.

Introduction
PerkinElmer spectrometers are designed for routine, trouble-free operation. Many
errors are diagnosed immediately as they occur and a message containing details
of the problem appears on the screen. Often this information enables you to solve
the problem quickly.

Some difficulties may not be so easily diagnosed and solved. For this purpose, the
following troubleshooting suggestions are included to help you determine whether
the difficulties are due to unsuitable analytical techniques, incorrect instrument
parameters, or a malfunctioning of the instrument. If, after checking the instrument
against the symptoms described below, the instrument appears to be
malfunctioning, we strongly recommend that you contact your local PerkinElmer
service representative.

Servicing of the instrument by someone other than a PerkinElmer trained and


authorized person will render the warranty null and void.
378 Troubleshooting

Performance Problems

Spectrometer

Problem Possible Cause(s) Corrective Action

Initialization process fails. Communication cables Make sure that you use the
between the computer, spec- correct cables, and connect
trometer, and accessories are them to the correct communi-
not connected correctly. cation ports. See Connecting
the Computer and Printer on
page 119.
Lamp connector does not fit Lamp is not a PerkinElmer Use the lamps recommended
in the socket. lamp. Lamp is the older series for your spectrometer.
For some older lamps you
may need an adapter cable.
Lamp will not light. Lamp connector not plugged Connect the lamp to the cor-
in. rect socket in the lamp com-
partment.
Lamp old or damaged. Install a new lamp. See
Lamps on page 160.
Lamp energy low or no Lamp starting to deteriorate. Allow the lamp to warm up.
energy. EDL lamps may need 45 min-
utes to warm up. May also
use the maximum current,
within the recommended
range.
Wrong EDL coding plug con- Connect the correct EDL cod-
nected. ing plug to the correct socket.
The lamp is old. Install a new lamp. See
Lamps on page 160.
Performance Problems 379

Problem Possible Cause(s) Corrective Action

Wrong entries in the Lamp Use the Lamp Setup window


Setup window or in the to set the correct wavelength,
method. slit, and current.
Dirty lamp end window. Clean the windows. See
Lamp Troubleshooting on
page 285.
Dirty furnace windows. Clean the windows. See
Graphite Furnace Mainte-
nance for the PinAAcle 900T/
900Z on page 295.
Dirty atomizer compartment Do not attempt to clean any
windows optical components inside the
optics compartment.
Something inside the graphite Remove the obstruction. If
tube is obstructing the beam the tube is damaged, install a
new tube. See Graphite Fur-
nace Maintenance for the
PinAAcle 900T/900Z on page
295.
Something in the atomizer Remove the obstruction.
compartment is obstructing
the beam.
The atomizer (furnace, quartz Align the atomizer as
tube (FIAS), burner) is not described on the help by
aligned. selecting F1 on the computer
keyboard.
Lamp energy fluctuating. Lamp starting to deteriorate. Allow the lamp to warm up
for 30 to 60 minutes, or install
a new lamp.
380 Troubleshooting

Problem Possible Cause(s) Corrective Action

The current setting is too low Use the Lamp Setup window
or high. to set the correct current. If
the current is too high, start
by reducing the current in
10% steps. With EDLs
reduce the current in 10-20
mA increments.
The system cannot find the EDL coding plug not con- Connect the correct EDL cod-
lamp nected, or the wrong EDL ing plug to the correct socket
coding plug is connected. as described in the user's
guide for your spectrometer.
The lamp is not coded, is an Use the lamps recommended
older lamp, or the lamp is not for your spectrometer.
from PerkinElmer.

Computer System

Problem Possible Cause(s) Corrective Action

Computer not communicating Communication cable is not Make sure that you use the
with spectrometer. connected correctly. correct cable, and connect it
to the correct communication
ports.
The software is in Simulator Reconfigure the software to
mode. communicate with the spec-
trometer. See the help by
selecting F1 on the computer
keyboard; keyword: Recon-
figure.
Performance Problems 381

Problem Possible Cause(s) Corrective Action

The software application Communication cable. Make sure that you use the
stops or hangs correct cable, and connect it
to the correct communication
ports.
An unsuitable power manage- Switch off the power manage-
ment system. ment feature of your com-
puter. Refer to the software
installation instructions for
your system.
The software is corrupted or Install the software correctly
not installed correctly. as described in the software
installation instructions for
the software.
Computer is not suitable or Make sure that the computer
has the wrong configuration. has the recommended specifi-
cation and configuration. See
the installation instructions
for the software.
The software application Use the Windows software to
stops or hangs. find the conflicts. For more
advice about suitable settings,
call your PerkinElmer office.
System is slow during data- The database has become In the Utilities tab select the
saving and data-recovery pro- very large. Data Manager icon to:
cedures. Make regular backups of the
data. Delete old, unwanted
data.
Archive wanted data on a dif-
ferent system, CDs or on
archiving devices to leave the
software database system free
to collect new data.
Pack the data.
382 Troubleshooting

Problem Possible Cause(s) Corrective Action

Problems with the network If you are using a network


connection. drive to store data, this can
sometimes be slow. You may
have to store data locally on
the hard disk during analyses,
then transfer the data to the
network drive later.
Refer to the software installa-
tion instructions for advice on
setting up your computer sys-
tem.
The printer or mouse do not Not installed correctly. See the instructions provided
operate correctly. with these devices.

