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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
09936985 D February 2012
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

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 © 2012 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.


WinLab32 for AA, AAnalyst, Lumina, and THGA are trademarks of affiliates of PerkinElmer, Inc.
Windows is a trademark and Microsoft is a registered trademark of Microsoft Corporation.
Introduction ....................................................................................... xiii
Safety and Regulatory Information ............................................. xiii
How this Guide is Organized ........................................................xv
Conventions Used in this Manual ............................................... xvi
Software Help ............................................................................. xvi

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


Overview ...............................................................................................1
Precautions ............................................................................................2
Environmental Conditions ....................................................................3
Electrical Safety ....................................................................................4
Fuses .....................................................................................................6
EMC Compliance .................................................................................6
Europe .............................................................................................6
United States (FCC) ..............................................................................7
Warning Labels on the Instrument ........................................................7
Warning Labels at the Front of the Instrument ...............................9
Warning Labels at the Rear of the Instrument ..............................12
Warning Labels at the Sides of the Instrument .............................13
Safe Handling of Chemicals ...............................................................14
Waste Disposal ..................................................................................16
Contents of Waste Containers .......................................................16
Disposing of Defective Lamps .....................................................16
UV Radiation ......................................................................................18
Magnetic Field ....................................................................................18
Zeeman Graphite Furnace Systems (PinAAcle 900T and
PinAAcle 900Z) ............................................................................18
High Temperatures .............................................................................19
Burner System ...............................................................................19
Graphite Furnace ...........................................................................19
Quartz Tube Atomizer Cell ...........................................................20
Handling Compressed Gases ..............................................................20
Summary of Gas Hazards .............................................................21
Identifying Cylinders ....................................................................22
Safe Handling of Gas Cylinders .........................................................22
Identification of Gas Cylinders .....................................................23
Storing Cylinders ..........................................................................23
Handling Cylinders .......................................................................24
Safety Practices for Flame Atomization .............................................24
Safety Interlocks ...........................................................................24
Safe Use of Burner Gases .............................................................24
Air Supply .....................................................................................25
Nitrous Oxide (dinitrogen monoxide, N2O) .................................25
Acetylene ......................................................................................26
Safe Operation of the Flame .........................................................26
The Drain System .........................................................................27
Flashbacks .....................................................................................28
Hazards with Flame Atomization .................................................28
Safety Practices for Electrothermal Atomization ...............................29
Safety Interlocks ...........................................................................29
Inert Gas ........................................................................................30
Safety Checks ...............................................................................30
Hazards with Electrothermal Atomization ...................................30
Safety Practices for FIAS and Mercury Hydride Systems ..................31
Safety Checks ...............................................................................31
Hazards with FIAS and Mercury Hydride Systems ......................32
Decontamination and Cleaning ...........................................................33
Decontamination ...........................................................................33
Cleaning the Instrument ................................................................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
Dimensions and Weights ..............................................................39
Fume Ventilation ................................................................................41
Vent Hood Dimensions .................................................................44
Magnetic Field (PinAAcle 900T and 900Z Only) ..............................46
Line Power Requirements ...................................................................47
Power Consumption: .....................................................................48
Power Specification PinAAcle 900T and PinAAcle 900Z ...........48
Power Specification PinAAcle 900H ...........................................48
Power Specification PinAAcle 900F ............................................49
Power Specification For The Cooling System ..............................49
Noise Specifications .....................................................................50
Line Conditioners .........................................................................50
UPS Systems .................................................................................52
Power Outlets ................................................................................52
Gas Requirements ...............................................................................52
Gas Line Connections ...................................................................53
Safety of Gas Cylinders and Gas Delivery Lines .........................53
Gas Specifications .........................................................................55
Furnace Gas Requirements .................................................................55
Gas Specifications: .......................................................................55
Flame Gas Requirements ....................................................................56
Atomic Absorption Source Lamps .....................................................63
Drain Vessels ......................................................................................64
Cooling Requirements ........................................................................65
Furnace Cooling ............................................................................65
Furnace Power Supply Cooling ....................................................65
Cooling System .............................................................................65
External Cooling ...........................................................................65
PC Configuration and Printer .............................................................66
Installation Preparation .......................................................................66
Check for Damage ........................................................................66
Product Line Experience .....................................................................67
PC Skills .......................................................................................67

Chapter 3. System Description ............................................ 69


The PinAAcle 900 Series Spectrometer System .................................69
Concept .........................................................................................69
Features of the PinAAcle 900 Series System ...............................69
System Components .....................................................................71
System Control .............................................................................71
Accessories ...................................................................................72
The Optical System .......................................................................72
Optical System Schematics for the PinAAcle 900 Series .............74
The Electrical Connectors and Switches ............................................78
Operational On/Off Switches ........................................................78
Connectors and Controls on the Rear Panel .................................80
The Gas and Cooling Connectors .......................................................81
Furnace Cooling ............................................................................81
Furnace Gases ...............................................................................81
Burner Gases .................................................................................81
Burner Assembly System ....................................................................82
How the Burner System Works ....................................................84
Burner Head Options ....................................................................86
The Burner Mount ........................................................................87
The Ignitor Assembly ...................................................................87
Specifications ......................................................................................91
System Design: ............................................................................91
Background Correction .................................................................92
Flame Atomizer ............................................................................92
Graphite Furnace Atomizer ..........................................................93
Furnace Autosampler ....................................................................94
Data System ..................................................................................95
Physical Data - Instruments ..........................................................96
Physical Data - Cooling System ...................................................97

Chapter 4. Installation .......................................................... 99


Introduction .........................................................................................99
Unpacking Instructions .....................................................................101
Inspecting the Shipment ..............................................................101
Unpacking the PinAAcle 900 Series Spectrometer ....................101
Banding on the Box ....................................................................102
How to Unpack the Instrument ...................................................102
Recycling the Instrument Box ....................................................103
Before You Install the Spectrometer ................................................103
When the spectrometer arrives ...................................................103
Before the service engineer arrives .............................................103
When the service engineer arrives ..............................................104
If You Must Move and Reinstall the Spectrometer ..........................104
Preparing the Spectrometer to be Moved ...................................105
Moving the Spectrometer to Another Location ..........................105
Reinstalling the Spectrometer .....................................................107
Connecting the Burner Gases .....................................................108
Connecting the Gases ........................................................................109
Air ...............................................................................................109
Nitrous oxide ...............................................................................109
Acetylene ....................................................................................110
Converting Standard U.S. Gas Lines to
European Requirements ..............................................................111
Connecting the Furnace Gases ....................................................112
To Connect Argon (or Nitrogen) Only .......................................113
To Connect Both Argon and a Special Gas ................................115
Connecting the Computer and Printer ..............................................117
Electrical Connections ......................................................................119
Installing the Cooling System ...........................................................124
Locating the Cooling System .....................................................124
Connecting and Disconnecting the Water Hoses ........................125
Filling the Cooling System .........................................................127
Connecting the Drain System to the Burner .....................................128
Preconditioning A Drain Tube ...................................................131
Adding Water to the Drain Trap .................................................131
Nebulizer Installation ........................................................................132
Installing AS 900 Furnace Autosampler ...........................................132
Installing the Drain Tube and the Waste Bottle ..........................138
Installing Sample Tray and Cover ..............................................141
Installing the Sample Capillary .........................................................143
Filling and Flushing the Rinsing System ....................................143
To Align the Autosampler Tip in the Graphite Tube .................145
Checking the solution droplet delivery .......................................153
Installing S10 Autosampler ..............................................................156
Lamps ................................................................................................156
Replacement Parts .............................................................................156
Shipping List for the PinAAcle 900F ...............................................157
Shipping List for the PinAAcle 900H ...............................................158
Shipping List for the PinAAcle 900T ...............................................160
Shipping List for the PinAAcle 900Z ...............................................163

Chapter 5. Preparing the System ...................................... 165


Switching on the System ...................................................................165
Installing the Lamps ..........................................................................168
Lamp Compartment ....................................................................169
Installing and Connecting HCLs .................................................170
Electrodeless Discharge Lamps (EDL) .......................................170
Installing and Connecting EDLs .................................................170
Removing lamps .........................................................................172
Tips for installing lamps .............................................................172
Installing Sample Trays ....................................................................173
To remove the tray ......................................................................176
Setting up the System for Analyses Using the Flame Technique .....176
Setting Up the Burner System ....................................................176
Safety Checks for the Flame Technique .....................................177
Igniting the Flame .......................................................................178
Extinguishing the Flame .............................................................179
Setting up the System for Analyses Using the Furnace Technique
For the PinAAcle 900 T/Z ................................................................181
Locking the Furnace Cover in Place ...........................................181
Setting up the Analysis ...............................................................183
Setting up the System for Analyses Using the Furnace Technique
For the PinAAcle 900 H ...................................................................184
To use the furnace .......................................................................184
Aligning the Graphite Furnace ...................................................186
Setting up the AS 900 Autosampler .................................................190
Shutting Down the System ...............................................................191
To shut down the flame system ..................................................191
To shut down the furnace system ...............................................191
To shut down the spectrometer ...................................................191
Emergency Shutdown .................................................................192

