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ICP Optical Emission

Optima 2000 DV

User’s Guide
 PerkinElmer Bodenseewerk is
registered for the design and
manufacture of laboratory analyti-
cal equipment under the quality
requirements of BS EN ISO 9001.

Certificate No. FM 22178

Notice
The information contained in this document is subject to change without notice.
PerkinElmer makes no warranty of any kind with regard to the material, including, but not limited to, the implied warranties
of merchantability and fitness for a particular purpose.
PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in connection with
furnishing, performance or use of this material.
Release history

Part Number Release Publication Date

0993-6226 1..0 January 2000

Trademarks
PerkinElmer is a trademark of PerkinElmer, Inc.
WinLab32, FIAS, GemCone, GemTip, are trademarks of affiliates of PerkinElmer LLC.
Meinhard is a registered trademark of J.E. Meinhard Associates, Inc. MS-DOS, Ryton is a registered trademark of Phillips
Petroleum Company. Teflon and Viton are registered trademarks of E.I. duPont deNemours & Co. Tygon is a registered
trademark of Norton Company. Windows is a trademark and Microsoft is a registered trademark of Microsoft Corporation.
Registered names, trademarks, etc. used in this document, even when not
specifically marked as such, are not to be considered unprotected by law.

Copyright information
This document contains proprietary information that is protected by copyright.
All rights are reserved. No part of this document may be reproduced in any form whatsoever
or translated into any language without the prior written permission of PerkinElmer LLC
or one of its affiliates.
Copyright © 2000 by affiliates of PerkinElmer LLC
Printed in the Federal Republic of Germany
Technical Documentation
PerkinElmer Bodenseewerk
88662 Ueberlingen, Federal Republic of Germany
 Contents
Using this Guide ............................................................................................ xi
Other Guides for the Optima 2000 DV ......................................................... xi

Chapter 1. Safety Information

Safety Information in the Manual ................................................................ 1-4
General Safety Practices .............................................................................. 1-5
Laboratory Hygene .............................................................................. 1-5
Electrical Safety .................................................................................... 1-5
Safe Operating Conditions .................................................................... 1-7
Radio Frequency Radiation ................................................................... 1-8
Ultraviolet Radiation ............................................................................. 1-8
High Temperatures ................................................................................ 1-9
Handling of the Instrument ................................................................... 1-9
Laboratory Ventilation .......................................................................... 1-9
Safety Interlocks ................................................................................... 1-9
Safe Use of Drain Systems ................................................................. 1-10
Safe Handling of Gas Cylinders ......................................................... 1-11
Safe Use of Chemical Reagents .......................................................... 1-13
Waste Disposal Procedures ................................................................. 1-15
Regulatory Information ............................................................................. 1-16
FCC Compliance (United States) ........................................................ 1-16
Electrical Protection ............................................................................ 1-16
Symbols Used on the Instrument ........................................................ 1-17
Warning Labels on the Instrument ...................................................... 1-19
Sample Preparation .................................................................................... 1-28
Dissolving Solid Samples in Organics ................................................ 1-28
Dissolving Solid Samples Using Acids .............................................. 1-29
Acid Digestions ................................................................................... 1-29
Fusion Mixtures .................................................................................. 1-32
References ................................................................................................. 1-32
vi Contents

Chapter 2. Preparing Your Laboratory

Environmental Conditions ...........................................................................2-4
Exhaust Vent Requirements .........................................................................2-5
Laboratory Space Requirements ..................................................................2-7
Cooling Water Requirements .......................................................................2-9
Electrical Requirements .............................................................................2-10
Pneumatic Requirements ............................................................................2-12

Chapter 3. System Description

Major Components .......................................................................................3-4
Spectrometer ................................................................................................3-6
Introduction ...........................................................................................3-6
Transfer Optics ......................................................................................3-8
Monochromator .....................................................................................3-8
Detector .................................................................................................3-9
Wavelength Correction ........................................................................3-11
ICP Source .................................................................................................3-12
RF Generator .......................................................................................3-12
RF Control Electronics ........................................................................3-13
Sample Introduction System ......................................................................3-14
Sample Compartment ..........................................................................3-14
Quick-Change Adjustable Torch Module ...........................................3-14
Torch ....................................................................................................3-14
Spray Chamber ....................................................................................3-14
Nebulizers ............................................................................................3-15
Nebulizer Heater ..................................................................................3-17
Peristaltic Pump ...................................................................................3-18
Autosampler ........................................................................................3-18
Switches and Controls ................................................................................3-19
Main On/Off Switch ............................................................................3-19
Interlocks .............................................................................................3-19
EMO Switch ........................................................................................3-20
Hardware Setup and Optimization ......................................................3-21
Connections to Electrical, Gas, and Cooling Water Supplies ....................3-22
Technical Data ...........................................................................................3-24
ICP Plasma Generator System .............................................................3-24
Gas Flow Controls ..............................................................................3-24
Sample Introduction System ................................................................3-25
Spectrometer .......................................................................................3-26
 vii

Chapter 4. Installation
Installation Summary ................................................................................... 4-4
Moving the Instrument ................................................................................ 4-5
Connecting the Gases and Cooling Water ................................................... 4-6
Connecting the Gases ............................................................................ 4-6
Connecting the Neslab Chiller ............................................................ 4-10
Filling the Neslab Chiller .................................................................... 4-15
Starting Up the Neslab Chiller ............................................................ 4-17
Connecting the System Components ......................................................... 4-17
Setting Up the Computer and Printer ........................................................ 4-20
Installing the Quick-Change Adjustable Torch Module ........................... 4-20
Installing the Quick-Change Adjustable Torch Module ..................... 4-20
Connecting the Nebulizer (Neb) Tubing ............................................. 4-24
Installing the Autosampler ........................................................................ 4-26
Setting Up the Autosampler ...................................................................... 4-28
To Fit the Sampling Probe .................................................................. 4-28
Adjusting the Sampling Probe Height ................................................ 4-29
Instrument Start-up .................................................................................... 4-30
Automatically Aligning the Torch Viewing Position ................................ 4-31
Setting Instrument Parameters ................................................................... 4-33
Plasma Parameters .............................................................................. 4-33
Important Considerations for Dual Viewing ....................................... 4-33
Shipping List ............................................................................................ 4-35

Chapter 5. Maintenance
Introduction ................................................................................................. 5-6
Daily Checks ............................................................................................... 5-6
Daily Cleaning ...................................................................................... 5-6
Argon Supply ........................................................................................ 5-6
Purge Gas Supply .................................................................................. 5-7
Shear Gas Supply .................................................................................. 5-7
Chiller ................................................................................................... 5-7
Vent ....................................................................................................... 5-8
Torch and RF Coil ................................................................................ 5-8
Nebulizer ............................................................................................... 5-8
Peristaltic Pump and Drain ................................................................... 5-8
Periodic Checks ........................................................................................... 5-9
Torch Assembly and RF Coil ............................................................... 5-9
Purge Viewing Window/Tubes .......................................................... 5-10
viii Contents

Nebulizer .............................................................................................5-10
Spray Chamber ...................................................................................5-10
Peristaltic Pump ...................................................................................5-10
Drains ..................................................................................................5-10
General System Maintenance ..............................................................5-10
Torch Viewing Position Alignment .....................................................5-11
Performance Checks ...........................................................................5-11
Cleaning the Sample Introduction System ..........................................5-12
Quick-Change Adjustable Torch Module ..................................................5-13
Plasma Torch .......................................................................................5-13
RF Coil ................................................................................................5-14
Removing the Scott Spray Chamber ..................................................5-15
Removing the Injector .........................................................................5-15
Removing and Disassembling the Torch .............................................5-17
Cleaning the Torch ..............................................................................5-19
Cleaning the Spray Chamber ...............................................................5-21
Replacing the Torch ............................................................................5-21
Replacing the Torch on the Mount ......................................................5-25
Replacing the Spray Chamber ............................................................5-28
Connecting the Nebulizer (Neb) Tubing .............................................5-28
Replacing the RF Coil .........................................................................5-30
Purge Window/Tubes .................................................................................5-33
Removing and Cleaning the Purge Windows ......................................5-33
Removing the Purge Windows ............................................................5-33
Cleaning the Purge Windows ..............................................................5-35
Adjusting the Position of the Shear Gas Nozzle ........................................5-39
Scott-Type Spray Chamber .......................................................................5-40
Removing the Spray Chamber .............................................................5-40
Removing the End Cap from the Spray Chamber ...............................5-40
Cleaning the Scott-Type Spray Chamber ............................................5-41
Cyclonic Spray Chamber ...........................................................................5-42
Installing the Cyclonic Spray Chamber ...............................................5-42
Etching the Cyclonic Spray Chamber .................................................5-45
Cleaning the Cyclonic Spray Chamber ...............................................5-46
Nebulizers ..................................................................................................5-47
GemTip Cross-Flow Nebulizer ..................................................................5-49
Removing the Nebulizer/End Cap .......................................................5-49
Checking the Spray Pattern .................................................................5-50
 ix

Disassembling the Cross-Flow Nebulizer .......................................... 5-51

Replacing the Nebulizer/End Cap ....................................................... 5-61
GemCone Nebulizer .................................................................................. 5-62
Daily Cleaning of the Low-Flow GemCone Nebulizer ...................... 5-62
Daily Cleaning of the High Solids GemCone Nebulizer .................... 5-62
Installing the GemCone Nebulizer on the Scott-Type Spray Chamber 5-63
Installing the GemCone Nebulizer on the Cyclonic Spray Chamber 5-64
Cleaning the GemCone Nebulizer ...................................................... 5-65
GemCone Liquid Fitting Maintenance ............................................... 5-66
Concentric Glass Nebulizer ...................................................................... 5-67
Installing the Concentric Nebulizer .................................................... 5-67
Cleaning the Concentric Glass Nebulizer ........................................... 5-69
Peristaltic Pump ......................................................................................... 5-71
Replacement Pump Tubing ................................................................. 5-71
Installing the Sample and Drain Tubing ............................................. 5-72
Adjusting the Pump Tubing ................................................................ 5-77
Cleaning the Pump .............................................................................. 5-79
Drain ................................................................................................... 5-79
General System Maintenance .................................................................... 5-81
Air Filters ........................................................................................... 5-81
Changing the RF Generator Air Filter ................................................ 5-81
Changing the Spectrometer Air Filter ................................................. 5-81
Changing the Neon Lamp ................................................................... 5-82
Chiller and Filters .............................................................................. 5-83
Fuses ................................................................................................... 5-84
Replacement Parts: General ................................................................ 5-84

Chapter 6. Troubleshooting
A Word on Troubleshooting ........................................................................ 6-4
What the Performance Checks Measure ...................................................... 6-4
Sodium Bullet Test ...................................................................................... 6-5
Performance Problems ................................................................................ 6-6
Checking the Sample Introduction System ........................................... 6-6
Performance Problems: Troubleshooting Table ........................................ 6-10
Plasma Ignition and Stability Problems .................................................... 6-14
Plasma Ignition Problems ................................................................... 6-14
Plasma Stability Problems .................................................................. 6-16
Printing Problems ...................................................................................... 6-17
Pump Problems .......................................................................................... 6-18
x Contents

Autosampler Problems ...............................................................................6-19

RF Generator/Sample Introduction System Troubleshooting Form ..........6-19
Troubleshooting Form .........................................................................6-20
General: ...............................................................................................6-20
Sample Introduction Configuration: ....................................................6-20
Operating Conditions: .........................................................................6-20
Instrument Environment: .....................................................................6-20
Troubleshooting Tasks Performed: .....................................................6-20
Common Setup Problems: ...................................................................6-21

Chapter 7. Error Messages

System Error (SYSERROR) Messages for RF Generator ...........................7-4

Index
 Using this Guide
xi

Using this Guide

Thoroughly read the Safety chapter before using the instrument.

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

1 Safety Practices Important safety information.
2 Preparing Your The preparation of your laboratory needed for the
Laboratory Optima 2000 DV. Environmental, electrical, space,
exhaust, gases, and cooling water requirements are
reviewed.
3 System The components of the instrument, how the echelle
Description spectrometer works and instrument specifications.
4 Installation This chapter includes information for installing or re-
installing the system components (autosampler,
computer, and printer) and is provided for your reference
should you ever need to move the system.
5 Maintenance Maintenance and cleaning procedures for the various
components of your system, particularly for the sample
introduction area.
6 Troubleshooting Performance checks and troubleshooting information for
both hardware and software problems.
7 Error Messages Explanations of software and system error messages.

Other Guides for the Optima 2000 DV

In addition to this guide, the following guides are also provided for the Optima
2000 DV.
• Winlab32 Software Guide (Part No. 0993-6335). This guide contains basic
information on the ICP WinLab software, step-by-step procedures, and
comprehensive chapters that cover each of the software windows and
parameters for reference.
• Winlab32 Software Installation and Administration Guide (Part No. 0993-
6397). This guide contains step-by-step procedures for software installation
and administration information on the ICP WinLab software.
xii
Safety Information 1
Safety Information
Contents
Safety Information in the Manual ................................................................ 1-4
General Safety Practices .............................................................................. 1-5
Laboratory Hygene .............................................................................. 1-5
Electrical Safety .................................................................................... 1-5
Safe Operating Conditions .................................................................... 1-7
Radio Frequency Radiation ................................................................... 1-8
Ultraviolet Radiation ............................................................................. 1-8
High Temperatures ................................................................................ 1-9
Handling of the Instrument ................................................................... 1-9
Laboratory Ventilation .......................................................................... 1-9
Safety Interlocks ................................................................................... 1-9
Safe Use of Drain Systems ................................................................. 1-10
Safe Handling of Gas Cylinders ......................................................... 1-11
Safe Use of Chemical Reagents .......................................................... 1-13
Waste Disposal Procedures ................................................................. 1-15
Regulatory Information ............................................................................. 1-16
FCC Compliance (United States) ........................................................ 1-16
Electrical Protection ............................................................................ 1-16
Symbols Used on the Instrument ........................................................ 1-17
Warning Labels on the Instrument ...................................................... 1-19
Sample Preparation .................................................................................... 1-28
Dissolving Solid Samples in Organics ................................................ 1-28
Dissolving Solid Samples Using Acids .............................................. 1-29
Acid Digestions ................................................................................... 1-29
Fusion Mixtures .................................................................................. 1-32
References ................................................................................................. 1-32
1-4 Safety Information

Safety Information in the Manual

Before setting up and operating this instrument, carefully read the safety
precautions described in this chapter and observe them at all times.

This chapter describes general practices designed to aid you in safely operating the
spectrometer and accessories.

This advice is intended to supplement, not supersede, the normal safety codes in the
user's country. 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 spectrometer 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.

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.

A warning indicates an operation that could cause personal injury if precautions are
! not followed.
Warning

Caution A caution indicates an operation that could cause instrument damage if precautions
are not followed.
 General Safety Practices 1-5

General Safety Practices

This section describes some general laboratory safety guidelines. For additional
information, we recommend The CRC Handbook of Laboratory Safety (1) and
Prudent Practices for Handling Hazardous Chemicals in Laboratories (2).

Laboratory Hygene
Always wear safety glasses when using the instrument. Safety glasses with side
shields will provide an extra margin of safety as well as mechanical protection for
your eyes.

For safety reasons and to avoid contaminating samples, be sure that the instrument
and work area are kept scrupulously clean. This is especially important when
working with toxic elements or when measuring trace amounts of any element.
Clean up spilled chemicals immediately and dispose of them properly.

Smoking is a source of significant contamination as well as a potential route for

ingesting harmful chemicals.

Food should not be stored, handled, or consumed in the work area.

Electrical Safety
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 authorized and trained person.
Warning
When the instrument is connected to line power, opening the instrument covers is
likely to expose live parts. Even when the power switch is off, high voltages can still
be present. Power supplies inside the instrument may still be charged even if the
instrument has been disconnected from all voltage sources.
1-6 Safety Information

Grounding circuit continuity is vital for safe operation of the equipment. Never
! operate equipment with grounding conductor disconnected.
Warning

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

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

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

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

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

Do not operate the instrument with any covers or parts removed. Disconnect
! supply wherever the cover is removed.
Warning

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 unless
required to do so.
 General Safety Practices 1-7

• Never leave the instrument unattended with the cover off and connected to AC
power!

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

in the manuals.

• Disconnect the instrument from all voltage sources before opening it for any
adjustment, replacement, maintenance, or repair. If afterwards, the opened
instrument must be operated for further adjustment, maintenance, or repair, this
must only be done by a qualified person who is aware of the hazards involved.

• Whenever it is possible that the instrument is no longer electrically safe for use,
make the instrument inoperative and secure it against any unauthorized or
unintentional operation. The electrical safety of the instrument is likely to be
impaired if, for example, the instrument shows visible damage; has been
subjected to prolonged storage under unfavorable conditions; or has been
subjected to severe stress during transportation.

Safe Operating Conditions

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

Operating Conditions
The instrument will operate safely under the following conditions:

• Indoors.

• Ambient temperature 15 C to 35 C (50 F to 95 F).

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

• Altitude in the range 0 to 2000 meters.

1-8 Safety Information

Storage Conditions
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 0 to 12,000 meters.

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

Radio Frequency Radiation

The instrument generates high levels of Radio Frequency (RF) energy, which is
potentially hazardous if allowed to escape. The instrument is designed to contain the
RF energy within the shielded enclosures of the sample compartment and the RF
power supply. Safety interlocks prevent you from operating the system without all
covers, doors, and shields in place.

Ultraviolet Radiation
The plasma generates high intensity ultraviolet radiation. A safety interlock is used
to automatically shut off the plasma if the sample compartment door is opened or the
torch is removed. The sample compartment has a viewing window for safely viewing
the plasma.

Directly viewing the plasma (without protection) may cause permanent

! impairment of eyesight.
Warning
 General Safety Practices 1-9

High Temperatures

The torch
The torch components remain hot for some time after the plasma has been shut off.
Allow sufficient time for these items to cool to room temperature before you handle
them.

Hot Exhaust Gases

When the plasma is on, hot gases are vented through the chimney above the sample
compartment. An efficient ventilation system must be provided, as referenced in the
Exhaust Vent Requirements part of the Preparing Your Laboratory chapter
(Chapter 2) in this manual. In addition, avoid this area of the instrument to prevent
burns.

Handling of the Instrument

Contact a PerkinElmer service engineer for assistance in installing or
evaluating the system after moving. The Optima 2000 DV weighs 146 kg (321
pounds), or 201 kg (442 pounds) with the shipping container. If the instrument needs
to be moved please contact PerkinElmer Service.

Laboratory Ventilation
Toxic combustion products, metal vapor, and ozone can be generated by the system,
depending upon the type of analyses. Therefore, an efficient ventilation system must
be provided for the instrument. Detailed specifications for a recommended venting
system are described in the section called Exhaust Vent Requirements in Preparing
Your Laboratory (Chapter 2).

Safety Interlocks
The instrument has safety interlocks to protect the operator from radio frequency
(RF) radiation and ultraviolet radiation, and to prevent access to high voltage areas.
1-10 Safety Information

Do not attempt to defeat the safety interlocks. This would place the operator's
! safety at risk.

Warning

The following interlocks must be satisfied in order to ignite the plasma. If any of
these interlocks is interrupted while the plasma is on, the plasma will automatically
be shut down.

• The front door on the torch compartment must be closed before the plasma can
ignite.

• Argon pressures for the torch must be correct.

• Emergency Off Switch must be released.

• Cooling water must be flowing to the RF coil and oscillator.

• Quick change torch must be installed.

• The shear gas must be flowing.

Safe Use of Drain Systems

For safe operation of the system, the pumped drain system should be properly
installed.

Never place the vessel in an enclosed cabinet. Doing so could result in a build-up
! of hazardous gases, which may result in a serious explosion or fire.

Warning Never use a glass drain vessel. A glass drain vessel may break and spill flammable,
toxic, or corrosive liquids.

Recommended safety practices for drain systems are given below.

 General Safety Practices 1-11

• Place the drain vessel in an area that is visible to the operators, who can observe
the level of collected effluent and empty the vessel when necessary.

• Check the condition of the drain tubing regularly to monitor deterioration.

Organic solvents deteriorate the tubing more quickly than aqueous solutions.
When the tubing becomes brittle or cracked, replace it.

• Empty the drain bottle regularly when using organic solvents. Before switching
from organic to aqueous solutions, always empty the drain bottle.

Safe Handling of Gas Cylinders

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

Gases commonly used with ICP instruments include argon and nitrogen. 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.

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

Warning Carefully use, store, and handle compressed gases in cylinders. Gas cylinders can
be hazardous if they are mishandled.

If liquid argon or nitrogen is used, the gas cylinder must be fitted with an over-
pressure regulator, which will vent the cylinder as necessary to prevent it from
becoming a safety hazard.

Listed below are some general safety practices for the proper identification, storage,
and handling of gas cylinders. Consult References 3 and 4 for more detailed
information and additional guidelines.
1-12 Safety Information

Identification of Gas Cylinders

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

Storing Cylinders
• Cylinders should be stored in accordance with the regulations and standards
applicable to the customer’s locality, state, and country.

• 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).

Handling Cylinders
• If it becomes necessary to move cylinders, do so with a suitable hand truck after
ensuring that the container cap is secured and the cylinder properly fastened to
the hand truck.

• Use only regulators, tubing, and hose connectors approved by an appropriate

regulatory agency.
 General Safety Practices 1-13

• Arrange gas hoses where they will not be damaged or stepped on, and where
objects will not be dropped on them.

• Do not refill gas 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 solution.

• 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.

Safe Use of Chemical Reagents

Before using any chemicals or solvents with the instrument, the customer should be
thoroughly familiar with all hazards and safety handling practices. Observe the
manufacturer’s recommendations for use, storage and disposal. These
recommendations are normally supplied in the material safety data sheets (MSDS)
supplied with the solvents.

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

Some definitions of terms used in "Hazardous Chemicals Warnings" above are given
next.

OSHA: Occupational Safety and Health Administration (United States)

ACGIH: American Conference of Governmental Industrial Hygienists

COSHH: Control of Substances Hazardous to Health (United Kingdom)

1-14 Safety Information

Responsible body: "Individual or group responsible for the use and maintenance of
equipment, and for ensuring that operators are adequately trained." [per IEC 1010-1,
Amendment 2].

Operator: "Person operating equipment for its intended purpose." [per IEC 1010-1
Amendment 2].

Protective Equipment
• Wear appropriate eye protection at all times while handling chemicals. Use
safety glasses with side shields, goggles, or full-face shields, according to the
types of chemicals being handled.

• Wear suitable protective clothing, including gloves specifically designed to

resist the chemicals being handled.

Use, Storage, and Disposal

Review the following information with the customer to ensure the safe use, storage,
and disposal of chemicals.

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

recommendations and regulations applicable to the locality, state, and/or
country.

• When preparing chemical solutions, always work in a fume hood that is suitable
for the chemicals you are using.

• Conduct sample preparation 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, as

required) away from the instrument.
 General Safety Practices 1-15

Waste Disposal Procedures

• Carefully monitor the collection of effluent in the drain vessel and empty the
drain vessel frequently. When switching between organic and aqueous solutions,
flush the drain tube thoroughly and empty and flush out the drain vessel.

• Drain vessels may contain flammable, acidic, caustic, or organic solutions, and
small amounts of the elements analyzed. The collected effluent may have to be
disposed of as hazardous waste.

Dispose of waste in accordance with the regulations applicable to your locality,

! state, and/or country.
Warning
1-16 Safety Information

Regulatory Information

FCC Compliance (United States)

This equipment has been tested and found to comply with the limits for a Class B
digital device, pursuant to Part 15 of the FCC [Link] 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 case the user will be required to correct the interference at his
or her own expense. Changes or modifications not expressly approved by the
manufacturer could void the user's authority to operate the equipment.

Electrical Protection
Insulation

Class I as defined in IEC-1010-1.

Installation Category

This instrument is able to withstand transient overvoltage according to Installation

Category II as defined in IEC 1010–1.

Pollution Degree

This equipment will operate safely in environments that contain nonconductive

foreign matter up to Pollution Degree 2 in IEC 1010–1.
 Regulatory Information 1-17

Symbols Used on the Instrument

The three different types of warning symbols that appear on the instrument are
shown below:

This symbol indicates an operation (or condition on the

! instrument) that could cause personal injury if precautions
are not followed. This can be any type of hazard.

When you see this symbol, refer to the safety pages or pertinent
information in the manual for further information.

Consulter les documents d’accompagnement.

This symbol indicates the danger of electric shock, if precautions

are not followed, due to the presence of high voltage.

AVERTISSEMENT: Risque de choc électrique.

This symbol indicates a hot surface.

AVERTISSEMENT: La surface est chaude.

1-18 Safety Information

The following graphic symbols are also found on the instrument:

Indicates the OFF position of the main power switch.

Indicates the ON position of the main power switch.

Indicates alternating current.

This protective grounding terminal must be connected to

earth ground before any other electrical connections are
made to the instrument.
 Regulatory Information 1-19

Warning Labels on the Instrument

Safety Labels on the Front of the Instrument

1

Figure A. Location of warning label on thefront of the instrument.

Label Location Hazard Instructions for Safety

On the front of Hot gases are vented through the Avoid this area of the
the chimney chimney into the venting system. instrument when the
(Label #1 on plasma is on.
Figure A). Les gaz chauds passent par la
cheminée dans l’installation de
ventilation.
The plasma generates high Do not view the plasma
intensity ultraviolet radiation. through the chimney.

Le plasma crée des rayons

ultraviolets a haute intensité.
1-20 Safety Information

Safety Labels on the Side of the Instrument

2
1

Figure B. Location of warning label on the right hand panel of the instrument.

Marking Location Hazard Instructions for Safety

Label #1 on Connect correct Shear gas must be air or nitrogen. See the
Figure B. gases. following table for translations of "air".

Label #2 on Electrical Do not exceed stated voltage and current.

Figure B. hazard Umax = 30 V AC, Imax = 0,5 A AC
Umax = 30 V DC, Imax= 2 A DC
 Regulatory Information 1-21

Translations of the word “Air” (for the shear gas connection) and the words “In” and
“Out” (for the coolant connections) are provided in the following table.

Language Air In Out

German Luft Eingang Ausgang

French Air Entrée Sortie

Danish Luft Indgang Udgang

Finnish Ilma Sisään Ulos

Greek ⊥βP⊥π βφπλαλπ βυλαλπ

Italian Aria Ingresso Uscita

Dutch Lucht In Uit

Norwegian Luft Inngang Avløp

Portuguese Ar Entrada Salída

Spanish Aire Entrada Salida

Swedish Luft In Ut
1-22 Safety Information

Safety Labels on the Back of the Instrument

6
5
4
3
2
1

Figure C. Location of warning labels on the back of the instrument.

The warning label shown below appears on the back of the instrument in the
locations indicated in Figure C (see label 1 on figure C).

WARNING:
All field wiring must have insulation suitable for at least 300V.

AVERTISSEMENT: Le cablage a pied d’ouvre doit etre certifiés

pour un minimum de 300V.
 Regulatory Information 1-23

The warning label shown below appears on the back of the instrument in the
locations indicated in Figure C (see label 2 on figure C).

WARNING:
Disconnect supply before servicing.

AVERTISSEMENT: Couper l’alimentation avant l’entretien.

The warning label shown below appears on the back of the instrument in the
locations indicated in Figure C (see label 3 on figure C).

WARNING:
This equipment must be
! de-energized for 60 seconds to
allow safe discharge of power
supplies before servicing.
AVERTISSEMENT:
Afin de permettre aux
condensateus de se décharger
entierement, mettez l’appareil
hors tension pendant 60
seconde de les réparer

The warning label shown below appears on the back of the instrument in the
locations indicated in Figure C (see label 4 on figure C).

WARNING:
Ground circuit continuity is vital for safe operation of equipment.
Never operate equipment with ground conductor disconnected.

AVERTISSEMENT: La continuité du circuit de mise a la terre est

essentielle pour le bon fonctionnement de l’appareil.
N’utilisez jamais l’appareil lorsque le cable de mise a la terre est
débranché.
1-24 Safety Information

The warning label shown below appears on the back of the instrument in the
locations indicated in Figure C (see label 5 and 6 on figure C).

CAUTION:
Do not restrict air intake
! or exhaust.
ATTENTION:
N’obstruez pas l’arrivée ou
l’évacuation d’air.

Additional Label: The following label is located on the power line cord:

SAFETY CODES REQUIRE

USE OF IEC-309 CONNECTOR.
! ATTENTION: Les codes de
sécurité prescrivent l’utilisation de
connecteurs CEI-309.

Additional Instructions: To provide adequate space for ventilation, allow at least

15 cm (6 in.) of space between the instrument and the laboratory wall. Do not
obstruct the two air filters. See Figure D for the location of the air filters.
 Regulatory Information 1-25

Spectrometer Air Filter

To remove, slide filter

in this direction.

Access Panel for Neon Lamp RF Generator Filter

Figure D. Location of the air filters on the back of the instrument.

Additional Instructions: The instrument has AC line surge suppressing

components which require disconnection before testing.

Additional Instructions: Lethal voltages are present in the instrument. For

safety reasons testing and servicing should be carried out only by a PerkinElmer
service engineer or similarly authorized and trained person.
1-26 Safety Information

Safety Labels in the Sample Compartment

Front of Instrument,
Sample Compartment
Door Open

Figure E. Location of warning labels in the sample compartment.

 Regulatory Information 1-27

The warning labels shown below appears appear in the sample compartment (for
location see Figure E).

WARNING – Do not defeat interlocks.

! AVERTISSEMENT: Ne pas desengager
les enclenchements de securite.