Burner System

Problem Possible Cause(s) Corrective Action

Flame will not ignite. No fuel or oxidant. Make sure that the fuel and
oxidant gas supplies are
turned on and set at the cor-
rect pressures.
Air has diffused into the fuel You may have to perform the
line while the instrument was ignite cycle a number of times
idle. before all the air is expelled
from the fuel line.
Performance Problems 383

Problem Possible Cause(s) Corrective Action

The igniter is not aligned cor- Make sure that the end of the
rectly. igniter moves exactly over the
burner slot and that the burner
head is installed correctly.
See the users guide for the
burner.
Interlocks on the burner sys- Install the burner and drain
tem or drain are open. systems correctly. See the
users guide for the burner.

Install the burner head. See To


Burner head is not installed
Install the Burner Head on
correctly.
page 229.

Flame extinguishes automati- Low gas pressures. Make sure that the fuel and
cally. oxidant gas supplies are
turned on and set at the cor-
rect pressures.
Safety interlocks are open Make sure that the burner sys-
because the burner system has tem is correctly installed and
been changed. all the interlocks are closed.
See Reassembling the Burner
System on page 226.
Flame unstable. Drain system is not operating If there is not a constant,
correctly. smooth flow down the drain
tube, extinguish the flame and
re-install the burner and drain
system correctly. See Drain
System Maintenance on page
229.
Burner head dirty. Clean the burner head. See
Cleaning the Burner Head on
page 218.
384 Troubleshooting

Problem Possible Cause(s) Corrective Action

Low acetylene pressure. Sol- The cylinder pressure should


vent is being carried over be above 600 kPa, 6.0 bar, 87
with the acetylene. psig. If necessary, connect a
new cylinder, then set the out-
let pressure recommended for
your burner; see the users
guide for the burner. Do not
set a pressure greater than 100
kPa, 1.0 bar, 14.5 psig.
Variable air pressure. Set the correct outlet gauge
pressure; see the users guide
for the burner. With an air
compressor, clean the oil and
water filters, or install new
ones.
Contaminated gases. With an air compressor, clean
the oil and water filters, or
install new ones. If necessary,
connect new cylinders, then
set the correct outlet pres-
sures; see the users guide for
the burner.
Nebulizer is partially Clean the nebulizer and fit
blocked, not optimized, or new components, or install a
damaged. new nebulizer; see the users
guide for the burner. Then
adjust and optimize the nebu-
lizer; see the Nebulizer
Removal and Reinstallation
on page 235 and the help by
selecting F1 on the computer
keyboard.
Performance Problems 385

Problem Possible Cause(s) Corrective Action

Flashback of flame. Leaks in fuel or oxidant lines, Check for leaks using an
or drain system. approved leak detection kit.
Install the gas lines correctly
using approved components.
Blocked burner slot. Clean the burner head slot.
See Cleaning the Burner
Head on page 218.
Cylinder air contains excess Use compressed air not
oxygen. breathing air, which may be
enriched with oxygen.
Wrong regulators. Use the correct regulator for
each type of gas.
Wrong gases connected. Make sure that the correct
gases are connected to the
correct inlets on the spec-
trometer. See Connecting the
Gases on page 111.
386 Troubleshooting

Furnace and Furnace Autosampler

Problem Possible Cause(s) Corrective Action

The furnace does not operate Normal or special gas pres- Make sure the connections
sures too low. and pressures are correct. See
Connecting the Gases on
page 111.
No graphite tube installed, or Insert a new graphite tube.
the tube is defective. See Inserting the Graphite
Tube on page 298.
The contact breaker switch on This switch is activated when
the rear of the spectrometer is the system draws too much
in the OFF position. current. Wait a few moments
before putting this switch to
the on position. If this switch
is activated frequently, call
your local PerkinElmer
office.
Furnace overheats The cooling system is not Wait at least 30 minutes to
switched on or not operating allow the furnace to cool,
correctly. then switch on the cooling
system. If the furnace contin-
ues to overheat, contact your
local PerkinElmer office.