Chapter 6. Maintenance ..................................................... 195


Introduction .......................................................................................195
General Maintenance Checklist ........................................................196
Instrument Maintenance Checklist ...................................................197
Cleaning the Instrument ....................................................................198
Checks ...............................................................................................198
Periodic Checks ..........................................................................198
Burner Maintenance Checklist ..........................................................199
Spectrometer Maintenance Checklists ..............................................202
General Preventative Maintenance Procedures ..........................202
Spectrometer Maintenance Checklist .........................................202
Changing the Air Filter .....................................................................203
Changing the Vent Filter ...................................................................205
Changing the Fuses ...........................................................................206
Cleaning the Burner Chamber ..........................................................208
Cleaning the Burner Chamber After Use With
Organic Solvents .........................................................................211
Cleaning the Burner Chamber After Aspirating Solutions
Containing Cu, Ag, or Hg ...........................................................212
Cleaning the Burner System .............................................................212
Flashbacks ...................................................................................213
Cleaning the Burner Head .................................................................214
Quick Cleaning Procedure ..........................................................214
Complete Cleaning Procedure ....................................................215
Checking the Slot Width .............................................................215
Pre-Conditioning a New Burner or Drain Tube ................................216
Removing the Burner Assembly From the Instrument .....................216
Removing the Burner Head ..............................................................219
Disassembling the Burner Chamber .................................................219
Reassembling the Burner System .....................................................221
To Install the Burner in the Spectrometer .........................................221
To Install the Burner Head ................................................................224
Drain System Maintenance ...............................................................224
Cleaning (or Flushing) the Drain System ...................................226
Emptying the Drain System ........................................................227
Replacing the Drain Tubing ........................................................228
Preparing the New Drain Tubing for Use ...................................229
Adding Water to the Drain Float Assembly ...............................229
Nebulizer Removal and Reinstallation .............................................230
Removing the Stainless Steel Nebulizer .....................................231
Reinstalling the Stainless Steel Nebulizer ..................................233
Cleaning the Stainless Steel Nebulizer .......................................235
Removing the High Sensitivity Plastic Nebulizer ......................236
Reinstalling the High Sensitivity Plastic Nebulizer ....................240
Cleaning the High Sensitivity Plastic Nebulizer .........................241
Complete Cleaning Procedure of High Sensitivity
Plastic Nebulizer .........................................................................243
Removing and Replacing the High Sensitivity
Plastic Nebulizer's Impact Bead .................................................244
Installing the High Sensitivity Plastic Nebulizer Spacer ..................245
Adjusting the Nebulizer for Maximum Absorbance .........................245
Using Organic Solvents ..............................................................246
Maintaining Optimum Nebulizer Performance ..........................247
Replacing Parts of Wear ...................................................................247
Burner System O-Rings ..............................................................247
Nebulizer O-Rings ......................................................................248
Maintaining the Acetylene Supply ...................................................249
Lamp Maintenance and Cleaning .....................................................250
Lamp Life ...................................................................................250
Lamp Troubleshooting ................................................................250
Replacing the Lamps ........................................................................250
Lamp Compartment Location .....................................................251
Removing and Replacing the Deuterium Arc Background
Corrector Lamp .................................................................................252
Removing the Deuterium Lamp Assembly ................................252
Replacing the Deuterium Lamp ..................................................255
Reassembling the Deuterium Lamp Assembly ...........................257
Aligning Deuterium Lamp ..........................................................257
Resetting the D2 Hours ...............................................................259
Graphite Furnace Maintenance for the PinAAcle 900T/900Z ..........260
Removing the Graphite Tube ......................................................260
Inserting the Graphite Tube ........................................................263
Cleaning the Graphite Tube and Contacts ..................................267
Cleaning the Contact Surfaces of the Graphite Tube and
Contacts ......................................................................................269
Changing the Contact Cylinders .................................................270
Tilting the Graphite Furnace Forward ........................................271
Resetting Cycles for Tubes and Contacts ...................................290
Conditioning the Graphite Tube .................................................291
Manually Heating the Graphite Tube .........................................292
Checking and Cleaning the Furnace Windows ...........................293
Tilting the Graphite Furnace Back Into Position ........................296
Graphite Furnace Maintenance for the PinAAcle 900H ...................296
Open the Furnace and Remove the Graphite Tube .....................296
Cleaning the graphite tube and graphite contacts ......................300
Changing the graphite tube ........................................................302
Conditioning the graphite tube ..................................................305
Changing the graphite contacts ..................................................306
Checking and cleaning the furnace windows .............................318
S10 Autosampler Maintenance .........................................................322
AS 900 Furnace Autosampler Maintenance .....................................322
Filling and flushing the rinsing system .......................................323
Valve Maintenance .....................................................................324
Routine Maintenance ..................................................................325
Checking the Valves ...................................................................325
Replacement Parts .............................................................................327
Replacement Parts for the PinAAcle 900 .........................................328

Chapter 7. Troubleshooting ............................................... 339


Overview ...........................................................................................339
Introduction ......................................................................................339
Performance Problems ......................................................................340
Spectrometer ...............................................................................340
Computer System ........................................................................342
Burner System .............................................................................344
Furnace and Furnace Autosampler .............................................348
Autosamplers for Flame and Flow Injection .............................350
Flow Injection System ...............................................................350
Analysis Flame Technique ..........................................................352
Analysis Furnace Technique .......................................................354
Analysis Flow Injection Technique ............................................362
Introduction xiii

Introduction

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.
xiv

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.
Introduction xv

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 System Description 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.
xvi

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.

• WinLab32-AA.chm. This software help file can be accessed by opening the


WinLab32 for AA 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 2000 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

Warning: Unauthorized Adjustments and Servicing


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

The instrument has been designed to protect the operator from potential electrical
hazards. This section describes some recommended electrical safety practices.

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.
Capacitors inside the instrument may still be charged even if the
instrument has been disconnected from all voltage sources.

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


supply must have a correctly installed protective conductor (earth ground) and
Electrical Safety 5

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.

Note Make sure that your laboratory has a matching receptacle for the IEC
60309 power plug.

The product is designed and manufactured, having regard to the state of the art, to
ensure that:

• the electromagnetic disturbance generated does not exceed the level above
which radio and telecommunications equipment or other equipment
cannot operate as intended;

• it has a level of immunity to the electromagnetic disturbance to be


expected in its intended use which allows it to operate without
unacceptable degradation of its intended use.

Use of this product in residential areas may cause interference and such use should
be avoided unless special measures are taken by the user to restrict emissions to a
level that allows the reception of broadcast emissions.

When working with the instrument:

• 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.

• Do not attempt to make internal adjustments or replacements except as


directed in the manuals.
6 Safety Practices

• 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 PerkinElmer Service engineer or a
similarly trained and authorized person.

• 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.

EMC Compliance

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

This equipment has been designed and tested to CISPR 11 Class A. In a


domestic environment it may cause radio interference, in which case,
! measures to mitigate the interference have to be taken.

Note Evaluate the electromagnetic environment prior to operation of the device.


United States (FCC) 7

United States (FCC)


This equipment has been tested and found to comply with the limits for a Class A
digital device, pursuant to part 15 of the FCC Rules. These limits are designed to
provide reasonable protection against harmful interference when the equipment is
operated in a commercial environment. This equipment generates, uses, and can
radiate radio frequency energy and, if not installed and used in accordance with the
instruction manual, may cause harmful interference to radio communications.
Operation of this equipment in a residential area is likely to cause harmful
interference in which user will be required to correct the interference at his own
expense.

Note Changes or modifications not expressly approved by PerkinElmer could


cause the instrument to violate FCC (U.S. Federal Communications
Commission) emission regulations, and because of this violation could
void the user's authority to operate this equipment.

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.

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.
8 Safety Practices

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.


Warning Labels on the Instrument 9

Warning Labels at the Front of the Instrument


Graphite Furnace Labels

1
3

Item Description Item Description


1 Warning - No Pacemakers. See Magnetic 3 Warning-Hot Surface
Field on page 18
2 Warning-Strong Magnetic Field

Item Description
1 Warning-Hot Surface (the PinAAcle 900H)
10 Safety Practices

Burner Locking Mechanism Label

Item Description
1 Press button to unlock the lever
Warning Labels on the Instrument 11

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
12 Safety Practices

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.
Warning Labels on the Instrument 13

Warning Labels at the Sides of the Instrument


Right Side of Instrument

Item Description
1 Caution-Do not restrict air intake or exhaust
14 Safety Practices

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.
Safe Handling of Chemicals 15

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.
16 Safety Practices

• 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
Waste Disposal 17

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.
18 Safety Practices

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.
High Temperatures 19

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.
20 Safety Practices

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.
Handling Compressed Gases 21

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.
22 Safety Practices

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.
Safe Handling of Gas Cylinders 23

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.
24 Safety Practices

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.
Safety Practices for Flame Atomization 25

• 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.
26 Safety Practices

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;
Safety Practices for Flame Atomization 27

• 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

The Drain System


• Always place the drain 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 vessel.

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

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


28 Safety Practices

• 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:
• 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.
Safety Practices for Electrothermal Atomization 29

• 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.
• 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.
30 Safety Practices

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;
• 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.
Safety Practices for FIAS and Mercury Hydride Systems 31

• 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.
• 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.
32 Safety Practices

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.

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 15 cm (6 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 141kg


(37.3 in) (26.7 in) (28.7 in) (310Ib.)
with AS 900 1038 mm
(40.9 in)
PinAAcle 900Z 950 mm 680 mm 730 mm 126kg
(37.3 in) (26.7 in) (28.7 in) (278Ib.)
with AS 900 1038 mm
(40.9 in)
PinAAcle 900H 950 mm 680 mm 730 mm 114kg
(37.3 in) (26.7 in) (28.7 in) (251Ib.)
with AS 900 1038 mm
(40.9 in)
PinAAcle 900F (No 950 mm 680 mm 730 mm 94kg
AS 900) (37.3 in) (26.7 in) (28.7 in) (207Ib.)
1038 mm
(40.9 in)
AS 900 280 mm 299 mm 317 mm 7.2 kg
(11.0 in) (11.7 in) (12.5 in) (15.8 Ib.)
Cooling System 200 mm 500 mm 375 mm 18.0 kg
(7.9 in) (19.7 in) (14.8 in) (39.6 Ib.)

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 840 mm (36 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 St. 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


laboratory.
Warning
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


For Vent Hood Alignment - Approximately 58 cm (23 in) from back of Instrument
to center of Atomizer. Approximately 29 cm (11.5 in) from tight side of Instrument
to center of Atomizer.
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 200 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 195 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 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 N9307511 10 KVA 50/60 Hz N0777613
900T/Z Conditioner True On-Line
Power
Conditioned
UPS
PinAAcle 6.0 KVA Line 220 50 Hz N9307523 10 KVA 50/60 Hz N0777613
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 3.8 KVA Line 120 60 Hz N9307512 5.2 KVA Line 50/60 Hz N0777511
900H Conditioner Conditioned
UPS
PinAAcle 3.8 KVA Line 220 50 Hz N9307522 5.2 KVA Line 50/60 Hz N0777511
900H Conditioner 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 (900T/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 N0777613.

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.

5.2 KVA Line Conditioned UPS 50/60Hz unit is currently available for the HGA
PinAAcle model 900H. The PerkinElmer part number for the 5.2 KVA UPS is
N0777511.

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 Requirements 53

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.