Additional Instructions: The instrument has safety interlocks to protect the

operator from exposure to radio frequency and ultraviolet radiation. Do not attempt
to defeat the safety interlocks.

Location of Instructions for

Warning Warning Label Hazard Safety

On the smooth Hot surface. Avoid this area of

metal surface the instrument
below the shear gas La surface est when the plasma is
assembly on the chaude. on.
transfer optics
radial snout. (Label
#2 on Figure D)
1-28 Safety Information

Sample Preparation
Sample preparation for ICP spectroscopy may require the handling of organic or
corrosive solutions. Dilution of samples and adding dilute acid to a liquid sample is
generally less hazardous than putting a solid sample into solution. This section will
deal specifically with the potential hazards associated with dissolving solid samples,
although the information can be applied to any sample handling situation. Also, refer
to the general precautions for handling chemicals described at the beginning of this
chapter.

Reference 6 contains general information on sample preparation procedures as well

as an appendix on laboratory safety. Reference 7 contains information on laboratory
safety and sample preparation methods prescribed by the United States
Environmental Protection Agency (EPA). Reference 8 contains information on
microwave sample preparation, which is not covered in this section.

Solid samples may be put into solution by dissolving the sample in an organic
solvent or acidic solution; digesting the sample; or reacting the sample with a fusion
mixture. Each of these techniques has certain hazards associated with it.

Always wear appropriate eye protection while preparing samples. Use safety
! glasses with side shields, goggles, or full-face shields, depending on the chemicals
you are handling.
Warning

Dissolving Solid Samples in Organics

• Always work in a fume hood so that flammable and/or toxic solvents do not
concentrate in the work area.

• Wear protective clothing and gloves. Some solvents are readily absorbed
through the skin.

When selecting a solvent, consider the following:

• Is the solvent compatible with the equipment?

Aliphatic hydrocarbons, ketones and esters, alcohols, and xylene, are the most
frequently used solvents. Make sure that all equipment that will come into
 Sample Preparation 1-29

contact with the solvent is compatible with the solvent, e.g., tubing, sample cups,
storage and waste containers, etc.

• Is the solvent toxic?

Avoid solvents known to be health hazards, such as benzene or methyl isobutyl

ketone (MIBK).

Some solvents, such as the halogenated hydrocarbons, generate toxic gases

when heated.

Consult the data sheets provided by the manufacturer for information on health
hazards (see Reference 5).

Dissolving Solid Samples Using Acids

Dissolving solid samples in aqueous solutions often requires the use of concentrated
acids.

Using Acids
When using acids, use the following precautions:

• Always work in an acid-resistant fume hood.

• Wear protective clothing, including gloves specifically designed to resist the

acid being used.

• Attempt to dissolve the sample in a dilute acid solution before using

concentrated acid.

• Add concentrated acid to a sample cautiously. Dissolving a sample in

concentrated acid may provoke a vigorous reaction.

Acid Digestions
Acid digestions, either at atmospheric pressure or at increased pressure, require
special care. Spattering and foaming of the sample/acid mixture may expose the user
to a hazard, as well as compromise the sample integrity. A digested sample
containing concentrated acid will react violently with water.
1-30 Safety Information

Perchloric acid and hydrofluoric acid are particularly hazardous to work with.

Perchloric Acid
Perchloric acid (HClO4) is extremely corrosive and a powerful oxidizing agent. It
presents severe fire and explosion hazards.

Before using perchloric acid, you should be thoroughly familiar with its
! hazards and safe handling practices. Observe the manufacturer's
recommendations for use, storage, and disposal.
Warning

• Use hoods, ducts, and other devices for removing vapors specifically designed
to accommodate this kind of fume. There is a severe explosion hazard if a normal
hood is used, or if the hood is not properly used and maintained.

• Use goggles and face shields. Wear protective clothing and polyvinyl chloride
gloves. Do not use rubber gloves.

• Additional hazards and precautions are given in References 1, 2, 9, 10 and 11.

Hydrofluoric Acid
Hydrofluoric acid (HF) is also used for digestions. It is toxic and extremely
corrosive. Hydrofluoric acid will readily burn skin, and if the fumes are inhaled, lung
tissue. Burns may not be immediately painful or visible. Contact with eyes could
result in blindness.

Before using hydrofluoric acid, you should be thoroughly familiar with its
! hazards and safe handling practices. Observe the manufacturer's
recommendations for use, storage, and disposal.
Warning

• Always wear suitable protective equipment, including goggles, a face shield,

acid-resistant gloves, and protective clothing when using hydrofluoric acid.

• Do not breathe HF vapors. Always work in a fume hood when using hydrofluoric
acid.
 Sample Preparation 1-31

• Do not use a glass beaker. Hydrofluoric acid attacks glass.

• Observe the additional hazards and precautions outlined in References 1, 2, 9, 10

and 11.

Performing Digestions
When carrying out sample digestions:

• Always work in a hood suitable for the type(s) of chemicals you are using.

• Add very small quantities of the acid dropwise, while observing the magnitude
of the reaction.

• Apply heat to a digestion solution slowly in case a further vigorous reaction is

initiated.

• Cool the completed digest before transferring it and diluting it. Add water
cautiously.

Digestions at Elevated Pressure

Acid digestions in a pressure digestion apparatus require special care at several
points, in addition to the precautions described above.

When using high pressure digestion vessels, consult the manufacturer's

! instructions and recommendations, particularly regarding organic material
and possible explosive reactions.
Warning
Never use perchloric acid in a pressure digestion.

• Use only the manufacturer's recommended amounts of sample and acid for the
type of sample you are preparing.

• Be sure the apparatus is in good condition and provides safe release of pressure
in the case of excess pressure buildup.

• Cool the apparatus to room temperature before attempting to open it.

1-32 Safety Information

• Open the apparatus in a fume hood to vent the entrapped fumes safely.

Fusion Mixtures
Dissolving a sample by reacting with a fusion-flux mixture is generally chosen when
other techniques for sample dissolution fail. The fusion-flux mixture should be
carefully selected. Knowledge of fusion-flux mixture/crucible compatibility is
essential. Heating the sample-flux mixture may initiate a vigorous or explosive
reaction.

• Heat the mixture slowly and intermittently until the system is characterized.

• If you use a muffle furnace rather than a flame for heating, make a trial using the
standard amount of flux but with a smaller amount of sample.

• Most reacted fusion mixtures are dissolved in acidic solutions. Observe the
precautions described previously for handling acids.

References
1. Furr, K., ed., CRC Handbook of Laboratory Safety, 3rd ed., The Chemical
Rubber Co. Press, Florida, USA, 1990.

2. National Research Council, Prudent Practices for Handling Hazardous

Chemicals in Laboratories, National Academy Press, Washington, D.C., USA,
1981.

3. Compressed Gas Association (USA), "Safe Handling of Compressed Gases in

Containers," pamphlet no. P-1, 1984.

4. Compressed Gas Association (USA), "The Inert Gases – Argon, Nitrogen and
Helium," pamphlet no. P-9, 1992.

5. Data sheets provided by chemical manufacturers, for example:

• Material Safety Data Sheets (MSDS), USA;

• DIN-Sicherheitsdatenblätter (genormte Formular DIN-Nr 52900), FRG;

• Product Information Sheets, UK.

 References 1-33

6. Helrich, K., ed., Official Methods of Analysis, 15th ed., Association of Official
Analytical Chemists, Inc., Arlington, VA, USA, 1990.

7. Standard Methods for the Examination of Water and Wastewater, 17th ed,
American Public Health Association et al., USA, 1989.

8. Kingston, H.M. and Jassie, L.B., eds., Introduction to Microwave Sample

Preparation, American Chemical Society, USA, 1988.

9. Bretherick, L., Bretherick's Handbook of Reactive Chemical Hazards, 4th ed.,

Butterworth & Co., Ltd., London, UK, 1990.

10. Sax, N., ed., Dangerous Properties of Industrial Materials, 7th ed., Van
Nostrand Reinhold, New York, USA, 1989.

11. Bretherick, L., ed., Hazards in the Chemical Laboratory, 3rd ed., Royal Society
of Chemistry, London, UK, 1981.

12. Roth, L., ed., Sicherheitsfibel Chemie, 4, Auflage, 1979

ecomed verlagsgesellschaft mbH, 8910 Landsberg/Lech.
1-34 Safety Information
Preparing your Lab 2
 Preparing Your
Laboratory
Contents
Introduction ................................................................................................. 2-4
Environmental Conditions ........................................................................... 2-4
Exhaust Vent Requirements ........................................................................ 2-5
Laboratory Space Requirements .................................................................. 2-7
Cooling Water Requirements ................................................................ 2-9
Electrical Requirements ............................................................................. 2-10
Pneumatic Requirements ........................................................................... 2-12
2-4 Preparing Your Laboratory

Introduction
The items listed below need to be considered when preparing the laboratory for the
Optima 2000 DV:
• Environmental Conditions
• Exhaust Vent Requirements
• Laboratory Space Requirements
• Cooling Water Requirements
• Electrical Requirements
• Pneumatic Requirements

Environmental Conditions
The laboratory in which the Optima 2000 DV Spectrometer system is located must
meet the following conditions:

• corrosive-free environment.

• The instrument will operate with a laboratory temperature between 15 and 35 C

(59 - 95 F). For optimum instrument performance, the room temperature should
be controlled at 20 2 C.

• The heat dissipated directly into the laboratory when properly vented by the
Optima 2000 DV is approximately 6600 BTU/hour (2200 W).

• Relative humidity between 20% and 80%, non-condensing. For optimum

instrument performance, the relative humidity should be between 35% and 50%.

• Dust levels not above 36 000 000 particles, 0.5 micron or larger, per cubic meter
of air. The environment should be relatively dust-free to avoid sample and
instrument contamination problems.

• Free of excessive vibration.

The Optima 2000 DV has been designed for indoor use. Do not use the instrument
in an area where explosion hazards may exist.
 Exhaust Vent Requirements 2-5

Exhaust Vent Requirements

The Optima 2000 DV has one vent. This exhaust vent for the ICP torch removes
combustion fumes and vapors from the torch housing.

Exhaust venting is important for the following reasons:

• It protects laboratory personnel from toxic vapors that may be produced by some
samples.

• It improves the stability of the ICP torch by removing the effects of room drafts
and laboratory atmosphere.

• It helps to protect the instrument from corrosive vapors that may originate from
the sample(s).

• It removes dissipated heat produced from the torch and power supply.

The use of ICP-OES instruments without adequate ventilation to

! outside air may constitute a health hazard. For example, the
combustion of halogenated hydrocarbons produces toxic vapors. Extreme
Warning care should be taken that exhaust gases are vented properly.

The maximum temperature for the ICP torch vent system is 200 C (392 F). To
withstand these temperatures stainless-steel tubing must be used.

ICP torch vent required minimum flow rate is 5600 liters/min (200 cubic feet/min)
at the end of the venting hood.

Note Local electrical codes do not allow PerkinElmer Service Engineers to

install the blower and vent assembly.

The blower capacity depends on the duct length and 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-
2-6 Preparing Your Laboratory

steel tubing where flexibility is not required to reduce system friction loss or "drag."
If smooth stainless steel is used, there must be a way to move the vent hood out of
the way for servicing. A length of smooth stainless-steel tubing 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 150 mm with a maximum bend angle of 45
degrees to reduce friction losses, and the number of elbows should be minimized.

Additional recommendations on the venting system include:

• Make sure duct casing is installed using fireproof construction. Route ducts
away from sprinkler heads.

• Locate the blower as close to the discharge outlet 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.

• 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 using an air flow meter.

• Equip the blower with a pilot light located near the instrument to indicate to the
operator when the blower is on.

The venting system for the ICP torch should be positioned over the Torch
Compartment Chimney located on top of the sample compartment. For proper
instrument venting, order PerkinElmer Venting Kit # 0303-0406. The minimum
distance from the top of the instrument’s Torch Compartment Chimney to the bottom
of the extraction vent should be 7.5-12.5 cm. (3-5 in.). Gas, water, and air lines are
 Laboratory Space Requirements 2-7

also provided. The gas line is 6 m (20 ft.) long. The water line is 1.4 m (4.5 ft.) long.
The air line is 3.6 m (12 ft.) long. Figure 2-1 shows the location of the ICP torch
exhaust vent. Figure 2-1 shows the location of the ICP torch exhaust vent.

Recommended Vent
Width: 30.6 cm (12 in.)
Depth: 15.3 cm ( 6 in.)
Height: 30.6 cm (12 in.)
Torch
Compartment
Chimney
7.5 - 12.5 cm (3 - 5 in.)

Figure 2-1. Location of the Torch Compartment Chimney and Vent.

Laboratory Space Requirements

The Optima 2000 DV system includes the Optima 2000 DV instrument, a Neslab
CFT-75 Recirculating Chiller (or equivalent), a computer, and a printer. The Optima
2000 DV instrument itself includes optics, electronics, a plasma torch, and an RF
power supply, all housed in a self-contained unit. The minimum door width must be
90 cm (36 in.).
2-8 Preparing Your Laboratory

Optima 2000 DV Instrument

The Optima 2000 DV is 132-cm long (52-in.), 76-cm high (30-in.), and 81-cm deep
(32-in.). The bottom of the vent must be a minimum of 75-cm (3-in.) from the top of
the torch compartment chimney. Figure 2-2 illustrates the dimensions of the
instrument. The Optima 2000 DV weighs 146 kg (321 pounds), or 201 kg (442
pounds) with the shipping container.

The Optima 2000 DV may be placed on a bench. A bench is available from

PerkinElmer (Part No. N077-3106).

The main power cable length is 2.4 m (8.0 ft.).

To provide access for servicing and space for ventilation, allow at least 61 cm (24
in.) of space between the instrument and the laboratory walls.

81 cm
(32 in.)

76 cm
(30 in.)

132 cm
(52 in.)

Figure 2-2. Outside Dimensions of the Optima 2000 DV Instrument.

 Cooling Water Requirements 2-9

Computer and Printer

Refer to the manuals supplied with your computer and printer for dimensions.

Neslab Chiller
The Neslab CFT-75 recirculating Chiller (or equivalent) is usually located on the
floor, to the right side of the instrument. Its dimensions are 37.8-cm (14 in.) wide,
65.4-cm (25.8 in.) deep and 67.3-cm (26.5 in.) high. It weighs 82 kg (181 lbs.). The
Chiller has air intakes and exhausts that need to be unobstructed. The power is 2200
watts. It requires a minimum of 45.7 cm (18 in.) on all sides for adequate ventilation.
The coolant hoses restrict the distance that the Chiller can be placed away from the
instrument (hose length = 1.4 meters or approximately 4 feet).

Cooling Water Requirements

A water supply is required to dissipate heat from the RF coil and the oscillator.

Recirculating System
A recirculating system (Chiller) must be used. The requirements for the Chiller are:

o
Cooling Capacity at 20 C 950 watts
o
Temperature Stability 1 C
Pump Rate 1 US gal/min. at 55 psi max (45 psi min).
Coolant: distilled water

A Neslab CFT-75 Recirculating Chiller meets these requirements and is

recommended for the instrument. The Neslab CFT-75 is available through
PerkinElmer in the following two configurations:

208/230V, 60 Hz PerkinElmer Part No. N812-2122

220/240V, 50 Hz PerkinElmer Part No. N812-2123 (For Europe the
PerkinElmer Part No. is ED00-0097)

For detailed information on Neslab Recirculating Chiller electrical requirements see

the following section, Electrical Requirements.
2-10 Preparing Your Laboratory

The Neslab Chiller comes with its own Instruction Manuals. The headquarters for
Neslab Instruments is located at:

NESLAB Instruments, Inc.

25 Nimble Hill Road
Newington, New Hampshire 03801

Service Assistance: (603) 427-2877

Ordering and
Product Information: (800) 258-0830
FAX: (603) 436-8411

Electrical Requirements
The following sections describe the power requirements for all the components that
make up the Optima 2000 DV Spectrometer system.

Optima 2000 DV Instrument

A means of electrically grounding the instrument must be available at

! the customer.
Warning

The Optima 2000 DV instrument is supplied with a 2.5 m (98 in.) power cable (Part
No. B081-0548) that supplies both the spectrometer and the RF Generator modules.
The Optima 2000 DV requires a 200-240VAC, 50/60 Hz electrical line with a
separate circuit breaker. Only single-phase power is needed. The line should be rated
at 15 Amps, though the instrument does not draw all of this capacity. The Optima
2000 DV draws 9 Amps at 240V. The maximum power consumption for the RF
generator and the spectrometer is 2800 volt-amperes.

Note The Optima 2000 DV must not have a Ground Fault Circuit Interruptor
(GFCI) protected outlet. The instrument will trip the interruptor if this type
of outlet protection is used.
 Electrical Requirements 2-11

The Optima 2000 DV is equipped with an IEC 309 250 V 16/20A 2 pole plus
protective earth (Hubbell Part No. C320P6SVL, PerkinElmer Part No. 0999-7530)
that inserts into a receptacle (Hubbell Part No. C320R6SVL, PerkinElmer Part No.
0999-7529).

To order directly from Hubble you can also use these two alternative Hubble part
numbers.

• For the US/Canada (20A service) use Hubble Part No. C320R6W.

• For Europe (16A service) use Hubble Part No. C316R6S.

A conduit box (PerkinElmer Part No. 0994-0914) is not provided with the
instrument but can be ordered through PE Express.

Grounding circuit continuity is vital for safe operation of this

instrument. Grounding is accomplished by use of an IEC309
instrument power plug furnished by the factory and not to be removed
during or after installation.

Note PerkinElmer instruments will normally operate within 10% of the

specified voltage and within 1 % of the specified frequency, unless
otherwise noted. If the power line is unstable, fluctuates in frequency or is
subject to surges, additional control of the incoming power may be
required.

Computer and Printer

Refer to the manuals supplied with your computer and printer for electrical
requirements.

Note The computer and printer must share a common ground with the Optima
2000 DV.
2-12 Preparing Your Laboratory

Neslab Chiller
The specific electrical requirements for the Neslab CTF-75 Chiller are printed on a
serial number label located on the back of the unit. The voltage of the power source
must meet the specified voltage 10%. In addition, an adequate ground connection
must be provided.

For 60 Hz installations, the Neslab CFT-75 208/230 V, 60 Hz, 15A unit is supplied
with a 15-ampere, 250-volt Hubbell #4570-C Twist-Lock power plug (NEMA L6-
15P configuration). A Hubbell #4560 or equivalent receptacle (NEMA L6-15R
configuration) is also required, and is supplied with the instrument.

For 50 Hz installations, to accommodate most countries which require 50Hz

installations, the Neslab CFT-75 220/240 V, 50 Hz, 15A unit is supplied with two
detachable line cords.

Note NEMA: The National Electrical Manufacturer’s Association; CEE:

International Commission on Rules for the Approval of Electrical
Equipment

Pneumatic Requirements

Argon
Liquid or gaseous argon can be used with the Optima 2000 DV system. The use of
liquid or gaseous argon tanks is determined primarily by 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 for safety reasons. The over-pressure regulator vents the tank as
necessary to keep the argon cool enough to remain in its liquid state, thus preventing
the cylinder from exploding due to pressure build-up. A tank of liquid argon
containing 160 liters will typically last for 80 hours of continuous running time.

Gaseous argon tanks do not require venting and consequently can be stored for
longer periods without loss. A tank of gaseous argon will last 5 to 6 hours of running
time. The normal argon usage is 16-20 liters/min. with a maximum of 25 liters/min
 Pneumatic Requirements 2-13

(0.04 - 1.0 cu. ft/min). The argon flow for the system (including the ICP) may vary
between 1 and 25 L/min.

Caution Gas delivery lines from the argon tank should be contaminant-free and
not made of plastic. Teflon delivery lines are acceptable.

Available argon pressure should be between 550 to 825 kPa (5.5 to 8.25 bar or 80 to
120 psig ).

Argon can be purchased from local suppliers. The argon for use with ICP systems
should be 99.996% pure.

Purge Gas
Nitrogen or argon can be used to purge the Optima 2000Optima 2000 DV
spectrometer optics. The purge gas high flow is 5 L/min. The low gas flow is 1.0 L/
min.
.
Caution Gas delivery lines from the purge gas tank should be contaminant-free and
not made of plastic. Teflon delivery lines are acceptable.

The available pressure should be between 275 and 825 kPa (2.75 to 8.25 bar or 40 to
120 psig).

The purge gas should be 99.999% pure and is available from local suppliers.

Shear Gas
Air or nitrogen can be used to shear the plasma for the Optima 2000 DV. The Optima
2000 DV RF generator typically consumes the shear gas at a rate of 25 L/min.

The flow rate should be approximately 25 L/min (1.0 cu. ft/min).

Available pressure should be between 550 and 825 (5.5 to 8.25 bar or 80 to 120 psig).
2-14 Preparing Your Laboratory

Regulator
A pressure regulator for use with either argon or nitrogen is available from
PerkinElmer as Part No. 0303-0264. To connect the regulator to the instrument gas
controls, use the 1/4-in. Swagelok connector. The gas tube provided has 1/4-in.
Swagelock fittings.
System Description 3
System Description
Contents
Major Components ...................................................................................... 3-4
Spectrometer ................................................................................................ 3-6
Introduction ........................................................................................... 3-6
Transfer Optics ...................................................................................... 3-8
Monochromator ..................................................................................... 3-8
Detector ................................................................................................. 3-9
Wavelength Correction ....................................................................... 3-11
ICP Source ................................................................................................. 3-12
RF Generator ....................................................................................... 3-12
RF Control Electronics ....................................................................... 3-13
Sample Introduction System ...................................................................... 3-14
Sample Compartment .......................................................................... 3-14
Quick-Change Adjustable Torch Module ........................................... 3-14
Torch ................................................................................................... 3-14
Spray Chamber .................................................................................... 3-14
Nebulizers ........................................................................................... 3-15
Nebulizer Heater ................................................................................. 3-17
Peristaltic Pump .................................................................................. 3-18
Autosampler ........................................................................................ 3-18
Switches and Controls ............................................................................... 3-19
Main On/Off Switch ........................................................................... 3-19
Interlocks ............................................................................................. 3-19
EMO Switch ........................................................................................ 3-20
Hardware Setup and Optimization ...................................................... 3-21
Connections to Electrical, Gas, and Cooling Water Supplies ................... 3-22
Technical Data ........................................................................................... 3-24
ICP Plasma Generator System ............................................................ 3-24
Gas Flow Controls ............................................................................. 3-24
Sample Introduction System ............................................................... 3-25
Spectrometer ...................................................................................... 3-26
3-4 System Description

Major Components
The Optima 2000 DV instrument consist of two major components: the ICP Source
andthe spectrometer. Each component is further divided into the different modules
described below. This modular system design facilitates system access, testing and
servicing.

The spectrometer consists of the following modules:

• Optics module
• Spectrometer electronics module
• Spectrometer pneumatics module

The ICP source consists of three modules:

• RF generator module
• High voltage power supply module
• Plasma pneumatics module

In addition, the sample compartment contains a Quick-Change Adjustable Torch

Module, which can be removed easily to replace the torch.
 Major Components 3-5

Sample Introduction Spectrometer

Compartment with
Quick Change
Adjustable Torch Module
Torch Compartment

Peristaltic Pump

Figure 3-1. The Optima 2000 DV.

3-6 System Description

Spectrometer

Introduction
The core of the optical system comprises a dual echelle monochromator with a dual,
backside-illuminated, cooled, CCD detector. The system is specifically designed for
ICP-OES. Computer controlled transfer optics direct the radiation from the plasma
into the monochromator. The optics housing is sealed and continuously purged with
high purity nitrogen.

Signals at the required analytical wavelengths are measured using a scanning CCD
(charged coupled device) based technology, with simultaneous measurement of the
background emission and a neon spectrum for active wavelength correction.
 Spectrometer 3-7

Echelle Grating
Parabolic
Collimators

Transfer Optics
Mirrors

Torch Prism
Detector
Radial View Entrance Slit
(Internally
reflective face)
Intermediate Slit
(This is where the neon reference beam enters.)

Echelle Grating
Parabolic
Collimators

Transfer Optics
Mirrors

Axial View

Torch Prism
Detector
(This mirror moves out of the (Internally
optical path for Axial viewing.)
Entrance Slit reflective face)
Intermediate Slit
(This is where the neon reference beam enters.)

Figure 3-2. Schematic diagram of the optical system.

3-8 System Description

Transfer Optics
The computer controlled transfer optics are used to select either radial or axial
viewing of the plasma and to direct the radiation from the plasma onto the entrance
slit of the monochromator. The exact viewing position, horizontal and vertical
position, can be selected in the software.

An automatic shutter closes between measurement cycles to reduce the exposure of

the optics to excess UV radiation.

Monochromator
In the dual echelle monochromator, the prism monochromator acts as a preselection
system to select the required wavelength range to pass on to the echelle
monochromator. Optimally positioned slits and baffles result in very low stray light
levels reaching the echelle monochromator. The prism and echelle dispersion
systems use Littrow configurations, designed to eliminate astigmatism, with
identical, 300 mm focal length, 10° off-axis, parabolic, collimating and focusing
mirrors.

The echelle grating has 79 lines/mm with a blaze angle of 63.4°. The grating is used
in the higher orders, where the high efficiency and high dispersion allow a relatively
short focal length resulting in a compact optical system.

Wavelength selection is achieved by simultaneous rotation of the prism and grating.

Since the maximum rotation required for either element is not more than +/– 2°, the
average wavelength selection time is less than 2 seconds. To further optimize the
analysis time, the wavelengths required are sorted to minimize the change-over time
between any two consecutive wavelengths.

The dual monochromator system enables relatively high slits to be used with no loss
of image quality, which contributes to the high optical throughput. In addition, part
of the slit height is used for the simultaneous measurement of a neon reference
spectrum for wavelength correction.

Two slit width settings are available, optimized for UV and visible wavelengths. The
system automatically selects the correct slit for each analytical measurement.
 Spectrometer 3-9

Figure 3-3. Monochromator

Detector
The detector is a two-dimensional CCD device containing approximately 25,600
pixels. The photosensitive area is separated into two differently sized arrays that are
used for separate reference and analytical measurements. The analytical signal is
measured in the larger, lower array.

The rear of the actual detector area is thinned to a few micrometers to allow
illumination from the rear. This prevents the absorption of radiation by components
other than the detector pixels and maximizes the quantum efficiency without the use
of a fluorescent coating.
3-10 System Description

Output Register for the

reference measurement

2 mm CCD array

3.5 mm CCD array

Output Register for the

analytical measurement

3 mm
↔

Figure 3-4. Detector

At 240 nm the array covers a wavelength range of approximately 0.52 nm, and at 850
nm, approximately 25 nm. Thus the emission line for the analyte of interest and
emission on each side of the analytical line fall simultaneously on the array. This
allows simultaneous measurement of the analyte and background signals.

To improve performance and reduce noise levels, the CCD detector is cooled
between –7 and –8 °C with an integrated Peltier cooler. The entire CCD is
hermetically sealed and the housing filled with dry nitrogen.

How the CCD works

Photons of radiation from the analyte emission strike the photosensitive area of the
detector where photoelectrons are produced in each pixel of the detector. The
electrons are moved into the register where they accumulate as electric charge. The
charge is allowed to accumulate for the period selected for the integration time. At
 Spectrometer 3-11

the end of the integration time, the charge is transferred out of the register to the
signal processing electronics. The pixels in each vertical row are binned into the
register for the respective array. This use of an effective pixel length of 3 mm results
in the low noise performance typical of CCD devices.

Photons

e- e-
e-
e-

Photosensitive Register
Register

Figure 3-5. Storage of photoelectrons during integration.

Wavelength Correction
The optical system uses a two-component, active wavelength stabilizing system. The
overall stability is controlled by temperature and pressure sensors in the optics
housing.

Any residual deviations are compensated for by measuring a neon reference

spectrum simultaneously with each measurement of an analytical emission line. The
output from a neon discharge lamp is collected by an optical fiber and projected onto
the top half of the intermediate slit in the monochromator, which is the entrance to
the echelle monochromator. The neon spectrum passes through the echelle system
with the analytical radiation and illuminates the top array of the detector. The neon
spectrum acts as a wavelength scale to enable active wavelength correction.
3-12 System Description

ICP Source

RF Generator
The Optima 2000 DV uses a 40-MHz free-running solid state RF generator. The RF
power from the solid state oscillator is used to ionize the argon in the torch and excite
the atoms of the liquid sample so that they emit energy at their atomic wavelength in
the form of photons. The photons from the torch are detected optically and measured
electronically in the spectrometer section of the Optima 2000 DV. It is displayed in
terms of wavelength and intensity, which are converted to sample concentration.

The RF generator provides a power output of 750 to 1500 watts. The power output
levels are computer-controlled and may be adjusted in one-watt steps for different
sample matrices.

The RF generator is designed with RF Power Control (RFPC), using a power control
loop which maintains the plasma setting regardless of line voltage fluctuations and
changes in the plasma.
 ICP Source 3-13

AC Power RF Power
Input to Load Coil
40 MHz
RF Power
Control Generator Power Plasma
Feedback Measurement
Signal Signals

RF Power
Control
Loop

Microprocessor

Figure 3-6. Block diagram illustrating the RF Power Control (RFPC)

RF Control Electronics
The RF generator uses solid-state circuits. The solid state RF generator is designed
to significantly increase reliability and reduce the need for recalibration.

The RF generator also monitors plasma conditions. If the plasma is unstable, the
system automatically shuts it off.