Insufficient coolant liquid in


the cooling system. The
coolant liquid should contain Fill up the cooling system to
10% glycerol and 90% water. the MAX mark.
See Filling the Cooling
System on page 129.
Performance Problems 387

Problem Possible Cause(s) Corrective Action

Rapid corrosion of tube Argon flow rate is too low. Set suitable flow rates in each
Make sure that the argon gas step of the furnace program.
(or Nitrogen gas, or any inert Set the correct inlet pressure
gas) is clean and DRY. The for the argon.
supply - piping and tubing, of
this clean and DRY gas to the
furnace must also be clean
and dry.
The drying step is not ade- With the software, use the
quate. Solvent fumes remain Method Editor to enter a suit-
in and around the tube after able furnace program. See the
drying, when raising to higher Recommended Conditions.
temperatures of pyrolysis and Ensure that there is 5 to 10
atomization. seconds left in the drying
step, for the vapor to come
completely out of the graphite
tube, before going to the
pyrolysis step when tempera-
ture can go up to above 550
°C.

The samples/solutions ana- Dilute the solutions, to reduce


lyzed may be very corrosive, its corrosiveness, the acid
and/or also contain high con- concentration, and to use
centration of acids, so the appropriate temperature pro-
tube life is shorter. gram that may contain slower
ramp, lower pyrolysis and
atomization temperatures.
Develop equitable tempera-
ture program. Please seek
advice from the PerkinElmer
Product Specialists.
388 Troubleshooting

Problem Possible Cause(s) Corrective Action

Autosampler does not go to The wrong configuration of Select the correct sample tray
the correct locations. the tray for the autosampler. exit the software and run the
Reconfigure utility. To run
the Reconfigure utility, click
on Start>All Programs >
PerkinElmer Syngistix for
AA> Reconfigure.r. See the
help by selecting F1 on the
computer keyboard.
Autosampler does not oper- The communication cable is Make sure that you use the
ate. not connected correctly. correct cable, and connect it
to the correct communication
port.

Autosamplers for Flame and Flow Injection

Problem Possible Cause(s) Corrective Action

Autosampler will not func- The autosampler is not Reconfigure the software to
tion. entered in the system configu- communicate with the spec-
ration or supported by this trometer. See the help by
version of software/system. selecting F1 on the computer
Use the system-supported keyboard; keyword: Recon-
autosampler. figure.
The autosampler is not If you are using the autosam-
switched on. pler with a controller, switch
this on.
The communication cable is Make sure that you use the
not connected correctly. correct cable, and connect the
cable to the correct communi-
cation port.
Performance Problems 389

Flow Injection System

Problem Possible Cause(s) Corrective Action

Computer cannot communi- FIAS not entered in the sys- Reconfigure the software to
cate with FIAS. tem configuration communicate with the spec-
trometer. See the help by
selecting F1 on the computer
keyboard; keyword: Recon-
figure or the software installa-
tion instructions.
Not switched on. Switch on.
Communication cable is not Make sure that you use the
connected correctly. correct cable, and connect the
cable to the correct communi-
cation port.
FIAS has the wrong IEEE or Set the correct address using
serial address. the DIP switches. Refer to the
user's guide for FIAS.

Gas pressure is too low. See No gas flow below.

No gas flow. Gas pressure is too low. The Switch off FIAS. If necessary,
gas supply is turned off or connect a new cylinder, then
empty. set the outlet pressure recom-
mended in the user's guide for
the flow-injection system.
Switch on FIAS.
The automatic gas stop is In the FIAS Control window,
active. click on Valve Fill/Inject.
Pump heads stop rotating. The pressure on the pump Use the pressure adjustment
magazines is too high screws to reduce the pressure.
390 Troubleshooting

Problem Possible Cause(s) Corrective Action

Solution is leaking from the The carrier flow rate exceeds Set the carrier flow rate to be
connections between the the aspiration rate of the neb- about 1-2 mL/min less than
flow-injection system and the ulizer. the aspiration rate of the neb-
nebulizer. ulizer.

Flame Analysis Technique

Problem Possible Cause(s) Corrective Action

Noisy, erratic signals. Contaminated burner If you aspirate aqueous solu-


tions after organic solvents or
oils, the absorption signals
generated can be noisy and
erratic. After aspirating
organic solvents or oils, fol-
low the cleaning procedure
described in the help by
selecting F1 on the computer
keyboard.
Unstable flame See Troubleshooting: See
Burner System on page 382.
The nebulizer sample tubing Install new tubing and make
is partially blocked, damaged, sure it remains immersed in
or not correctly immersed in the measurement solution.
the measurement solution.
The nebulizer is partially Clean the nebulizer or install
blocked or damaged. a new one. See Nebulizer
Removal and Reinstallation
on page 235.
Performance Problems 391

Problem Possible Cause(s) Corrective Action

Autosampler sample probe is Clean the probe and sample


partially blocked, damaged or tube or install new ones. Set
not correctly immersed in the the sample probe to the cor-
measurement solution. rect depth in the sample con-
tainers. See AS 900 Furnace
Autosampler Maintenance on
page 289.