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.
54 Preparing Your Laboratory

• 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.
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
thoroughly after analyzing solutions with high silver or mercury
Warning 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.
Furnace Gas Requirements 55

• 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.
• 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


produced when the furnace temperature is above 2300 °C.
Warning
Make sure that the main laboratory fume ventilation system removes
all gases and fumes emitted by the furnace.
56 Preparing Your Laboratory

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.

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
Flame Gas Requirements 57

PinAAcle 900H and PinAAcle 900T systems require a minimum air pressure of
350 kPa (50-58 psig).

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
58 Preparing Your Laboratory

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.

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.

Suitable acetylene typically has a minimum purity specification of 99.6% with the
actual assay being about 99.8%. In general, ordinary welding-grade acetylene is
adequate for most AA analyses, though sometimes a particular tank may be
contaminated. Special higher purity "atomic absorption" grade acetylene is also
available from some vendors, and its use is recommended when the available
welding-grade acetylene is not sufficiently pure.

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
fittings is recommended.
Warning

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: Explosion Danger

! Acetylene line pressure from the tank to the instrument should never
exceed 103 kPa (1.03 bar, 15 psig). At the higher pressures, acetylene
Warning 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.

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.


Flame Gas Requirements 61

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.

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.
62 Preparing Your Laboratory

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


Atomic Absorption Source Lamps 63

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.
64 Preparing Your Laboratory

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). The PerkinElmer Atomax 1.5 inch lamps do not
require an adapter. The use of other 1.5 inch HCLs you will need an adaptor kit to
connect in the lamp compartment area. 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.
Cooling Requirements 65

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 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 makes 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.
66 Preparing Your Laboratory

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 14 °d or 2.5 mol/L

If the water is too cold or flowing too fast, moisture may condense on the
Caution 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 95.

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
warned about the weight of the instrument and informed that at least three and
preferably four adults are necessary to lift the instrument.
Product Line Experience 67

• 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 WinLab32 for AA.
The customer should have a fundamental knowledge of atomic absorption
spectroscopy.
68 Preparing Your Laboratory
System Description 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 analyses. The complete
system is operated from the associated computer using the Winlab32 for AA
software.

Features of the PinAAcle 900 Series System


Table 3-1. PinAAcle Instrument Configurations and Models

Part Number Model Configuration Nebulizer Recirculator


N3160080 PinAAcle 900T THGA + Flame Stainless Steel With
Recirculator
N3160081 PinAAcle 900T THGA + Flame Stainless Steel Optional
Recirculator
N3160082 PinAAcle 900T THGA + Flame High With
Sensitivity Recirculator
Plastic
70 System Description

Part Number Model Configuration Nebulizer Recirculator


N3160083 PinAAcle 900T THGA + Flame High Optional
Sensitivity Recirculator
Plastic
N3160070 PinAAcle 900H HGA + Flame Stainless Steel With
Recirculator
N3160071 PinAAcle 900H HGA + Flame Stainless Steel Optional
Recirculator
N3160072 PinAAcle 900H HGA + Flame High With
Sensitivity Recirculator
Plastic
N3160073 PinAAcle 900H HGA + Flame High Optional
Sensitivity Recirculator
Plastic
N3160060 PinAAcle 900Z THGA N/A With
Recirculator
N3160061 PinAAcle 900Z THGA N/A Optional
Recirculator
N3160050 PinAAcle 900F Flame Only Stainless Steel N/A
N3160051 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.
The PinAAcle 900 Series Spectrometer System 71

• 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 WinLab32 for AA software with which you control the
spectrometer system. WinLab32 for AA 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:

• 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 WinLab32 for AA software.

• The printer; this is optional but strongly recommended.

System Control
To control the spectrometer and perform your analyses, you use the WinLab32 for
AA application program, which runs under the Microsoft Windows operating
system. The computer keyboard, the screen, and the mouse form the user interface.
72 System Description

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 in the WinLab32
for AA online help.

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
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
EDL lamps. 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 900 Series Spectrometer System 73

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 74. In addition to the HCL and EDL source lamps
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.

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.
74 System Description

Optical System Schematics for the PinAAcle 900 Series

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


The PinAAcle 900 Series Spectrometer System 75

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


76 System Description

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


The PinAAcle 900 Series Spectrometer System 77

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


78 System Description

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.
The Electrical Connectors and Switches 79

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.
80 System Description

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
The Gas and Cooling Connectors 81

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 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.
82 System Description

Item Designation Function

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)


Burner Assembly System 83

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
84 System Description

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. As the heat produced by the
flame converts the sample 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 Winlab32 for AA 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.
Burner Assembly System 85

Figure 3-8. Block diagram of the burner system


86 System Description

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).

• N3161040: 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.
Burner Assembly System 87

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 N0400101
air-acetylene flame)
3 10-cm, single-slot burner head N0400102
4 10-cm, three-slot burner head N0400103
5 Burner head adjustment tool N3161040
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.

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
88 System Description

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 WinLab32 for AA 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.
Burner Assembly System 89

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


Item Description
1 Drain Interlock
2 Drain hose
3 Drain cap
4 Drain bottle
90 System Description

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.
Specifications 91

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.
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.
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 WinLab32 for AA™ software.
Lamp elements and recommended operating currents are
automatically recognized and set when using PerkinElmer
Lumina™ hollow cathode lamps.
92 System Description

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.
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.
Specifications 93

Flame Atomizer Description

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.
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.
94 System Description

Graphite Furnace Atomizer Description

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.

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.
Specifications 95

Furnace Autosampler Description

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

Data Control: Complete PC control using WinLab32 for AA software


operating under the Microsoft® Windows.
System Environment: Provides complete control of the instrument and its major
accessories plus data handling and storage.
Data Handling: Instrument readings linear in absorbance (-0.500 A to +2.000
A), concentration or emission intensity with continuously
variable scale expansion from 0.01 to 100 times. Integration
times operator-selectable from 0.1 to 120 sec. in increments of
0.1 sec. Reading modes include time-averaged integration,
non-averaged integration (peak area), and peak height
measurement. Includes built-in statistics. Up to thirty (30)
standards and a choice of proven calibration equations.
Reslope of the analytical curve using a single operator-selected
calibration standard.
Minimum PC Configuration
for system testing:
Factory Installed Operating System: Microsoft® Windows®7
Memory: 2 GB, Non-ECC, 1066 MHz, DDR3, 2 x 1GB, Four
DIMM slots
96 System Description

Data System Description

Hard Drive: 160 GB SATA, 7200 RPM


Networking: Integrated Gigabit Ethernet
External I/O Ports: 8 USB 2.0 (2 front, 6 rear), 1 Ethernet
(RJ45), 2 serial (9-pin), 1 VGA (DB-15, Display Port) out
Expansion Slots:
Slot 1: half-length, full-height, PCIe 2.0 x16 (75w max)
Slot 2: half-length, full-height, PCIe x1
Slot 3: half-length, full-height, 32-bit PCI 2.3
Slot 4: half-length, full-height, 32-bit PCI 2.3
Removable Media: DVD+/-RW SATA
Video: Integrated video, Intel® GMA4500
Mouse: USB optical mouse with scroll
Keyboard: USB Keyboard
Audio: Integrated High Definition Audio

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.
Specifications 97

Specifications Descriptions

Weight: PinAAcle 900T: 141 kg (instrument only).


PinAAcle 900Z: 126 kg (instrument only).
PinAAcle 900H: 114 kg (instrument only).
PinAAcle 900F: 94 kg (instrument only).
Electronics: The autosampler is powered from the spectrometer and is software-
controlled.
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 WinLab32 for AA 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.
98 System Description

Specifications Description

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.
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 101

• Before You Install the Spectrometer on page 103

• If You Must Move and Reinstall the Spectrometer on page 104

• Connecting the Gases on page 109

• Connecting the Computer and Printer on page 117

• Electrical Connections on page 119

• Installing the Cooling System on page 124

• Connecting the Drain System to the Burner on page 128

• Nebulizer Installation on page 132

• Installing AS 900 Furnace Autosampler on page 132

• Installing the Sample Capillary on page 143


100 Installation

• Installing S10 Autosampler on page 156

• Lamps on page 156

• Replacement Parts on page 156

• Shipping List for the PinAAcle 900F on page 157

• Shipping List for the PinAAcle 900H on page 158

• Shipping List for the PinAAcle 900T on page 160

• Shipping List for the PinAAcle 900Z on page 163


Unpacking Instructions 101

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 PinAAcle 900 Series in the box, can weigh as much as 160 kg (352
! lbs). When using a forklift to move the instrument between the unloading
area and the installation site, the instrument must remain on the shipping
Warning platform. Position the hand truck or forklift under the end of the box. The
instrument should not be lifted without the shipping platform.

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


102 Installation

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.

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 94 kg (207 lbs). Use proper lifting
! posture when lifting the instrument out of the carton. Be aware that most
of the weight is located at the right side of the instrument. It will want to
Warning tip forward when it is lifted out of the carton, so be prepared to support
that corner.
Before You Install the Spectrometer 103

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.

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.
104 Installation

• 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.

• 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.
If You Must Move and Reinstall the Spectrometer 105

Preparing the Spectrometer to be Moved


1. Close the WinLab32 for AA 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.

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 94 kg (207 lbs).
! Improper lifting can cause painful and sometimes permanent back injury.
Use proper lifting techniques and always use the handles to lift or
Warning move the instrument.
106 Installation

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.

For instructions on reinstallation see Reinstalling the Spectrometer on page 107.

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.
If You Must Move and Reinstall the Spectrometer 107

Figure 4-1. Furnace locking knob


Item Description
1 Furnace locking knob

Reinstalling the Spectrometer

Tools Needed

• Phillips screwdriver

• Adjustable wrench

• Flat bladed screwdriver


108 Installation

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.

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.
Connecting the Gases 109

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 111.

Connecting the Gases


Refer to the figure on page 110, 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.
110 Installation

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.

3
2

Figure 4-2. Connecting the gas lines


Item Description Item Description
1 Acetylene (C2H2) 3 Air

2 Nitrous Oxide (N2O)


Connecting the Gases 111

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.
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)
112 Installation

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

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.
Connecting the Gases 113

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

• 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 114 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 114.

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 114.