To ensure operator safety and to protect the instrument from damage, the system
includes extensive use of RF shielding and safety interlocks. Proper RF shielding
and filtering are provided so that the system complies with FCC and CE regulations
regarding radio frequency radiation.
3-14 System Description

Sample Introduction System

Sample Compartment
The sample compartment has a side door to provide easy access to the sample
introduction module. The front door has a window so that the operator can safely
view the plasma. The front door has safety interlocks that shut down the plasma if a
door is opened during operation. The front door has a finger lock to secure it when
it is closed. The torch compartment has extensive shielding to prevent exposure to
radio frequency radiation.

Quick-Change Adjustable Torch Module

The Quick-Change Adjustable Torch Module is the quartz torch, injector, spray
chamber, and nebulizer/end cap – all in one assembly. This module can be quickly
removed from the sample compartment. This adjustable mount allows the torch an
adjustment of up to 8 mm.

In addition, adapters are available for special applications, such as the use of an
ultrasonic nebulizer or an external spray chamber.

Torch
The torch has a standard alumina injector with a 2.0 mm inner diameter. Other
injectors available include alumina injectors in different sizes for optimum sample
flow rate, and quartz injectors for different sample types.

Spray Chamber
A Ryton, double-pass Scott-type spray chamber and the GemTip Cross-Flow
pneumatic nebulizer are the standard components supplied with the instrument. This
rugged combination provides the best results for a variety of elements. Depending
on the instrument configuration ordered the instrument may include a Scott-type
spray chamber or GemTip Cross-Flow pneumatic nebulizer and a cyclonic spray
chamber. Other combinations will also be available.
 Sample Introduction System 3-15

Nebulizers
PerkinElmer offers these nebulizers for a wide variety of applications:

Description/Part No. Uses/Advantages

GemTip Cross-Flow Good general purpose nebulizer for the analysis of

Nebulizer end cap strong mineral acids (including HF) and samples
N068-0503 with less than 5% dissolved solids. Uses GemTips
made of sapphire and ruby in a Ryton end cap for
maximum chemical resistance.
GemCone High Solids GemCone is for samples with high
(Conespray) dissolved solids (up to 20%). Low Flow GemCone
Nebulizer permits lower nebulizer gas flow rates, useful for
High Solids: N069-0670 spectral lines with high excitation energies and for
Low Flow: N069-0671 providing a more robust plasma. GemCone
nebulizers require an end cap (Part No. N068-0343).
Concentric Glass Provides excellent sensitivity and precision for
Nebulizer aqueous solutions and samples with few dissolved
(MEINHARD) solids (less than 1%). Self-aspirating. Not to be used
with solutions containing hydrofluoric acid.
PerkinElmer offers three types, Meinhard A, C, and
K, which are described below. All require an end cap
(Part No. N068-0343).
MEINHARD Type A General purpose Meinhard nebulizer.
0047-2020
MEINHARD Type C Used for samples containing high dissolved solids
0047-2022 (up to 20%).
MEINHARD Type K Optimized for samples that require reduced nebulizer
N068-1574 gas flow rates, such as organic-based samples.

U-6000AT+ Ultrasonic For samples with low analyte and low matrix
Nebulizer concentrations. Typically improves detection limits
N069-1709 (115 V) by a factor of 10 over conventional pneumatic
N069-1710 (230 V) nebulizers.
3-16 System Description

Figure 3-7. GemTip Cross-Flow nebulizer and end cap N068-0503 (also shown in
cross-sectional view).

Figure 3-8. GemCone nebulizer and end cap N068-0343 (also shown in cross-sec-
tional view).
 Sample Introduction System 3-17

Figure 3-9. Concentric glass nebulizer and end cap N068-0343 (also shown in
cross-sectional view).

Note The MEINHARD nebulizer will aspirate liquid sample naturally. The
nebulizer may also be operated with externally pumped sample, provided that
the sample flow is not significantly below the natural aspiration rate.

Nebulizer Heater
The nebulizer heater allows you to set the temperature of the spray chamber
enclosure to provide a constant temperature for the spray chamber. The nebulizer
heater ensures maximum long-term stability even as room temperature varies.

The use of the nebulizer heater also ensures that the sample aerosol is uniformly
maintained with respect to temperature and aerosol droplet size. The heater can be
used with the cyclonic and the Scott-type spray chamber. The nebulizer heater
temperature can be controlled via the software and the spray chamber door must be
closed for the heater to work properly. The heater should always be on for inorganic
analyses.
3-18 System Description

For organic, high solids or salt analyses the spray chamber should be as cool as
possible, therefore we recommend that you do not use the heater to achieve the best
performance. We also recommend that you leave the sample compartment door open
when running organic analyses. Also do not use the nebulizer heater when using an
ultrasonic nebulizer.

Peristaltic Pump
The peristaltic pump is fully computer-controlled. As an added feature, the pump
speed can be programmed to run at a fast speed for the read or rinse cycle. The
TubingSaver mode is a feature for extending the life span of pump tubing.

Autosampler
The PerkinElmer AS-90, AS-90 plus and AS-91 Autosamplers are available for
automated sample handling. These autosamplers consist of a sample table, a sample
tray, and a motorized sampling arm with an attached probe. Three sample trays are
available for each autosampler, covering a variety of sample volume and total sample
capacity requirements. All sample trays have one location for a 150-mL wash vessel.

AS-90 and 90 Plus

Number of Locations
Sample Trays

Sample Tray A 152 total locations / 144 sample locations

Sample Tray B 106 total locations / 98 sample locations
Sample Tray C 44 total locations / 44 sample locations

AS-91 Sample Trays Number of Locations

Sample Tray E 226 total locations / 218 sample locations

Sample Tray F 160 total locations / 152 sample locations
Sample Tray G 63 total locations / 63 sample locations
 Switches and Controls 3-19

Switches and Controls

Main On/Off Switch

The Main Instrument switch is used to turn on the spectrometer (and is normally left
on). Once the plasma has been ignited, you should wait one half hour for the system
to stabilize before running samples.

Interlocks
Interlocks are designed to ensure operator safety and protect the instrument from
damage. The main system interlocks are described below.

The following interlocks must be satisfied in order to ignite the plasma. If any of
these interlocks is interrupted while the plasma is on, the plasma will automatically
be shut down.

• The front door on the sample compartment must be closed before you can ignite
the plasma.

• Argon pressures for the torch must be correct.

• Cooling water must be flowing to the RF coil and oscillator.

• Torch must be installed.

• Shear gas pressure must be correct.

• Emergency Plasma Off switch on front of instrument must be released.

3-20 System Description

EMO Switch
The Optima 2000 DV has one illuminated switch, the red Emergency Off Switch.
If it is blinking slowly the instrument is in the middle of an ignition cycle. It blinks
rapidly after the Emergency Off Switch is depressed. This is an indication that the
switch has been depressed and to remind you to push the switch again to release it.
This switch shuts off the plasma in an emergency by disconnecting the main voltage
circuitry in the RF generator. To restart, you must release the switch by pressing the
switch again. Reset the RF generator using the software Reset button. (The
spectrometer stays on.)

Emergency Off Switch

Figure 3-10. Location of Red Emergency Plasma Off Switch.

 Switches and Controls 3-21

Hardware Setup and Optimization

The following hardware settings are controlled by the software.

• RF Power: Power levels can be adjusted in 1-watt increments.

• Plasma and auxiliary argon flow rates: Flow rates can be automated during the
analysis with specific flow rates for each element if desired. Plasma argon is
adjustable in 1 L/min increments. Auxiliary argon is adjustable in 0.1 L/min
increments.

• Nebulizer argon flow rate: The flow rate is automatically controlled using a
mass flow controller in 0.01 L/min increments.

• Pump rate: By specifying the desired flow rate (adjustable in 0.1 mL/min
increments) and the tubing diameter, the software calculates the pump speed.

• Nitrogen purge rate: A high or normal flow rate can be specified.

• Dark current measurement: A shutter under software-control can be closed to

block light from the plasma from reaching the detector in order to measure dark
current.

• TubingSaver: A feature for extending the life span of pump tubing for the
peristaltic pump.

• The area of the plasma viewed by the optical system can be adjusted horizontally
and vertically using a computer-controlled moveable transfer optic. The
software also has a built-in optimization function for plasma viewing.
3-22 System Description

Connections to Electrical, Gas, and Cooling Water Supplies

Note All gas lines supplied with the instrument are 6.5m (20 ft.) long. Ensure
that the gas connections are located in close range (within 6.5 m) to the
instrument.

Label reads... Use... To connect...

Electrical IEEE (on side IEEE-488 cable Instrument to the

Connections of spectrometer) 0999-1355 computer
(spectrometer Power cable Instrument to 200-
side of (attached to 240 VAC, 16 amp
instrument) instrument) IEC-309 connector
outlet
Gas Connections N2 Supply Nitrogen hose Nitrogen inlet to
N069-0275 nitrogen supply
Shear Gas Air hose Require a supply of
Supply 0077-0348 air (typically) or
included with Air nitrogen for the
Dryer Filter and shear gas.
regulator assembly
Ar Supply Argon hose Argon inlet to argon
N069-0274 supply
Cooling Water H2O IN (Red Tubing Chiller or cooling
Connections Tie) N077-0341 water supply
(spectrometer side
of instrument)
H2O OUT Tubing Chiller or cooling
(White Tie) N077-0342 water return
 Connections to Electrical, Gas, and Cooling Water Supplies 3-23

Gas Connections
Shear Gas Supply
Ar Supply N2 Supply

Coolant IN
Coolant OUT

Instrument
Power to 200-240 VAC
Switch 16 AMP
Computer IEC-309 Outlet
Connection
INLET

OUTLET

Filter

Neslab CFT-75
Chiller

Figure 3-11. Electrical, gas, and cooling water connections on the spectrometer
side of the instrument.
3-24 System Description

Technical Data

ICP Plasma Generator System

Frequency: 40 MHz, free-running

Output Power Stability: <0.1%

Power Output: 750 to 1500 watts, computer-controllable in 1 watt increments. RF

generator is located in the left side of the instrument for efficient use of laboratory
space.

RF Shielding: Meets all FCC certification requirements for RF emission (Part 18 of

FCC rules and Regulations). Also complies with VDE 0871 Class B Requirements
and CE Marking Requirements.

Coil: 2-turn 3/[Link] tubing.

Cooling Water: System requires a flow of 1 gal/min at 310 to 550 kPa at a

temperature between 15 °C and 25 °C. A recirculating cooling system is required
(Neslab CFT 75 or equivalent is recommended). A filter for removing sediment is
supplied with the system.

Automatic Ignition: Plasma ignition is computer controlled and totally automated.

The plasma can be turned on at a set time, warming up the system prior to an
analysis, and can be turned off automatically after an analysis.

Safety Interlocks: System checks water flow, shear gas flow, argon pressures, torch
compartment door interlocks, torch installed and plasma stability. The status of these
interlocks is constantly monitored and text information is displayed on the computer
screen. If any interlock is interrupted, the plasma is shut down automatically.

Gas Flow Controls

Plasma Argon Flow: Closed-loop flow control using a proportional valve and a
measured pressure across a known resistor. Computer-controlled to regulate the flow
automatically within the range of 0 to 20.0 liter/minute in 1 liter/minute
[Link] flow system is interlocked to prevent ignition without plasma gas
flowing.
 Technical Data 3-25

Auxiliary Argon Flow: Closed-loop flow control using a proportional valve and a
measured pressure across a known resistor. Computer-controlled to regulate the flow
automatically within the range of 0 to 2.0 liter/minute in 0.1 liter/minute increments.

Nebulizer Argon Flow: Computer-controlled, using a mass flow controller, and is

variable between 0 and 2.0 liter/minute in 0.01 liter/minute increments.

Shear Gas: A compressed-air shear gas (18-20 liters/minute) is used to push the
plasma plume out of the optical path, minimizing the impact of self-absorption in the
cooler plasma plume.

Sample Introduction System

Torch: Demountable design using one-piece quartz tubing for plasma and auxiliary
gas flow. The standard torch is supplied with a 2.0-mm alumina injector for full
corrosion resistance to all acids, including hydrofluoric and aqua regia. A 0.8-mm
injector is available as an option for analysis of very volatile organic solutions. As
options, 3.0-mm, 1.6-mm and 1.2-mm quartz injectors are available.

Spray Chamber: Scott-type designed to minimize pulsations from the peristaltic

pump and constructed of Ryton for complete corrosion resistance to most acids,
including HF, and all organic solvents normally used in ICP analyses.

Nebulizer: Cross-flow design with chemically resistant GemTips manufactured

from corrosion-resistant (sapphire tips in a PEEK body) material. The system can
routinely handle 50% (v/v) solutions of HCl, HNO3, H2SO4, H3PO4, 20% (v/v) HF
and 30% (v/v) NaOH. Up to 20% NaCl can be aspirated by the nebulizer for 1 hour
without clogging. The system is fully compatible for use with other nebulizers such
as ultrasonics, concentrics (MEINHARD) and GemCone types. A low flow
GemCone nebulizer is included the instrument.

Peristaltic Pump: A three-channel, variable speed, computer-controlled pump.

Speed is variable from 0.2 to 5 mL/minute in 0.1 mL/minute increments using 0.76
mm (0.030 inch) tubing.

Torch Mount: In Quick-Change Torch Module both horizontal and vertical viewing
of the plasma are optimized by computer-controlled movement of the first transfer
mirror.
3-26 System Description

User Plasma Viewing: The full plasma is viewed through a UV-blocking, low-
transmittance window located in the sample compartment door.

Spectrometer
Monochromator: Wavelength range: 165 nm – 800 nm. High throughput, f/6, dual
echelle monochromator. Echelle grating: 79 line/mm, blaze angle: 63.8 °. Dispersing
prism: 30 ° calcium fluoride. Spectral bandpass: 0.009 nm at 200 nm, 0.027 nm at
700 nm.

Transfer Optics: Computer-controlled toroidal mirrors. Adjustable viewing

position: +/– 15mm along the plasma; +/– 10 mm across the plasma.

Detector: Dual, backside-illuminated, cooled, CCD detector. Cooling to between -

7 and -8 °C with integrated Peltier cooler. Detector area: approximately 3 x 5 mm
split into a reference and an analyte array with separate read-out registers. Reference
array: 64 x 192 pixels of 18 x 32 ←m. Analyte array: 64 x 192 pixels of 18 x 56 ←m.
Read-out noise: 30 electrons. Dark current: 150 electrons/pixel/second. Read-out
time: 64 ←s. Full well capacity: 1.1 million electrons. Charge transfer efficiency:
0.99995.

Wavelength correction: Temperature and pressure sensors for the optics housing.
Spectrum from a neon discharge lamp is collected with each analytical
wavelength measurement and acts as a wavelength scale to enable active
wavelength correction.
Installation 4
 Installation
Contents
Installation Summary ................................................................................... 4-4
Moving the Instrument ................................................................................ 4-5
Connecting the Gases and Cooling Water ................................................... 4-6
Connecting the Gases ............................................................................ 4-6
Connecting the Neslab Chiller ............................................................ 4-10
Filling the Neslab Chiller .................................................................... 4-15
Starting Up the Neslab Chiller ............................................................ 4-17
Connecting the System Components ......................................................... 4-17
Setting Up the Computer and Printer ........................................................ 4-20
Installing the Quick-Change Adjustable Torch Module ........................... 4-20
Installing the Quick-Change Adjustable Torch Module ..................... 4-20
Connecting the Nebulizer (Neb) Tubing ............................................. 4-24
Installing the Autosampler ........................................................................ 4-26
Setting Up the Autosampler ...................................................................... 4-28
To Fit the Sampling Probe .................................................................. 4-28
Adjusting the Sampling Probe Height ................................................ 4-29
Instrument Start-up .................................................................................... 4-30
Automatically Aligning the Torch Viewing Position ................................ 4-31
Setting Instrument Parameters ................................................................... 4-33
Plasma Parameters .............................................................................. 4-33
Important Considerations for Dual Viewing ....................................... 4-33
Shipping List ............................................................................................ 4-35
4-4 Installation

Installation Summary
A PerkinElmer service engineer should install your system for the first time or help
you in moving the system. This chapter is provided for your reference should you
need information on moving the system, or reinstalling accessories. 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:

The installation of the system is divided into the following steps:

• Moving the Instrument

• Connecting the Gases and Cooling Water

• Connecting the System Components

• Installing the Quick-Change Torch Module

• Installing and Setting Up the Autosampler

• Setting Up the Printer

• Instrument Start-up

• Automatically Aligning the Torch Viewing Position

Note Procedures for installing the software are in Winlab32 Software

Installation and Administration Guide (Part No. 0993-6397).
 Moving the Instrument 4-5

Moving the Instrument

Caution If moving the Optima 2000 will subject the instrument to any freezing
temperatures you must contact a PerkinElmer service engineer to assist
you in the move. The PerkinElmer service engineer will flush all traces of
cooling water from the RF generator to prevent freezing of RF generator
components.

If you must move the instrument any great distance, especially if the instrument may
be subject to vibration or jolts contact a PerkinElmer service engineer to assist
you in moving your system.

If you are only moving the instrument within the lab or to a laboratory nearby you
may use the following procedure.

• Remove the Quick-Change Torch module.

• Remove the chiller.

• Remove any accessories, for example an autosampler.

• Disconnect all gas and water lines.

• Remove the computer and printer.

• Attach the handles.

• Lift the instrument onto a movable table or put it in the wooden platform
originally shipped with the instrument. See the Unpacking Instructions (Part No.
0993-6390).

• Lift into position at the new location. Make sure that the new location complies
with the laboratory requirements; see Chapter 2, Preparing Your Laboratory.

• Remove the handles.

• At the new location reconnect the Quick-Change Torch module, the chiller, any
accessories, gas and water lines, the computer and the printer; see the procedures
later in this chapter.
4-6 Installation

Connecting the Gases and Cooling Water

After the instrument has been moved into its position, it can be connected to the
various services in the laboratory.

Connecting the Gases

Note All gas hose connections use 1/4 inch Swagelok fittings.

Use two wrenches when making Swagelok connections. Use a space collar (Part No.
0992-0125, supplied in the hose kit) at each Swagelok connection. Tighten the
Swagelok nut until you can no longer turn the knurled space collar. Only if you
cannot locate a space collar, tighten the nut until it is finger-tight, then turn it an
additional 1/4 turn with a wrench. Pre-swaged fittings should be turned 1/8 turn past
finger-tight. Do not over-tighten fittings. Check for leaks with all the connections
made.

Caution The pneumatic tubing kinks easily. Install it so that it is less likely
to twist, fold and kink.

Connect the gases to the instrument as described in the following procedures.

Connecting the Nitrogen Supply

1. Connect the instrument to the nitrogen supply using the nitrogen hose (Part No.
N069-0275, uses 1/4-in. Swagelok fitting) using a 1/4-in. space collar (Part No.
0992-0125) on both ends of the tubing. Refer to Figure 4-1.

2. Set the nitrogen supply regulator between 275 kPa and 825 kPa (2.75 to 8.25 bar
or 40-120 psig).

3. Check for leaks using a proprietary leak testing fluid for high purity gas lines.
 Connecting the Gases and Cooling Water 4-7

Figure 4-1. Pneumatic, water and shear gas connections.

4-8 Installation

Connecting the Argon Supply

Use the following procedure to connect the argon supply.

Caution Gas delivery lines from the argon tank must be contaminant-free
and not made of plastic, although Teflon lines are acceptable.

1. Connect the instrument to the argon supply using the argon hose (Part No. N069-
0274, uses a 1/4-in. Swagelok fitting) using a 1/4-in. space collar (Part No. 0992-
0125) on both ends of the tubing.

2. Set the argon supply regulator between 550 kPa and 825 kPa (5.5 to 8.25 bar or
80-120 psig).

3. Check for leaks using a proprietary leak testing fluid for high purity gas lines.

Connecting the Shear Gas Supply

The shear gas used is typically compressed air; however, nitrogen may also be used.
The shear gas must be clean and dry, so the instrument includes an air dryer filter
assembly (Part No. N077-0198) and is included in the Pre-Installation kit (Part No.
N077-0431). For more information on the requirements for the shear gas supply,
refer to Pneumatic Requirements in the Preparing Your Laboratory, Chapter 2.

An air hose with 1/4-in. Swagelok fittings at each end is supplied in the hose kit that
is shipped with the instrument. A second air hose is included with the PerkinElmer
Air Dryer Filter in the Pre-Installation kit (Part No. N077-0431). The following
procedure describes how to connect the PerkinElmer air compressor, filter and
regulator.

Note If you are using house air, it must be clean and dry. The instrument
includes an air dryer assembly (Part No. N077-0198). Refer to Connecting
the Shear Gas Supply later in this chapter.

1. Install the Air Dryer Filter as described in the instructions that are included with
the filter.
 Connecting the Gases and Cooling Water 4-9

2. Locate the air hose (Part No. N077-0348, uses 1/4-in. Swagelok fittings at each
end) that is shipped with the Air Dryer Filter. Connect the air hose from the air
compressor to the AIR IN fitting on the Air Dryer Filter using a 1/4-in. space
collar at both ends. Make sure the air flow is in the proper direction, as indicated
by arrows on top of the filters.

3. Locate the air hose (Part No. N077-0348, uses 1/4-in. Swagelok fittings at each
end) that is shipped with the instrument in the hose kit. Connect the air hose from
the AIR OUT fitting on the Air Dryer Filter using a 1/4-in. space collar at both
ends.

Setting the Shear Gas Pressure

The following procedure describes how to set the shear gas pressure when using the
PerkinElmer Air Dryer Filter.

1. Make sure the shut-off valve on the Air Dryer Filter is closed (knob turned fully
clockwise), then set the air pressure on the air compressor to between 550 kPa
and 825 kPa (5.5 to 8.25 bar or 80-120 psig).

Do not set the air compressor pressure higher than 690 kPa
(100 psig). The maximum pressure and temperature that the filter
! bowls can withstand is 1035 kPa (150 psig) at 50 °C
Warning (125 °F). At a higher pressure, the filter bowls can be blown off
and cause injury.

2. Check that the metal covers are in position on the filter bowls and the filter bowl
holding rings are properly locked.

Before opening the shut-off valve, always check to make sure

! the filter bowls are properly secured. Injury can result if the
bowls are blown off.
Warning

3. Open the shut-off valve fully (turn counterclockwise). Partial opening may
defeat the action of the water separator portion of the system.
4-10 Installation

4. Close the shut-off valve fully (knob turned fully clockwise), then set the air
pressure on the air compressor to between 550 kPa (5.5 bar and 80 psig) and 825
kPA (8.25 bar and 120 psig).

5. Connect the air hose from the Air Dryer Filter to the SHEAR GAS SUPPLY
fitting on the side of the spectrometer.

6. Open the shut-off valve fully (turn counterclockwise).

Connecting the Neslab Chiller

The Neslab CFT-75 Chiller must be used to supply cooling water to the instrument.
The Neslab Chiller comes with a complete instruction manual. You should be
familiar with this manual before proceeding.

Note You are required to have your electrician install the single wall
receptacle for the Neslab CFT-75 chiller.

The Neslab CFT-75 is available through PerkinElmer in the following two

configurations:

208/230V, 60 Hz PerkinElmer Part No. N812-2122

220/240V, 50 Hz PerkinElmer Part No. N812-2123 (For Europe the
PerkinElmer Part No. is ED00-0097)

Note Teflon tape (PTFE tape) should be used for all pipe-thread
fittings (NPT). Use of Teflon tape can prevent leaks.

Connecting the Water Filter on the Chiller

It is required to install a water filter (Part No. 0990-4845) on the chiller on the water
input line. Refer to Figure 4-2 and 4-3.

The supplied filter, Part No. 0990-4845, consists of three parts; the filter cap, the
filter tank and filter element. A spare filter element (Part No. 0990-4846) is available
separately as a replaceable item. The hose kit (Part No. N077-0183) includes the
Swagelok fittings and Teflon tape (PTFE tape).
 Connecting the Gases and Cooling Water 4-11

Note Use teflon tape on all pipe thread fittings.

1. Install the fitting on chiller port marked "INLET," the 1/2" male NPT to 3/8"
Swagelock tube connector (Part No. 0992-0867).

2. Install the fitting on chiller port marked "OUTLET," the 1/2" male NPT to
3/8" female NPT reducing bushing (Part No. 0992-0868) on the outlet of the
chiller. Into that fitting put the 3/8" NPT Hex nipple (Part No. 0992-0869).

o
3. Mount the 90 3/8 male NPT x 3/8" Swagelock (Part No. 0992-9866) to the top
center port on the filter cap.

4. Remove the filter cap from the filter tank. See the following figure.

Filter
Cap

Filter Element

Filter Tank

Figure 4-2. Installation of the filter cartridge.

4-12 Installation

5. Screw the filter cap sideport to the 3/8" NPT Hex nipple (on the outlet of the
chiller). Orient the filter cap so that the filter tank will hang below. See Figure
4-3 (detail area).

6. Reassemble the filter. (A spare filter element is available as Part No. 0990-
4846.)

o
7. Add 3/8-in. space collars (Part No. 0992-0584) to the 90 elbow on the filter cap
and the connector on the inlet port of the chiller.

8. Connect coolant hoses, N077-0342 (white tie wrap) and N077-0341 (red tie
wrap) as shown in Figure 4-3.
 Connecting the Gases and Cooling Water 4-13

Coolant Supply Hose

(White Tie Wrap)
(Part No. N077-0342)
From
OPTIMA "OUT"

To
OPTIMA "IN"
Chiller
50 Hz N812-2123
60 Hz N812-2122
Coolant Drain Hose
(Red Tie Wrap)
(Part No. N077-0341)

Line Cord
Plug

90° Elbow, 3/8-in. Male NPT x

3/8-in. Swagelok
(Part No. 0992-0866)
1/2-in. Male x
3/8-in. Swagelok
(Part No. 0992-0867)

1/2-in. Male NPT x

3/8-in. Female NPT
Reducing Bushing
(Part No. 0992-0868)

3/8-in. NPT x 2-in. Hex Nipple

(Part No. 0992-0869)

Water Filter
(Part No. 0990-4845)
Figure 4-3. Chiller connections.
4-14 Installation

Connecting the Chiller to the Instrument

1. Connect the instrument’s Water Return Line to the chiller inlet using coolant
drain hose (Part No. N077-0342). See Figures 4-3 and 4-4. The instrument water
outputs have a fitting and tubing to connect them to the return or drain. Use 3/8-
in. space collars (Part No. 0992-0584) at the instrument. See the following
figure.

2. Connect the chiller outlet to the Instrument's Water Input line using the coolant
supply hose (Part No. N077-0341, uses 3/8-in. Swagelok fittings). Use 3/8-in.
space collars (Part No. 0992-0584) at the instrument. See Figures 4-3 and 4-4.
Figure 4-3 shows the chiller connections. Figure 4-4 shows the water supply
connections at the instrument.
 Connecting the Gases and Cooling Water 4-15

3/[Link] Collars
(Part No. 0992-0584)

Coolant IN

Coolant OUT INLET

OUTLET

Filter

Neslab CFT-75
Chiller

Figure 4-4. Water Flow Diagram with Neslab Chiller.

Filling the Neslab Chiller

Use the following procedure to fill the Neslab Chiller.

1. Unscrew the two thumbscrews and remove the Reservoir Access Panel. Refer to
Figure 4-5.
4-16 Installation

2. Remove the Reservoir Plug. Refer to Figure 4-5.

Fill the reservoir to the bottom of the fill hole threads. Use only distilled water with
an addition of Chloramine-T, one gram per US gallon, as an algaecide. The chiller
reservoir has a capacity of 6.8 liters (1.8 US gallons). This would require 1.8 grams
of chloramine-T to be added to the distilled water.

Caution Do not use deionized or tap water in the chiller. Do not use an
algaecide other than that specified above.

3. Keep some coolant fluid beside the unit and proceed to Starting Up the Neslab
Chiller. The reservoir tank may need to be topped off once the unit has been
started.

Reservoir Access Panel

Reservoir Plug

Figure 4-5. Filling the Neslab chiller.

 Connecting the System Components 4-17

Starting Up the Neslab Chiller

Check the following before starting up the Neslab Chiller:

• All plumbing connections are tight.

• The chiller reservoir is full.

• The chiller power cord is plugged in.

1. Turn the On/Off switch to the On position. The refrigeration system and the
recirculation pump will start.

2. With the chiller running, top off the Reservoir Tank and screw in the Reservoir
Plug.

3. Install the Reservoir Access Panel and secure it with its thumbscrews.

Connecting the System Components

Electrical Hazard
To prevent potential injury to yourself and damage to the
! instrument, switch OFF all instruments in the system and
Warning disconnect them from the line power supply before you alter, or
make any new electrical connections.

The system component connections are as follows (see the following figure):

• IEEE cable from the computer to the instrument IEEE connector on the
spectrometer side of the instrument.

• IEEE cable from an optional autosampler to the instrument IEEE connector.

• Centronics Parallel cable from the computer to the printer.

• The Optima 2000 DV is equipped with an IEC 309 250 V 16/20A 2 pole plus
protective earth (Hubbell Part No. C320P6SVL, PerkinElmer Part No. 0999-
7530) that inserts into a receptacle (Hubbell Part No. C320R6SVL, PerkinElmer
4-18 Installation

Part No. 0999-7529). A conduit box, Hubbel PN SP20301, PerkinElmer PN

0994-0914 is not provided with the instrument. These two parts can be ordered
through PE Express.

To order directly from Hubble you can also use these two alternative Hubble part
numbers.

For the US/Canada (20A service) use Hubble Part No. C320R6W.

For Europe (16A service) use Hubble Part No. C316R6S.