The source lamp or the deute- With the software, use the
rium lamp is failing, or the Lamp Setup window to set
current is too high or too low the correct current. Install
new lamps. See Lamp Life on
page 285.
Characteristic concentration Wrongly prepared reference Prepare new fresh, correct
is too high. solution or blank. concentration solutions.
Poor sensitivity.
Poor detection limit.
See the sections above on
noisy, erratic signals.
Unsuitable measurement With the software, use the
parameters in the method. Method Editor to select suit-
able measurement parame-
ters.
Unsuitable flame conditions. With the software, use the
Method Editor to select suit-
able measurement parame-
ters. See the Recommended
Conditions.
Burner position is not opti- To optimize the burner; see
mized. the help by selecting F1 on
the computer keyboard.
392 Troubleshooting

Problem Possible Cause(s) Corrective Action

Nebulizer sample tubing is Install new tubing of the cor-


too long. rect length. With the soft-
ware, use the Method Editor
to select suitable values for
the read time and read delay.
See Nebulizer Removal and
Reinstallation on page 235.
The lamp current is too high From the Instrument tab
(line broadening) or too low. select the Lamp Setup icon
to open the Lamp Setup win-
dow to set the correct current.
A low-sensitivity wavelength With the software, use the
is selected. Method Editor to select the
correct wavelength. See the
Recommended Conditions.

Furnace Analysis Technique

Problem Possible Cause(s) Corrective Action

Poor sensitivity. Characteris- Wrongly prepared reference Prepare a new proven stan-
tic mass is too high. solution or blank. dard, freshly and accurately
prepared.
The standard solutions are too Prepare new standard solu-
"old" - solutions not prepared tions correctly.
fresh daily.
The standard and reference Prepare fresh acidified solu-
solutions are not acidified. tion daily.
The elements may drop out of
the solution.
Performance Problems 393

Problem Possible Cause(s) Corrective Action

See the sections on bad preci-


sion and erratic signals.
Poor sensitivity. Characteris- Unsuitable time/temperature With the software, use the
tic mass is too high (contin- program in the method. Method Editor to enter a suit-
ued). Matrix modifiers are not used able furnace program. See the
as recommended. Recommended Conditions. If
this does not work, seek
advice from the PerkinElmer
Product specialists.
Poor contact between the Clean the contact faces of the
graphite tube and the con- graphite tube and the con-
tacts. tacts. If the contacts show
signs of pitting or cracks,
replace them. Install a new
graphite tube and/or contact
cylinders if the change in the
tube does not resolve the
issue. See Inserting the
Graphite Tube on page 298.
Analyte has been lost during Use a lower pyrolysis tem-
the pyrolysis step. perature, especially if you are
not using a matrix modifier.
Unsuitable measurement With the software, use the
parameters in the method. Method Editor to select suit-
able measurement parame-
ters. See the Recommended
Conditions.
Gas flow during atomization Use zero flow during the
too high. atomization step. Select this
on the Furnace page in the
Method Editor.
394 Troubleshooting

Problem Possible Cause(s) Corrective Action

Low sensitivity wavelength Select the correct wavelength


selected. on the Instrument page in the
Method Editor. See the Rec-
ommended Conditions.
Poor sensitivity. Characteris- Graphite tube is old or faulty. Install a new tube.
tic mass is too high (contin-
ued).
The lamp current is too high From the Instrument tab
or too low. select the Lamp Setup icon
to open the Lamp Setup win-
dow to set the correct current.
Old or faulty lamp. Use a new lamp.
Unsuitable sample volume. For example, a volume of 5
uL will spread out less than
50 uL, which can affect the
sensitivity.
Accurate volume dispensed. Ensure that the autosampler
Dirty autosampler probe probe (pipette tip) is clean,
(Pipette tip), such that the and also the volume dis-
volume dispensed is lower pensed is accurate.
than intended, so resulting in
lower signal, so higher char-
acteristic mass.
Characteristic mass is too The reference solution or sol- Prepare new fresh standard
low. vent is contaminated. solutions accurately.
Signal is too high.
Performance Problems 395

Problem Possible Cause(s) Corrective Action

Contaminated during sample Metal parts of pipets can be


preparation. attacked by acidic fumes.
Plastic pipet tips may be con-
taminated. Rinse utensils
before using them and rinse
pipet tips several times with
sample solution before finally
dispensing the sample solu-
tion. Beware of the environ-
mental contaminants, in a
less-than ideal clean labora-
tory (dirty laboratory)
Autosampler cups contami- Rinse the cups in 10% v/v
nated and also the autosam- HNO3 overnight, then rinse
pler probe (pipette tip) is with deionized water
contaminated.
Increased baseline level, The lamp current is too high Check the current, the lamp
increased noise. or too low. might be failing and need
replacement. See also Trou-
bleshooting: Spectrometer on
page 378.
Carbon build-up in the tube is Install a new tube.
causing emission.
The furnace is not correctly Check the peak plot from a
aligned. dry firing using a Cr lamp at
357.9 nm. If necessary align
the furnace.
Contaminated contact cylin- Clean the contacts, or replace
ders. with a new pair of contacts.
See Cleaning the Graphite
Tube and Contacts on page
302.
396 Troubleshooting

