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ICP OPTICAL EMISSION

OPTIMA 5000 SERIES

Hardware Guide
Release Information
Part Number Release Publication Date
0993-6762 A April 2006
0993-6762 B April 2006 Valid for Software Version 3.3
0993-6762 C January 2007
0993-6762 D February 2007 Valid for Software Version 3.4
Any comments about the documentation for this product should be addressed to:

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

or emailed to: [email protected]

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

Copyright Information
This document contains proprietary information that is protected by copyright. All rights are reserved. No parts of this document may
be reproduced in any form whatsoever or translated into any language without the prior written permission of
Perkin Elmer, Inc.
Copyright © 2007 Perkin Elmer, Inc.

Printed in the USA.

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Registered names, trademarks, etc. used in this document, even when not specifically marked as such, are protected by
law
PerkinElmer is a trademark of Perkin Elmer, Inc.
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WinLab is a trademark of Perkin Elmer, Inc.
 Contents iii

Customer Service .............................................................................. xiii

Safety and Regulatory Information ................................................... xiv
Safety Information in the Manual .................................................xv
FCC Compliance (United States) .................................................xv
Europe ...........................................................................................xv
Environment ................................................................................ xvi
Operating Conditions ............................................................ xvi
Symbols Used on the Instrument ............................................... xvii
Warning Labels on the Instrument .............................................. xix
Safety Labels on the Front of the Instrument ....................... xix
Safety Labels on the Side of the Instrument ......................... xxi
Safety Labels on the Back of the Instrument ...................... xxiv
Safety Labels in the Sample Compartment ........................ xxvii
Safety Label in the Spray Chamber Compartment for the
Optima 5100DV, 5200DV and 5300DV ..............................xxx
Using this Guide ............................................................................. xxxi
Documents to Help You ................................................................. xxxi
How this Guide is Organized ......................................................... xxxii
Using the Index ....................................................................... xxxiii
A Word on Troubleshooting ................................................... xxxiii

Chapter 1. Safety Practices ................................................. 1-3

Laboratory Guidelines ...................................................................... 1-3
General ....................................................................................... 1-3
Environmental Conditions .......................................................... 1-4
Handling of the Instrument ......................................................... 1-4
Laboratory Ventilation ................................................................ 1-4
Instrument Safety Practices .............................................................. 1-5
Safety Interlocks ......................................................................... 1-5
Radio Frequency Radiation ........................................................ 1-6
Ultraviolet Radiation ................................................................... 1-6
Electrical Safety .......................................................................... 1-6
High Temperatures ..................................................................... 1-9
Hot Exhaust Gases ...................................................................... 1-9
Safe Use of Drain Systems ......................................................... 1-9
Waste Disposal Procedures ....................................................... 1-10
iv Contents

Safe Handling of Gas Cylinders ............................................... 1-11

Identification of Gas Cylinders ........................................... 1-12
Storing Cylinders ................................................................ 1-12
Handling Cylinders ............................................................. 1-13
Hazardous Chemicals Warnings ............................................... 1-14
Safe Use of Chemical Reagents ................................................ 1-15
Protective Equipment .......................................................... 1-15
Use, Storage, and Disposal ................................................. 1-15
Sample Preparation ......................................................................... 1-16
Dissolving Solid Samples in Organics ...................................... 1-16
Dissolving Solid Samples Using Acids .................................... 1-17
Using Acids ......................................................................... 1-17
Acid Digestions ......................................................................... 1-17
Perchloric Acid ................................................................... 1-18
Hydrofluoric Acid ............................................................... 1-18
Performing Digestions ........................................................ 1-19
Digestions at Elevated Pressure .......................................... 1-19
Fusion Mixtures ........................................................................ 1-20
References ....................................................................................... 1-20

Chapter 2. Preparing Your Laboratory ............................ 2-3

Chapter Overview ............................................................................. 2-3
Preparing the Laboratory .................................................................. 2-3
Environmental Conditions .......................................................... 2-3
Exhaust Vent Requirements ........................................................ 2-4
Vent Positions ............................................................................. 2-6
Laboratory Space Requirements ................................................. 2-7
Optima 5000 Instrument ....................................................... 2-7
Computer and Printer ............................................................ 2-9
PolyScience Chiller ............................................................... 2-9
Drain Vessels ........................................................................ 2-9
Location ................................................................................ 2-9
Recirculating System .......................................................... 2-10
Electrical Requirements ............................................................ 2-11
Optima 5000 Series Instrument .......................................... 2-11
Computer and Printer .......................................................... 2-12
 Contents v

PolyScience Chiller ............................................................. 2-12

Pneumatic Requirements .......................................................... 2-13
Argon .................................................................................. 2-13
Purge Gas ............................................................................ 2-14
Shear Gas ............................................................................ 2-15
Regulator ............................................................................. 2-15