Do not connect the instrument. Contact a PerkinElmer service engineer.

• Computer and printer to electrical power 120 V, 50/60Hz or 220/240 V, 50 Hz.

The computer and printer must share a common ground with the
instrument.

• The chiller can be turned on and off via the software if the chiller has been
connected via pluggable terminal strip on the instrument. This cable is provided
with the chiller and cannot exceed three meters.

Caution Extending IEEE cable lengths by making tandem connections

will compromise instrument communication.
 Connecting the System Components 4-19

Instrument to 200-240
VAC
16 AMP (EUROPE)
20 AMP (US)
IEC-309 Outlet

Figure 4-6. System component connections.

4-20 Installation

.
Note The 12-pin instrument connector next to the IEEE connector on
the spectrometer side is a pluggable terminal strip for use with
accessory devices.

Setting Up the Computer and Printer

To install the ICP WinLab software, computer, and printer, refer to Winlab32
Software Installation and Administration Guide (Part No. 0993-6397).

Installing the Quick-Change Adjustable Torch Module

The Quick-Change Adjustable Torch Module is shipped pre-assembled as one unit.
It includes the torch, Scott-type spray chamber, injector, and cross-flow nebulizer.

Installing the Quick-Change Adjustable Torch Module

Before installing the Quick-Change Adjustable Torch Module in the sample
compartment, check that the RF coil is in place and the bonnet is properly seated on
the coil and held in place with the O-ring.

To install the Quick-Change Adjustable Torch Module:

Note The torch is not supplied with the copper foil ignitor in place on the torch
glassware. You must put a piece of copper foil ignitor tape (Part No. N077-
5297) over the ignitor hole in the torch.

1. Open the torch compartment and the sample compartment door.

When installing the Torch Module in the next steps, do so

! carefully so you will avoid breaking the torch and risking
possible injury.
Warning
 Installing the Quick-Change Adjustable Torch Module 4-21

2. With two hands firmly grasping the torch coupler make sure that the markings
visible on the outside of the torch coupler are facing up, the two locking lugs on
the inside of the torch coupler are in an east-west position and the guide pin is in
a south position.

Caution When installing the torch make sure that you do not push the bonnet out
of the RF coil, against the radial window, or up against the ground pointer.

3. Firmly slide the torch coupler, clockwise, into the torch mount so the two
locking lugs and guide pin in the torch coupler engage the channels in the torch
mount. Rotate the torch coupler completely clockwise until it cannot be rotated
any further. See the following figure.

Note For proper ignition, turn the torch coupler fully clockwise and continue an
additional 2 mm from where you want to go. For example, to set at -3
loosen the locking thumbscrew nut (but do not unthread) and move the
torch clockwise to the 1 position. Then go back to the desired position of
-3 and tighten the locking thumbscrew nut.

If in the future when you remove the torch coupler and then gently rotate
to the locked position you will not have to reset it. The torch coupler will
return to the locked position that you set earlier.

For typical applications the following torch positions are recommended:

Analysis System Torch Position

Scott-Cross Flow Sample -2
Introduction System
Cyclonic/Low Flow Gem -1
Cone
High Dissolved Solids* -1
Organics* -3

*For the analysis of high dissolved solids and organics the sample compartment door
must remain open while the instrument is in operation.
4-22 Installation

See Setting Instrument Parameters later in this chapter for more information on
plasma parameters.

Figure 4-7. Installing the torch through the torch mount.

4. Make sure that the Ground Pointer is in close proximity to the end of the torch
glass but not inside the torch glass. If needed, push the Ground Pointer gently
slightly towards the rear of the torch box. Also make sure that the inner glass
tube in the torch is positioned 1.5 mm from the last turn of the RF coil. See the
following figure. The torch assembly is now installed on the instrument.
 Installing the Quick-Change Adjustable Torch Module 4-23

O-Ring
Bonnet
Copper Foil Torch
Ignitor Contact RF Coil

Ground
Pointer
Front of Instrument,
Torch Compartment
Door Open

Ignitor
Contact
Finger

Figure 4-8. Installing the torch into the sample compartment.

5. Slide the bonnet into position around the torch. Angle the bonnet so that it will
not touch the radial window.
4-24 Installation

6. Connect the sample capillary tubing to the nebulizer sample inlet.

7. To the spray chamber drain connect the barbed fitting (Part No. 0992-0528).

8. Attach the Solvent Flex tubing (Part No. 0998-5729) to the barbed fitting. Attach
the other end of the Solvent Flex tubing to the tubing coupler (Part No. 0992-
0865).

9. Use the other end of the tubing coupler (Part No. 0992-0865) to connect the drain
tubing to the peristaltic pump tubing. For more detailed instructions on
connecting the tubing to the peristaltic pump see the section on the Peristaltic
Pump, in Chapter 5, Maintenance.

Connecting the Nebulizer (Neb) Tubing

To connect the nebulizer (Neb) tubing follow these steps and refer to the next figure.

1. Connect one end of the nebulizer (NEB) argon tubing to the nebulizer end cap
and the other end to the quick disconnect.

2. Make sure that the teflon tubing is in good condition. Replace the tubing if
necessary.

3. Connect the drain tubing to the spray chamber.

For instructions on connecting tubing to the peristaltic pump see the section on the
Peristaltic Pump, in Chapter 5, Maintenance.
 Installing the Quick-Change Adjustable Torch Module 4-25

Nebulizer (NEB)
Argon Tubing
Quick Disconnect

Quick Disconnect

Nebulizer (NEB)
Drain Tubing Argon Tubing

Sample
Capillary
Tubing
Waste
Vessel

Figure 4-9. Nebulizer (Neb) connections to torch and nebulizer end cap.
4-26 Installation

Installing the Autosampler

The instrument can be used with the PerkinElmer AS-90, AS-91 or 90 plus
Autosamplers. The following procedures describe the electrical connections
necessary to install the PerkinElmer autosamplers.

After the autosampler is installed, the software must be configured for the type of
autosampler you are using. This can be done during the software installation or, in
the ICP WinLab software, by selecting the Configure Autosampler command from
the System menu. See the AS-90 Series Autosampler Users Guide (Part No. 0993-
5264) for detailed information on installing the autosamper..

To connect the AS-90, AS-91 or 90 plus Autosampler via the IEEE-488 interface:

1. Connect the IEEE-488 cable supplied with the autosampler from the
autosampler to the instrument as follows:

a. Connect one end of the cable to the receptacle on the rear panel of the
autosampler labeled IEEE-488.

b. Connect the other end of the cable to the receptacle on the rear panel of the
computer or the rear panel of the instrument labeled IEEE-488. The IEEE
cables can be stacked.

2. Set the DIP switches on the autosampler as follows:

DIP Switch Settings

1 2 3 4 5 6 7 8

off on on on off off off on

3. Check that the voltage selector on the rear panel of the autosampler is set to the
correct operating voltage.

4. Connect the power receptacle on the autosampler to an AC power source of the

correct operating voltage using the power cord supplied with the autosampler.
 Installing the Autosampler 4-27

Instrument to 200-240
VAC
16 AMP (EUROPE)
20 AMP (US)
IEC-309 Outlet

Figure 4-10. Electrical Connection: PerkinElmer Autosampler to Computer via the

IEEE interface.
4-28 Installation

Setting Up the Autosampler

Caution Never move the sampling probe holder by hand. You may damage
the autosampler if you move the sampling arm tower by hand
when it is under system control.

Turn off the power to the autosampler if you need to move the
tower manually (Unplug the plug-in power supply or disconnect
the autosampler from the spectrometer.)

To Fit the Sampling Probe

After you have completed the installation and electrical connections of the
autosampler, fit the sampling probe as follows and see the next figure:

Caution When you fit the sampling probe, take care not to press forcefully
in any direction on the autosampler arm since this can damage the
arm.

The sampling probe is a complete assembly. Do not attempt to

take the probe apart since this can damage it; reassembly is not
possible.

1. If not already done, carefully insert the sampling probe arm and push it down
fully.

2. Carefully insert the sampling probe from above into the probe guide. Push the
sampling probe down until about 20 mm protrude from the bottom end of the
probe guide. Use the O-ring on the probe to prevent it from slipping.

Note The standard probe is a PTFE-lined epoxy polymer tube. This polymer is
resistant to the acids, alkalis and organic solvents normally used in
analysis. If your samples contain an organic solvent that attacks this
polymer, a PTFE-lined stainless steel sampling probe is offered as an
option (Part No. B300-0152).
 Setting Up the Autosampler 4-29

Autosampler Tower Sample

Tube
Autosampler
Arm Screw
Connector

O-Ring

Holder
Sampling
Probe Guide

Sampling
Probe

Figure 4-11. Inserting the sampling probe.

Adjusting the Sampling Probe Height

1. Turn on the autosampler. Turn on the computer, spectrometer and start the ICP
WinLab software. Check that the software is configured for the tray you are
using.

2. Holding the sample tray so that the location for the wash beaker (location 0) is
at the rear left, place the tray on the autosampler.

3. Place the wash beaker in location 0 in the sample tray.

4-30 Installation

4. Move the autosampler probe to location 0. In the Analysis menu, click on

Autosampler Go To Location. In this window select either Go to Wash
(probe will then go to the wash) or Go To Location (enter the autosampler
location where the autosampler should be moved).

5. Carefully push the sampling probe down until the tip is about 5 mm above the
bottom of the beaker. The sampling probe is now at the correct height.

6. To remove the sample tray, first click on Load Tray to raise the sampling probe,
then remove the tray.

This completes the installation of the sampling probe. See the AS-90 Series
Autosampler Users Guide (Part No. 0993-5264) for detailed information on
connecting the sample tube between the sample probe and the spectrometer’s sample
input system.

Instrument Start-up
First turn on the gases and water [Link] use the Main Instrument switch to turn
on the spectrometer. Launch the Winlab32 software to begin your analyses. Once the
plasma has been ignited, you should wait one half hour for the system to stabilize
before running samples.

When you switch on the spectrometer:

1. The peltier cooling system for the detector starts to cool the detector.

2. The system sets up all the motors for the optics at the default positions for the
axial viewing mode.

3. The system has been continuously monitoring the detector temperature. When
the temperature is stable at about -8 °C, the system continues with the
initialization.

4. The system performs a dark current measurement; this takes about 30 seconds.

5. The system switches on the neon reference lamp and measures the intensity. If
the intensity is too low, the system will attempt to switch on the lamp up to 8
times. If the energy is still too low, the system displays an error message. When
the measured intensity is above the lower limit, the system is ready for use.
 Automatically Aligning the Torch Viewing Position 4-31

The spectrometer initialization is completed when the spectrometer sends a "system

ready" message to the computer.

Automatically Aligning the Torch Viewing Position

This procedure adjusts the torch viewing position for the highest signal intensity.
Perform this procedure when:

• the instrument or software is first installed

• the instrument is moved to a new location

• the torch is removed or replaced

• the RF coil is replaced

1. Switch on the computer and spectrometer, and if required, the autosampler.

2. Switch on the exhaust ventilation system.

3. Start the ICP Winlab software.

4. In the Options menu, click on Autosampler, and make sure that the software is
configured for the autosamper tray you are using.

5. In the Tools menu, click on Plasma Control and ignite the plasma. Allow the
torch to warm up for half an hour before you start the alignment.

6. Prepare a solution containing 1 ppm manganese.

7. In the Tools menu, click on Spectrometer Control.

The Spectrometer Control window appears.

8. Select Axial or Radial. We recommend that you first do the alignment in one
viewing mode, then select the other viewing mode and repeat the procedure.

9. To view spectra collected during the procedure, open the Spectra Display
window.
4-32 Installation

10. Click on Align View in the Spectrometer Control window to open the Align
View dialog.

11. Select the element and wavelength. This is the wavelength that the system will
use to measure the intensities at different viewing positions and locate the
position that gives the highest intensity. Your options are:

Select Manganese, which is typically used as the alignment wavelength for the
majority of analyses.

-or-

Select another element from the drop-down list. This feature is for specialized
analyses where you want to optimize the intensity for an individual analyte of
interest. This may adversely affect the intensities of other analytes.

12. Set the Read Delay time.

13. Aspirate a solution containing the element you have selected.

When using radial viewing, the system adjusts the lateral viewing position only.

When using axial viewing, the system adjusts both coordinates.

The system will determine the intensity at the selected wavelength, while
adjusting the viewing position in incremental steps. In the Results window, a
report is generated that gives the intensities found at each position. The system
changes the Torch Viewing Position to the position that gives the highest
intensity. In the Spectrometer Control window, the software resets the
coordinates so that the 0 and 15 position is at the location of highest intensity.
 Setting Instrument Parameters 4-33

Setting Instrument Parameters

You use the ICP WinLab software to set up the instrument parameters. The
following settings are general recommendations.

Plasma Parameters

Value (Optima 2000 Value (Optima 2000

Parameter
DV) Radial DV) Axial

RF power: 1300 watts 1300 watts

Nebulizer Flow: 0.8 L/min 0.8 L/min
(for Cross-Flow
Nebulizer)
Auxiliary Flow: 0.5 L/min 0.2 L/min
Plasma Flow: 15 L/min 15 L/min
Pump Rate: 1.5 mL/min 1.5 mL/min
Equilibration Time: 15 sec 15 sec

For more information on the above parameters, refer to the Winlab32 Software
Guide (Part No. 0993-6335).

Note Recheck Interelement Corrections (IECs) if you change the

source conditions after the IEC data is collected.

Important Considerations for Dual Viewing

The following recommendations are for the Optima 2000 DV (Dual View)
instrument. Optimum conditions will depend on the type of analyses being
performed.

The following parameters are set in the method:

• Auto integration times are recommended, using the following settings:

4-34 Installation

Read Parameters
Time: Auto: Min: 2 sec, Max: 10 sec

Note A Max time of 100 seconds may be required for detection limit work.

• Check that the read delay, wash time, and rinse times you are using are
sufficient. In general, either longer times are required or a fast pump speed. In
addition, check that the sample waste is being drained properly to avoid solution
filling the torch.

In addition, see the following operating considerations:

• Check the Interelement Corrections (IECs) if you make any changes to the
ionization or excitation characteristics of the plasma after IEC data is collected.
This would include changing the source conditions or changing the nebulizer or
torch.

• To compensate for spectral interferences, use Background Correction,

Interelement Correction (IEC), or Multi-component Spectral Fitting (MSF).
Confirm using interference check standards.

• To compensate for matrix effects, use internal standardization.

 Shipping List 4-35

Shipping List

Table 4-1. Items Shipped with Instruments

Part No. Description
0993-6390 Unpacking Instructions

N080-0500 Instrument

N077-0432 Installation Kit

N077-0433 Spares Kit

N080-0439 Dual View Spares Kit

0993-6226 Hardware Guide

Table 4-2. Items Included in Installation Kit (Part No. N077-0432)

Part No. Description

N077-0183 Hose Kit (includes gas and cooling water

hoses)

N069-0271 Drain Bottle Cap Assembly (includes

PTFE drain tubing, Part No. N822-1152)

N077-3061 Drip Tray for Peristaltic Pump

0990-4991 Drain Bottle

N077-0198 Air Duct Filter Assembly

0993-6225 ICP-OES Instrument Maintenance Log

4-36 Installation

Table 4-3. Spare Parts Available

Part No. Description

N069-0676 Cross-Flow Nebulizer GemTip Kit

N077-0437 Torch Glassware O-Ring Kit

N077-0438 Injector Adapter O-Ring Kit

N077-0600 Adjustable Torch Assembly

N077-0602 Injector Positioning Tool Kit

N077-0603 Torch Injector Assembly

N077-0604 Adjustable Torch Holder Assembly

N077-0605 Cyclonic Adapter Assembly Kit

N069-0288 Axial Drain Assembly Kit

N077-0338 Quartz Torch (Tulip)

N077-5289 Quartz Bonnet

N077-6052 Cyclonic Spray Chamber Assembly

N077-5299 RF Load Coil

0940-1066 Card-PCI GPIB/WIN NT Driver

0999-1355 IEEE Cable

N069-1870 CD-ROM ICP Winlab32

N077-5177 Alumina Injector, 2.0 mm i.d.

 Shipping List 4-37

Table 4-3. Spare Parts Available

N077-5228 Alumina Injector, 1.2 mm i.d

N077-5227 Alumina Injector, 0.8 mm i.d

N077-5247 Sapphire Injector, 2.0 mm i.d

N077-5225 Quartz Injector, 0.8 mm i.d.

N077-5226 Quartz Injector, 1.2 mm i.d.

N077-5223 Quartz Injector, 1.6 mm i.d.

N077-5014 Quartz Injector, 2 mm i.d.

N077-5224 Quartz Injector, 3 mm i.d.

0992-1045 Small O-Ring for Gem Tips

N069-0671 Low Flow Gemcone Nebulizer

N068-0504 Endcap Assembly

N077-0336 Gemcone Nebulizer Tubing

N822-1152 Teflon Tubing, 1 mm i.d., for Spray

Chamber Drain (after pump tubing)

N077-6027 Knurled Nut

N077-0604 Torch Holder Assembly

N077-0603 Injector Adapter Assembly

N077-5297 Copper Foil (1 foot-48 squares)

N077-6036 Injector O-Ring Plug

4-38 Installation

Table 4-3. Spare Parts Available

N077-0438 Injector Adapter O-Ring Kit

0992-3383 Injector Adapter Cap

0998-5729 Solvent Flex Tubing, 1.5 mm i.d. for

Spray Chamber Drain (before pump tub-
ing)

0250-6241 Tubing for Drain Connection to Sample

Bottle

N077-5220 Air Filter for RF Generator

0990-2001 O-Ring, Cross-Flow Nebulizer,

2 included

0990-2033 End Cap O-Ring

0990-4846 Filter Element, Cooling Water

0998-5729 Solvent Flex Tubing

0992-3037 Solvent Flex Tubing, 1.14 mm (PVC drain

tubing)

0998-5708 Teflon Tubing Piece, Nebulizer

0990-8143 Teflon Tape

0999-5098 Air Filter for Spectrometer Fan

0998-5730 Solvent Flex Tubing, 0.76 mm i.d.

0047-3550 Solvent Flex Pump Tubing, 0.76 mm

(PVC sample tubing)

0999-2731 Purge Window, Axial

 Shipping List 4-39

Table 4-3. Spare Parts Available

N069-0672 Purge Window, Radial

0992-1057 Purge Extension O-Ring

0992-1036 Radial Window O-Ring

0992-1062 Axial Window O-Ring

A Spares Parts Kit is available and the Part Number is N077-0433.

4-40 Installation
Maintenance 5
 Maintenance
Contents
Introduction ................................................................................................. 5-6
Daily Checks ............................................................................................... 5-6
Daily Cleaning ...................................................................................... 5-6
Argon Supply ........................................................................................ 5-6
Purge Gas Supply .................................................................................. 5-7
Shear Gas Supply .................................................................................. 5-7
Chiller ................................................................................................... 5-7
Vent ....................................................................................................... 5-8
Torch and RF Coil ................................................................................ 5-8
Nebulizer ............................................................................................... 5-8
Peristaltic Pump and Drain ................................................................... 5-8
Periodic Checks ........................................................................................... 5-9
Torch Assembly and RF Coil ............................................................... 5-9
Purge Viewing Window/Tubes .......................................................... 5-10
Nebulizer ............................................................................................. 5-10
Spray Chamber ................................................................................... 5-10
Peristaltic Pump .................................................................................. 5-10
Drains .................................................................................................. 5-10
General System Maintenance ............................................................. 5-10
Torch Viewing Position Alignment .................................................... 5-11
Performance Checks .......................................................................... 5-11
Cleaning the Sample Introduction System .......................................... 5-12
Quick-Change Adjustable Torch Module ................................................. 5-13
Plasma Torch ...................................................................................... 5-13
RF Coil ................................................................................................ 5-14
Removing the Scott Spray Chamber .................................................. 5-15
Removing the Injector ......................................................................... 5-15
Removing and Disassembling the Torch ............................................ 5-17
Cleaning the Torch .............................................................................. 5-19
Cleaning the Spray Chamber .............................................................. 5-21
5-4 Maintenance

Replacing the Torch ............................................................................5-21

Replacing the Torch on the Mount ......................................................5-25
Replacing the Spray Chamber ............................................................5-28
Connecting the Nebulizer (Neb) Tubing .............................................5-28
Replacing the RF Coil .........................................................................5-30
Purge Window/Tubes .................................................................................5-33
Removing and Cleaning the Purge Windows ......................................5-33
Removing the Purge Windows ............................................................5-33
Cleaning the Purge Windows ..............................................................5-35
Adjusting the Position of the Shear Gas Nozzle ........................................5-39
Scott-Type Spray Chamber .......................................................................5-40
Removing the Spray Chamber .............................................................5-40
Removing the End Cap from the Spray Chamber ...............................5-40
Cleaning the Scott-Type Spray Chamber ............................................5-41
Cyclonic Spray Chamber ...........................................................................5-42
Installing the Cyclonic Spray Chamber ...............................................5-42
Etching the Cyclonic Spray Chamber .................................................5-45
Cleaning the Cyclonic Spray Chamber ...............................................5-46
Nebulizers ..................................................................................................5-47
GemTip Cross-Flow Nebulizer ..................................................................5-49
Removing the Nebulizer/End Cap .......................................................5-49
Checking the Spray Pattern .................................................................5-50
Disassembling the Cross-Flow Nebulizer ..........................................5-51
Replacing the Nebulizer/End Cap .......................................................5-61
GemCone Nebulizer ...................................................................................5-62
Daily Cleaning of the Low-Flow GemCone Nebulizer .......................5-62
Daily Cleaning of the High Solids GemCone Nebulizer .....................5-62
Installing the GemCone Nebulizer on the Scott-Type Spray Chamber 5-63
Installing the GemCone Nebulizer on the Cyclonic Spray Chamber .5-64
Cleaning the GemCone Nebulizer .......................................................5-65
GemCone Liquid Fitting Maintenance ................................................5-66
Concentric Glass Nebulizer ......................................................................5-67
Installing the Concentric Nebulizer .....................................................5-67
Cleaning the Concentric Glass Nebulizer ............................................5-69
Peristaltic Pump .........................................................................................5-71
Replacement Pump Tubing .................................................................5-71
Installing the Sample and Drain Tubing ..............................................5-72
Adjusting the Pump Tubing ................................................................5-77
 5-5

Cleaning the Pump .............................................................................. 5-79

Drain ................................................................................................... 5-79
General System Maintenance .................................................................... 5-81
Air Filters ........................................................................................... 5-81
Changing the RF Generator Air Filter ................................................ 5-81
Changing the Spectrometer Air Filter ................................................. 5-81
Changing the Neon Lamp ................................................................... 5-82
Chiller and Filters .............................................................................. 5-83
Fuses ................................................................................................... 5-84
Replacement Parts: General ................................................................ 5-84
5-6 Maintenance

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.

You should perform only the maintenance procedures described in this chapter.
Record your daily maintenance procedures in the ICP-OES Maintenance Log (Part.
No. 0993-6225). If additional maintenance is required, contact a PerkinElmer service
engineer.

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

Daily Checks
The following maintenance procedures should be done on a daily basis.

Daily Cleaning
At the end of each working day, it is recommended that you flush out the sample
introduction system for five minutes with the plasma on. After analyzing aqueous
solutions, flush with deionized water or a 2% nitric acid solution, followed by
deionized water. After analyzing organic solutions, flush the system using clean
solvent. Also clean the spectrometer housing using a mild lab detergent.

Argon Supply
Make sure that an adequate supply of argon is available and connected to the system.
Check that the argon tank(s) have sufficient pressure, and that a spare tank is ready
if necessary.
 Daily Checks 5-7

Argon can be purchased from local suppliers. The argon for use with ICP systems
should be 99.996% pure.

Argon output pressure: 550-825 kPa (80-120 psig)

Purge Gas Supply

The optical path must be purged with either nitrogen or argon. Nitrogen is the
recommended purge gas due to its lower cost. Make sure that an adequate supply of
purge gas is available and connected to the system. Check that the cylinder has
sufficient pressure, and that a spare cylinder is ready if necessary.

The purge gas should be 99.999% pure and is available from local suppliers.

Nitrogen output pressure: 275-825 kPa (40-120 psig)

Shear Gas Supply

The Optima 2000 DV requires a supply of shear gas. The shear gas used is typically
compressed air; however, nitrogen may also be used. Make sure that an adequate
supply of shear gas is available and connected to the system. Check that the supply
has sufficient pressure, and that a spare cylinder is ready if necessary.

Shear Gas output pressure: 550-825 kPa (80-120 psig)

Chiller
Check the plumbing connections for the chiller. Check for leaks. Check the electrical
connections, and make sure the chiller has been filled with distilled water with an
addition of Chloramine-T, one gram per US gallon, as an algaecide. The chiller
reservoir has a capacity of 6.8 liters (1.8 US gallons). This would require 1.8 grams
of chloramine-T to be added to the distilled water.

On a monthly basis drain out and replace the coolant. This insures maximum chiller
efficiency.
5-8 Maintenance

Caution Do not use deionized or tap water in the chiller. Do not use an algaecide other
than that specified above.

Cooling water pressure: 310-550 kPa (3.1 to 5.5 bar or 45-80 psig)

Vent
Check that your vent system is switched on and is not blocked. Check regularly for
proper flow rate of the vent system.

Torch and RF Coil

Inspect the torch, glassware, and aerosol injector tube. The glassware should be
clean, with no traces of deposits or signs of melting.

Caution To extend the life and aid in preventing devitrification of glassware, it is necessary
to remove all traces of alkali on glassware caused by handling it with bare hands. To
remove the alkali, wipe the glassware clean with cotton wool dipped in alcohol.

Caution When the humidity in your lab is high, water can condense on the RF coil when the
torch is not in operation. To prevent damage to the coil, use a soft dry cloth to
gently dry the coil before igniting the torch. Be careful not to change the position
of the coil.

Nebulizer
Check that the nebulizer is not clogged and that the sample capillary tubing is clean
and in good condition. Flush the nebulizer daily with deionized water.

Peristaltic Pump and Drain

Inspect the pump tubing before operating and after every few hours of use. Replace
the tubing when flat spots develop (approximately every eight hours of use). Refer
to the section on the peristaltic pump for the appropriate tubing for different solvents.
 Periodic Checks 5-9

When the pump is not in use, release the pressure plate and release the tubing to
prevent flat spots from forming. For optimal running conditions use the TubingSaver
feature where the pump tubing is flushed out at the end of the day with deionized
water at the fast pump speed.

Always remove the sample capillary or the autosampler probe from the solution it is
in when you are finished using the pump. Otherwise, the solution will siphon into the
spray chamber and flood it.

Be sure the drain tubing is firmly attached to the spray chamber and liquid flows
smoothly through the pump. Keep the drain tubing clear of debris. Empty the drain
bottle as needed.

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. You should consider the usage of your spectrometer and
establish a suitable maintenance schedule, with particular emphasis on the following
areas of the system.

Torch Assembly and RF Coil

Clean the torch components periodically according to the instructions given later in
this chapter to remove accumulated deposits. If using organic solvents, check the
injector and torch regularly for carbon buildup. Replace any cracked or worn O-rings
on the torch assembly.

Caution To extend the life and aid in preventing devitrification of glassware, it is necessary
to remove all traces of alkali on glassware caused by handling it with bare hands. To
remove the alkali, wipe the glassware clean with cotton wool dipped in alcohol.

The RF coil must be kept clean to prevent arcing across the coils. Inspect the RF coil
for any deformations or carbon buildup. Replace the RF coil if there are any signs of
pitting. Pitting causes weakness in the coil which can result in a hole in the coil and
a water leak.
5-10 Maintenance

Purge Viewing Window/Tubes

Remove and examine the window or purge tube for deposits. If you notice a drop in
UV performance clean or replace the windows. Clean according to the instructions
given later in this chapter or replace as necessary.

Nebulizer
Check the nebulizer spray pattern with deionized water. Clean or replace the
nebulizer as necessary.

Spray Chamber
Check for leaks around the nebulizer and drain fitting. Inspect the spray chamber for
deposits and check the condition of the O-rings.

Peristaltic Pump
Check that the pump rollers are clean, not scored, free from deposits due to spills,
and move freely. Remove and clean the pump head if necessary. Replace the pump
rollers if necessary.

Periodically observe the drain tubing. Liquid should drain smoothly from the spray
chamber. If not, adjust the pump tension on the pump tubing.

Drains
Check the spray chamber drain fittings, tubing and connections and replace if
necessary.

General System Maintenance

Regularly check the following:

• Air filters: clean or replace the spectrometer and generator air filters as
necessary.
 Periodic Checks 5-11

• Neslab Chiller: Flush out the chiller every 6 months. Inspect the water filter
(Part No. 0990-4845) installed on the chiller and replace the water filter element
(Part No. 0990-4846) every 3 months or as needed. To fill the chiller, use only
distilled water with an addition of Chloramine-T, one gram per gallon, as an
algaecide. The chiller reservoir has a capacity of 6.8 liters (1.8 US gallons). This
would require 1.8 grams of chloramine-T to be added to the distilled water.

Caution Do not use deionized or tap water in the chiller. Do not use an algaecide other
than that specified above.

Refer to Chapter 4, Installation for more information on filling the chiller.

Torch Viewing Position Alignment

The torch viewing position alignment procedure is used to set the plasma viewing
position of the spectrometer entrance optics for the highest signal intensity. Torch
Viewing Position Alignment procedure is described in Chapter 4, Installation.