Problem Possible Cause(s) Corrective Action

Very high blank signal for a Graphite tube or contacts are Install a new tube, and if nec-
dry firing contaminated. essary, new contacts. See
Inserting the Graphite Tube
on page 298.
Increased background signal Build up of matrix due to Increase the clean-out tem-
after several replicates inadequate clean-out. perature or time. Make a dry
firing to measure the signal.
Temperature above 2500 °C
for periods longer then 10
seconds will decrease the life-
time of the tube.
Poor precision The autosampler pipet tip is Make sure that the pipet tip
not aligned correctly. injects the solution at the cor-
rect place within the graphite
tube. Make sure that the pipet
tip enters the solution in the
sample cup. See AS 900 Fur-
nace Autosampler Mainte-
nance on page 357 or the help
by selecting F1 on the com-
puter keyboard.
The autosampler probe is not Flush the inside and outside
clean. of the autosampler probe with
isopropyl alcohol for five
minutes before re-use. Should
consider to add 1% methanol
in the rinsing solution for rou-
tine operation.
Performance Problems 397

Problem Possible Cause(s) Corrective Action

Large symmetrical double A chemical modifier or lower


peak could also mean roll- atomization temperature may
over, indication of exceed- eliminate this problem.
ingly high concentration, for
Zeeman background correc-
tion system.
Poor precision Lamp current is too low. Old See Troubleshooting: Spec-
or faulty lamp. trometer on page 378.
Build up of matrix due to Increase the clean-out tem-
inadequate clean-out. perature or time. Make a dry
firing to measure the signal.
Temperature above 2500 °C
for periods longer then 10
seconds will decrease the life-
time of the tube.
Spattering during the drying With the software, use the
or pyrolysis step. Method Editor to increase
the ramp time for the step.
Optimize the temperatures.
Spattering when the sample is The tube is too hot. With the
injected. software, use the Method
Editor to set the injection
temperature for the tube.
Make sure that the cooling
system cools the tube to the
correct temperature before the
autosampler injects the next
sample.
Samples are highly acidic Acidic samples cause more
rapid degredation of the tube.
High acid concentrations
have an influence on the opti-
mal drying temperature.
398 Troubleshooting

Problem Possible Cause(s) Corrective Action

Samples are in an organic sol- Organic solvents require indi-


vent. vidually optimized drying
temperatures.
Poor precision Poor drying conditions caus- Remedy is to carefully moni-
ing sample spattering. tor the drying with a dental
mirror and modify the time/
temp program in the software
as needed.

No rinse solution Fill the rinse bottle and prime


the rinsing system correctly.
The autosampler pipet tip is Make sure that the pipet tip
partly blocked or damaged. and the sample tube are clean
and undamaged. Replace
them if necessary. See AS 900
Furnace Autosampler Main-
tenance on page 357.
Air bubbles in the pumps Flush the air out of the
pumps. Prime the rinsing sys-
tem correctly. See AS 900
Furnace Autosampler Main-
tenance on page 357.
Valves: dirty or worn. Clean the valves or fit new
valves. See the user's guide
for the furnace. See Valve
Maintenance on page 359.
The furnace is not correctly Align the furnace. See
aligned. Graphite Furnace Mainte-
nance for the PinAAcle 900T/
900Z on page 295.
Performance Problems 399

Problem Possible Cause(s) Corrective Action

Erratic signals, In some situations, multiple In many situations, raising the


double peaks. peaks cannot be avoided. The atomization temperature will
errors from multiple peaks are eliminate the multiple peaks.
much less pronounced when Use appropriate matrix modi-
integrated absorbance is used fiers, and Temperature Pro-
as opposed to peak height. gram.
Spattering during the drying With the software, use the
or pyrolysis step. Method Editor to increase
the ramp time for the step.
Optimize the temperatures.
Poor contact between the Clean the contact faces of the
graphite tube and the con- graphite tube and the con-
tacts. tacts. If the contacts show
signs of pitting or cracks,
replace them. Install a new
graphite tube. See Inserting
the Graphite Tube on page
298.
Element is present as more A matrix modifier may elimi-
than one chemical species. nate this problem.
Build up of matrix due to Increase the clean-out tem-
inadequate clean-out perature or time. Make a dry
firing to measure the signal.
Temperature above 2500 °C
for periods longer then 10
seconds will decrease the life-
time of the tube.
Graphite tube was not condi- Condition the graphite tube.
tioned correctly. See Conditioning the Graph-
ite Tube on page 326 or the
help by selecting F1 on the
computer keyboard.
400 Troubleshooting

Problem Possible Cause(s) Corrective Action

Contaminated graphite tube Install a new graphite tube or


or contacts. new contacts. See Inserting
the Graphite Tube on page
298.