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.
114 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 115

To Connect Both Argon and a Special Gas


Refer to the figure on page page 116 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.
116 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 117

Connecting the Computer and Printer


We recommend placing the computer to the right of the instrument on the
workbench. See the figure on page 118 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.
118 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 119

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.
120 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 121

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.
122 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 123

Figure 4-9. Instrument on/off switch


Item Description
1 Instrument on/off switch

7. Start up the computer to install the WinLab32 for AA software.


124 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 125

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
126 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 127

See the following procedure Filling the Cooling System on page 127 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
128 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 125.

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 116.

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.
Connecting the Drain System to the Burner 129

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.
130 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 131

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.

• 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.
132 Installation

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.
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 230.

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.
Installing AS 900 Furnace Autosampler 133

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.


134 Installation

Figure 4-15. Autosampler mounting arm


Item Description
1 Front of instrument
2 Autosampler mounting arm
3 Boom receptacle
Installing AS 900 Furnace Autosampler 135

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.
136 Installation

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
Installing AS 900 Furnace Autosampler 137

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 136 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
138 Installation

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.
Installing AS 900 Furnace Autosampler 139

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.
140 Installation

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.
Installing AS 900 Furnace Autosampler 141

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 Options > Furnace Autosampler dialog in the WinLab32 software.

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.
142 Installation

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.

1 2

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


Item Description Item Description
1 Notch 2 Hub
Installing the Sample Capillary 143

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
2.5 mL; polypropylene 1–80 121, 124, 126, 129, 131,
134, 136, 139
7 mL; polypropylene 81–88 141–148

• Polypropylene containers are suitable for organic solvents

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.

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
144 Installation

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). 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.

4. Flush the system:


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.
Installing the Sample Capillary 145

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


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.

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:


• In the Furnace Control window, click on Align Tip.
The Align Autosampler Tip Wizard appears.
146 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 147

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.
148 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 149

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 WinLab32 for AA
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.
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
150 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 Align the
autosampler 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 151

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.
152 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 153

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 Online Help in WinLab32 for AA on how to create a method.

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


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

3. In the Automated Analysis Control window, on the Setup page, in the Locations
column, enter the autosampler location of the blank solution.

4. Start the method:


In the Automated Analysis Control window, on the Analyze 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 150.

7. Repeat step 4 through step 8 to dispense further aliquots of blank solution until
you are satisfied with the delivery.
154 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 155

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
156 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).

For information on adding or replacing see Replacing the Lamps on page 250.

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 157

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 N20 Burner Head Cleaner 1

09902219 Viton Burner Head O-Ring Kit 1


B0147498 Insert For Plastic Hose 2
B0190413 Organic Solvent Agent Card 1
N3161040 Burner Head Handle 1
B0501696 Air and Vent Filter (Felt) 1
09903004 Hose Clamp 7/32-5/8 SST 1
158 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 N20 Burner Head Cleaner 1

09902219 Viton Burner Head O-Ring Kit 1


B0147498 Insert For Plastic Hose 2
B0190413 Organic Solvent Agent Card 1
N3161040 Burner Head Handle 1
Shipping List for the PinAAcle 900H 159

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


160 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 161

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 N20 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


162 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 HGA Graphite Tubes Standard 5 Pack

B3120410 Press-In Gage THGA 1

B3120416 Press-In Sleeve 1

B3120420 Press-Out Tool 1

N3161040 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 163

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
164 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 HGA Graphite Tubes Standard 5 Pack

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 127).

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 167.

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 168 .

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.
166 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 Online Help in
WinLab32 for AA).

12. Start WinLab32 for AA: In the WinLab32 for AA group, double click on the
WinLab32 for AA icon.

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 168.

• Set up the burner system. See Setting up the System for Analyses Using the
Flame Technique on page 176.

• 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 181.

Procedures for shutting down the system are described see Shutting Down the
System on page 191.
Switching on the System 167

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


Shutdown on page 192

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
168 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 230.
Installing the Lamps 169

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)
170 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 171

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
172 Preparing the System

4. Connect the lamp cable to an EDL cable connection (see the previous figure)
to the EDL driver power supply connection. Use the Lamp Setup window in
WinLab32 for AA 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 169 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. On the Toolbar, click on Lamps. 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.

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


contamination can reduce the intensity of the radiation.
Installing Sample Trays 173

• 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.


174 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 175

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
176 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 165).

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


technique, go into WinLab32 for AA and select File > Change Technique >
flame.

3. Create or open a method (see the Online Help in WinLab32 for AA).

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


Inst page, for Signal Type, select Emisssion.

5. If you intent to make absorption measurements, install the lamps that you
require (see Installing the Lamps on page 168).

6. Set up the burner system (see Setting Up the Burner System on page 176)

7. Perform the safety checks (see Safety Checks for the Flame Technique on page
177).

8. Ignite the flame (see Igniting the Flame on page 178)

You should now set up the nebulizer, then optimize the burner and nebulizer before
checking the sensitivity. Refer to the Online Help in WinLab32 for AA.

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 132).
Setting up the System for Analyses Using the Flame Technique 177

2. Perform the safety checks (see Safety Checks for the Flame Technique on page
177).

3. Ignite the flame (see Igniting the Flame on page 178).

For the correct procedure to extinguish the flame see Extinguishing the Flame on
page 179.

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.

If WinLab32 indicates an interlock error, one or more of the following may be the
cause:

• 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.


178 Preparing the System

Igniting the Flame

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 177.

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 192 for the procedure to
follow after an emergency shutdown.

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 176).

2. Perform the safety checks (see Safety Checks for the Flame Technique on page
177).

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
167).

4. On the Toolbar, click on Flame. 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.
Setting up the System for Analyses Using the Flame Technique 179

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.

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 179.

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.
180 Preparing the System

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.

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.
Setting up the System for Analyses Using the Furnace Technique For the 181

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.

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.
182 Preparing the System

Figure 5-1. 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)

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.
Setting up the System for Analyses Using the Furnace Technique For the 183

Figure 5-2. 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 165).

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


technique go into WinLab32 for AA and select File > Change Technique >
furnace.
184 Preparing the System

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 Online Help in WinLab32 for AA).

5. Install the lamps that you require (see the procedure, Installing the Lamps on
page 168).

6. If required, install or change and condition a graphite tube (see Changing the
Contact Cylinders on page 270 and Conditioning the Graphite Tube on page
291).

7. Set up the furnace autosampler. Refer to the Online Help in WinLab32 for AA).

You should now optimize the analytical conditions. Refer to the Online Help in
WinLab32 for AA.

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 Online Help in WinLab32 for
AA).

2. Remove the burner assembly from the spectrometer (see Removing the Burner
Head on page 219).

3. Lift the furnace cover up.


Setting up the System for Analyses Using the Furnace Technique For the 185

Figure 5-3. 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
186 Preparing the System

4. Move In/Place the auto-sample. Lock the auto-sampler 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.


Setting up the System for Analyses Using the Furnace Technique For the 187

2
3

Figure 5-4. 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 properly aligned.

2. Where applicable, switch off the deuterium lamp background corrector.


188 Preparing the System

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 293).

5. Autozero the spectrometer:


1. In the Tools menu, click on Continuous Graphics.
2. Click on Autozero.
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.
Setting up the System for Analyses Using the Furnace Technique For the 189

Figure 5-5. 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 320).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.
190 Preparing the System

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 143).

2. Align the autosampler arm (see To Align the Autosampler Tip in the Graphite
Tube on page 145).

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 150).

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 152).

5. Check delivery of the solution droplet (see the procedure, Checking the
solution droplet delivery on page 153).
Shutting Down the System 191

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 192 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 179). Either aspirate the
solutions manually or use the flame autosampler.

2. Extinguish the flame and bleed the gas lines:

• In the Flame Control window, click on the Flame 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 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 322).

2. Shut down the furnace gases to the spectrometer at source.

To shut down the spectrometer


1. Exit WinLab32 for AA:
In the File menu, click on Exit.

2. Switch off the spectrometer at the operational on/off switch on the front panel.
192 Preparing the System

3. Switch off any accessories.

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 227).

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

Note Only use the on/off switch in an emergency. Do not use the on/off switch
as a routine shutdown procedure.

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.
Shutting Down the System 193

Figure 5-6. Location of instrument on/off switch


Item Description
1 Instrument On/Off switch
194 Preparing the System
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.
196 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.

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.

In accordance with safe laboratory practices, spilled material should be


cleaned up and disposed of 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 197

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 alignment. 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.

Caution If optic surfaces become dirty (e.g., from exposure to


laboratory vapors), cleaning should be done only by a
PerkinElmer service engineer.
198 Maintenance

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 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 199

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.


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.
200 Maintenance

Part Maintenance

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 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 stainless steel 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

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.
Burner Maintenance Checklist 201

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.


202 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 203

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 327, for the part number.

2. Locate the air filter on the right side of the instrument.


204 Maintenance

4
3

Figure 6-7. 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 Vent Filter 205

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 6-8. Location of Furnace Power Supply vents


Item Description
1 Furnace Power Supply vents

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.
206 Maintenance

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 6-9. Location of vent filter


Item Description
1 Vent filter

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.
Changing the Fuses 207

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 6-10. 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)

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:


208 Maintenance

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 209

Figure 6-11. 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.
210 Maintenance

1 2

3 4

Figure 6-12. Lever positions


Item Description
1-2 Latches closed position
3-4 Latches open position
Cleaning the Burner Chamber 211

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.
212 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
226.

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


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.
Cleaning the Burner System 213

• 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

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.

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.


214 Maintenance

• 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 217.

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.

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.


Cleaning the Burner Head 215

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 206.
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)
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.
216 Maintenance

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


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.
Removing the Burner Assembly From the Instrument 217

1
2

3
4

Figure 6-13. 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
218 Maintenance

4. The burner assembly is now accessible for maintenance. Remove the burner
assembly.

Figure 6-14. 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.
Removing the Burner Head 219

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 86.

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 216
220 Maintenance

2. Unscrew the retaining ring (see figure below) and pull out the burner o-ring.

3 1
5
4

Figure 6-15. Exploded view of the burner chamber assembly


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
Reassembling the Burner System 221

3. Remove the nebulizer from the end cap assembly. Refer to Removing the
Stainless Steel Nebulizer on page 231. Refer to Removing the High Sensitivity
Plastic Nebulizer on page 236

4. Clean the chamber. Place the parts in a detergent solution until they are
completely clean. See Cleaning the Burner Chamber on page 208 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. Pull the locking level forward until
it locks the burner assembly in place. The locking pin automatically locks.
222 Maintenance

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.
To Install the Burner in the Spectrometer 223

2
3

Figure 6-16. Drain hose attached


Item Description
1 Clamp
2 Drain hose
3 Drain Interlock
224 Maintenance

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 86.