Perform this procedure when:

• the instrument is first installed or moved to a new location, or

• the torch is removed or replaced, or

• the RF coil is replaced (important)

Performance Checks
Several checks should be done periodically to check instrument performance. These
include the sodium bullet test to check the nebulizer argon flow, the Background
Equivalent Correction (BEC) test, and Coefficient of Variation (CV) test. These tests
are described in Chapter 6, Troubleshooting.
5-12 Maintenance

Cleaning the Sample Introduction System

See the following table for the recommended cleaning procedures for the sample
introduction system.
Table 5-1. Recommended Cleaning Procedure
Daily cleaning After analyzing aqueous solutions, flush with
deionized water, or 2% nitric acid, followed by
deionized water. After analyzing organic
solutions, flush using a clean solvent.
Torch Soak in 5-20% nitric acid or aqua regia; use an
Bonnet ultrasonic cleaner if available. For more detailed
Injector information, see Cleaning the Torch later in
Spray Chamber this chapter.
O-Rings Clean with soap and water, rinse thoroughly.
GemTips for Clean with soap and water, rinse thoroughly; or
Cross-Flow use a 2% solution of nitric acid.
Nebulizer
GemTip or Clean with soap and water; rinse thoroughly.
GemCone
Nebulizer/End Cap
Assembly
Concentric Glass Do not use an ultrasonic cleaner. Do not use a
(MEINHARD) cleaning wire. See Concentric Glass Nebulizer
Nebulizer later in this chapter.
Spray Chamber By handling the spray chamber oil and dirt can
accumulate on it and this will affect
performance. To assure proper wetting wipe the
spray chamber with acetone to remove all oils
and dirt.
Pump Head Remove and clean with water or a mild solvent.
Purge Viewing Clean with deionized water and dry with a soft
Windows/Tubes cloth. To clean difficult stains, refer to the
information in this chapter.
 Quick-Change Adjustable Torch Module 5-13

Quick-Change Adjustable Torch Module

The Quick-Change Adjustable Torch Module consists of the torch assembly, spray
chamber, and nebulizer. These components are easily removed from the system for
regular inspection and maintenance. Normal wear on these components is shown by
metal or salt deposits on the quartzware or injector, glazed or devitrified quartz, worn
O-rings, or clogged nebulizer tips.

All the O-rings in the sample introduction system must be in place and be in good
condition. Otherwise, pressure leaks may occur, which can cause difficulties in
igniting the plasma and poor performance.

It is good practice to have spare parts available before removing any of the parts of
this module, particularly the torch, since it may be accidentally broken. Replacement
parts are listed at the end of this chapter.

Plasma Torch
The plasma torch assembly is comprised of a quartz torch with an inner quartz tube,
injector, and adapter for securing the injector into an inlet in the spray chamber. The
injector supplied is an alumina injector with a 2.0 mm inner diameter. Other injectors
available include alumina injectors of different inner diameter for varying sample
flow rate, quartz injectors for different sample types and sapphire injectors for silicon
applications. For more volatile solvents, use a smaller diameter injector.

Regularly inspect the torch glassware and aerosol injector tube. The glassware
should be clean, with no traces of deposits or signs of melting. Give particular
attention to the inner quartz tube. Before removing the torch for cleaning, be sure to
have a spare torch available, in case it should break.

The quartz torch is shown in the next figure. The quartz torch has one slot and a glass
bonnet. The torch glassware is slotted so the plasma is viewed optically through the
slot and not the quartz, for best performance while maintaining optimum shielding
of the plasma from entrained air.
5-14 Maintenance

Figure 5-1. Quartz torch.

RF Coil
Regularly inspect the RF coil. It should not show any signs of deforming or pitting.

If your lab has high humidity, check the coil to make sure it is dry. Use a soft dry
cloth to dry the coil if necessary. To replace and adjust the RF coil refer to the
procedure, Replacing the RF Coil discussed later in this chapter.
 Quick-Change Adjustable Torch Module 5-15

Removing the Scott Spray Chamber

1. Place the sample tubing in deionized water and turn on the pump to flush the
spray chamber. Remove the sample tubing from the deionized water and
continue to run the pump a few minutes until the spray chamber is fully drained.
Then turn off the pump.

2. Disconnect the spray chamber drain tubing from the pump tubing for the drain.
Be careful not to have liquid spill out of the disconnected drain tubing. Spilled
liquid should be cleaned up immediately.

3. Disconnect the sample tubing from the nebulizer inlet.

Note Carefully disconnect the sample tubing and nebulizer argon fitting at the quick
disconnect so that the jeweled orifices do not fall out. They are not interchangeable.

4. Disconnect the nebulizer argon fitting from the gas fitting on the quick
disconnect.

5. Pull open the clamp that holds the spray chamber in place. The action of opening
the clamp will partially push the spray chamber out.

6. Firmly hold onto the spray chamber and lift it all the way out of the spray
chamber mounting block, which will disconnect it from the injector adaptor.

Removing the Injector

Once the spray chamber has been removed, the injector can be removed without
removing the entire torch assembly. To do this procedure follow these steps.

1. Push and hold the injector lock with your right thumb while holding the base of
the injector adapter with your left hand.

2. Firmly pull the injector adapter out with your left hand.

Note If the injector adapter pulls off the injector, remove the glassware and grab the
injector and push through. The injector adapter can be pulled off the injector if the
nut on the injector adapter is not tight or the O-rings on the adapter and the base of
the torch are worn.
5-16 Maintenance

Instrument
Left Side

Front of
Instrument

C la m p
To r c h
Sp ra y C h a m b e r C o u p le r

D ra in T u b in g

To r c h
I n je c t o r C o u p le r

In je c to r L o c k

Figure 5-2. Removing the spray chamber assembly.

 Quick-Change Adjustable Torch Module 5-17

Removing and Disassembling the Torch

1. Turn off the plasma if it is on.

If the plasma has been on, the torch glass will be very hot and can cause serious
burns. Wait five minutes after turning off the plasma before you begin these
! maintenance procedures.
Warning

2. Open the side door to the sample compartment.

3. With two hands firmly grasping the torch coupler turn in a counterclockwise
direction. Allow the two locking lugs, located on the side of the torch coupler
and guide pin to pass through the torch coupler channels and out. The torch is
mounted on an assembly that slides out. Carefully slide the torch out of the RF
coil. The torch coupler and torch are now separated from the instrument. See the
following figure.

Torch Coupler
Nebulizer
Spray Chamber
Clamp Torch Glass

Torch Holder

Torch Mount
Spray
Chamber

Figure 5-3. Removing the torch coupler from the torch mount.
5-18 Maintenance

4. Pull open the clamp that holds the spray chamber in place. The action of opening
the clamp will partially push the spray chamber out.

5. Firmly hold onto the spray chamber and lift it all the way out of the spray
chamber mounting block, which will disconnect it from the injector adaptor.

6. Press in the injector lock on the torch coupler and remove the injector. See
Figure 5-2 for a view of the injector lock.

Inspect the O-rings on the injector adapter for cracks and wear. If the O-rings
need to be removed, carefully remove them using a small paper clip with a hook
bent on one end or a mico-spatula. Do not use a knife blade because the blade
will cut the O-rings and damage the O-ring seats. Replace with new O-rings. An
injector O-ring kit is available from PerkinElmer (Part No. N077-0438).

In the next step, be sure to carefully remove the torch so you will avoid breaking the
glassware and risking possible injury. If the torch does break, discard the broken
! torch and replace (Part No. N077-0338). Remove the knurled nut, sleeve and
Warning washers on the torch mounting shaft to make sure that all glass fragments are
removed.

7. Loosen the knurled nut on the torch holder and carefully remove the torch.
Inspect the torch, if it is cracked replace with a new one (Part No. N077-0338).
If the torch needs to be cleaned see the next section Cleaning The Torch for
more information.

8. Inspect the O-rings on the torch mounting shaft for cracks and wear. If the O-
rings need to be removed, carefully remove them using a small paper clip with a
hook bent on one end or a mico-spatula. Do not use a knife blade because the
blade will cut the O-rings and damage the O-ring seats. Replace with new O-
rings. A torch O-ring kit is available from PerkinElmer (Part No. N077-0437).

Caution When the torch glassware is removed from the coil, the bonnet may be on the coil
with nothing securing it. Be careful not to knock it off and break it. There is an O-
ring that can be used to secure the bonnet. (Included with O-ring kit, Part No. N077-
0437.)

Inspect the bonnet, if it is cracked replace with a new one (Part No. N077-5289).
 Quick-Change Adjustable Torch Module 5-19

Figure 5-4. Disassembling the torch.

After installation, you will need to perform the Torch Viewing Position Alignment
Procedure described in Chapter 4, Installation.

Cleaning the Torch

The torch components should be cleaned regularly to remove accumulated deposits.
After prolonged use, a torch may lose its transparency and become crystalline. In this
condition, called devitrification, the torch is very fragile. You should not attempt to
clean a devitrified torch, but it can still be used. If the torch is cloudy, this generally
does not affect performance because the plasma is either viewed through the slot on
the torch, or, for axial viewing, through the open end of the torch.

Caution The copper foil ignitor (Part No. N077-5297) contact must be removed from the
torch glassware before it is cleaned in acid. Replace a new piece of copper foil tape
over the ignitor hole in the torch after the glass is clean and dry.
5-20 Maintenance

If you have been analyzing aqueous solutions, the torch glassware and injector tube
should be cleaned in an acid bath. An ultrasonic bath may be used. Start with a
solution of 5% nitric acid or aqua regia and, if deposits persist, increase the acid
concentration, up to 20% if necessary. Acid solutions must be used with care.
Observe all of the manufacturer's safety recommendations. These recommendations
are normally provided in a material safety data sheet (MSDS) supplied with the
chemical.

Caution To extend the life and aid in preventing devitrification of glassware, it is necessary
to remove all traces of alkali on glassware caused by handling it with bare hands. To
remove the alkali, wipe the glassware clean with cotton wool dipped in alcohol.

Use of hydrofluoric acid for cleaning the torch is not recommended.

If you have been analyzing organic solutions, the torch glassware and injector tube
can be cleaned using a solvent or diluted soap solution. Be sure to inspect the torch
and injector daily for carbon buildup. A muffle furnace can be used if necessary to
remove organic deposits on the torch or injector. Place the torch or injector in a
muffle furnace at 500 C to 550 C for several hours.

After cleaning the torch, dry it thoroughly using clean air or nitrogen. No moisture
should be present.

O-rings may be cleaned with soap and water. An ultrasonic bath may be used.
Replace if cracked or worn. A torch O-ring kit is available. See the list of
replacement parts later in this section.
 Quick-Change Adjustable Torch Module 5-21

Cleaning the Spray Chamber

See page 40.

Replacing the Torch

1. Loosen the knurled nut and firmly grasp the torch and push it slowly into the
torch mount. The glass inlets should face to the front. Rotate the torch so that the
strip on the torch lines up with the index mark on the torch mount and the guide
pin on the torch coupler. Firmly tighten the knurled nut. See the following figure.

Torch Glass

Torch Cutout
Knurled Nut

Washer
O-Ring

Spacer

O-Ring Stripe on Torch

Index Mark
on Torch Holder

Torch
Coupler

Guide Pin

Figure 5-5. Replacing the torch.

5-22 Maintenance

Note If the torch glass does break, discard the broken torch and replace (Part No. N077-
0338). Remove the knurled nut, sleeve and washers to make sure that all glass
fragments are removed.

2. From the back of torch coupler push the injector into the torch adapter until it
locks in place. Press the injector lock to seat the injector. You may use the
Injector Positioning tool (Part No. N077-0602) to accurately locate the tip of the
injector relative to the inner glassware. Press down on the tool to completely seat
the injector in place. See figure 5-7.

Note The Injector Positioning tool (Part No. N077-0602) has a dual purpose. One end is
used to position the injector. The other end can be inserted into the torch holder to
remove O-rings if needed. Also if the injector is stuck in the torch holder due to a
damaged O-ring, the Injector Positioning tool can be used to loosen the injector for
removal (use the O-ring removal end of the tool). See the following two figures.
 Quick-Change Adjustable Torch Module 5-23

Figure 5-6. Using the injector positioning tool to remove O-rings.

5-24 Maintenance

Figure 5-7. Inserting the injector.

 Quick-Change Adjustable Torch Module 5-25

Replacing the Torch on the Mount

The following steps describe how to replace the torch in the mount. Refer to the next
two figures.

1. With two hands firmly grasping the torch coupler make sure that the markings
visible on the outside of the torch coupler are facing up, the two locking lugs on
the inside of the torch coupler are in an east-west position and the guide pin is in
a south position.

Caution When installing the torch make sure that you do not push the bonnet out of the RF
coil, against the radial window, or up against the ground pointer.

2. Firmly slide the torch coupler, clockwise, into the torch mount so the two
locking lugs and guide pin in the torch coupler engage the channels in the torch
mount. Rotate the torch coupler completely clockwise until it cannot be rotated
any further. See the following figure.

Note For proper ignition, turn the torch coupler fully clockwise and continue an additional
2 mm from where you want to go. For example, if you want the torch set in the -3
position, turn clockwise to -5 position and then return the torch coupler to -3
position. Then lock the torch coupler to set the hard stop for the -3 position.

If in the future you remove the torch coupler and then return it to the instrument you
will not have to reset it. The torch coupler will return to the locked position that you
set earlier.
5-26 Maintenance

Figure 5-8. Assemble the torch assembly to the mount.

3. Carefully slide the torch through the RF coil and bonnet. Make sure that the
Ground Pointer is in close proximity to the end of the torch glass but not inside
the torch glass. If needed, gently push the Ground Pointer slightly towards the
rear of the torch box. See the following figure. The torch assembly is now
installed on the instrument.

4. Slide the bonnet into position around the coil and torch. Angle the bonnet so that
it will not touch the radial window.
 Quick-Change Adjustable Torch Module 5-27

O-Ring
Bonnet
Copper Foil Torch
Ignitor Contact RF Coil

Ground
Pointer
Front of Instrument,
Torch Compartment
Door Open

Ignitor
Contact
Finger

Figure 5-9. Positioning of torch in the sample compartment.

5-28 Maintenance

5. Check that the injector is flush or slightly below the inner glass tube of the torch.
If the injector tube is not seated properly an air leak could occur or sample could
drip into the torch.

Replacing the Spray Chamber

1. Orient the spray chamber so that the drain connection is facing down and
towards the rear of the sample compartment. See the following figure.

2. Check the condition of the two O-rings (Part No. 0992-1028) on the spray
chamber/injector adapter. If the O-rings need to be removed, carefully remove
them using a small paper clip with a hook bent on one end or a micro-spatula.
Do not use a knife blade because the blade will cut the O-rings and damage the
O-ring seats.

3. Firmly push the spray chamber into the spray chamber mounting block. Close
the clamp around the spray chamber until it is locked into place. The action of
closing the clamp will secure the spray chamber to the spray chamber mounting
block.

4. Make sure that the sample capillary tubing is in good condition. Replace the
tubing if necessary. Connect the sample capillary tubing to the nebulizer sample
inlet.

5. Attach the drain tubing assembly to the spray chamber drain. Check that the
drain tubing is in good condition and replace if necessary.

Connecting the Nebulizer (Neb) Tubing

To connect the nebulizer (Neb) tubing follow these steps and refer to the next figure.

1. Connect one end of the nebulizer (NEB) argon tubing to the nebulizer end cap
and the other end to the quick disconnect.

2. Make sure that the teflon tubing is in good condition. Replace the tubing if
necessary. Connect the sample capillary tubing to the nebulizer sample inlet.

3. Connect the drain tubing to the spray chamber.

For instructions on connecting tubing to the peristaltic pump see the section on the
Peristaltic Pump, later in this chapter.
 Quick-Change Adjustable Torch Module 5-29

Nebulizer (NEB)
Argon Tubing
Quick Disconnect

Quick Disconnect

Nebulizer (NEB)
Drain Tubing Argon Tubing

Sample
Capillary
Tubing
Waste
Vessel

Figure 5-10. Nebulizer (Neb) connections to torch and nebulizer end cap.
5-30 Maintenance

Replacing the RF Coil

The RF coil may need to be replaced occasionally as a result of overheating, pitting,
or arcing. To replace the RF coil follow these steps and refer to the next figure.

1. Turn off the plasma if it is on.

If the plasma has been on, the torch will be very hot and can cause serious burns.
! Wait five minutes after turning off the plasma before you begin these maintenance
Warning procedures.

2. Turn off the instrument.

3. Remove the torch.

4. Remove the bonnet from the load coil.

5. Turn off the water supply to the instrument.

6. Place paper towels below the load coil to absorb any water that is spilled.

Caution Use a backing wrench on the stationary part of the Swagelok fitting when removing
or installing the load coil. This will prevent any excess pressure from being exerted
on the load coil which could damage the load coil.

7. Loosen the two 1/2-inch Brass Swagelok nuts that hold the RF coil in place.

Caution Do not overtighten the Brass Swagelok nuts when replacing the RF Coil since this
can damage the coil.

8. Replace with a new RF coil (Part No. N077-5299) and tighten the Brass
Swagelok nuts until hand-tight then tighten an additional 1/4 turn.

9. Turn on the water supply and power to the instrument.

Caution If you cannot align the RF coil with the torch and bonnet contact a PerkinElmer
Service Engineer.
 Quick-Change Adjustable Torch Module 5-31

Emergency
Of f Switch

RF Coil
Micro
Switches
(Torch Door
Interlock)

1/2-inch
Swagelok Nuts

Figure 5-11. Replacing the RF coil.

5-32 Maintenance

Table 5-2. Replacement Parts: Torch Module

Part No. Description

N077-0606 Torch Module (includes torch, glassware, injector (Alumina
Injector, 2.0 mm i.d.), Scott-type spray chamber, & GemTip cross-
flow nebulizer)
N077-0600 Torch Module (without torch, glassware, spray chamber or
nebulizer)
N069-0770 Dry Aerosol Adapter
N077-0338 Quartz Torch
N077-5289 Quartz Bonnet
N077-5177 Alumina Injector, 2.0 mm i.d. (standard injector)
N077-5014 Quartz Injector, 2.0 mm i.d.
N077-5223 Quartz Injector, 1.6 mm i.d.
N077-5226 Quartz Injector, 1.2 mm i.d.
N077-5225 Quartz Injector, 0.8 mm i.d.
N077-6027 Knurled Nut

N077-0604 Torch Holder Assembly

N077-0603 Injector Adapter Assembly

N077-5299 RF Load Coil

N077-5297 Copper Foil (1 foot-48 squares)

N077-6036 Injector O-Ring Plug

N077-0438 Injector Adapter O-Ring Kit

N077-0437 Torch Glassware O-Ring Kit

N077-0602 Injector Positioning Tool Kit

 Purge Window/Tubes 5-33

Purge Window/Tubes

Removing and Cleaning the Purge Windows

If the plasma has been on, the torch will be very hot and can cause serious burns.
Wait five minutes after turning off the plasma before you begin these maintenance
! procedures.
Warning

Gradually, deposits may accumulate on the windows, for example, metallic oxides,
and the windows may become etched. You must remove the windows to clean or
replace them.

If you notice a drop in UV performance the purge windows may needed to be cleaned
or replaced even if the windows still look clear. Clean the windows first, if the UV
performance does not improve replace the windows.

The axial window mount is also the purge outlet for the spectrometer. The radial
window is a cylinder with one closed end; this end being the actual window.

Removing the Purge Windows

Note These windows are important parts of the optical system. Handle them carefully, as
you would any sensitive optical component. Do not directly touch the windows.
Always remove the axial window before the radial window and refit the radial
window before the axial window. This will help avoid objects or contamination
falling into the radial snout.

Removing the Shear Gas Nozzle and Torch

1. Remove the torch assembly; see the section Removing and Disassembling the
Torch earlier in this chapter.
5-34 Maintenance

2. Remove the two Torx-head screws that hold the shear gas nozzle
assembly in position and move the assembly carefully to one side. See the
following figure.

Axial Window
to Purge Extension
Shear Gas
Nozzle

Radial Window

Torch

Torx Screws

Retaining Ring

Figure 5-12. Purge Window

Removing the Axial Window

1. Carefully unscrew the axial window [Link] may need to use the key
provided.

2. Remove the O-ring that holds the axial window in the mount and remove the
window.
 Purge Window/Tubes 5-35

Removing the Radial Window

Normally you should remove the axial window before you remove the radial
window. This releases the pressure in the spectrometer and helps avoid objects or
contamination falling into the radial snout.

1. Unscrew and remove the radial window retaining ring. You may need to use the
key provided.

2. Lift the radial window and O-ring out of the mount — take care if the
spectrometer purge is set to high and you have not removed the axial window,
the pressure inside the spectrometer may force out the radial window.

Cleaning the Purge Windows

Note Do not rub the surfaces of the windows before you have cleaned them as described
below. The more you rub the surface of the windows, the more chance there is of
scratching them. You must discard scratched windows.

1. Rinse the windows thoroughly with deionized water.

2. To remove more stubborn marks:

Soak the windows in warm — 40°C, 10-20% nitric acid for one hour.
Rinse the windows thoroughly with deionized water.

3. Dry them with an optical-quality cloth.

Caution Allow to drycompletely before reinstalling. If there is any moisture on the inside of
the window it can degrade the UV performance and/or damage the optics.

4. If the windows are scratched or badly etched, discard them and install new ones.
5-36 Maintenance

Replacing the Radial Window

Note Do not leave fingermarks on the window. Use an optical cloth to handle the window.
Normally you should install the radial window before the axial window. This helps
avoid objects or contamination falling into the radial snout. If the axial window is
already installed, and the spectrometer purge is set to high, the pressure inside the
spectrometer may lift the radial purge window unless you hold it in place until you
have tightened the retaining ring.

1. Install the O-ring in the radial window mount.

2. Place the retaining ring loosely over the mount.

3. Hold the radial window with an optical-quality cloth. Carefully push the open
end of the cylinder through the O-ring right to the base of the mount. The closed
end must be at the top.

4. Screw the radial window retaining ring onto the mount — handtighten firmly.
Do not overtighten. Hold the radial window with an optical-quality cloth and
push the window through the O-ring right to the base of the mount.
 Purge Window/Tubes 5-37

Radial Window

O-Ring

Figure 5-13. Replacing the radial window.

Replacing the Axial Window

Note Do not leave fingermarks on the window. Use an optical cloth to handle the window.

1. Hold the axial window with an optical-quality cloth and refit the window in the
mount.

2. Install the O-ring that holds the window in the mount.

3. Check the purge outlet O-ring. If it is damaged install a new one.

4. Screw the axial window mount onto the axial snout. — handtighten firmly. Do
not overtighten.
5-38 Maintenance

Axial Snout

Radial Window

O-Ring Axial Window O-Ring

Purge Outlet
O-Ring

Radial Window
Mount Axial Window

Figure 5-14. Replacing the axial window.

Replacing the Shear Gas Nozzle and Torch

1. Place the shear gas assembly back into position and insert the two Torx screws.
Slide the shear gas nozzle to the required position, then tighten the screws. The
normal position is when the shear gas nozzle is very near the radial window.
Approximately a 1 mm gap should be between the nozzle and the radial window.
For special analyses you may want to move the nozzle to a different position.

2. Reinstall the torch assembly; see the section Replacing the Torch earlier in this
chapter.

3. Align the torch and perform an axial and radial alignment refer to chapter 4,
Installation.
 Adjusting the Position of the Shear Gas Nozzle 5-39

Note Before you perform an analysis at wavelengths below 190 nm, purge the optics
overnight on high purge. For other analyses, purge the system until you obtain a
steady signal.

Table 5-3. Replacement Parts: Purge Components

0999-2731 Purge Window, Axial
N069-0672 Purge Window, Radial
0992-1057 Purge Extension O-Ring
0992-1036 Radial Window O-Ring
0992-1062 Axial Window O-Ring

Adjusting the Position of the Shear Gas Nozzle

The basic shear gas nozzle position is with a 2 mm gap between the nozzle slit and
the front edge of the axial window mount. For some special analyses you may want
to move the nozzle, for example, for samples containing organics or salts, set the
nozzle slit 4 mm in front of the front edge of the axial window mount.

Note Never set the nozzle slit behind the front edge of the axial window mount.

1. Loosen the two Torx-head screws that hold the shear gas nozzle assembly in
position.

2. Slide the assembly to the position you require, then tighten the screws.
5-40 Maintenance

Scott-Type Spray Chamber

Check the spray chamber periodically for leaks around the nebulizer end cap and
drain fitting. Examine the end cap O-ring for cracking and wear and replace if
necessary. Deposits and plated out metals can accumulate in the spray chamber,
which can introduce “memory effects.” Usually, aspirating a strong acid or solvent
will clean out these deposits. If not, remove the spray chamber and clean it in a 5%
to 20% nitric acid bath.

Removing the Spray Chamber

Refer to the instructions for your instrument, provided earlier in this chapter.

Removing the End Cap from the Spray Chamber

1. Loosen, but do not remove, the two knurled screws in the nebulizer end cap.
Support the spray chamber with one hand as you twist the end cap and end cap
ring, together, off the spray chamber.

2. Examine the spray chamber for any obstructions or wear.

3. The spray chamber has an inner tube that is pressure fitted and difficult to
remove. The outer chamber can be damaged if you attempt to remove a tightly
fitting inner tube. If the inner tube is damaged, the complete spray chamber
should be replaced.
 Scott-Type Spray Chamber 5-41

End Cap Ring

(Part No. 0047-3543)
End Cap
(Part No. N068-1688,
not complete assembly)
Knurled Screw (2)

Spray Chamber

O-Ring
(Part No. 0990-2033)

Figure 5-15. Spray chamber, end cap, and associated parts. (Illustration shows
cross-flow nebulizer end cap assembly, Part No. N077-0546.)

Cleaning the Scott-Type Spray Chamber

If you have been analyzing aqueous solutions, the spray chamber should be cleaned
in an acid bath. An ultrasonic bath may be used. Start with a solution of 5% nitric
acid or aqua regia and, if deposits persist, increase the acid concentration, up to 20%
if necessary. Acid solutions must be used with care. Observe all of the
manufacturer's safety recommendations. These recommendations are normally
provided in a material safety data sheet (MSDS) supplied with the chemical.

If you have been analyzing organic solutions, the spray chamber can be cleaned
using a solvent or diluted soap solution. Be sure to inspect the torch and injector daily
for carbon buildup.

O-rings may be cleaned with soap and water. An ultrasonic bath may be used.
Replace if cracked or worn. A torch O-ring kit is available. See the list of
replacement parts at the end of this chapter.
5-42 Maintenance

Cyclonic Spray Chamber

The cyclonic spray chamber is a glass spray chamber. The cyclonic spray chamber
may be used with the concentric glass, low-flow GemCone, and high flow GemCone
nebulizers. Use a baffled cyclonic spray chamber for organic solvent analysis and a
cyclonic spray chamber without a baffle for aqueous solutions analysis.

Installing the Cyclonic Spray Chamber

The following steps describe how to remove the Scott-type spray chamber and
replace it either with a cyclonic spray chamber assembly (Part No. N077-6052) or a
baffled cyclonic spray chamber assembly (Part No. N077-6053). See the following
two figures.

1. Pull open the clamp that holds the Scott-type spray chamber in place. The action
of opening the clamp will partially push the spray chamber out. Remove the
Scott-type spray chamber.

2. Slide open the cyclonic spray chamber cap. Insert the cyclonic spray chamber
into the cyclonic spray chamber cap. Slide the cap closed. See the following
figure.
 Cyclonic Spray Chamber 5-43

Cyclonic Spray Chamber

Cyclonic Spray
Chamber Cap
(opened position)

Cyclonic Spray Chamber

(seated in cap)

Cyclonic Spray
Chamber Cap
(closed position)

Figure 5-16. Installing the cyclonic spray chamber into the cyclonic spray chamber
cap.

3. Close the clamp to secure the cyclonic spray chamber assembly in place. Tighten
the nut at the end of the cyclonic spray chamber assembly. This allows you to
lock in place the angle of the cyclonic spray chamber. This angle will remain
locked even if you later remove the cyclonic spray chamber from the instrument.
Future installations will not require any readjustments.
5-44 Maintenance

4. On the drain end of the cyclonic spray chamber attach Tygon tubing (Part No.
0250-6516). To the other end of the Tygon tubing attach the tubing coupler (Part
No. 0992-0865). See the following figure.

Figure 5-17. Installing the cyclonic spray chamber.

 Cyclonic Spray Chamber 5-45

5. To the open end of the tubing coupler (Part No. 0992-0865) connect the drain
tubing to the peristaltic pump tubing. See the procedure Installing the Drain
Tubing later in this chapter for information on connecting the drain tubing to the
drain bottle.

6. After you install the cyclonic spray chamber, install the concentric glass or
GemCone nebulizer. See the procedure, Installing the GemCone Nebulizer on
the Cyclonic Spray Chamber, later in this chapter. Insert the nebulizer, as far
as it will go, through the O-rings of the spray chamber.

Etching the Cyclonic Spray Chamber

The cyclonic spray chamber can be etched in order to improve drainage using the
following procedure. However, if you will be using the cyclonic spray chamber in
determinations of silicon, this procedure should not be used.

1. Prepare a 0.5% solution of Hydrofluoric acid (HF), observing the precautions

listed below.

Before using hydrofluoric acid, you should be thoroughly familiar with its
hazards and safe handling practices. Observe the manufacturer's
! recommendations for use, storage and disposal. These recommendations are
Warning normally provided in a material safety data sheet (MSDS) supplied with the
chemical.

Hydrofluoric acid (HF) is toxic and extremely corrosive. Hydrofluoric acid will
readily burn skin, and if the fumes are inhaled, lung tissue. Burns may not be
immediately painful or visible. Contact with eyes could result in blindness.