Flow Injection Analysis Technique

Problem Possible Cause(s) Corrective Action

Poor sensitivity. Reagents


Characteristic mass is too Old or wrongly prepared Prepare fresh solutions with
high. reagents, reference solution, the correct concentration.
or blank.
Wrong oxidation state of ele- See the recommended condi-
ment in the measurement tions for a suitable sample
solution. preparation procedure and
analytical conditions.
FIAS-flame system
Burner system is not opti- See the Troubleshooting sec-
mized when using Flame- tions: Burner System on page
FIAS technique. 382; Flame Analysis Tech-
nique on page 390.

Worn pump tubing. Install new pump tubing.


Performance Problems 401

Problem Possible Cause(s) Corrective Action

Leaks in the fluid system. Make sure that all the connec-
tions are tight. Tighten them
by hand or with the tube con-
nector key. Do not over-
tighten or distort the
connectors. If necessary,
install new connectors.
Contaminated or blocked Clean the entire fluid system
fluid system. as described in the users
Examples: guide for the flow-injection
Tin II chloride was previously system. Install the Reductant
used in the system. Change Kit.
A precipitate has blocked the
manifold.
FIAS-valve is blocked.
FIAS-MHS components
Poor sensitivity. The waste flow rate from the Adjust the flow; see the user's
Characteristic mass is too gas/liquid separator is too guide for the flow-injection
high. high - sample vapor is escap- system or the help by select-
ing with the waste. ing F1 on the computer key-
board.
The waste flow rate from the Adjust the flow. Clean and
gas/liquid separator is too low dry the sample transfer tube.
- liquid is entering the sample If it is contaminated, install a
transfer tube. new tube.
The membrane in the gas/liq- Install a new, dry membrane.
uid separator is wet.
The carrier gas flow is wrong. Optimize the carrier gas flow;
see the user's guide for the
flow-injection system or the
help by selecting F1 on the
computer keyboard.
402 Troubleshooting

Problem Possible Cause(s) Corrective Action

The carrier or reductant flow Make sure that the feed tubes
rates are wrong. for the carrier and reductant
are in the correct containers.
Set the correct flow rates as
described in the user's guide
for the flow-injection system
or the help by selecting F1 on
the computer keyboard.

FIAS-MHS: Quartz tube


Wrong quartz tube Use the correct quartz tube
recommended for the flow-
injection system.
The sample vapor in the Reduce the extraction rate
quartz tube is being extracted from the exhaust outlets of
too quickly, reducing the resi- the quartz tube.
dence time of the sample.
The cell windows and the Clean the windows and quartz
inside of the quartz tube are tube, and if necessary condi-
contaminated. tion the tube, as described in
the user's guide for the flow-
injection system.
Characteristic mass is too The reference solution or sol- Prepare new solutions cor-
low. vent is contaminated. rectly.
Signal is too high.
Performance Problems 403

Problem Possible Cause(s) Corrective Action

Contamination during sam- Metal parts of pipets can be


ple preparation. attacked by acidic fumes.
Plastic pipet tips may be con-
taminated. Rinse utensils
before using them and rinse
pipet tips several times with
sample solution before finally
dispensing the sample solu-
tion.
The autosampler containers Rinse the containers in 10%
are contaminated. v/v HNO3 overnight, then
rinse with deionized water.
The first replicate of a series The Fill step in the FIAS pro- With the software, use the
gives a high reading. grams is too short. Method Editor to increase the
time for the Fill step in the
FIAS program.
The first replicate of a series The Prefill step in the FIAS Use the Method Editor to
gives a low reading. programs is too short. increase the time for the Pre-
fill step in the FIAS program.
If possible, use a shorter tube
between the sample container
and the FIAS-valve.
Baseline shift. Air is trapped in the system. Make sure that all the connec-
tions are tight. Tighten them
by hand or with the tube con-
nector key. Do not over-
tighten or distort the
connectors. If necessary,
install new connectors. Flush
the fluid system thoroughly to
remove trapped air.
404 Troubleshooting