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 full. 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.
Drain System Maintenance 225

2
1

Figure 6-17. Drain bottle attached


Item Description
1 Drain Interlock
2 Drain hose
3 Drain bottle
226 Maintenance

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.


Drain System Maintenance 227

Emptying the Drain System

Figure 6-18. 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
226.
228 Maintenance

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.
Drain System Maintenance 229

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.

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 229.

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.


230 Maintenance

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.

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 stainless steel or a high
sensitivity plastic nebulizer.

Table 6-2. Nebulizer Configurations


Model and Part No. Configuration Nebulizer
PinAAcle 900T- THGA + Flame Stainless Steel
N3160080 or N3160081
PinAAcle 900T- THGA + Flame High Sensitivity Plastic
N3160082 or N3160082
PinAAcle 900H- HGA + Flame Stainless Steel
N3160070 or N3160071
PinAAcle 900H- HGA + Flame High Sensitivity Plastic
N3160072 or N3160073
PinAAcle 900Z- THGA Only N/A
N3160060 or N3160061
PinAAcle 900F- Flame Only Stainless Steel
N3160050
PinAAcle 900F- Flame Only High Sensitivity Plastic
N3160051

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.
Nebulizer Removal and Reinstallation 231

Removing the Stainless Steel 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
stainless steel side arm upwards 90 degrees to the unlock position.

3
4

Figure 6-19. Stainless steel nebulizer


Item Description Item Description
1 Nebulizer in locked position 4 Nebulizer stainless steel arm in up
position
2 Nebulizer stainless steel arm 5 Nebulizer Interlock sensor
in locked position

3 Nebulizer in unlock position


232 Maintenance

3. Pull the nebulizer out from the nebulizer assembly end cap.

2 7 10
3 8
5

1 4 6 9 11

Figure 6-20. Exploded view of the stainless steel nebulizer


Item Description Item Description
1 Fine adjustment nut 7 Nebulizer body o-rings (2)
2 Sample capillary 8 O-ring
3 Washer 9 Venturi
4 Needle valve 10 Cap
5 Spring 11 O-ring
6 Nebulizer body

Note 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
capillary.

4. Inspect all the o-rings in the nebulizer assembly end cap. Replace any cracked
or damaged o-rings.
Nebulizer Removal and Reinstallation 233

5. Apply a small amount of Apiezon grease (Part No. 03030405) onto the o-rings
(Part No. 09902015). The nebulizer will then slide easily into the end cap.

6. Inspect the needle valve and replace if needed.

7. For information on cleaning the nebulizer, see Cleaning the Stainless Steel
Nebulizer on page 235.

Reinstalling the Stainless Steel 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.
234 Maintenance

1
2

4 3

Figure 6-21. Needle valve


Item Description
1 Needle valve assembly
2 Beveled edge of the hypodermic needle in the middle
needle valve assembly
3 Stainless steel nebulizer body
4 Needle valve in 1 o’clock position
Nebulizer Removal and Reinstallation 235

Note 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
capillary.

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 WinLab32 for AA software will indicate
that the safety lock is not satisfied.
A checked green box in the WinLab32 for AA software will indicate that
the safety locks are engaged and the instrument can be run.

The stainless steel nebulizer reinstallation is complete.

Cleaning the Stainless Steel Nebulizer


A low or erratic absorbance reading may indicate that the burner head or the
nebulizer and capillary tubing require cleaning. If you find that the burner slot is
clean, the problem is probably due to an obstruction in the nebulizer or capillary.

To clear an obstruction in the nebulizer

1. Aspirate pure solvent with the flame on until a stable baseline signal is
achieved. Then aspirate a known standard solution, within the linear range for
this element. Please refer to the Analytical Methods for AA Spectroscopy (Part
No. 03030152) for this concentration. The achieved absorbance should be +/-
236 Maintenance

20% the expected absorbance for this known concentration as shown in the
Analytical Methods for AA Spectroscopy (Part No. 03030152).

2. If you cannot obtain a satisfactory absorbance for this standard, 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


1. After you have taken the nebulizer apart, clean the components as follows:

2. Clean the capillary assembly using a mild laboratory detergent solution, or a


solvent such as isopropanol, preferably in an ultrasonic bath.

3. 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.

4. Rinse all the cleaned components thoroughly with deionized water.

5. 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.

6. After you have cleaned the components, reassemble the 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.
Nebulizer Removal and Reinstallation 237

3. Grasp the plastic arm from the locked position and firmly rotate it up (the arm
will be tightly in place).

2 1

6
7
5
8
9

Figure 6-22. 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 7 Nebulizer interlock sensor
position
4 Locking clamp 8-9 Latch
238 Maintenance

4. Wiggle the nebulizer out from the nebulizer assembly end cap.

5. The nebulizer assembly end cap is secured to the burner chamber by the latches
located on each side. Push both latches 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.

2 1
4
5
3

Figure 6-23. Plastic nebulizer assembly end cap 0-rings


Item Description
1 Nebulizer assembly end cap
2-6 O-rings

7. Take apart the nebulizer.


Nebulizer Removal and Reinstallation 239

4 5 7
9

1 2 3
6 8

11
10

Figure 6-24. Exploded view of the plastic nebulizer


Item Description Item Description
1 Sample capillary 7 Nebulizer body
2 Knurled needle valve adjustment knob 8 Spacer
3 Capillary holder 9 Impact bead
4 Spring and o-rings (2) 10 Apiezon grease
5 Locking washer 11 Cleaning wire
6 Nebulizer body o-rings (2)

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 grease (Part No.
03030405) is not applied on the needle valve.
240 Maintenance

8. Inspect the all the o-rings. Replace any cracked or damaged o-rings. Apply a
small amount of Apiezon grease (Part No. 03030405) 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 241.

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 capillary assembly (if it was removed).

2. Slide the assembled capillary assembly into the nebulizer body.

3. Line up the alignment key with the keyway in the nebulizer body.

4. Push the capillary assembly in until it bottoms out in the nebulizer body.

5. If you inserted the capillary 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. Where applicable, refit the fragile impact bead and spacer onto the plastic
nebulizer.

8. Reattach the nebulizer sample capillary to the nebulizer by screwing the


connector into the nebulizer needle valve.

9. Take the plastic arm on the nebulizer and lower it into the lock position and
lock it in place with the locking clamp.
Nebulizer Removal and Reinstallation 241

10. 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 WinLab32 for AA software will indicate
that the safety lock is not satisfied.
A checked off green box in the WinLab32 for AA 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


To maintain optimum nebulizer performance you must periodically clean the
sample capillary assembly, and occasionally replace it as needed.

When you aspirate concentrated samples with complex matrices, it is especially


important to keep the burner chamber and nebulizer free of deposits. 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 will encourage constant
drainage, which is essential for optimum burner system performance.

If you suspect that the nebulizer is causing poor sensitivity (e.g. cannot obtain
expected characteristic concentration) or poor precision (fluctuating absorbances),
before cleaning the nebulizer check that:

• The sample tube is in good condition (i.e. no kinks), is not too long, and is
clean. With a longer sample tube, the rate of sample uptake, and thus the
sensitivity, will decrease. Recommended length: 20 cm.

• The burner head is clean.

• The burner is correctly optimized.

• Correct operating parameters are used.


242 Maintenance

Clearing an Obstruction in the High Sensitivity Plastic Nebulizer


Clean the nebulizer capillary whenever you notice degradation in absorbance
values due to blockage of the capillary. There are two ways to clean the capillary
holder:

• The first (simplified) way should be used if the nebulizer is not difficult to
clear. This method involves simply passing one of the cleaning wires,
supplied, through the capillary holder.

• The second (complete) procedure requires shutting down the spectrometer,


removing the nebulizer from the end cap, and replacing the capillary
tubing. This procedure must be performed if you have no success with the
first method.

Simplified Cleaning Procedure For Nebulizer


For a simplified (light) cleaning of a standard the nebulizer sample capillary holder
see the following procedure:

Caution In the simplified method of cleaning the nebulizer the impact bead is not
removed. Use the cleaning wire carefully so as not to damage the impact
bead.

1. Unscrew the sample capillary from the nebulizer.

2. Take one of the cleaning wires (Part No. 03030135) supplied, and push it
through the capillary holder from its wider (open) end.

Note It may take several attempts to pass the wire through the nebulizer.

3. Repeat step 2 several times. Then replace the capillary (sample) tubing.

4. Run one or more standards to determine if the capillary holder has been
cleared. If it has been cleared, proceed with normal spectrometer operation;
otherwise, proceed with the next procedure.
Nebulizer Removal and Reinstallation 243

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 of the Nebulizer


1. Turn off the spectrometer and turn off all gas supplies.

2. Pull back the locking clamp that secures the nebulizer in place.

3. Rotate counter clockwise to the unlock position and gently pull the nebulizer
out of the burner end cap.

4. Remove the impact bead from the plastic nebulizer and, if using the impact
bead spacer, remove the spacer as well. Handle with care. (See the next page
for instructions.)

5. Unscrew the capillary tubing.

6. See the figure on page 239 and loosen and then remove the knurled needle
valve adjustment knob and locking washer.

7. Remove the capillary assembly from the nebulizer body.

Cleaning
1. While holding the capillary assembly in one hand, take one of the cleaning
wires (Part No.03030135) supplied.

2. Push it through the capillary assembly from its wider (open) end.

Note It may take several attempts to pass the wire through the nebulizer.
244 Maintenance

Cleaning the Nebulizer


1. After you have taken the nebulizer apart, clean the components as follows:

2. Clean the capillary assembly using a mild laboratory detergent solution, or a


solvent such as isopropanol, preferably in an ultrasonic bath.

3. 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.

4. Rinse all the cleaned components thoroughly with deionized water.

5. Inspect the all o-rings and clean them if necessary in mild laboratory detergent
solution, followed by a thorough rinsing with deionized water. If they look
damaged, replace them.