2. Ignite the plasma.

3. Aspirate the HF solution. At first, you will see beads of water inside the cyclonic
spray chamber, then after approximately 30 seconds, the beads will begin to
disappear. Pump the HF solution for 1 to 2 minutes maximum.

4. Aspirate a rinse solution for several minutes.

5-46 Maintenance

Cleaning the Cyclonic Spray Chamber

If you have been analyzing aqueous solutions, the spray chamber should be cleaned
in an acid bath. An ultrasonic bath may be used. Start with a solution of 5% nitric
acid or aqua regia and, if deposits persist, increase the acid concentration, up to 20%
if necessary. Acid solutions must be used with care. Observe all of the
manufacturer's safety recommendations. These recommendations are normally
provided in a material safety data sheet (MSDS) supplied with the chemical.

If you have been analyzing organic solutions, the spray chamber can be cleaned
using a solvent or diluted soap solution.

Caution Do not use solvents that will attack quartz or glass. The cyclonic spray chamber
is not HF resistant.

O-rings may be cleaned with soap and water. An ultrasonic bath may be used.
Replace O-rings if they are cracked or worn.

Table 5-4. Replacement Parts: Spray Chambers

Part No. Description

N077-5180 Ryton Double-Pass Scott-Type Spray
Chamber
N077-6052 Cyclonic Spray Chamber for aqueous
solutions
N077-6053 Baffled Cyclonic Spray Chamber for
organic solvents
N077-0605 Cyclonic Adapter Kit
N077-0608 External Spray Chamber Mount
For use with high-volatility organic
solutions.
 Nebulizers 5-47

Nebulizers
PerkinElmer offers different types of nebulizers for a wide variety of applications.
For descriptions of the nebulizers and their different uses and advantages, refer to
Chapter 3, System Description. Part numbers and replacement parts for the different
types of nebulizers are listed on the next page.

Recommended flow rates for the nebulizers are given in the table below. If you find
that a flow rate is insufficient, this often indicates that the nebulizer has clogged and
requires cleaning. On GemTip and GemCone nebulizers, you should also check that
the argon gas fitting is properly tightened. If a space collar is used, tighten the fitting
with a wrench until you can no longer turn the knurled space collar. If a space collar
is not used, finger-tighten the fitting, then using a wrench, turn clockwise 1/8-turn.

Table 5-5. Nebulizer Flow Rates

Argon Flow Rate

Typical Value Operating Range

Nebulizer

GemTip Cross-Flow 0.8 L/min 0.7 - 1.3 L/min

Low-Flow GemCone 0.6 L/min 0.4 - 0.95 L/min
High Flow GemCone 1 L/min 0.7 - 1.0 L/min
Concentric Glass 0.8 L/min 0.7 - 1.3 L/min
(MEINHARD)
Type A
Concentric Glass 0.8 L/min 0.7 - 1.3 L/min
(MEINHARD) Type C
Concentric Glass 0.6 L/min 0.4 - 0.95 L/min
(MEINHARD)
Type K
Ultrasonic 0.5 L/min n/a
5-48 Maintenance

Table 5-6. Replacement Parts: Nebulizers and End Caps

Part No. Description
N077-0546 GemTip Cross-Flow Nebulizer Assembly (in-
cludes end cap, end cap ring, O-rings, and
GemTips)

N069-0676 GemTip Replacement Nebulizer Tips for

GemTip Cross-Flow Nebulizer

N069-0670 High Solids GemCone Nebulizer

N069-0671 Low-Flow GemCone Nebulizer

N068-0343 Scott-Type Spray Chamber End Cap for Gem-

Cone and concentric glass nebulizers

0047-2020 Concentric Glass Nebulizer, MEINHARD

Type A

0047-2022 Concentric Glass Nebulizer, MEINHARD

Type C

N068-1574 Concentric Glass Nebulizer, MEINHARD

Type K

0990-2033 End Cap O-Ring for Scott-type spray chamber

0047-3194 Small O-Ring for MEINHARD Nebulizers

N069-1709 CETAC U-6000AT+ Ultrasonic Nebulizer

System, 115 V, 50/60 Hz

N069-1710 CETAC U-6000AT+ Ultrasonic Nebulizer

System, 230 V, 50/60 Hz
 GemTip Cross-Flow Nebulizer 5-49

GemTip Cross-Flow Nebulizer

The following procedures cover the maintenance of the GemTip Cross-Flow
nebulizer supplied with the instrument.

To check the performance of the nebulizer, aspirate a standard and note the intensity
reading. If the intensity is significantly lower than it should be, first check that:

• The pump tubing is in good condition (has no flat spots).

• The sample capillary is in good condition (has no kinks) and is clean.

• The horizontal plasma viewing position is set properly (using the software's
horizontal alignment function).

Also try flushing out the nebulizer by aspirating for several minutes using either:

• a 1% acid solution, if you have been analyzing aqueous solutions, or

• a solvent, if you have been analyzing organic solutions.

Recheck the intensity of the standard. If the intensity is still too low, you should
check the nebulizer spray pattern. Before removing the nebulizer/end cap to check
the spray pattern, be sure to pump deionized water for several minutes to thoroughly
flush it out.

Removing the Nebulizer/End Cap

To remove the nebulizer/end cap assembly:

1. Turn off the plasma if it is on.

If the plasma has been on, allow one minute for the Quick-Change Adjustable Torch
! Module to cool and an additional two minutes for the torch to cool before handling.
Warning

2. Open the door on the left side to the sample compartment.

5-50 Maintenance

3. Loosen, but do not remove, the two knurled screws in the nebulizer end cap.
Support the spray chamber with one hand as you twist the end cap and end cap
ring, together, off the spray chamber.

Cross-Flow GemTip Nebulizer

End Cap Assembly
(Part No. N077-0546)

Knurled Screw

Spray Chamber

Knurled Screw

Figure 5-18. The nebulizer/end cap assembly removed from the spray chamber. Il-
lustration shows cross-flow nebulizer end cap assembly.

4. To check the spray pattern, leave the sample capillary tubing and the nebulizer
argon tubing connected. Then refer to the next procedure.

Checking the Spray Pattern

Once you have thoroughly flushed out the nebulizer with deionized water and
removed the nebulizer/end cap, you can follow these steps to check the nebulizer
spray pattern:

1. Set the nebulizer argon flow to 1.0 L/min.

2. Place the sample capillary tubing in a beaker of deionized water and start the
pump at a rate of 1.0 mL/min.
 GemTip Cross-Flow Nebulizer 5-51

3. Check the spray pattern on a paper towel. You should see a fine, even spray of
uniform sample droplets.

If the spray pattern is not even or the nebulizer is sputtering, the nebulizer tips should
be inspected for clogging, and cleaned or replaced as necessary. See the following
procedure.

Complete replacement of the nebulizer/end cap assembly may be necessary if the

GemTips are not seated properly inside the cap (see the next figure) or if the end cap
does not fit properly on the spray chamber.

Disassembling the Cross-Flow Nebulizer

Disassemble the nebulizer if it is necessary to clean or replace the GemTips. The
Cross-Flow nebulizer has two GemTips. The sample tip is a clear sapphire and the
argon tip is a red ruby. These tips are not interchangeable. For this reason, we
recommend that you first remove one GemTip, clean or replace it, then remove the
other.
5-52 Maintenance

Red GemTip
Argon
Clear GemTip Inlet

Sample
Inlet

Figure 5-19. Cross-section of GemTip Cross-Flow Nebulizer shown with Cross-

Flow End Cap, N077-0546.

To begin disassembling the nebulizer:

1. If you have not already done so, remove the nebulizer/end cap assembly from
the spray chamber.

2. Disconnect the sample capillary tubing by removing it from the pump tube.

3. Disconnect the nebulizer argon tubing at the gas fitting. Do not disconnect
nebulizer argon tubing from the end cap because the GemTip could fall out.

4. Inspect the inside of the end cap. If metal or salt deposits are found, clean the cap
using a dilute acid solution.
 GemTip Cross-Flow Nebulizer 5-53

Removing the Sample Tip from the End Cap, N077-0546

1. Loosen the nut on the sample inlet. Remove the nut along with the tubing piece
and ferrule. See the next figure.

2. Using your fingers, push the sample tip out from the inside of the end cap, being
careful not to damage it. Do not use any metal tools to remove the nebulizer tips
because this may damage the tips or end cap.

3. Inspect the sample tip. Clean the tip using soap and water or a dilute solution of
nitric acid. An ultrasonic bath may be used.

If you need to replace the sample tip, be sure to replace it with a clear GemTip.
GemTips must be purchased in a set (Part No. N069-0676). They are not
available separately.

4. Inspect the O-ring (Part No. 0992-1045), replace if it is worn or cracked.

5-54 Maintenance

O-Ring
(Part No. 0992-1045)

Clear GemTip Nebulizer

(Sample Inlet)
Available in GemTip Kit
(Part No. N069-0676)
Ferrule
(Part No. 0992-0518)

Nut
(Part No. 0992-0546)

1/16" O.D.
Teflon Tubing Piece
(Part No. 0998-5708)
Sample
Capillary
Tubing

Figure 5-20. Clear GemTip for sample inlet and associated parts for Cross-Flow
End Cap, N077-0546.
 GemTip Cross-Flow Nebulizer 5-55

5. Check the condition of the tubing piece (Part No. 0998-5708). If the tubing is
worn, replace it as follows:

a. Obtain a new piece of 1/16-in. O.D. teflon tubing (Part No. 0998-5708).

b. Using a razor blade, make a straight cut on one end of the tubing.

c. Insert a nut (Part No. 0992-0546) and ferrule (Part No. 0992-0518) on the
newly cut end of the tubing with the ferrule oriented as shown in the figure
below.

Ferrule
(Part No. 0992-0518)
Nut
(Part No. 0992-0546)

Sample
Capillary
Tubing

1/16" O.D.
Teflon Tubing Piece
(Part No. 0998-5708)

Figure 5-21. Installing new tubing for the sample inlet. Cross-Flow End Cap, N077-
0546.

6. To reassemble the nebulizer make sure that the O-ring is completely seated on
the base of the sample tip, then insert the sample tip into the sample inlet.

7. With the tubing and ferrule assembled as shown in the previous figure, screw the
nut into the sample inlet making a finger-tight connection. Do not use any tools
to tighten the nut.

8. Examine the two GemTips in the end cap. These tips should almost butt up to
each other at an angle of 90 .

9. If you have installed new 1/16-in. tubing, cut the tubing so that it extends
approximately 1/2 in. beyond the nut.
5-56 Maintenance

10. For the sample capillary tubing, use a piece of 0.023 in. (inner diameter)
polyethylene tubing (Part No. 0990-8265). Using a razor blade, bevel the tubing
by cutting it at an angle. Insert the sample capillary tubing into the tubing piece.

Removing the Argon Tip from the End Cap, N077-0546

1. Loosen the nut on the argon inlet. Remove the nut along with the tubing and
ferrule. See the next figure.

2. Using your fingers, push the argon tip out from the inside of the end cap, being
careful not to damage it. Do not use any metal tools to remove the nebulizer tips
because this may damage the tips or end cap.

3. Inspect the argon tip. Clean the tip using soap and water or a dilute solution of
nitric acid. An ultrasonic bath may be used.

If you need to replace the tip, be sure to replace it with a red GemTip. GemTips
must be purchased in a set (Part No. N069-0676). They are not available
separately.

4. Inspect the O-ring (Part No. N0992-1045), replace if it is worn or cracked.

 GemTip Cross-Flow Nebulizer 5-57

End Cap O-Ring (Part No. 0990-2033)

O-Ring
(Part No. 0992-1045)

Red GemTip Nebulizer

(Argon Inlet)
(Part No. N069-0676)
Ferrule
(Part No. 0992-0515)
Nut
(Part No. 0992-0545)

1/8" O.D. Teflon Tubing

(Part No. 0250-6483)

Figure 5-22. Red GemTip for argon inlet and associated parts for Cross-Flow End
Cap, N077-0546.

5. To reassemble the nebulizer make sure that the O-ring is completely seated on
the base of the argon tip, then insert the argon tip into the argon inlet.

6. Check the condition of the argon inlet tubing (Part No. 0250-6483). If the tubing
is worn, replace it as follows. See the next figure.

a. Obtain a new piece of 1/8-in. O.D. teflon tubing (Part No. 0250-6483).

b. Using a razor blade, make a straight cut on one end of the tubing. Wire
cutters or scissors do not make acceptable cuts.

c. Insert a nut (Part No. 0992-0545) and ferrule (Part No. 0992-0515) on the
newly cut end of the tubing, with the ferrule oriented as shown in the figure
below.
5-58 Maintenance

Ferrule (Part No. 0992-0515)

Nut (Part No. 0992-0545)

1/8-in. O.D. Tubing

(Part No. 0250-6483)

Figure 5-23. Installing new tubing for the argon inlet. Cross-Flow End Cap, N077-
0546.

7. With the tubing and ferrule assembled as shown in the figure above, screw the
nut into the argon inlet making a finger-tight connection. Do not use any tools to
tighten the nut.

8. Examine the two GemTips in the end cap. These tips should almost butt up to
each other at an angle of 90 .

Connecting the Nebulizer Argon Tubing (Cross-Flow End Cap, N077-0546)

1. Pass the tubing (Part No. 0250-6483) through the nut (Part No. 0992-0545) and
attach the ferrule on the end of the tubing. See the following figure.

2. Insert the ferrule with the tubing and nut to the Quick Disconnect (Part No.
N077-5206). Connect the entire Quick Disconnect to the smaple introduction
system. See the following figure.
 GemTip Cross-Flow Nebulizer 5-59

Replacing the Nebulizer Argon Tubing (Cross-Flow End Cap, N077-0546)

If you replace the argon tubing with new tubing, you will need to replace the
Swagelok nut as follows. See the previous figure.

1. Using a razor blade, make a straight cut on one end of the tubing. Wire cutters
or scissors do not make acceptable cuts.

2. Put the 1/8-in. Swagelok nut (Part No. 0990-3128), rear ferrule, front ferrule, and
tubing insert onto the tubing as shown in the figure below.

3. Finger-tighten the nut on the Brass Reducer Fitting.

4. Connect the nebulizer argon tubing to the NEB connection. Using a wrench,
tighten the 1/8-in. nut an additional 3/4 turn.
5-60 Maintenance

Ferrule (Part No. 0992-0515)

Nut (Part No. 0992-0545) Quick Disconnect (Part No. N077-5206)

1/8-in. Tubing
(Part No. 0250-6483)

Instrument
Left Side
Nut (Part No. 0992-0545)

Ferrule (Part No. 0992-0515)

Figure 5-24. Connecting the nebulizer argon tubing. Cross-Flow End Cap, N077-
0546.
 GemTip Cross-Flow Nebulizer 5-61

Replacing the Nebulizer/End Cap

Before replacing the end cap:

• Check the end cap O-ring (Part No. 0990-2033) for nicks or cracks. If you need
to replace the O-ring, remove the two knurled screws and the end cap ring. When
placing the end cap ring back on the end cap, install it with the flat side against
the O-ring and the molding marks (small circular indentations) against the end
cap.

• If you have just replaced the nebulizer tips, connect the sample capillary tubing
and the nebulizer argon tubing to the nebulizer and check the spray pattern to
make sure it is even. See Checking the Spray Pattern earlier in this chapter.

To replace the end cap:

1. Moisten the O-ring to make replacing the end cap easier. Make sure that the two
knurled screws that hold the end cap and the ring together are loose.

2. With one hand supporting the far end of the spray chamber, push and twist the
nebulizer/end cap onto the spray chamber so that the end cap seats firmly onto
the spray chamber.

3. Alternately hand-tighten the two knurled screws until the end cap ring is pulled
snug against the end cap.

4. If you have not already done so, connect the sample capillary tubing and
nebulizer argon tubing.
5-62 Maintenance

GemCone Nebulizer

Daily Cleaning of the Low-Flow GemCone Nebulizer

Each day after use, the low-flow GemCone nebulizer should be rinsed out by
pumping deionized water to the nebulizer for several minutes. This should be done
with both the plasma on and the nebulizer gas on. This helps prevent the formation
of salt crystals near the exit of the nebulizer gas orifice. The plasma should be on to
prevent aerosol from condensing on the purge window. This is important for axial
and dual view instruments since the aerosol is aimed directly at the purge window.

Daily Cleaning of the High Solids GemCone Nebulizer

It is important to rinse the high solids nebulizer after use, particularly when working
with solutions containing high levels of solids. You do this by pumping deionized
water for several minutes to wash out any solid material that may have crystallized
on the inside surface of the nebulizer. If a stronger cleaning solution is required, a
solution of 1% acid in deionized water may be used in place of the deionized water.
The plasma should be on to prevent aerosol from condensing on the purge window.
This is important for axial and dual view instruments since the aerosol is aimed
directly at the purge window.

To rinse the argon orifice:

1. Place the sample capillary tube in deionized water or 1% acid in deionized water
and operate the pump.

2. Momentarily shut off the nebulizer gas flow for about 30 seconds.

3. Turn the nebulizer gas back on.

This procedure can be performed more than once a day in cases where very high
levels of dissolved solids are aspirated through the nebulizer for prolonged
periods of time.
 GemCone Nebulizer 5-63

Installing the GemCone Nebulizer on the Scott-Type Spray Chamber

To install the GemCone nebulizer on the Scott-type spray chamber, the end cap
assembly (Part No. N077-0546) and the tubing assembly (Part No. N077-0336) must
be used.

1. Remove the existing nebulizer/end cap assembly (if the wrong one is installed)
by loosening the knurled screws on the end cap. Use a gentle twisting action to
remove the assembly from the spray chamber.

2. Assemble the correct end cap (Part No. N077-0546) to the spray chamber with
a twisting [Link] hand-tighten the knurled screws until the end cap
ring is pulled snugly against the end cap.

3. Before inserting the GemCone nebulizer into the cap, connect the argon gas
fitting to the threads on the nebulizer where shown in the next figure. First,
tighten the gas fitting by hand. Tighten the fitting another 1/8 of a turn using a 9/
16-in. open-end wrench. Support the nebulizer with a back-up wrench when
tightening or loosening fittings. Do not overtighten the fitting as this may cause
leaking and poor ICP performance.

4. Connect the capillary tubing to the nebulizer. Be sure not to crimp or bend the
tubing as you insert it. Crimps may reduce flow to the tip of the nebulizer or may
cause air to enter the liquid stream during operation.

5. Insert the nebulizer as far as it will go through the opening in the end cap.

6. Tighten the nut on the end cap so that it is finger-tight.

5-64 Maintenance

Figure 5-25. Installing the GemCone nebulizer to a Scott-type spray chamber.

Installing the GemCone Nebulizer on the Cyclonic Spray Chamber

1. Before inserting the GemCone nebulizer into the chamber, connect the argon gas
fitting to the nebulizer threads. First, tighten the gas fitting by hand. Tighten the
fitting another 1/8 of a turn using a 9/16-in. open-end wrench. Support the
nebulizer with a back-up wrench when tightening or loosening fittings. Do not
overtighten the fitting as this may cause leaking and poor ICP performance.

2. Connect the capillary tubing to the nebulizer. Be sure not to crimp or bend the
tubing as you insert it. Crimps may reduce flow to the tip of the nebulizer or may
cause air to enter the liquid stream during operation.
 GemCone Nebulizer 5-65

3. Insert the nebulizer into the cyclonic spray chamber as shown in the next figure.
The nebulizer may be inserted to its fullest extent.

Figure 5-26. Connecting the GemCone nebulizer to the cyclonic spray chamber.

Cleaning the GemCone Nebulizer

With routine use it may become necessary to perform a thorough cleaning.

1. Remove the nebulizer from the end cap (loosen both thumbscrews).

2. Disconnect the argon gas fitting and the capillary tube connection from the
nebulizer.
5-66 Maintenance

3. Immerse the nebulizer in a solution of liquid laboratory cleaner (such as

"Microcleaning" solution, Cole-Parmer). Use the recommended concentration
of cleaning solution.

4. Apply ultra-sonication to the solution containing the nebulizer for about 5

minutes.

5. Rinse the nebulizer thoroughly using deionized water.

6. Dry the gas passages of the conespray nebulizer by connecting the argon gas
fitting and turning on the argon flow to 1 L/min. Allow the argon flow to dry the
internal passages for several minutes.

GemCone Liquid Fitting Maintenance

It is possible to remove the liquid inlet fitting to the nebulizer. The clear plastic
fitting has a knurled head and can be unscrewed by hand. Before reconnecting the
fitting, make sure that about 1-2 mm of tubing protrudes out from the sealing side of
the fitting. Screw the fitting back into the nebulizer and snug to hand tightness.
 Concentric Glass Nebulizer 5-67

Concentric Glass Nebulizer

Installing the Concentric Nebulizer

Handle the concentric nebulizer carefully to avoid breaking the glassware and
! possible injury.
Warning

1. Wet the outside of a short length of Viton Orange-Orange I.D. 0.89 mm (0.036
in.) pump tubing (Cole Parmer Part No. P-07606-26). Insert this tubing as far
into the concentric nebulizer as possible.

2. After you have inserted this Viton Orange-Orange tubing, cut the tubing so that
one inch extends out from the nebulizer. Insert a section of capillary tubing (Part
No. 0990-8265) inside this short piece of peristaltic pump tubing.

3. Connect the supplied Tygon tubing (Part No. 0250-6515) to the argon inlet of
the nebulizer. Secure this tubing to the nebulizer by using the snap clamp
provided with the nebulizer. Cut the tubing to a sufficient length using a razor
blade.
5-68 Maintenance

Concentric Nebulizer Viton Orange-Orange Tubing

Capillary Tubing

Clamp

Argon Line

Figure 5-27. Installing the concentric nebulizer.

4. With an adapter connect the argon tubing from the nebulizer to the NEB/
NEBULIZER fitting.

5. Insert the Concentric Glass nebulizer, as far as it will go, through the opening in
the end cap. See the next figure.

6. Tighten the nut on the end cap so that it is finger-tight.

 Concentric Glass Nebulizer 5-69

Meinhard
Concentric Nebulizer

Figure 5-28. Installation of the Concentric Glass Nebulizer in the End Cap.

Cleaning the Concentric Glass Nebulizer

For detailed information on cleaning MEINHARD Concentric Glass nebulizer, see
Maintenance Tips for Users of the MEINHARD Concentric Glass Nebulizer
(PerkinElmer Part No. 09993-6334), which is also available upon request from J.E.
Meinhard Associates, Inc.

J.E. Meinhard Associates, Inc.

1900-J East Warner Ave.
Santa Ana, CA 92705 U.S.A.
(800) 634-6427
(714) 250-3332
Internet address: [Link]
5-70 Maintenance

The following table summarizes the cleaning procedures for the MEINHARD
Concentric Glass nebulizer.

1. Disengage nebulizer
Examine visually (20 - 30X)

a. No visible foreign matter

b. Particle wedged in passage
c. Deposits in capillary
d. Cryst. Deposit on nozzle

2. Particulate 3. Deposits 4. Crystalline 5. Organic 6. Plugged 7. Lodged

Matter in Capillary Deposit Matter Capillary Particle

a. Tapping a. Dissolution a. Solvent rinse CrO3 /H 2 SO 4 Melt & expel Probe

b. Gas Pressure b. Solvent + Heat b. Prolonged soak ~100 C
O

c. Backflushing c. Hf + gas pressure

d. PTFE d. Organic? c. Unyielding?
e. HF
f. Organic?
g. Unyielding?

Figure 5-29. Cleaning Strategy for the MEINHARD Nebulizer.

(Reprinted with the permission of JE Meinhard Assoc., Inc.)

Caution When cleaning the concentric glass nebulizer, do not use ultrasonic cleaning. This
can adversely affect nebulizer performance.

Do not attempt to clean out the concentric nebulizer with any wire instrument. This
can cause irreparable damage to the nebulizer.
 Peristaltic Pump 5-71

Peristaltic Pump
The peristaltic pump requires routine maintenance to ensure that the system will run
properly. The pump tubing should be replaced when flat spots develop (on a daily
basis or after approximately eight hours of use). When replacing the pump tubing,
the drain tubing should be replaced at the same time since uneven wear can cause the
spray chamber to back up.

Replacement Pump Tubing

Replace the pump tubing when flat spots develop (after approximately eight hours
of use). When replacing the pump tubing, both the sample and drain tubing should
be replaced at the same time since uneven wear can cause the spray chamber to back
[Link] following table gives part numbers for pump tubing for the sample and drain.

Table 5-7. Pump Tubing

Solvent
Pump Tubing
Type Inner Diameter Part No.

Standard Inorganic Sample: 0.76 mm (0.030 in.) 0990-8587

Drain: 1.14 mm (0.045 in.) 0990-8585
Solvent Flex Kerosene or Sample: 0.76 mm (0.030 in.) 0047-3550
Xylene Drain: 1.14 mm (0.045 in.) 0992-3037
Silicone Organic Sample: 0.76 mm (0.030 in.) 0047-3552
solvents, Drain: 1.14 mm (0.045 in.) N069-1595
including
MIBK.*
Viton Kerosene or Sample: Orange-Orange 0992-3511
Xylene 0.89 mm (0.035 in.)
not MIBK.* Drain: Yellow-Yellow 0992-3512
1.40 mm (0.056 in.)

*Silicone tubing is not recommended for use with kerosene or xylene.

5-72 Maintenance

Installing the Sample and Drain Tubing

The peristaltic pump is used to pump sample into the nebulizer and pump the waste
out of the spray chamber.

From
Spray Chamber

To Drain Bottle
To Nebulizer

From Sample
Container

Figure 5-30. Tubing installed on pump for sample and drain (side view).

Installing the Sample Tubing

To install the sample tubing refer to the instructions below and the next two figures:

1. Turn off the peristaltic pump using the software control.

2. Take a piece of 0.76 mm (0.030 in.) pump sample tubing. New pump tubing will
work better if it is pre-stretched and analytical precision will be improved. Grasp
the tubing, with one clip in each hand, and stretch the tubing gently a few times.

3. Install the pump tubing on an open channel of the pump. To do this, carefully
stretch the new tubing around the pump head and place the clips on the pump
tubing into the slots, using the slots in the same position on each side of the pump
 Peristaltic Pump 5-73

head. Carefully thread the pump tubing through the lip of the cover (see the next
figure). Be careful not to twist or kink the pump tubing during this process.

Cover Door
Spray Chamber

Lip

Peristaltic
Pump Tubing

Figure 5-31. Peristaltic pump tubing installed with cover in place.

Caution Make sure that the closed cover door does not pinch the tubing. If the tubing is
pinched, pressure will build up in the pump tubing and liquid will not flow.
5-74 Maintenance

4. Take two pieces of 0.58 mm i.d. (0.023 in.) polyethylene tubing (Part No. 0990-
8265), one for the sample capillary and one for the nebulizer capillary. Using a
razor blade, bevel one end of each piece of capillary tubing by cutting it at an
angle. See the next figure.

5. Insert the beveled end of the sample capillary tubing into one end of the pump
tubing. Lead the capillary tubing to the sample bottle.

Spray Chamber

Pump Tubing 0.76 mm i.d.

(different part nos. available) Polyethylene Tubing
(Included with Nebulizer),
0.58 mm i.d.
(Part No. 0990-8265)

Polyethylene Tubing
(Included with Nebulizer),
0.58 mm i.d.
(Part No. 0990-8265)

To Sample Inlet

Figure 5-32. Tubing assembly for sample.

6. Insert the beveled end of the nebulizer capillary tubing into the other end of the
pump tubing.

7. Attach the capillary tubing to the sample inlet of the nebulizer.

Using the Spray Chamber Drain Spare Parts

See the following table for a list of the spare parts needed for the spray chamber. The
fittings screw in to the drain adapter and can be used with different sized tubing.
 Peristaltic Pump 5-75

Table 5-8. Spray Chamber Drain Spare Parts

Part No. Drain Spare Part

0992-0528 Barbed Fitting
0998-5729 Solvent Flex Tubing
0992-0865 Tubing Coupler
0998-5729 PVC Tubing
0990-8143 Teflon Tape
N822-1152 Teflon Tubing

Drain tubing with 1 mm i.d. (0.04 in.) can also be used by following these steps:

1. Attach a small piece of 1.5 mm (0.06 in.) i.d. PVC tubing (Part No. 0998-5729)
to the barbed fitting (Part No. 0992-0528).

2. Cut the 1 mm i.d. tubing at an angle and insert it into the 1.5 mm tubing.

Connecting the Drain Tubing Assembly

To connect the drain tubing assembly, use the following steps and refer to the next
figure.

1. Connect the barbed fitting (Part No. 0992-0528) to the spray chamber drain.
Wrap a small piece of teflon tape around the barbed fitting. See the table above.

2. Attach the Solvent Flex tubing (Part No. 0998-5729) to the barbed fitting. Attach
the other end of the Solvent Flex tubing to the tubing coupler (Part No. 0992-
0865). See the following figure.

3. Use the other end of the tubing coupler (Part No. 0992-0865) to connect the drain
tubing to the peristaltic pump tubing. See the following figure.
5-76 Maintenance

Barbed Fitting (Part No. 0992-0528)

Wrap Teflon Tape (Part No. 0990-8134)
on Threaded Barbed Fitting.

Teflon Tubing, 1 mm i.d. (Part No. N822-1152)

Figure 5-33. Drain tubing assembly.