Problem Possible Cause(s) Corrective Action

Double peaks - FIAS MHS. The concentration of the ana- Dilute the samples.
lyte is too high.
The temperature of the quartz See the Recommended Con-
tube is too low for atomiza- ditions. Use the Method Edi-
tion to occur. tor to set the correct
temperature on the FIAS
page. If necessary, increase
the temperature setting
slightly.
Air is trapped in, or entering Make sure that all the connec-
the fluid system. tions are tight. Tighten them
by hand or with the tube con-
nector key. Do not over-
tighten or distort the
connectors. If necessary,
install new connectors. Flush
the fluid system thoroughly to
remove trapped air.
The carrier or reductant flow Make sure that the feed tubes
rates are wrong. for the carrier and reductant
are in the correct containers.
Set the correct flow rates as
described in the users guide
for the flow-injection system
or the help by selecting F1 on
the computer keyboard.
No acid in the sample solu- See the Recommended Con-
tions, or the acid concentra- ditions. Use more concen-
tion is too low. trated or more acid in the
sample solutions.
Index: A I-1

A Burner Assembly System 83


Accessories 73 Burner Chamber
Acetylene 25 cleaning 212
Acetylene Supply disassembling 224
maintenance 284 Burner Gases
Air Filter connecting 109
changing 207 Burner Head 221, 224
Air Supply 24 cleaning 218
aligning autosampler arm 148 installing 229
Aligning the Graphite Furnace 191 removing 224
alignment controls Burner Head Options 87
autosampler 152, 153 Burner Mount 88
Argon Gas Burner System
connect 115 cleaning 217
AS 900 Autosampler high temperatures 18
installing 135 introduction 85
Autosampler maintenance checklist 203
alignment controls 152, 153 reassembling 226
troubleshooting 388 setting up 180
unlocking autosampler arm 149 troubleshooting 382
autosampler C
adjusting immersion depth in sample Capillary Assembly
cup 156 cleaning 242
adjusting penetration depth in graphite changing
tube 148 graphite contacts 341
aligning autosampler arm 148 graphite shield ring 340
checking penetration depth in graphite graphite tube 337
tube 154 Checks
sample cups and reagent containers 146 periodic 202
setting up ??–159 Chemicals
B safety 13
Background Correction 93 Cleaning
Burner furnace windows 356
preconditioning 220 Graphite Contact surfaces 336
Burner Assembly instrument 33
removal 221
I-2 Index: D

cleaning removing 287


graphite contact surfaces 304 replacing 290
graphite contacts 335 E
graphite tube 335 EDL
closing the furnace installing 174
after contact change 324, 352 Electrical Connectors 79
Compressed Gases electrical protection xvi
handling 19 Electrical Safety 4
Computer System electromagnetic compatibility xvi
troubleshooting 380 Electrothermal Atomization
conditioning the graphite tube 340 hazards 30
Contact Cylinders safety practices 29
changing 305 Environmental Conditions 3
Cooling Connectors 82 Environmental Requirements 37
Cooling Requirements 66 European Requirements
Cooling System gas lines 112
filling 129 F
installing 126 Features
installtion 126 PinAAcle 900 Series System 71
D FIAS
Data System 96 safety practices 31
Decontamination 33 Flame
Dimensions 39 safe operation 25
Drain System 27, 89 Flame AnalysisTechnique 390
cleaning 231 Flame Atomization
emptying 232 hazards 28
Drain System Maintenance 229 safe practices 23
Drain Tube Flame Atomizer 93
installing 141 Flame Autosampler
precondition 133 troubleshooting 388
preconditioning 220 Flame Gas Requirements 56
replacing 233 Flame System
Drain Vessels 65 shut down 196
DRC Lamp Flame Technique
aligning 292 setting up 180
reassembling 290, 292 troubleshooting 390
Index: G I-3

Flashbacks 27 G
Flow Injection Autosampler Gas Connectors 82
troubleshooting 388 Gas Controls 89
Flow Injection System Gas Cylinders
troubleshooting 389 handling 23
Flow Injection Technique identiying 21
troubleshooting 400 safe handling 21
Fume Ventilation 41 safety 53
Furnace storing 22
troubleshooting 386 Gas Delivery Lines
furnace safety 53
closing after contact change 324, 352 Gas Hazards
opening for contact change 342 summary 20
Furnace Analysis Technique Gas Requirements 52
troubleshooting 392 graphite contact surfaces
Furnace Autosampler 96 cleaning 304, 336
troubleshooting 386 graphite contacts
Furnace Gas Requirements 55 changing 341
Furnace Gases cleaning 335
connecting 114 Graphite Furnace
Furnace System high temperatures 18
shut down 196 maintenance for the PinAAcle 900H
Furnace Systems 331
Zeeman Graphite 17 Graphite Furnace Atomizer 94
Furnace Technique Graphite Furnace Maintenance 295
setting up for the PinAAcle H 189 graphite shield ring
setting up for the PinAAcle T/Z 186 installing 340
Furnace Windows Graphite Tube
cleaning 328, 356 changing for the PinAAcle 900H 337
furnace windows cleaning 302, 335
cleaning 356 conditioning 326
refitting 355 conditioning for the PinAAcle 900H
removing 353 340
Fuses heating manually 327
changing 211 inserting 298
safety 6
I-4 Index: H