6. After you have cleaned the components, reassemble the nebulizer.

Removing and Replacing the High Sensitivity Plastic Nebulizer's


Impact Bead
The PinAAcle plastic nebulizer utilizes a ceramic, one-piece, impact-bead
structure (Part No. B0505086) which improves nebulization efficiency. The bead
itself is held by two fragile support arms.

The bead structure mounts directly on the plastic nebulizer's body assembly, see
the figure on page 239.

To Remove the Impact Bead


1. Hold the impact bead by its base only.

2. Rotate it approximately 1/8 turn counter clockwise before carefully lifting it


from the nebulizer's body assembly.

To Install the Impact Bead


1. Hold the impact bead by its base and carefully push it onto the body of the
plastic nebulizer in front of the venturi.
Installing the High Sensitivity Plastic Nebulizer Spacer 245

2. Then rotate it, holding only the base, approximately 1/8 turn clockwise, i.e.,
until it reaches a stop and "locks" itself.

Installing the High Sensitivity Plastic Nebulizer Spacer


The plastic nebulizer assembly can be used with or without the spacer. Maximum
sensitivity for Air-Acetylene elements can be achieved without the use of the
spacer.

The addition of the spacer reduces the amount of sample delivered to the flame. It
is recommended to use the spacer for all elements analyzed with the nitrous oxide-
acetylene flame and for elements which are air-acetylene flame sensitive such as
calcium, chromium and gold. When analyzing some complex sample matrices, it
may be desirable to add the spacer to reduce chemical interferences.

To Install the Spacer


1. Hold the impact bead by its base only.

2. Rotate it approximately 1/8 turn counter clockwise before carefully lifting it


from the nebulizer's body assembly.

3. Place the spacer onto the back of the nebulizer and replace the impact bead.

4. Rotate the bead 1/8 turn clockwise to "lock" the bead in place.

Adjusting the Nebulizer for Maximum Absorbance


Adjust the nebulizer to achieve maximum absorbance as follows:

1. Ignite the flame.

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.

3. Aspirate a blank and let the flame stabilize.


246 Maintenance

4. If you see bubbles at the end of the capillary tube (in the sample solution),
loosen the nebulizer locking nut and slowly turn the adjustment nut clockwise
until the bubbling stops.

5. Aspirate a standard and adjust the burner position. Optimize the burner head
position through the WinLab32 for AA software.

6. While still aspirating the standard, turn the nebulizer locking nut clockwise
until it is free of the nebulizer adjustment nut.

7. Slowly turn the nebulizer adjustment nut counter clockwise until bubbles begin
to appear at the end of the capillary tube in the sample solution.

8. Slowly turn the nebulizer adjustment nut clockwise until the absorbance goes
to a maximum and then begins to decrease.

9. Lock the nebulizer adjustment nut in its current (optimum) position by turning
the nebulizer locking nut counter-clockwise while carefully holding the
nebulizer adjustment nut, until this locking nut locks the adjustment nut.

10. Check the characteristic concentration as instructed in your spectrometer


manual. 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. These organic solvents can also act as a fuel for the flame as well. The
normal nebulizer uptake rate is typically 6-8 mL/min.

By reducing the uptake rate to 2-4 mL/min, it is usually possible to operate with a
leaner (blue) flame than is possible with higher nebulizer uptake rates. This leaner
flame typically provides improved precision, particularly when aspirating xylene.

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.
Replacing Parts of Wear 247

Note The uptake rate is easily measured by using a graduated cylinder.

Maintaining Optimum Nebulizer Performance


To maintain optimum nebulizer performance, you must periodically clean the
capillary assembly, and occasionally replace the capillary (sample) tubing. See the
figure on page 239 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 heads, 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 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
capillary holder 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.
248 Maintenance

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 is 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.

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 249

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.
250 Maintenance

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 are warrantied 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
Replacing the Lamps 251

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 6-25. Accessing the lamp compartment


Item Description
1 Lamp compartment cover
252 Maintenance

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. Using the WinLab32 for AA software click on the Lamp icon to display the
Lamp Setup page.

3. In the LampSetup 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. N3160803

• ultraviolet-absorbing safety glasses

• phillips head screwdriver

Removing the Deuterium Lamp Assembly


1. Turn OFF the power switch and unplug the power cord.
Removing and Replacing the Deuterium Arc Background Corrector Lamp 253

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 6-26. 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.
254 Maintenance

4. Carefully slide the D2 lamp assembly away from the instrument.

3
2

Figure 6-27. Deuterium lamp assembly


Item Description
1 Thumbscrew
2 D2 Lamp

3 Bracket
Removing and Replacing the Deuterium Arc Background Corrector Lamp 255

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.
256 Maintenance

1 2

Figure 6-28. Accessing the D2 lamp compartment

Item Description
1 D2 lamp

2 Cutout
3 Alignment pin

6. Plug in the lamp.


Removing and Replacing the Deuterium Arc Background Corrector Lamp 257

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 lam, see Removing the Deuterium Lamp Assembly on page 252 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.


258 Maintenance

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.
Removing and Replacing the Deuterium Arc Background Corrector Lamp 259

Figure 6-29. Location of the alignment screws of the deuterium lamp


Item Description
1 Horizontal alignment
2 Vertical alignment

The alignment procedure is now complete.

Resetting the D2 Hours

After aligning the deuterium lamp you need to reset the hours.

1. Select Tools > Diagnostics > Spectrometer tab.


260 Maintenance

2. Click the Advanced Tools... 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 side. Tilt the front contact housing downward.
See the following figure.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 261

2
1

Figure 6-30. 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.
262 Maintenance

Figure 6-31. Insertion/removal tools


Item Description
1 Graphite tube holder (insertion/removal tool)
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 263

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 6-32. 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.
264 Maintenance

Figure 6-33. Graphite tube


Item Description
1 Optical path
2 Rear contact
3 Sample Injection closing hole

2. Use the insertion/removal tool provided to insert the graphite tube into the rear
contact.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 265

Figure 6-34. 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).
266 Maintenance

2 1

Figure 6-35. 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 291.
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 292).
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 267

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.
268 Maintenance

1
4

4
3

Figure 6-36. Graphite components


Item Description
1 Rear contact
2 Graphite tube
3 Front contact
4 Optical path
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 269

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 292).
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 260).

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 270).
270 Maintenance

3. Heat out the graphite tube to remove contamination (see Manually Heating the
Graphite Tube on page 292).

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.

To Open the Furnace For Contact Changes


1. Make sure that the furnace is cool.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 271

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 296.

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.
272 Maintenance

Figure 6-37. 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 .


Graphite Furnace Maintenance for the PinAAcle 900T/900Z 273

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 271.

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

Figure 6-38. 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.
274 Maintenance

Figure 6-39. 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.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 275

Figure 6-40. 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.
276 Maintenance

Figure 6-41. 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
271.

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).
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 277

Figure 6-42. Contact removal tool

Note Make sure that you do not bend or twist the temperature sensor connector.
Also, do not damage the insulating washers.
278 Maintenance

1
4

3 5

Figure 6-43. 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
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 279

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 6-44. Furnace removal tool


Item Description
1 Furnace removal tool
2 Rear contact housing
280 Maintenance

7. Use the hex-driver to screw the bolt on the removal tool into the tool to push
out the contact.

Figure 6-45. 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.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 281

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 271.

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.
282 Maintenance

4
1
2
3

Figure 6-46. 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.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 283

Figure 6-47. 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.
284 Maintenance

Figure 6-48. 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 327.

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.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 285

Figure 6-49. 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:


286 Maintenance

• 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 6-50. 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.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 287

1
2
4

Figure 6-51. 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.
288 Maintenance

Figure 6-52. 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 327.

11. Push the optical sensor into the rear contact housing. Make sure that you do not
damage the O-ring.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 289

Figure 6-53. 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 296).

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 263).
290 Maintenance

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 291).

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 292).

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.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 291

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 292) 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 Toolbar, click on Furnace.

2. In the Furnace Control window, click on Condition Tube.


The system uses a special furnace program to heat the tube to successively
higher temperatures.
292 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

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 Toolbar, click on Furnace.

2. In the Furnace Control window, click on the Cleanout Temp. entry field and
type the required temperature (e.g. 2500 °C).
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 293

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 296).

4. Use the key provided to unscrew the left-hand and the right-hand windows
from the furnace.
294 Maintenance

Figure 6-54. Window key


Item Description
1 Window key
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 295

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 6-55. 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.
296 Maintenance

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 296).

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 272.

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
Graphite Furnace Maintenance for the PinAAcle 900H 297

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 6-56. 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.
298 Maintenance

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
sample introduction hole in the tube.
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 6-57. Speed Reducer


Item Description
1 Speed Reducer
Graphite Furnace Maintenance for the PinAAcle 900H 299

1
2

3 4 6
5

Figure 6-58. 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
300 Maintenance

5. If you have installed a new graphite tube, perform the procedure outlined in
Conditioning the graphite tube on page 305.
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
186).
8. Check alignment of the furnace autosampler (see To Align the Autosampler
Tip in the Graphite Tube on page 145).

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 301.

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.
Graphite Furnace Maintenance for the PinAAcle 900H 301

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 318).
2. Open the furnace and remove the graphite tube (see Open the Furnace and
Remove the Graphite Tube on page 296).
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 306).
302 Maintenance

5. Insert the graphite tube and close the furnace (see Open the Furnace and
Remove the Graphite Tube on page 296).
6. Refit the windows (see To refit the windows: on page 320).
7. Condition the graphite tube (see Conditioning the graphite tube on page 305).
Changing the graphite tube

2 3
1

Figure 6-59. 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.
Graphite Furnace Maintenance for the PinAAcle 900H 303

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 296).
304 Maintenance

Figure 6-60. Installing the graphite shield


Item Description
1 Graphite shield ring
2 Graphite shield ring installed
Graphite Furnace Maintenance for the PinAAcle 900H 305

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 296).

4. If you have installed a new graphite tube, perform the procedure outlined in
Conditioning the graphite tube on page 305.
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
306 Maintenance

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 Toolbar, click on Furnace Control.