Installing the Drain Tubing

Install the drain tubing on an open channel of the peristaltic pump as follows:

1. Pre-stretch a piece of 1.14 mm (0.045 in.) pump drain tubing.

 Peristaltic Pump 5-77

2. Carefully stretch the new tubing around the pump head and place the clips on the
pump tubing into the slots, using the slots in the same position on each side of
the pump head. Be careful not to twist or kink the pump tubing during this
process.

3. Attach the Teflon tubing to the pump tubing for the drain.

Make sure you install the tubing on the pump so that the waste liquid is
pumped out of the spray chamber. See Figure 5-33. If the tubing is installed
in the wrong direction, the spray chamber will flood.

4. For the tubing that leads to the drain bottle, use one piece of 1.07 mm i.d. (0.042
in.) teflon tubing (Part No. N822-1152). Bevel one end by cutting it at an angle.

5. Insert the teflon tubing into the other side of the pump tubing. Lead this tubing
to the drain bottle. Refer to Figure 5-34 in the Drain section.

6. Adjust the tubing as described in the next procedure.

Adjusting the Pump Tubing

Adjust the tension on the sample and drain tubing, one at a time, using deionized
water as follows:

Adjusting the Sample Tubing

1. Make sure the sample tubing is centered in the channel, then place the clamp
around the tubing and swing back the cam lever.

2. Place the sample capillary (SAMPLE IN side) in a container of deionized water.

3. Set the pump speed to 1.5 mL/min and start the pump.

4. Dip the tubing in DI water a few times to let bubbles form. As you watch the
bubbles form loosen the adjustment screw in a counterclockwise direction until
the bubbles stop or do not flow smoothly.

5. Tighten the adjustment screw slowly (turn clockwise) until droplets just start
forming at the end of the SAMPLE OUT side of the sample tubing.
5-78 Maintenance

6. Tighten the adjustment screw until you see a smooth flow of bubbles (about 1/2
to 1 turn more on the peristaltic pump).

7. Turn off the pump. The tension is now correctly set. No bubbles should be seen
in the sample tubing once the sample tube is kept in the solution.

Adjusting the Drain Tubing

1. Make sure the drain tubing is centered in the channel without disturbing the
sample tubing, then place the clamp around the drain tubing and swing back the
cam lever.

2. Loosen the adjustment screw (turn counterclockwise) for the drain tubing
channel so that the cam lever can be easily opened and closed with little
resistance.

3. Set the pump speed to 1.5 mL/min and start the pump.

4. Tighten the adjustment screw (turn clockwise) up to three turns so that moving
bubbles are visible in the drain tubing. It may take up to one minute to see
bubbles if the spray chamber is dry.

5. Loosen the adjustment screw until the bubbles stop moving.

6. Tighten the adjustment screw slowly until the bubbles just start moving again.

7. Tighten the adjustment screw until the bubbles move in a segmented flow (about
1/2 to 1 turn on the peristaltic pump).

8. Turn off the pump. The tension is now correctly set.

 Peristaltic Pump 5-79

Cleaning the Pump

Periodically inspect the pump rollers to make sure they are clean and move freely.
Clean the exterior of the pump with a cloth moistened with water.

The pump head on the peristaltic pump can be removed and cleaned if necessary.
Replacement pump heads are also available (Part No. N069-0284 – has plastic
rollers). A stainless-steel pump head is also available (Part No. N069-0360).

Caution If a spill occurs on the pump, immediately clean it up. A corrosive spill could
damage the rollers and interior parts of the pump.

Removing the Pump Head on the Peristaltic Pump

To remove the pump head on the peristaltic pump:

1. Remove the pump tubing.

2. Unscrew the large screw in the center of the pump head. Place the screw and
washer in a secure place.

3. Lift the pump head off. To clean the pump head, use water or a mild solvent and
dry thoroughly.

4. Return the pump head to the pump. Orient the pump head by aligning the notch
on the bottom of the pump head with the pin on the shaft. The pump head must
click in this slot for a proper fit. Replace the washer and tighten the screw.

Drain
One drain is used on the Optima 2000 DV. This pumped drain leads from the spray
chamber.

To connect the drain to the drain bottle, refer to the next figure and follow the steps
below:

1. Connect the drain tubing leading from below the sample compartment to one of
the large fittings on the drain bottle.
5-80 Maintenance

2. Insert the drain tubing from the pump into the 1.6 mm (0.0625 in.) i.d. tubing
piece on the drain bottle shown in the next figure.

Figure 5-34. Tubing connections to the drain bottle.

 General System Maintenance 5-81

Table 5-9. Replacement Parts: Peristaltic Pump

Part No. Description

N069-0360 Peristaltic Pump Head, stainless-steel
rollers
N069-0284 Peristaltic Pump Head, plastic rollers

General System Maintenance

Air Filters
To ensure that the electrical components in the spectrometer and the RF generator
are properly cooled, check the air filters regularly to see if they are clogged or dirty.
There are two air filters on the instrument as shown in Figure 5-35. The one filter is
for the RF generator and the other for the spectrometer.

Changing the RF Generator Air Filter

Two generator air filters are provided with the instrument. Refer to Figure 5-35.

1. Remove the filter from the back of the instrument.

2. Clean or replace the filter. The filter may be washed with water, but replacing it
with the other filter provided is recommended. This insures that a completely dry
filter is in the instrument.

3. When replacing the filter make sure that the fine screen side is towards the
instrument, with the open mesh facing the outside of the instrument.

Replacement filters (Part No. N077-5220) are included in the spares kit.

Changing the Spectrometer Air Filter

The filter for the spectrometer cooling is inside the snap-on plastic grid. Refer to
Figure 5-35.
5-82 Maintenance

1. Shut down and switch off the spectrometer.

2. Carefully pull off the plastic grid on the ventilator.

3. Remove the filter and insert a new one (Part No. B051-1305).

4. Carefully push the plastic grid onto the ventilator.

Changing the Neon Lamp

The neon lamp is in an assembly that plugs into a connector on the right-hand side
of the optics tub. A panel in the side of the spectrometer housing gives access to the
neon lamp. Refer to Figure 5-35.

1. Shut down and switch off the spectrometer.

2. Remove the screw that secures the access panel on the right-hand side of the
spectrometer and remove the panel. Place the screw in a secure location.

3. The neon lamp assembly is the metal box that is visible inside the access hole.
Loosen the large screw on the metal box inside the access panel and pull the
metal box off the side of the optics tub.

4. Carefully slide a new neon lamp assembly (Part No. B081-0144) onto the tub
using the metal plates on the tub as guides. Tighten the large screw securely.

5. Replace the access panel and secure it with the screw.

 General System Maintenance 5-83

Spectrometer Air Filter

To remove, slide filter

in this direction.

Access Panel for Neon Lamp RF Generator Filter

Figure 5-35. Location of the air filters on the back of the instrument.

Chiller and Filters

Inspect the water filter (Part No. 0990-4845) installed on the chiller and replace the
water filter element (Part No. 0990-4846) every 3 months or as needed. Flush out the
chiller every 6 months.

To fill the chiller, use only distilled water with an addition of Chloramine-T, one
gram per US gallon, as an algaecide. The chiller reservoir has a capacity of 6.8 liters
(1.8 US gallons). This would require 1.8 grams of chloramine-T to be added to the
distilled water. Refer to Chapter 4, Installation for more information on filling the
chiller.

Caution Do not use deionized or tap water in the chiller. Do not use an algaecide other
than that specified above.

For additional information on the chiller, refer to the manufacturer's maintenance

guidelines.
5-84 Maintenance

Fuses
Fuses may only be replaced by a PerkinElmer service engineer.
Replacement Parts: General
The following replacement parts are required for general system maintenance. For
other replacement parts, refer to the appropriate sections earlier in this chapter.

Table 5-10. Filters

Part No. Description

N077-5220 Air Filter for Generator
0990-4845 Cooling Water Filter
0990-4846 Cooling Water Filter Cartridge,
replacement for Water Filter 0990-4845

Table 5-11. Gas and Water Supply Connections

N077-0342 Coolant Supply Hose

N077-0341 Coolant Drain Hose

N069-0274 Argon Supply Hose

N069-0275 Nitrogen Supply Hose

N077-0348 Shear Gas Supply Hose

0303-0313 Air compressor, 115 V, 60 Hz

0303-0314 Air compressor, 230 V, 50 Hz

N077-5220 Air filter-RF Generator

0990-5098 Air filter-Spectrometer

0992-0125 Space Collar for 1/4-in. Swagelok fittings

 General System Maintenance 5-85

Table 5-12. Miscellaneous

Part No. Description

N077-0434 Fresh Air Kit (which includes the Flex Hose
and Hose Clamp)
N077-3061 Drip Tray for Sample Compartment
0992-0044 Clamp for RF Generator Exhaust Hose

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

PerkinElmer using the eight-digit part numbers provided in this manual.

PE XPRESS, PerkinElmer's catalog service, offers a full selection of high quality

atomic spectroscopy supplies through the Atomic Spectroscopy Supplies Catalog. To
place an order, request a free catalog, or ask for information:

• If you are located within the U.S., call toll free 1-800-762-4002, from 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 office.
5-86 Maintenance
Troubleshooting 6
 Troubleshooting
Contents
A Word on Troubleshooting ........................................................................ 6-4
What the Performance Checks Measure ...................................................... 6-4
Sodium Bullet Test ...................................................................................... 6-5
Performance Problems ................................................................................ 6-6
Checking the Sample Introduction System ........................................... 6-6
Performance Problems: Troubleshooting Table ........................................ 6-10
Plasma Ignition and Stability Problems .................................................... 6-14
Plasma Ignition Problems ................................................................... 6-14
Plasma Stability Problems .................................................................. 6-16
Printing Problems ...................................................................................... 6-17
Pump Problems .......................................................................................... 6-18
Autosampler Problems .............................................................................. 6-19
RF Generator/Sample Introduction System Troubleshooting Form ......... 6-19
Troubleshooting Form ........................................................................ 6-20
General: ............................................................................................... 6-20
Sample Introduction Configuration: ................................................... 6-20
Operating Conditions: ......................................................................... 6-20
Instrument Environment: .................................................................... 6-20
Troubleshooting Tasks Performed: ..................................................... 6-20
Common Setup Problems: .................................................................. 6-21
6-4 Troubleshooting

A Word on Troubleshooting
We recommend that you consult the troubleshooting information included here
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.

If after using the troubleshooting techniques in this chapter your instrument is still
not performing properly fill out the form at the end of this chapter and contact
PerkinElmer service.

Use the following table to guide you to the appropriate section or manual.

Problem Refer to section

You are not getting the desired Optimizing and Verifying Performance in the
results. WinLab32 Software Guide or Performance
Problems: Troubleshooting Table in this
chapter.
You cannot ignite the plasma, Plasma Ignition and
or the plasma is unstable. Stability Problems in this chapter.
A red fault icon appears in the Operating Status Problems in the WinLab32
Instrument Diagnostics window Software Guide.
or the system is not ready.
There is a software error. Software Troubleshooting in the Winlab32
Software Guide.
The printer is not working. Printer Problems in this chapter.
The pump is not working. Pump Problems in this chapter.

What the Performance Checks Measure

The tests in this section allow the operator to measure performance aspects of the
instrument. If you are experiencing problems with your results, these tests can
pinpoint the cause of the problem.
 Sodium Bullet Test 6-5

The tests include the following:

• Sodium Bullet Test: This test allows you to visualize the sample flow in the
plasma, so that you can check that the sample introduction system is working
correctly.

• Background Equivalent Concentration (BEC) Test: The BEC value is the

concentration of an element which would produce the same emission intensity
as the plasma background measured at the analyte wavelength. The BEC serves
as an indication of instrument sensitivity. It checks torch alignment, plasma
viewing height, nebulizer gas flow rate, and incident RF power. Refer to the
Winlab32 Software Guide (Part No. 0993-6335) for details.

• Precision Test: This test indicates the Relative Standard Deviation (RSD) of the
instrument's analyte emission intensity or concentration measurements. The
RSD may also be referred to as the CV (Coefficient of Variation). A high RSD
or CV is usually indicative of a problem with the sample introduction system
such as improper drainage, leaks, improper tension on the pump tubing, worn
pump tubing, or nebulizer problems. Refer to the Winlab32 Software Guide for
details.

• Detection Limit Test: This test measures the baseline signal for a blank solution
to give an indication of the lowest concentration of an element which can be
measured. The detection limit is calculated as three times the standard deviation
of the blank. Refer to the Winlab32 Software Guide for details.

Sodium Bullet Test

To run the sodium bullet test:

1. For aqueous analyses, aspirate a 1000 mg/L solution of sodium. For organic
analyses, aspirate an appropriate organic blank.

2. Examine the plasma through the viewing window in the sample compartment
door.

A yellow-orange bullet (or green, in the case of organic compounds) should be

visible in the center of the discharge, and should extend from the base of the
discharge to about 2-3 mm above the top of the RF coil. If the bullet height is
6-6 Troubleshooting

unsatisfactory, adjust the nebulizer argon flow in the Method Editor or Plasma
Control windows.

If no bullet appears or the bullet is faint:

• Check that your sample does contain sodium at the required concentration.

• Check that sample is being pumped to the nebulizer. Make sure that the pump
lever is engaged and that the pump tubes are connected appropriately.

• Check that the drain is being pumped properly. You should see a segmented flow
of bubbles through the tubing.

If the above checks fail to make an improvement, turn off the plasma, then check the
following:

• Check that the nebulizer end cap is connected tightly.

• Check the nebulizer spray pattern: run deionized water for several minutes, then
remove the nebulizer end cap. If the nebulizer spray is sputtering or uneven,
inspect the nebulizer tips for clogging and clean or replace them as necessary.

If the plasma has been on, allow one minute for the Quick-
! Change Torch Module to cool and an additional two minutes
for the torch to cool before checking the following.
Warning

• Check that the injector is not clogged. You will need to remove the Quick-
Change Torch Module and disassemble the torch as described in Chapter 5,
Maintenance.

Performance Problems

Checking the Sample Introduction System

Many performance problems (such as poor precision or loss of signal) can be traced
to the setup and condition of the sample introduction system.
 Performance Problems 6-7

The following list describes general checks for the sample introduction system,
which should be done on a regular basis. Typical symptoms of problems are listed to
help you determine whether maintenance is required.

If you have already done performance checks, refer to the Winlab32 Software Guide
for details.

The sodium bullet test is also a good way of visually checking the sample flow in the
plasma and, therefore, indicates problems in sample introduction. This test is
described earlier in this chapter.

Pump and Pump Tubing

Is the tubing overstretched or does it have flat spots, leaks, or discoloration?

Install new tubing, stretching it gently beforehand. If using organics, special tubing
should be used. See the list of replacement parts at the end of Chapter 5,
Maintenance.

Is the flow of liquid irregular?

Refer to the adjustment procedure in Chapter 5, Maintenance.

Do the pump rollers bind or not roll easily? Are there grooves in the pump rollers?

On the PerkinElmer pump, the pump head may be removed for cleaning. The pump
head may also be replaced. A pump head with stainless steel rollers is available. See
Chapter 5, Maintenance.

Capillary Tubing

Are the nebulizer and sample capillary tubing properly connected? Is the tubing
discolored or clogged? Is tubing crimped or pinched?

If the capillary tubing is not in good condition, replace it.

Nebulizer and Spray Chamber

Is there leakage around the end cap? Is there leakage from the spray chamber drain?
Is fluid accumulating in the torch?
6-8 Troubleshooting

Make sure the end cap is on securely. If you cannot get a secure fit, the end cap O-
ring may need to be replaced. Check the drain fitting and tubing to be sure the spray
chamber is being properly drained. Check that the waste is being pumped in the
proper direction.

Check the nebulizer spray pattern: run deionized water for several minutes, then
remove the nebulizer end cap. Is the nebulizer spray sputtering or uneven?

If the spray pattern is uneven, the nebulizer tips may be clogged or worn.
Disassemble the nebulizer and clean or replace the GemTips. See Chapter 5,
Maintenance.

Are there deposits inside the end cap or spray chamber?

Clean out deposits. See Chapter 5, Maintenance for recommended cleaning

procedures (Table 5-1).

Torch Assembly

Are the torch fittings for the gas inlets secure?

Finger-tighten the fittings. Do not overtighten them.

Is the quartz torch cloudy or dirty?

Check for deposits, particularly if running organics, alloys, or samples with high
dissolved solids. See Chapter 5, Maintenance for cleaning procedures.

Is the injector dirty? Is it deformed due to overheating?

The injector may be clogged and require cleaning. If you are running organics, check
for carbon buildup. If running samples with high dissolved solids, check for deposits.
See Chapter 5, Maintenance for cleaning procedures.

If the torch requires disassembly, check the O-rings. Are they cracked or worn? Is
the injector adapter discolored?

Replace worn parts. See Chapter 5, Maintenance.

 Performance Problems 6-9

Purge Window

Is the purge window cloudy or dirty?

Rinse with deionized water and dry with a soft cloth. Or, replace if necessary. Do not
touch the window. If oils from the skin are deposited on the window, this can cause
inaccurate results. A 10% solution of hydrofluoric acid may be used to clean the
window. Observe the following warning statement. Soak the window briefly, then
rinse thoroughly.

Has UV performance dropped?

Even if the purge windows look clean a drop in UV performance indicates that the
windows should be cleaned or replaced. First rinse with deionized water and dry with
a soft cloth. If the UV performance does not improve replace the purge windows. Do
not touch the window. If oils from the skin are deposited on the window, this can
cause inaccurate results. A 10% solution of hydrofluoric acid may be used to clean
the window. Observe the following warning statement. Soak the window briefly,
then rinse thoroughly.

Before using hydrofluoric acid, you should be thoroughly

familiar with its hazards and safe handling practices. Observe
! the manufacturer's recommendations for use, storage and
Warning disposal.

Bonnet

Is the bonnet cloudy or dirty?

Remove the bonnet and clean in a 20% nitric acid solution. Rinse well.
6-10 Troubleshooting

Performance Problems: Troubleshooting Table

Table 6-1. Performance Problems: Troubleshooting Table

Problem Possible Cause(s) Corrective Action

RSD (Relative The sample introduction Refer to Chapter 5, Maintenance.
Standard Deviation) system may not be set up
greater than 1%. correctly or may require
maintenance.
Does the sample have a high Try increasing the integration time.
viscosity or high percentage of Refer to the Winlab32 Software Guide
dissolved solids? for details.
For high dissolved solids, try the cone
spray nebulizer.
Add 0.05% surfactant to your samples,
standards, and blanks.
Try running other samples with normal
characteristics to determine if the
sample matrix is really the problem.
The standard and blank may need to be
matrix-matched. Or, internal
standardization may be required.
Look for carryover – check if Increase the Read Delay to flush the
concentrations of replicates sample introduction system
increase from one to the next. completely. Increase the rinse time if
using an autosampler. Prepare the rinse
solution in the same acid matrix used
for the standards, samples, and blank.
Refer to the Winlab32 Software Guide
for details.
RF power and/or nebulizer Adjust as necessary. Also, check that
argon flow may require you are using the recommended
adjustment. settings for your instrument.
 Performance Problems: Troubleshooting Table 6-11

Table 6-1. Performance Problems: Troubleshooting Table

Problem Possible Cause(s) Corrective Action

Cannot obtain You may not be comparing the Refer to the Winlab32 Software Guide
suggested BEC value appropriate BEC value for the for details.
wavelength you are using.
The torch position may need Refer to the torch adjustment
adjustment. procedures for your instrument.
The plasma viewing position Refer to the Lateral (radial view mode)
may need to be optimized. and X/Y (axial view mode) torch view
procedures. See "Automatically
Aligning the Torch Viewing Position"
in Chapter 4, Installation.
RF power, nebulizer argon Adjust as necessary. Also, check that
flow, and/or plasma viewing you are using the recommended
height may need adjustment. settings for your instrument.
The purge windows may Refer to the instructions for removing
require cleaning. and cleaning the purge windows for
your instrument.
Results Corrections may not have been Aspirate a blank and rerun standards
erroneously made for the reagent blank. and samples.
high
Standard solutions may have Restandardize with a proven standard.
deteriorated or may have been
improperly made.
Background emission may be Use background correction.
present.
6-12 Troubleshooting

Table 6-1. Performance Problems: Troubleshooting Table

Problem Possible Cause(s) Corrective Action

Results Standard solutions may have Rerun proven standards.
erroneously low been improperly made.
Blank solution may be Remake the blank solution. Acidify the
contaminated or not matrix- blank if the sample matrix is acidified.
matched to the standards.
Does the matrix composition If possible, prepare the standard and
of the samples vary from that blank in the same acid matrix used for
of the blanks and standards? the samples. Or, internal
standardization may be required.
Is the concentration for the Increase the Read Delay to flush the
second standard lower than sample introduction system
that for the first? completely. Alternatively, aspirate a
blank between standards.
Is background correction being Check the placement of background
used? correction points. Refer to the
Winlab32 Software Guide for details.
Are you analyzing aluminum Run a high nitrogen purge for one hour
at 167 nm? before starting the analysis. Refer to the
Winlab32 Software Guide for details.
Undetectable The sample introduction Refer to Chapter 4, Maintenance.
emission signal system may not be set up
correctly, or may require
maintenance.
The shutter may be closed. Check the shutter position set in the
software. Refer to the Winlab32
Software Guide for details.
Memory effects Spray chamber may not be Check drain fittings and drain tubing.
being drained properly, or may Clean the spray chamber if necessary.
need cleaning.
 Performance Problems: Troubleshooting Table 6-13

Table 6-1. Performance Problems: Troubleshooting Table

Cannot get suggested The sample introduction Refer to Chapter 4, Maintenance.
detection limits system may not be set up
correctly, or may require
maintenance.
The BEC may be high. Run the BEC test. Refer to the
Winlab32 Software Guide for details.
Look for carryover – check if Increase the Read Delay to flush the
concentrations for the sample sample introduction system
replicates increase from one to completely. Refer to the Winlab32
the next. Software Guide for details.
The standard and blank may Prepare the standard and blank in the
need to be matrix-matched. same acid matrix used for the samples.
The integration time may be Increase the minimum and maximum
too short. times for integration. Refer to the
Winlab32 Software Guide for details.
Cannot get suggested The standard may have too Dilute the standard to approximate the
detection limits high a concentration. anticipated concentration of samples.
(continued)
You may not be comparing the Confirm that you are using the
appropriate value for the appropriate wavelength and recheck
wavelength you are using. the value. Refer to the Winlab32
Software Guide for details.
General performance Performance problems such as See the section "Checking the Sample
problems poor precision or loss of signal Introduction System" earlier in this
can often be traced to the setup chapter.
and condition of the sample
introduction system.
Unexplained The torch or injector may be Replace the torch and injector.
background shift coated with a deposit that
reflects light, resulting in a
periodic background shift.
6-14 Troubleshooting

Plasma Ignition and Stability Problems

Plasma Ignition Problems

Possible reasons for unsuccessful ignition follow. Correct the problem, if possible,
and then try to ignite the plasma again.

• If the plasma will not light check the ignitor. Open the door to the sample
compartment. Check that the ignitor finger is making contact with the tape on
the bottom of the torch glassware. Also, check the ignitor ground. If necessary,
use a brush to clean it.

• If the plasma is unstable check the exhaust vent. Be certain that your exhaust
vent is operating properly and is not blocked. Operation of the exhaust vent is
required to establish proper argon gas flow patterns as well as for safety reasons.

• Torch Connections. Verify that all gas fittings to the torch are finger-tight.
Leakage of air into any part of the torch, nebulizer or spray chamber will cause
ignition problems. The torch should be clean and in good condition. Do not use
tools to tighten, the nebulizer fittings may be damaged.

• If the plasma will not light check the RF coil. Check the RF coil for
condensation, particularly in labs with high humidity. Dry the RF coil with a soft
cloth if necessary.

• Torch Glassware. Check the condition of the torch glassware. If it is cloudy or

dirty, clean it in a 5-20% nitric acid solution. See Chapter 5, Maintenance for
instructions on removing these components.

• If the plasma is unstable check the drain. Check the drain tubing for flat spots
and replace the tubing if necessary. Check that the drain fitting on the spray
chamber drain is secure. Be sure that the pump is properly draining the spray
chamber and that the drain liquid is not backing up into the spray chamber or
building up in the torch.

• Argon. Check that the argon supply is on. Check the argon hose connections.
Make sure that they are not obstructed. Check that the pressure at the cylinder
regulator is 550-825 kPa (80-120 psig).

• Injector. Check that the injector is not clogged. You will need to remove the
injector and injector adaptor as described in Chapter 5, Maintenance. In addition,
 Plasma Ignition and Stability Problems 6-15

try pumping solutions with the Nebulizer, Auxiliary, and Plasma gas flows on
for approximately two minutes. Then turn off the pump and try to reignite the
plasma again.

• Optics Interlock. Check that the optics is centered over the torch. Problems
with ignition may be due to the optics having been bumped out of the correct
position. If this has happened carefully move the optics to the correct position.

• Nebulizer End Cap and Fittings. Check that it is tightly secured to the spray
chamber.

• Sample Capillary. Check that it is attached to the nebulizer.

• Organics. If you analyzing organic solutions and cannot ignite the plasma, run
the nebulizer argon for a couple of minutes with the pump off to purge the spray
chamber.

• Organic Vapors. If these remain in the torch from an earlier analysis, they can
sometimes cause ignition problems. If you suspect this, purge the sample
introduction system with argon for several minutes.

• Spray Chamber. Remove the spray chamber and cap the injector. Now try to
light the plasma. If the plasma now lights and is stable the ignition problem is in
the spray chamber, nebulizer or the sample introduction system. If the problem
persists check the torch O-rings and gas connections to the torch mount.
6-16 Troubleshooting

Plasma Stability Problems

If periodic pulsations of the torch are observed:

• Poor sample drainage may be the problem. Make sure that waste drainage is not
backing up into the spray chamber and that the waste is draining properly.

• Check the condition of the peristaltic pump tubing. If it is flattened, stretched, or

damaged by abrasion, replace the tubing.

• Air leaks may be causing the pulsation. Check the O-rings on the torch assembly
and ensure that the nut on the end of the torch is firmly in place. Do not use a
tool to tighten. Make sure the nebulizer/end cap assembly fits tightly to the spray
chamber.

If using organics, you may see an irregular pulsation:

• Be sure that the injector you are using is recommended for the types of solvents
you are using. The quartz injector, 1.2 mm i.d., is recommended for typical
organic analyses. The alumina injector, 0.85 mm i.d., should be used with
volatile organic solvents, for example, methanol.

• Try increasing the RF power, using less solvent, slowing down the pump speed,
or adjusting the torch height.
 Printing Problems 6-17

Printing Problems

Table 6-2. Printing Problems

Problem Possible Cause(s) Corrective Action

Printer does not print The correct printer driver may Check the printer drivers in Windows.
not be installed or selected in For more information, see the
Windows. WinLab32 Software Installation and
Administration Guide.
The printer may have been Check the power cable and the cable
disconnected. connecting the printer to the computer.
Make sure the power is on.
The printer may be out of Check printer status.
paper or off-line.
The pins on the printer cable Check the connector. If the pins are
connector may be broken. broken, order a replacement cable.
Printout is missing The printer may not be set to See the printer manufacturer’s
information the correct emulation mode. information or refer to the WinLab32
Software Installation and
Administration Guide.
6-18 Troubleshooting

Pump Problems

Table 6-3. Pump Problems

Problem Possible Cause(s) Corrective Action

Pump does not start The software may not be In the System menu, click on
configured for the pump you Configure Pump. In the dialog, make
are using. the appropriate selections.
Pump rollers stick A spill may have occurred or Clean the pump head, or replace if
the pump head may be worn necessary.
and may need to be replaced.
Liquid is not flowing The tension on the pump Use the adjustment screw to adjust the
freely tubing is too high or low. tension. See Chapter 5, Maintenance
for more information.
Tubing may not be installed
correctly in the channel. Reinstall tubing.

Tubing may be worn. Replace tubing.

Pump tubing is The tension on the pump Loosen the adjustment screw.
stretched on one end tubing is too tight.
and slack on the Check the rollers in the pump head to
other end Rollers may be stuck. see if they roll freely.

Tubing may be worn. Replace tubing.

Pump makes A mechanical problem may Call a PerkinElmer service engineer.
excessive noise have occurred.
 Autosampler Problems 6-19

Autosampler Problems

Table 6-4. Autosampler Problems

Problem Possible Cause(s) Corrective Action

Autosampler does not There may be a GPIB Use the Instrument Diagnostics
respond communication problem. window to reset the autosampler.
The software may not be In the System menu, click on
configured for the autosampler Configure Autosampler. In the
you are using. dialog, make the appropriate selections.
One of the cables may have Check the power cable and the cable
been disconnected or the connecting the autosampler to the
autosampler may have been computer. Make sure the power is on.
turned off.
The DIP switches may be set Check the DIP switch settings given in
incorrectly. Chapter 4, Installation.
The pins on the autosampler Check the connector. If the pins are
cable connector may be broken, order a replacement cable.
broken.
Autosampler does not The software may not be In the System menu, click on
go to the correct configured for the correct Configure Autosampler. In the
location. autosampler tray. dialog, select the appropriate tray.