graphite tube Instrument Cleaning 202


changing 337 L
conditioning 340 Lab Space Requirements 38
heating 304, 336 Laboratory Safety Practice
removing contamination by heating 336 references 35
H Lamp
HCL replacing 285
installing 174 Lamp Cleaning 285
Heating the Graphite Tube 304, 336 Lamp Maintenance 285
High Sensitivity Plastic Nebulizer 257 Lamps
cleaning 262, 263 disposing 15
reinstalling 261 removing 176
removing 257, 270 left-hand contact
with Chemical Resistant O-Rings 269 installing 348
High Sensitivity Plastic Nebulizer with removing 346
Chemical Resistant O-Rings Line Power Requirements 47
cleaning 275 locating the system 126
I M
Ignitor Assembly 89 Magnetic Field 17, 46
immersion depth of pipet tip in sample cup Maintenance
156 graphite furnace 295
Impact Bead Maintenance Checklist 200
installing 265, 277 Mercury Hydride Systems
removing 266 safety practices 31
removing and replacing 264, 277 Metal Body Nebulizer
Inert Gas 29 adjusting for maximum absorbance 244
Installation optimum performance 256
general information 105 organic solvents 255
unpacking 103 removing 247
Installation Preparation 67 Metal Body Nebulizer with Organic Sol-
installing graphite components vent Resistant O-Rings
graphite shield ring 340 reinstalling 250
left-hand contact 348 Metal Nebulizer
right-hand contact 350 cleaning 243
Index: N I-5

N Nitrogen Gas
Nebulizer connect 115
high sensitivity nebulizer 257 Nitrous Oxide 24
high sensitivity plastic nebulizer with O
chemical resistant o-rings 269 opening the furnace
impact bead,removing and replacing for contact change 342
277 Optical Schematics 75
installation 135 Optical System 73
metal body 238 Organic Drain Vessel 235
reinstallling 241 Organic Solvents 255
removing 238 plastic nebulizer 268
metal body adjusting fir maximum ab- plastic nebulizer with chemical resis-
sorbance 244 tant o-rings 281
metal body removing 247 P
metal body, optimum performance 256 PC Configuration 67
metal cleaning 243 penetration depth of pipet tip in graphite
metal, reinstalling 241 tube 148, 154
metal, removing 238 pipet tip
performance 246 immersion depth in sample cup 156
plastic nebulizer with chemical resis- penetration depth in graphite tube 148,
tant o-rings adjust to maximum 154
absorbance 280 placing the system 126
plastic nebulizer with chemical resis- Plastic Nebulizer
tant o-rings to maintain opti- with chemical resistant o-rings adjust to
mum performance 282 maintain optimum performance
plastic, adjusting for maximum absor- 282
bance 267 with chemical resistant o-rings adjust to
plastic, cleaning 262, 263, 275 maximum absorbance 280
plastic, optimum performance 269 Power Consumption
plastic, reassembling 279 48
plastic, reinstalling 261 Precautions
plastic, removing 257, 270 Safety 2
removal 235
removing and replacing the impact
bead 264
I-6 Index: Q

Printer 67 setting up the autosampler ??–159


Product Line Experience 68 Source Lamps 64
Q Spacer
Quartz Tube Atomizer Cell 19 installing 266, 278
R Specifications 92
reagent containers 146 Spectrometer
regulatory information installation 105
electromagnetic compatibility xvi reinstalling 109
removing shut down 196
left-hand contact 346 troubleshooting 378
right-hand contact 344 Spectrometer Maintenance Checklist 206
Replacement Parts 160 Switches 79
right-hand contact System
installing 350 shut down 196
removing 344 System Components 72
S System Control 73
Safety U
precautions 2 unlocking autosampler arm 149
warning labels 6 Unpacking Instructions 103
Safety Checks 29 UV Radiation 17
Safety compliance xvi V
Safety Information xiv Vent Filter
Safety Interlocks 23, 29 changing 210
Sample Capillary Vent Hood Dimensions 44
installing 146 W
Sample Cove Waste Bottle
installing 144 installing 141
sample cups 146 Waste Disposal 15
Sample Tray Water Hoses
installing 144, 177 connecting 127
removing 180 WEEE Instructions 34
Sample Trays Weights 39
installing 177 windows
cleaning 356
refitting 355
removing 353
PerkinElmer, Inc.
710 Bridgeport Avenue
Shelton, CT 06484-4794, U.S.A.

Internet: http://www.perkinelmer.com
email: info@perkinelmer.com

PerkinElmer is a registered trademark of PerkinElmer, Inc.