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 307).
Graphite Furnace Maintenance for the PinAAcle 900H 307

2. Remove the right-hand contact (see To remove the right-hand contact: on page
308).
3. Remove the left-hand contact (see To remove the left-hand contact: on page
311).
4. Install a new left-hand contact (see To install the left-hand contact: on page
313).
5. Install a new right-hand contact (see To install the right-hand contact: on page
315).
6. Insert the graphite tube and close the furnace (see To close the furnace after
contact change: on page 317).
7. Condition the graphite tube (see Conditioning the graphite tube on page 305).
8. Align the furnace (see Aligning the Graphite Furnace on page 186).
9. Align the autosampler (see To Align the Autosampler Tip in the Graphite Tube
on page 145).
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 WinLab32 for AA:
In the File menu, click on Exit.
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 318).

5. Open the furnace manually and remove the graphite tube:


1. Turn off the normal and special gas supplies.
308 Maintenance

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 6-61. Contact change


Item Description
1 Graphite shield ring

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
Graphite Furnace Maintenance for the PinAAcle 900H 309

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.


310 Maintenance

2
3

4
1

Figure 6-62. Remove the right-hand contact


Item Description Item Description
1 Bolt 4 Optical sensor
2 Extractor 5 Traction nut
3 Right-hand contact
Graphite Furnace Maintenance for the PinAAcle 900H 311

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.


312 Maintenance

2
1

4
3

Figure 6-63. Remove the left-hand contact


Item Description Item Description
1 Bolt 3 Left-hand contact
2 Extractor 4 Traction nut
Graphite Furnace Maintenance for the PinAAcle 900H 313

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.


314 Maintenance

2 3
4
1

Figure 6-64. 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
Graphite Furnace Maintenance for the PinAAcle 900H 315

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.
316 Maintenance

1 2
3

Figure 6-65. 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
Graphite Furnace Maintenance for the PinAAcle 900H 317

6. Slide the graphite shield ring with its large flat face toward the furnace block
over the left-hand contact.

Figure 6-66. 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 296).

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 320).

5. Switch on the instrument power.


318 Maintenance

6. Start WinLab32 for AA.

7. Condition the graphite components (see Conditioning the graphite tube on


page 305).

8. Check alignment of the furnace (see Aligning the Graphite Furnace on page
186).

9. Check alignment of the furnace autosampler (see To Align the Autosampler Tip
in the Graphite Tube on page 145).

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.


Graphite Furnace Maintenance for the PinAAcle 900H 319

Figure 6-67. 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.


320 Maintenance

Figure 6-68. 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.
Graphite Furnace Maintenance for the PinAAcle 900H 321

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
318).

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 6-69. 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.
322 Maintenance

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 320).

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 94.

For AS 900 installation information see Installing AS 900 Furnace Autosampler


on page 132.

Table 6-3. 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.
AS 900 Furnace Autosampler Maintenance 323

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.


324 Maintenance

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. 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.
AS 900 Furnace Autosampler Maintenance 325

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.
The Align Autosampler Tip Wizard appears.
326 Maintenance

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 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.
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.


Replacement Parts 327

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.

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.
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
328 Maintenance

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 6-4. Consumables for the PinAAcle 900

Part No. Description Quantity


03031573 N20 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
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
Replacement Parts for the PinAAcle 900 329

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 STD-HGA 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
N3161040 Burner Head Handle 1
B0501696 Air and Vent Filter (Felt) 1
09290587 USB Extension Cable 1
N3160143 Nebulizer Adjustable Stainless Steel 1
Kit Tested
N3160144 Nebulizer Adjustable Plastic Kit 1
Tested
N3160162 Electric Heated FIAS MHS Cell Kit 1
Assembly
N3160161 Zeeman Heated Cell Assembly 1
Adapter
330 Maintenance

N3160809 Burner Chamber Holder Assembly 1


N3160102 Endcap Assembly - Stainless Steel 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
B3130086 HGA Contact Cylinders 5 Pair
N3160182 Flame Burner Assembly - Stainless 1
Steel NEB Kit Tested
N3160179 Flame Burner Assembly - Plastic NEB 1
Kit Tested
Replacement Parts for the PinAAcle 900 331

09908265 Nebulizer Capillary Tubing 1


03030135 Nebulizer Cleaning Wires 1
03030405 Nebulizer Grease (Apiezon-L) 1
B3150458 High Sensitivity Nebulizer Capillary 1
Assembly
N3160143 Stainless Steel Nebulizer Assembly 1
N3160144 High Sensitivity Nebulizer Assembly 1

Table 6-5. 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
N3050121 Copper
N3050107 Gold
N3050126 Iron
N3050157 N3050657 Lead
N3050144 Magnesium
N3050145 Manganese
N3050134 N3050634 Mercury
N3050152 Nickel
332 Maintenance

Table 6-5. Single Element Lamps

N3050139 Potassium
N3050172 N3050672 Selenium
N3050148 Sodium
N3050191 N3050691 Zinc

Table 6-6. 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
Replacement Parts for the PinAAcle 900 333

Table 6-7. 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
334 Maintenance

Table 6-8. 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

Table 6-9. THGA Contact Cylinder

Standard Standard with Description


Part No. End Caps
Part No.
B0504035 B3002103 1 Pair
B0504036 B3002102 5 Pairs
Replacement Parts for the PinAAcle 900 335

Table 6-10. 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 5-Pack

Table 6-11. HGA Graphite Contact

Standard Description (Left Hand


Part No. and Right Hand)
B0128495 1 Pair

Table 6-12. Nebulizers

Assembly End Caps Description


Part No. Part No.
336 Maintenance

Table 6-12. Nebulizers

N3160143 N3160102 Stainless Steel Nebulizer


N3160144 N3160111 High Sensitivity Nebulizer

Table 6-13. 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 6-14. 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
Replacement Parts for the PinAAcle 900 337

Table 6-15. Matrix Modifiers

Part No. Volume Concentration Modifiers


B0190634 100 mL 1% Mg (as Mg (NO3)2
nitrate)
B0190635 50 mL 1% Pd (as nitrate) Pd
N9303445 100 mL 10% NH4H2PO4 NH4H2PO4
338 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.
340 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 117.
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 156.
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 156.
Performance Problems 341

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. Lamp
Troubleshooting on page 250.
Dirty furnace windows. Clean the windows.Graphite
Furnace Maintenance for the
PinAAcle 900T/900Z on page
260.
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. Graphite Furnace
Maintenance for the PinAA-
cle 900T/900Z on page 260
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 online help.
aligned.
Lamp energy fluctuating. Lamp starting to deteriorate. Allow the lamp to warm up
for 30 to 60 minutes, or install
a new lamp.
342 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.
WinLab32 for AA software is Reconfigure WinLab32 for
in Simulator mode. AA to communicate with the
spectrometer. See the online
help; keyword: Reconfigure.
WinLab32 for AA application Communication cable. Make sure that you use the
stops or hangs correct cable, and connect it
to the correct communication
ports.
Performance Problems 343

Problem Possible Cause(s) Corrective Action

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
WinLab32 for AA.
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 WinLab32 for AA.
WinLab32 for AA 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 Use the Data Manager to:
saving and data-recovery pro- very large. Make regular backups of the
cedures. data. Delete old, unwanted
data.
Archive wanted data on a dif-
ferent system, CDs or on
archiving devices to leave the
WinLab32 for AA database
system free to collect new
data.
Pack the data.
344 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 345

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 224.

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 221.
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
224.
Burner head dirty. Clean the burner head. See
Cleaning the Burner Head on
page 214.
346 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 230 and the online
help.
Performance Problems 347

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 214.
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 109.
348 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 109.
No graphite tube installed, or Insert a new graphite tube.
the tube is defective. See Inserting the Graphite
Tube on page 263.
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 127.
Performance Problems 349

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 insert 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 WinLab32 for AA, use
quate. Solvent fumes remain the Method Editor to enter a
in and around the tube after suitable furnace program. See
drying, when raising to higher the Recommended Condi-
temperatures of pyrolysis and tions.
atomization.
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.
Autosampler does not go to The wrong configuration of Select the correct sample tray
the correct locations. the tray for the autosampler. in WinLab32 > Options >
Furnace Autosampler. See
the online help.
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.
350 Troubleshooting

Autosamplers for Flame and Flow Injection

Problem Possible Cause(s) Corrective Action

Autosampler will not func- The autosampler is not Reconfigure WinLab32 for
tion. entered in the system configu- AA to communicate with the
ration or supported by this spectrometer. See the online
version of software/system. help; keyword: Reconfigure.
Use the system-supported
autosampler.
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.

Flow Injection System

Problem Possible Cause(s) Corrective Action

Computer cannot communi- FIAS not entered in the sys- Reconfigure WinLab32 for
cate with FIAS. tem configuration AA to communicate with the
spectrometer. See the online
help; keyword: Reconfigure
or the software installation
instructions.
Not switched on. Switch on.
Performance Problems 351

Problem Possible Cause(s) Corrective Action

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.
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.
352 Troubleshooting

Analysis Flame 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 online help.
Unstable flame See Troubleshooting: Burner
System on page 344
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 230.
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.
Performance Problems 353

Problem Possible Cause(s) Corrective Action

The source lamp or the deute- With WinLab32 for AA, use
rium lamp is failing, or the the Lamp Setup window to
current is too high or too low set the correct current. Install
new lamps. See Lamp Life on
page 250.
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 WinLab32 for AA, use
parameters in the method. the Method Editor to select
suitable measurement param-
eters.
Unsuitable flame conditions. With WinLab32 for AA, use
the Method Editor to select
suitable measurement param-
eters. See the Recom-
mended Conditions.
Burner position is not opti- To optimize the burner; see
mized. the online help.
Nebulizer sample tubing is Install new tubing of the cor-
too long. rect length. With WinLab32
for AA, use the Method Edi-
tor to select suitable values
for the read time and read
delay. See Nebulizer Removal
and Reinstallation on page
230.
354 Troubleshooting

Problem Possible Cause(s) Corrective Action

The lamp current is too high With WinLab32 for AA, use
(line broadening) or too low. the Lamp Setup window to
set the correct current.
A low-sensitivity wavelength With WinLab32 for AA, use
is selected. the Method Editor to select
the correct wavelength. See
the Recommended Condi-
tions.