RF Generator/Sample Introduction System Troubleshooting Form

Fill out the following form before you contact PerkinElmer service.
6-20 Troubleshooting

Troubleshooting Form
General:
Instrument Serial Number:
Site:
Date:

Sample Introduction Configuration:

Nebulizer Type: CROSS FLOW / LF GEMCONE / MEINHARD
Spray Chamber Type: SCOTT / CYCLONIC / BAFFLED CYCLONIC
Injector Type: QUARTZ / ALUMINA
Injector Bore (mm): 0.8 / 1.2 / 1.6 / 2.0 / 3.0
Glassware (number of slots): NO SLOT / ONE SLOT / THREE SLOT
Sample Type: AQUEOUS / ORGANICS / HIGH SOLIDS

Operating Conditions:
RF Power: W
Plasma Gas Flow: l/min
Aux Gas Flow: l/min
Nebulizer Gas Flow: l/min
Sample Uptake Rate: ml/min
Sample Compartment Heater: C
Torch Position: mm
Distance between Injector tip and Aux Tube: mm

Instrument Environment:
Lab Temperature: C  C
Vent Distance from Exhaust: mm
Line Voltage: V
Line Frequency Hz
Chiller Temperature Setting: C

Troubleshooting Tasks Performed:

Did the plasma light: Yes/No
Did the plasma stay lit after ignition: Yes/No
Plasma went out after pump turned on: Yes/No
 RF Generator/Sample Introduction System Troubleshooting Form 6-21

Plasma went out after how long of operation:

Plasma went out with Warm Wet Plasma (neb on, pump on, heat on): Yes/No
Plasma went out with Cold Wet Plasma (neb on, pump on, no heat): Yes/No
Plasma went out with Dry Plasma (neb on, no pump): Yes/No
Plasma went out when injector capped off: Yes/No
Referring to the figures on the following pages, the plasma looked like FIGURE:

Common Setup Problems:

Glassware bottomed out in torch body (Glassware Holder): Yes/No
Glassware aligned with notch in torch body (Glassware Holder): Yes/No
Copper tape covering igniter spark hole: Yes/No
Igniter finger contacting copper tape: Yes/No
Ground rod located near end of glassware but outside of glassware Yes/No
Fiber Optic located over glassware and is not melted or recessed: Yes/No
Torch position appropriate for sample type: Yes/No
Aqueous = -3, Organics = -3, High Solids = -1
Injector O-Rings not worn, cracked, or cut: Yes/No
Torch Body (Glassware Holder) O-Rings not worn, cracked, or cut: Yes/No
Injector Dry: Yes/No
Spray Chamber draining properly: Yes/No
Pump Tubing clamped: Yes/No
Pump Tubing not worn out: Yes/No
Pump Tubing pumping in proper direction: Yes/No
Radial and Axial windows installed and clean: Yes/No

Figure 6-1. Normal Plasma Conditions at 0 torch position

6-22 Troubleshooting

Figure 6-2. Normal Plasma at -3mm position

Figure 6-3. Rounded Plasma due to sample or air getting around the outside (typ-
ically subtle air leak)

Figure 6-4. Aux Gas too high, Air Leak, or Spray Chamber Temperature too high
 RF Generator/Sample Introduction System Troubleshooting Form 6-23

Figure 6-5. Injector too far forward

Figure 6-6. No Aux Gas (Torch may be glowing)

Figure 6-7. Air Leak or Spray Chamber Temperature too high

6-24 Troubleshooting

Figure 6-8. Thin Plasma due to leak in Plasma Gas Line

Chapter 7
 Error Messages
Contents
System Error (SYSERROR) Messages for RF Generator .......................... 7-4
7-4 Error Messages

System Error (SYSERROR) Messages for RF Generator

In the following chart, the first column lists the error code. The second column lists
the error messages that appear in the generator diagnostics software. The third
column gives the meaning of the error messages. The fourth column gives
suggestions for corrective action.

Note For every error message reported, four pieces of information are given; the
error code, the error value, the time the error occurred and the error
message.

In some cases, the error value is 0 and therefore meaningless. However, in cases
where the RF generator is operating out of range, the value of the parameter is
reported. For example, if the error code is "01", Vds out of voltage range, the value
is the actual Vds voltage.
 System Error (SYSERROR) Messages for RF Generator 7-5

The following messages are listed numerically by error code.

Error Code Error Meaning Corrective Action

Messages

00 No Error There is no error. No corrective action is needed.

01 Vds out of The drain to source Contact PerkinElmer Service.
voltage voltage across the
tolerance power FET transistor
window is out of the
Tolerance window.
02 Ids 1 out of The drain to source Contact PerkinElmer Service.
level 1 current across the
window power FET transistor
1 is out of the level 1
Tolerance window.
03 Ids 2 out of The drain to source Contact PerkinElmer Service.
level 1 current across the
window power FET transistor
2 is out of the level 1
Tolerance window.
04 Failed to Instrument failed Ignition failure may be caused by incorrect argon
ignite after ignition sequence. flows, air leaks, weak/no ignition spark, cracked or
all attempts damaged glass torch, or no RF power.
Verify that the Ignitor spring finger is making
connection with the torch contact.
Check that the Ignitor wire has not broken or shorted
to ground. Check the condition of the torch
glassware for cracks or signs of sputtering metal
onto the glass around the load coil. Check the
condition of the load coil bonnet, check it for cracks
or sputtering of metal around the load [Link] the
proper flows of argon in the plasma and auxiliary
lines; excessive argon pressure can “blow” a plasma
out. Check the torch, torch mount assembly and
argon fittings for air leaks.
7-6 Error Messages

Error Code Error Meaning Corrective Action

Messages

05 Ids 1 out of The drain to source Observe the plasma discharge during ignition
level 2 current across the through the viewing window; if the plasma forms
window power FET transistor properly but extinguishes right away, check the
1 is out of the level 2 argon flows, torch condition, and test for air leaks. It
Tolerance window. may be possible to see the plasma being blown out
of the torch, or that it is unstable during ignition in
which case the cause is probably pneumatic related.
If the plasma appears stable during the ignition, but
still extinguishes, it is possible that the one of the RF
transistors has been damaged and is therefore
drawing a different current than normal. In this case,
the RF Oscillator Assembly must be replaced.
Contact PerkinElmer Service.
06 Ids 2 out of The drain to source Contact PerkinElmer Service.
level 2 current across the
window power FET transistor
2 is out of the level 2
Tolerance window.
07 Ids 1 out of The drain to source Contact PerkinElmer Service.
level 3 current across the
window power FET transistor
1 is out of the level 3
Tolerance window.
08 Ids 2 out of The drain to source Contact PerkinElmer Service.
level 3 current across the
window power FET transistor
2 is out of the level 3
Tolerance window.
 System Error (SYSERROR) Messages for RF Generator 7-7

Error Code Error Meaning Corrective Action

Messages

09 Ids 1 higher The drain to source Contact PerkinElmer Service.

than ids current across the
maximum power FET transistor
1 is higher than the
maximum allowable
current.
10 Ids 2 higher The drain to source Contact PerkinElmer Service.
than ids current across the
maximum power FET transistor
2 is higher than the
maximum allowable
current.
11 Failed to Failed to set power to Contact PerkinElmer Service.
reach/ a value specified in
maintain the Plasma Controls
power at Dialog window.
specified
level
12 Failed to Failed to set AUX to Check argon supply, argon pressure, AUX flow
set AUX a value specified in tubing and connections. If this does not correct the
flow to the AUX Setting problem, contact PerkinElmer Service.
specified Flow Controls
level window.
13 Failed to Failed to set Plasma Check the argon supply, argon pressure, plasma
set Plasma flow to a value flow tubing, and connections. If this does not correct
flow to specified in the Flow the problem, contact PerkinElmer Service.
specified Controls window.
level
7-8 Error Messages

Error Code Error Meaning Corrective Action

Messages

14 Failed to Failed to set Neb Check the nebulizer tips for blockage.
set Neb flow to a value Check the argon supply, argon pressure, neb flow
flow to specified in the Flow tubing, and connections. Verify that the Nebulizer
specified Controls window. Quick Disconnect fitting is connected. See Figure 5-
level 11. If this does not correct the problem, contact
PerkinElmer Service.
15 The Attempted ignition Reset the Emergency Off Switch to correct this error
Emergency sequence with the message.
Off Switch Emergency Off If resetting the Emergency Off Switch does not clear
is still Switch pressed. the error message, check the operation of the switch.
pressed
16 Emergency Release and reset the Emergency Off Switch to
Off Switch correct this error message.
pressed If resetting the Emergency Off Switch does not clear
the error message, check the operation of the switch.
17 Emergency Reset the Emergency Off Switch to correct this error
Off Switch message.
latched If resetting the Emergency Off Switch does not clear
the error message, check the operation of the switch.
18 Torch not Torch interlock Contact PerkinElmer Service.
installed switch not satisfied.
19 Door open Door ajar or not Close the RF door to correct this error message.
sensed closed. If closing the door does not clear this error message,
contact PerkinElmer Service.
20 Water not Water shut off. Check the water flow.
flowing Verify that the water pressure is adequate, and the
water level in the chiller is filled. Check the water
lines for obstructions, especially the tubing inserts at
the Swagelok fittings. If this does not correct the
problem, contact PerkinElmer Service.
 System Error (SYSERROR) Messages for RF Generator 7-9

Error Code Error Meaning Corrective Action

Messages

21 Shear gas Shear gas is not Check the shear gas flow.
not flowing flowing. If this does not correct the problem, contact
PerkinElmer Service.
Caution: Running the plasma without shear gas
actually flowing for more than a few seconds may
cause damage to the purge glass.
22 Failed to The instrument has Verify that the NEB Quick-Disconnect fitting is
maintain failed to maintain or correctly mated. Examine the nebulizer tips for
Neb flow attain the nebulizer blockage. Check the argon lines from Pneumatics
flow. board for crimping. If this does not correct the
problem, contact PerkinElmer Service.
23 Failed to The instrument has Check the argon lines for crimping. If this does not
maintain failed to maintain or correct the problem, contact PerkinElmer Service.
AUX flow attain the AUX flow.
24 Failed to The instrument has Check the argon lines for crimping. If this does not
maintain failed to maintain or correct the problem, contact PerkinElmer Service.
Plasma attain the plasma
flow flow.
25 Heatsink A temperature Verify that the water chiller temperature is set
temperature problem with the correctly. Verify that the chiller is holding that
out of cooling water is temperature. Check the water lines (and water filter
limits detected. The RF if installed). If this does not correct the problem,
generator will be shut contact PerkinElmer Service.
down when the
temperature is out of
limits.
26 +24V This warning Contact PerkinElmer Service.
supply out message will appear
of range if the RF Control
(Warning) Electronics Supply is
+/-10% out of range.
7-10 Error Messages

Error Code Error Meaning Corrective Action

Messages

27 DC supply This warning Contact PerkinElmer Service.

out of range message will appear
(Warning) if the Instrument
Control Electronics
Supply is +/-10% out
of range.
29 Fiber optic The firmware expects Check the Optics Interlock. See Chapter 6, Plasma
not the plasma to be on Ignition Problems for more information. If this
detecting but the plasma is not does not correct the problem contact PerkinElmer
plasma on. The fiber optic Service.
during will do a hardware
ignition shutdown.
30 Not used
31 Neb In this hardware Verify that the NEB Quick-Disconnect fitting is
Pressure failure the nebulizer correctly mated. Examine the nebulizer tips for
out of range back pressure is out blockage. If this does not correct the problem,
of the acceptable contact PerkinElmer Service.
range of 0 to 65 psi.
32 Ids 1 is Drain to source Contact PerkinElmer Service.
non-zero current across the
power FET transistor
1 is a non-zero
current. This
transistor should be
off but current is still
going through it.
 System Error (SYSERROR) Messages for RF Generator 7-11

Error Code Error Meaning Corrective Action

Messages

33 Ids 2 is Drain to source Contact PerkinElmer Service.

non-zero current across the
power FET transistor
2 is a non-zero
current. This
transistor should be
off but current is still
going through it.
34 Shear gas In the Plasma Control The Shear Control must be turned on. If this does
not enabled Dialog window the not correct the problem, contact PerkinElmer
Shear Control is off. Service.
35 Water still May indicate Check the operation of the water flow soleinoid in
flowing hardware failure. the RF generator. Chiller pressure set too high.
36 Shear gas May indicate Check the operation of the shear gas soleinoid on the
still hardware failure. Pneumatics PC board.
flowing
37 Interlocks The interlocks are not Check that the torch door access door is closed and
set satisfied. the torch is in position.
38 Ids The current in one Check the position of the plasma during ignition. If
imbalance transistor is larger it is being pushed out of the load coil correct the air
than the other leak or AUX flow. If this does not correct the
transistor. Both problem, contact PerkinElmer Service.
transistors should
have an equal current
within tolerance
limits.
39 +24 V This fatal message Contact PerkinElmer Service.
Supply out will appear if the 24
of range V Supply is 10% out
(Fatal) of range (24V +/-2.4
V).
7-12 Error Messages

Error Code Error Meaning Corrective Action

Messages

40 +DC This fatal message Contact PerkinElmer Service.

Supply out will appear if the DC
of range Supply is 10% out of
(Fatal) range (24V +/-2.4 V).
41 Watchdog The microprocessor Contact PerkinElmer Service.
Timeout malfunctioned and
the instrument lost
functions, but
recovered.
42 Fiber optic Hardware error. The Check the Optics Interlock. See Chapter 6, Plasma
detecting fiber optic is Ignition Problems for more information. If this
plasma detecting the plasma does not correct the problem contact PerkinElmer
but the plasma is not Service.
on.
43 Ids 1 not 0 Drain to source Contact PerkinElmer Service.
current across the
power FET transistor
1 is turned off but
current is still
flowing through this
transistor.
44 Ids 2 not 0 Drain to source Contact PerkinElmer Service.
current across the
power FET transistor
2 is turned off but
current is still
flowing this
transistor.
 System Error (SYSERROR) Messages for RF Generator 7-13

Error Code Error Meaning Corrective Action

Messages

45 Watchdog A hardware/firmware Contact PerkinElmer Service.

not failure. The safety
working timer that protects the
instrument in case the
firmware fails is not
working.
46 Plasma The Flow Controls Check inlet pressure and the output regulators and
flow low Setting in the Plasma that there is enough pressure into the instruments. If
(<10 L/m) Control Dialog this does not solve the problem, contact PerkinElmer
window is too low, or Service.
not enough inlet
pressure and flow to
sustain the plasma
gas flow.
47 Neb flow The Neb flow should Something is wrong with the Neb flow control.
not zero be zero but the Check that the Neb tubing is properly connected to
hardware detects a the Quick Disconnect to allow for flow. If this does
flow. not solve the problem, contact PerkinElmer Service.
48 Plasma Flow control setting The ignite flow must be at least 10 L/m. See Error
flow < 10 is below 10 L/m. Message 46.
while
plasma lit
49 FLASH The Flash has been Contact PerkinElmer Service.
Checksum corrupted,
error redownload the
software.
50 AUX flow The Flow Controls The ignite flow must be at least 0.5 L/m. See Error
too low to Setting for AUX in Message 46.
ignite (0.5 the Plasma Controls
L/m) Dialog window is <
0.5 L/m.
7-14 Error Messages

Error Code Error Meaning Corrective Action

Messages

51 Operating In the General and Contact PerkinElmer Service.

parameters System Parameters
checksum the BRAM was
error corrupted or not
loaded correctly.
52 Backup In the System Contact PerkinElmer Service.
parameters Defaults the BRAM
checksum was corrupted or not
error loaded correctly.
53 Learn AUX The AUX calibration Contact PerkinElmer Service.
checksum table has been
error corrupted, relearn
AUX gas.
54 Learn The Plasma Contact PerkinElmer Service.
Plasma calibration table has
checksum been corrupted,
error relearn Plasma gas.
55 Parameter This warning This warning indicates that an error occurred earlier
validation message indicates and may need to be investigated.
error, that the Parameter
parameter Validation at start up
was fixed was changed back to
a valid range.
56 Lifetime The Lifetime log has Data is lost.
log been corrupted.
checksum
error
57 Manufac- The Manufacturing Data is lost.
turing log log has been
checksum corrupted.
error
 System Error (SYSERROR) Messages for RF Generator 7-15

Error Code Error Meaning Corrective Action

Messages

58 Vds too The supply voltage Contact PerkinElmer Service.

high for should be closer to
ignition (>5 zero.
volts)
59 Shear gas Check the shear gas valve.
stuck on
60 Water flow Check the water valve. The valve maybe frozen
stuck on open or the flow switch may need to be replaced. If
the solid-state relay is on and the water is on, the
flow sensor could be stuck on flow. Contact
PerkinElmer Service.
61 Error Parameters for the Contact PerkinElmer Service.
reading ignite command for
post-ignite the power setting are
power invalid.
setting
62 Error Parameters for the Contact PerkinElmer Service.
reading ignite command for
post-ignite the AUX flow are
AUX flow invalid.
63 Error Parameters for the Contact PerkinElmer Service.
reading ignite command for
post-ignite the neb flow are
neb flow invalid.
64 Error Parameters for the Contact PerkinElmer Service.
reading ignite command for
post-ignite the plasma flow are
plasma invalid.
flow
7-16 Error Messages

Error Code Error Meaning Corrective Action

Messages

65 Learn AUX There is a fault in the Contact PerkinElmer Service.

failed range pneumatics system.
checking
66 Learn There is a fault in the Contact PerkinElmer Service.
Plasma pneumatics system.
failed range
checking
67 Learn AUX The system calculates Verify that the AUX gas is turned on. Otherwise the
failed slope a slope to verify that plasma will not ignite.
checking the AUX flows are
actually increasing.
68 Learn The system calculates Verify that the plasma is turned on. Otherwise the
Plasma a slope to verify that plasma will not ignite.
failed slope the plasma flows are
checking actually increasing.
69 Fiber Optic The firmware cannot Check that the fiber optics is in line with the laod
not detect the plasma coil. If the problem persists contact PerkinElmer
detecting after ignition. The Service.
plasma in fiber optic will do a
the monitor hardware shutdown.
70 Neb back- The nebulizer has Check the sample introduction system for leaks and
pressure been shut off once the blockage and correct. Check that all the fittings are
>60 psi nebulizer tight and check if the nebulizer spray pattern is
(413 kPa) backpressure has correct. If the problem persists contact PerkinElmer
& shut off fallen below 60 psi Service.
neb (413 kPa).
71 Neb heater The nebulizer If there is a large variance in room temperature you
sensor is compartment heater might experience instrument drift if the nebulizer
not sensor is not working compartment heater is off. Otherwise the instrument
working- properly and the is fully functional.
heater off heater is now off. Contact PerkinElmer Service to have the nebulizer
compartment heater repaired.
System Error (SYSERROR) Messages for RF Generator 7-17
7-18 Error Messages
In d e x
 Index
A B
Acid Digestions 1-29 Bonnet
Air Filters inspecting 6-9
general maintenance 5-81 C
maintenance 5-81 Capillary Tubing
periodic checks 5-10 inspecting 6-7
RF generator, changing 5-81 Chemical Reagents 1-13
spectrometer, changing 5-81 Chiller
Alignment connecting 4-10, 4-14
torch viewing position 4-31 connections at back of instrument 4-15
Argon coolant recommended 4-15
checking 6-14 daily checks 5-7
Argon Supply electrical requirements 2-12
connecting, instructions 3-22, 4-8 filling 4-15, 4-16
daily checks 5-6 filters 5-83
requirements 2-12 requirements 2-9
Autosampler starting 4-17
connecting to computer 4-27 Coil, RF
description 3-18 see RF Coil 5-9
DIP switch settings, IEEE 4-26 Computer
inserting sampling probe 4-29 configuration and setup 4-20
installing 4-26 Connections
sampling probe fit 4-28 cooling water 4-6
sampling probe height adjustment 4-29 cooling water supplies 3-22
setting up 4-28 electrical 3-22
troubleshooting problems with 6-19 gases 3-22, 4-6
Axial Window Cooling Water
replacing 5-37 connections at back of instrument 4-7
flow diagram with chiller 4-15
In-4 Index

Cyclonic Spray Chamber replacing 5-61

cleaning 5-46 Environmental Conditions
etching 5-45 laboratory requirements 2-4
installing 5-42 Exhaust Vent
maintenance 5-42 checking 6-14
D daily checks 5-8
Daily Cleaning 5-6 requirements 2-5
Dark Current F
measuring 3-21 Filters
Detector 3-9 air 5-81
Digestions part numbers 5-84
at elevated pressure 1-31 replacement parts 5-84
performing 1-31 water 5-83
Dissolving Solid Samples Fuses
in organics 1-28 maintenance 5-84
using acids 1-29 Fusion Mixtures 1-32
Drain G
daily checks 5-8, 6-14 Gas Cylinders
periodic checks 5-10 handling 1-12
safety practices 1-10 identification 1-12
tubing, connecting 5-79 storing 1-12
Drain Tubing Gas Supply
adjusting 5-78 replacement parts 5-84
connecting 5-75 Gases
installing 5-72, 5-76 connecting, instructions 4-6
Dual View connections at back of instrument 4-7
recommendations 4-33 H
E Hardware Settings
Electrical Requirements controlled by software 3-21
laboratory preparations 2-10 Hazards
Electrical Safety ultraviolet radiation 1-8
safety practices 1-5 High Temperatures
Emergency Off Switch 3-20 safety practices 1-9
End Cap Hoses, Gas and Water
removing from Scott spray chamber 5-40 part numbers 5-84
replacement parts 5-48
 I In-5

Hot Exhaust Gases L

safety practices 1-9 Labels on the Instrument 1-18
Hydrofluoric Acid 1-30 Laboratory Guidelines 1-5
I Laboratory Preparation
ICP Source electrical requirements 2-10
RF control electronics 3-13 exhaust vent requirements 2-5
RF generator 3-12 Laboratory Requirements
Ignitor argon supply 2-12
checking cable 6-14 chiller 2-9, 2-12
Initialization of Instrument 3-19 environmental conditions 2-4
initialization steps 3-19 pneumatics 2-12
interlocks 3-19 purge gas 2-13
Injector regulator 2-14
checking 6-14 shear gas 2-13
removing 5-15 space 2-7
Installation Laboratory Ventilation 1-9
autosampler 4-26 M
connecting cooling water 4-6 Maintenance
connecting gases 4-6 air filters 5-81
connecting the system components 4-17 cleaning procedures 5-12
general information 4-4 concentric glass nebulizer 5-67, 5-69
moving the instrument 4-5 cyclonic spray chamber 5-42
Quick-Change Adjustable Torch Mod- cyclonic spray chamber, cleaning 5-46
ule 4-20 cyclonic spray chamber, etching 5-45
shipping list 4-35 cyclonic spray chamber, installing 5-42
summary 4-4 daily checks 5-6
Instrument Handling 1-9 end cap, removing 5-40
Instrument Parameters end cap,replacing 5-61
setting 4-33 fuses 5-84
Instrument Startup 4-30 GemCone nebulizer 5-62
Interlocks GemCone nebulizer, cleaning 5-62
description 3-19 GemTip Cross-Flow nebulizer 5-49
general system 5-81
nebulizer 5-47
periodic checks 5-9, 5-10
peristaltic pump 5-71
In-6 Index

purge window 5-33 end cap, removing 5-49

replacement parts 5-84 GemCone liquid fitting, maintenance 5-
RF coil 5-30 66
Scott spray chamber, cleaning 5-41 GemCone nebulizer, cleaning 5-65
shear gas nozzle, replacing 5-38 GemCone nebulizer, installing on cy-
spray chamber 5-15, 5-21 clonic spray chamber 5-64
spray chamber, replacing 5-28 GemCone nebulizer, installing on Scott
spray chamber,removing 5-40 spray chamber 5-63
torch, cleaning 5-19 GemCone, maintenance 5-62
torch, removing 5-17 GemTip Cross-Flow, maintenance 5-49
torch, replacing 5-21 High Solids GemCone nebulizer, clean-
water filter 5-83 ing 5-62
Meinhard Nebulizer inspecting 6-7
maintenance 5-67 low-flow GemCone nebulizer, cleaning
Monochromator 3-8 5-62
Moving maintenance 5-47
instrument 4-5 periodic checks 5-10
N replacement parts 5-48
Nebulizer tubing,connecting 5-28
argon flow rate 3-21 Nebulizer End Cap
argon tubing, connecting 5-58 checking 6-15
argon tubing, replacing 5-59 Nebulizer Heater 3-17
comparison of different types 3-15 Nebulizer Tubing
concentric glass nebulizer, maintenance connecting 4-24
5-67 Neon Lamp
concentric glass, cleaning 5-69 changing 5-82
concentric glass, installing 5-67 Nitrogen Purge Rate 3-21
Cross-Flow nebulizer argon tip, remov- Nitrogen Supply
ing 5-56 connecting, instructions 3-22, 4-6
Cross-Flow nebulizer sample tip, remov-
ing 5-53
Cross-Flow nebulizer spray pattern,
checking 5-50
Cross-Flow nebulizer, disassembling 5-
51
daily checks 5-8
 O In-7

O Plasma Torch
Optics Interlock periodic maintenance 5-13
checking 6-15 Pneumatic Requirements
Optimization 3-21 laboratory requirements 2-12
Organic Vapors Printer
checking 6-15 configuration and setup 4-20
Organics troubleshooting problems with 6-17
and plasma stability 6-16 Pump Tubing
checking 6-15 adjusting 5-77
P Pump, Peristaltic
Perchloric Acid 1-30 maintenance 5-71
Performance Checks Purge Gas
periodic checks 5-11 daily checks 5-7
Peristaltic Pump laboratory requirements 2-13
cleaning 5-79 Purge Window
daily checks 5-8 axial window, replacing 5-37
description 3-18 cleaning 5-35
flow rate 3-21 inspecting 6-9
inspecting 6-7 maintenance 5-33
maintenance 5-71 periodic checks 5-10
part numbers 5-81 radial window, replacing 5-36
periodic checks 5-10 removal 5-33
pump head, removing 5-79 Purge Windows
replacement parts 5-81 instruments 5-33
troubleshooting problems with 6-18 replacement parts 5-39
TubingSaver 3-21 Q
Peristaltic Pump Tubing Quick-Change Adjustable Torch Module 3-
inspecting 6-7 14
replacing 5-71 description 3-14
Plasma installation 4-20
troubleshooting ignition problems 6-14 periodic maintenance 5-13
troubleshooting stability problems 6-14
Plasma Argon Flow Rates 3-21
Plasma Parameters
recommendations 4-33
In-8 Index

R hot exhaust gases 1-9

Radial Window hydrofluoric acid 1-30
replacing 5-36 instrument handling 1-9
Regulator laboratory guidelines 1-5
laboratory requirements 2-14 laboratory ventilation 1-9
Replacement Parts perchloric acid 1-30
peristaltic pump 5-81 RF radiation 1-8
purge windows 5-39 safety interlocks 1-9
torch module 5-32 sample preparation 1-28
RF Coil ultraviolet radiation 1-8
daily checks 5-8 waste disposal procedures 1-15
inspecting 6-14 Sample Capillary
periodic checks 5-9 checking 6-15
periodic maintenance 5-14 Sample Compartment
replacing 5-30 description 3-14
RF Control Electronics 3-13 Sample Introduction System
RF Generator 3-12 autosampler 3-18
RF Power 3-21 cleaning 5-12
RF Radiation description 3-14
safety practices 1-8 inspection of 6-6
S nebulizer 3-15
Safety Interlocks 1-9 peristaltic pump 3-18
burner system 1-8 Quick-Change Adjustable Torch Mod-
Safety Practices ule 3-14
acid digestions 1-29 torch 3-14
chemical reagents 1-13 Sample Preparation 1-28
digestions 1-31 Sample Tubing
dissolving solid samples in organics 1-28 adjusting 5-77
dissolving solid samples using acids 1- installing 5-72
29 Shear Gas
drain system 1-10 adjusting nozzle 5-39
electrical safety 1-5 connecting, instructions 3-22, 4-8
environmental conditions 1-7 connection at back of instrument 4-7
fusion mixtures 1-32 daily checks 5-7
general practices 1-5 laboratory requirements 2-13
high temperatures 1-9 setting pressure 4-9
 T In-9

Shear Gas Nozzle Symbols

replacing 5-38 graphics on the instrument 1-18
Shipping List 4-35 used on the instrument 1-17
Space Collar warnings on the instrument 1-17
used in gas connections 4-6 T
Specifications 3-24 Torch
argon flow controls 3-24 alignment 4-31
ICP system 3-24 cleaning 5-19
sample introduction system 3-25 daily checks 5-8
spectrometer 3-26 description 3-14
Spectrometer disassembling 5-17
air filter, changing 5-81 inspecting 6-8
CCD 3-9 inspecting glassware 6-14
description 3-6 periodic checks 5-9
detector 3-9 removing 5-17
monochromator 3-8 replacing 5-21
transfer optics 3-8 Torch Connections
wavelength correction 3-11 checking 6-14
Spray Chamber Torch Module
checking 6-15 part numbers 5-32
cleaning 5-21, 5-41 Torch Viewing Position Alignment Proce-
description 3-14 dure 4-31, 5-11
end cap,removing 5-40 Transfer Optics 3-8
inspecting 6-7 Troubleshooting
maintenance 5-40 autosampler problems 6-19
periodic checks 5-10 general information 6-4
removing 5-15, 5-40 performance problems 6-6
replacement parts 5-46 performance problems, table 6-10
replacing 5-28 plasma ignition problems 6-14
spare parts 5-74 plasma stability problems 6-14
Spray Chamber, Cyclonic printing problems 6-17
maintenance 5-42 pump problems 6-18
Spray Chamber, Scott
cleaning 5-41
maintenance 5-40
replacing 5-28
In-10 Index

U
Ultraviolet Radiation
safety practices 1-8
V
Viewing 4-31
W
Warnings
symbols used on instrument 1-17
Waste Disposal Procedures 1-15
Water Filter
general maintenance 5-83
installing filter cartridge 4-11
Water Supply
replacement parts 5-84
Wavelength Correction 3-11