Analysis Furnace Technique

Problem Possible Cause(s) Corrective Action

Poor sensitivity. Characteris- Wrongly prepared reference Prepare new standard solu-
tic mass is too high. solution or blank. tions correctly.
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.
See the sections on bad preci-
sion and erratic signals.
Performance Problems 355

Problem Possible Cause(s) Corrective Action

Poor sensitivity. Characteris- Unsuitable time/temperature With WinLab32 for AA, use
tic mass is too high (contin- program in the method. the Method Editor to enter a
ued). suitable furnace program. See
the Recommended Condi-
tions. If this does not work,
seek advice from the Perki-
nElmer 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 263.
Analyte has been lost during Use a lower pyrolysis temper-
the pyrolysis step. ature, especially if you are not
using a matrix modifier.
Unsuitable measurement With WinLab32 for AA, use
parameters in the method. the Method Editor to select
suitable measurement param-
eters. See the Recom-
mended Conditions.
Gas flow during atomization Use zero flow during the
too high. atomization step. Select this
on the Furnace page in the
Method Editor.
Low sensitivity wavelength Select the correct wavelength
selected. on the Instrument page in the
Method Editor. See the Rec-
ommended Conditions.
356 Troubleshooting

Problem Possible Cause(s) Corrective Action

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 With WinLab32 for AA, use
or too low. the Lamp Setup window 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 357

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 340.
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
267.
358 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 263.
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 322 or the
online help.
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.
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.
Performance Problems 359

Problem Possible Cause(s) Corrective Action

Poor precision Lamp current is too low. Old See Troubleshooting: Spec-
or faulty lamp. trometer on page 340.
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 WinLab32 for AA, use
or pyrolysis step. the Method Editor to
increase the ramp time for the
step.
Optimize the temperatures.
Spattering when the sample is The tube is too hot. With
injected. WinLab32 for AA, use the
Method Editor to set the
injection temperature for the
tube. Make sure that the cool-
ing 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.
Samples are in an organic sol- Organic solvents require indi-
vent. vidually optimized drying
temperatures.
360 Troubleshooting

Problem Possible Cause(s) Corrective Action

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 WinLab32
for AA 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 322.
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 322.
Valves: dirty or worn. Clean the valves or fit new
valves. See the user's guide
for the furnace. See Valve
Maintenance on page 324.
The furnace is not correctly Align the furnace. See
aligned. Graphite Furnace Mainte-
nance for the PinAAcle 900T/
900Z on page 260.
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.
Performance Problems 361

Problem Possible Cause(s) Corrective Action

Spattering during the drying With WinLab32 for AA, use


or pyrolysis step. the Method Editor to
increase the ramp time for the
step. Optimize the tempera-
tures.
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
263.
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 291 or the
online help.
Contaminated graphite tube Install a new graphite tube or
or contacts. new contacts. See Inserting
the Graphite Tube on page
263.
362 Troubleshooting

Analysis Flow Injection 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. 344; Analysis Flame Tech-
nique on page 352.

Worn pump tubing. Install new pump tubing.

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.
Performance Problems 363

Problem Possible Cause(s) Corrective Action

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 online help.
ing with the waste.
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
online help.
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 online help.
364 Troubleshooting

Problem Possible Cause(s) Corrective Action

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.
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.
Performance Problems 365

Problem Possible Cause(s) Corrective Action

The first replicate of a series The Fill step in the FIAS pro- With WinLab32 for AA, use
gives a high reading. grams is too short. the 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.
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.
366 Troubleshooting

Problem Possible Cause(s) Corrective Action

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 online help.
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 82


Accessories 72 Burner Chamber
Acetylene 26 cleaning 208
Acetylene Supply disassembling 219
maintenance 249 Burner Gases
Air Filter connecting 108
changing 203 Burner Head 216, 219
Air Supply 25 cleaning 214
aligning autosampler arm 145 installing 224
Aligning the Graphite Furnace 186 removing 219
alignment controls Burner Head Options 86
autosampler 148, 149 Burner Mount 87
Argon Gas Burner System
connect 113 cleaning 212
AS 900 Autosampler high temperatures 19
installing 132 introduction 84
Autosampler maintenance checklist 199
adjusting immersion depth in sample reassembling 221
cup 152 setting up 176
adjusting penetration depth in graphite troubleshooting 344
tube 145 C
aligning autosampler arm 145 changing
alignment controls 148, 149 graphite contacts 306
checking penetration depth in graphite graphite shield ring 305
tube 150 graphite tube 302
sample cups and reagent containers 143 Checks
setting up 155 periodic 198
troubleshooting 350 Chemicals
unlocking autosampler arm 145 safety 14
B Cleaning
Background Correction 92 furnace windows 321
Burner graphite contacts 300
preconditioning 216 graphite contact surfaces 269, 301
Burner Assembly instrument 33
removal 216 graphite tube 300
I-2 Index: D

Closing the Furnace E


after contact change 289, 317 EDL
Compressed Gases installing 170
handling 20 Electrical Connectors 78
Computer System Electrical Safety 4
troubleshooting 342 Electrothermal Atomization
Conditioning the Graphite Tube 305 hazards 30
Contact Cylinders safety practices 29
changing 270 EMC Compliance 6
Cooling Connectors 81 safety 6
Cooling Requirements 65 Emergency Shutdown 192
Cooling System Environmental Conditions 3
filling 127 Environmental Requirements 37
installing 124 European Requirements
installtion 124 gas lines 111
D F
Data System 95 Features
Decontamination 33 PinAAcle 900 Series System 69
Dimensions 39 FIAS
Drain System 27, 88 safety practices 31
cleaning 226 Flame
emptying 227 safe operation 26
Drain System Maintenance 224 Flame AnalysisTechnique 352
Drain Tube Flame Atomization
installing 138 hazards 28
precondition 131 safe practices 24
preconditioning 216 Flame Atomizer 92
replacing 228 Flame Autosampler
Drain Vessels 64 troubleshooting 350
Drainage of Spray Chamber 131 Flame Gas Requirements 56
DRC Lamp Flame System
aligning 257 shut down 191
reassembling 255, 257 Flame Technique
removing 252 setting up 176
replacing 255 troubleshooting 352
Index: G I-3

Flashbacks 28 G
Flow Injection Autosampler Gas Connectors 81
troubleshooting 350 Gas Controls 88
Flow Injection System Gas Cylinders
troubleshooting 350 handling 24
Flow Injection Technique identiying 22
troubleshooting 362 safe handling 22
Fume Ventilation 41 safety 53
Furnace storing 23
closing after contact change 289, 317 Gas Delivery Lines
opening for contact change 307 safety 53
troubleshooting 348 Gas Hazards
Furnace Analysis Technique summary 21
troubleshooting 354 Gas Requirements 52
Furnace Autosampler 94 Graphite Contact Surfaces
troubleshooting 348 cleaning 269, 301
Furnace Gas Requirements 55 Graphite Contacts
Furnace Gases changing 306
connecting 112 cleaning 300
Furnace System Graphite Furnace
shut down 191 high temperatures 19
Zeeman Graphite 18 maintenance for the PinAAcle 900H
Furnace Technique 296
setting up for the PinAAcle H 184 Graphite Furnace Atomizer 93
setting up for the PinAAcle T/Z 181 Graphite Furnace Maintenance 260
troubleshooting 354 Graphite Shield Ring
Furnace Windows installing 305
cleaning 293, 321 Graphite Tube
refitting 320 changing for the PinAAcle 900H 302
removing 318 cleaning 267, 300
Fuses conditioning 291
changing 206 conditioning for the PinAAcle 900H
safety 6 305
heating manually 292
inserting 263
removing contamination by heating 301
I-4 Index: H

H Line Power Requirements 47


HCL Locating The System 124
installing 170 M
Heating the Graphite Tube 269, 301 Magnetic Field 18, 46
High Sensitivity Plastic Nebulizer Maintenance
bead 244 graphite furnace 260
cleaning 241 Maintenance Checklist 196
removing 236, 240 Maximum Absorbance
spacer 245 adjusting 245
I Mercury Hydride Systems
Ignitor Assembly 87 safety practices 31
Immersion Depth of Pipet Tip In Sample N
Cup 152 Nebulizer
Inert Gas 30 high sensitivity plastic, cleaning 241
Installation high sensitivity plastic, impact bead
general information 103 244
unpacking 101 high sensitivity plastic, reinstalling 240
Installation Preparation 66 high sensitivity plastic, removing 236
Installing Graphite Components high sensitivity plastic, spacer 245
graphite shield ring 305 installation 132
left-hand contact 313 maximum absorbance 245
right-hand contact 315 removal 230
Instrument Cleaning 198 stainless steel, cleaning 235
L stainless steel, reinstalling 233
Lab Space Requirements 38 stainless steel, removing 231
Laboratory Safety Practice Nitrogen Gas
references 35 connect 113
Lamp Nitrous Oxide 25
disposing 16 O
removing 172replacing 250 Opening The Furnace
Lamp Cleaning 250 for contact change 307
Lamp Maintenance 250 Optical Schematics 74
Left-Hand Contact Optical System 72
installing 313 P
removing 311 PC Configuration 66
Penetration Depth of Pipet Tip In Graphite
Index: Q I-5

Tube 145, 150 Sample Cups 143


Pipet Tip Sample Tray
immersion depth in sample cup 152 installing 141, 173
penetration depth in graphite tube 145, removing 176
150 Setting Up The Autosampler ??–155
Placing The System 124 Source Lamps 63
Power Consumption Specifications 91
48 Spectrometer
Precautions installation 103
Safety 2 reinstalling 107
Preconditioning 131 shut down 191
Printer 66 troubleshooting 340
Product Line Experience 67 Spectrometer Maintenance Checklist 202
Q Stainless Steel Nebulizer
Quartz Tube Atomizer Cell 20 cleaning 235
R reinstallling 233
Reagent Containers 143 removing 231
Removing Switches 78
left-hand contact 311 System
right-hand contact 308 shut down 191
Replacement Parts 156 System Components 71
Right-Hand Contact System Control 71
installing 315 U
removing 308 Unlocking Autosampler Arm 145
S Unpacking Instructions 101
Safety UV Radiation 18
precautions 2 V
warning labels 7 Vent Filter
Safety Checks 30 changing 205
Safety Information xiii Vent Hood Dimensions 44
Safety Interlocks 24, 29 W
Sample Capillary Waste Bottle
installing 143 installing 138
Sample Cove Waste Disposal 16
installing 141 Water Hoses
connecting 125
I-6 Index: W

WEEE Instructions 34
Weights 39
Windows
cleaning 321
refitting 320
removing 318
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.

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