Chapter 3. System Description ........................................... 3-3

Optima 5000 Series Instruments ....................................................... 3-4
Plasma Viewing Configurations ................................................. 3-5
Spectrometer ................................................................................... 3-10
Optical System .......................................................................... 3-10
Optics Housing ................................................................... 3-11
Detector Cooling and Purging .................................................. 3-13
ICP Source ...................................................................................... 3-14
RF Generator ............................................................................. 3-14
RF Control Electronics ............................................................. 3-15
Sample Compartment ..................................................................... 3-16
Sample Introduction System ........................................................... 3-16
Quick-Change Adjustable Torch Module ................................. 3-16
Torch ......................................................................................... 3-16
Spray Chamber ......................................................................... 3-16
Nebulizers ................................................................................. 3-17
Nebulizer Compartment Heater (optional) ............................... 3-20
Peristaltic Pump ........................................................................ 3-21
Autosampler .............................................................................. 3-21
System Initialization and Setup ...................................................... 3-22
Interlocks .................................................................................. 3-22
Initialization Steps .................................................................... 3-22
Hardware Setup and Optimization ............................................ 3-23
How the Echelle Spectrometer and SCD Work .............................. 3-23
Introduction ............................................................................... 3-23
Transfer Optics ......................................................................... 3-29
Input Module ............................................................................. 3-29
UV Module ............................................................................... 3-31
Visible Module (5300 model only) ........................................... 3-33
vi Contents

Segmented-array Charge-coupled-device Detector (SCD) ....... 3-33

Indicator Light ................................................................................ 3-37
Connections to Electrical, Gas, and Cooling Water Supplies ......... 3-38
Specifications .................................................................................. 3-42
ICP System Specifications ........................................................ 3-42
Gas Flow Controls ................................................................... 3-42
Sample Introduction System ..................................................... 3-43
Spectrometer ............................................................................ 3-44

Chapter 4. Installation ........................................................ 4-3

Installation Summary ........................................................................ 4-4
Moving the Instrument ...................................................................... 4-4
Connecting the Gases and Cooling Water ........................................ 4-5
Connecting the Gases .................................................................. 4-6
Connecting the PolyScience Chiller ......................................... 4-11
Filling the PolyScience Chiller ................................................. 4-16
Starting Up the PolyScience Chiller ......................................... 4-17
Connecting the System Components .............................................. 4-18
Setting Up the Computer and Printer .............................................. 4-20
Installing the Quick-Change Adjustable Torch Module ................. 4-21
Installing the Quick-Change Adjustable Torch Module on the
Optima 5100, 5200 and 5300 DV ............................................. 4-21
Torch Positions ................................................................... 4-22
Connecting the Nebulizer (NEB) Tubing ................................. 4-26
Installing the Torch Module for the Optima 5300V ....................... 4-28
Installing the Torch Module Assembly .................................... 4-29
Installing the Cyclonic Spray Chamber Assembly ................... 4-31
Connecting the Nebulizer (NEB) Tubing to
the Optima 5300V ................................................................... 4-34
Installing The Autosampler ............................................................ 4-34
Fitting and Connecting the Autosampler Sampling Probe ............. 4-37
Fitting the Sampling Probe ....................................................... 4-38
Instrument Start-up ......................................................................... 4-41
Automatically Aligning the Torch Viewing Position ..................... 4-41
Detector Calibration .................................................................. 4-43
Wavelength Calibration for all Optima 5000 Series Models .... 4-43
 Contents vii

Setting Instrument Parameters ........................................................ 4-46

Aqueous Setting Instrument Parameters ................................... 4-46
Plasma Parameters .............................................................. 4-46
Organic Setting Instrument Parameters .................................... 4-47
Plasma Parameters .............................................................. 4-47
High Dissolved Solids Setting Instrument Parameters ............. 4-48
Plasma Parameters .............................................................. 4-48
Torch Positions ................................................................... 4-48
Important Considerations for Dual Viewing ............................ 4-49
Shipping List ................................................................................... 4-51

Chapter 5. Maintenance ...................................................... 5-3

Daily Checks ..................................................................................... 5-4
Exterior of Instrument Cleaning ................................................. 5-4
Daily Cleaning ............................................................................ 5-4
Argon Supply .............................................................................. 5-5
Purge Gas Supply ........................................................................ 5-5
Shear Gas Supply ........................................................................ 5-5
RF Coil Cooling Gas ................................................................... 5-6
Chiller ......................................................................................... 5-6
Vent ............................................................................................. 5-6
Torch and RF Coil ...................................................................... 5-6
Nebulizer ..................................................................................... 5-7
Peristaltic Pump and Drain ......................................................... 5-7
Periodic Checks ................................................................................ 5-7
Torch Assembly and RF Coil ..................................................... 5-8
Purge Viewing Window/Tubes .................................................. 5-8
Nebulizer ..................................................................................... 5-8
Spray Chamber .......................................................................... 5-8
Peristaltic Pump .......................................................................... 5-9
Drains .......................................................................................... 5-9
General System Maintenance ..................................................... 5-9
Wavelength Calibration .............................................................. 5-9
Torch Viewing Position Alignment .......................................... 5-10
Performance Checks ................................................................ 5-10
Cleaning the Sample Introduction System ................................ 5-10
viii Contents

Quick-Change Torch Module for the Optima 5000 Series DV ...... 5-12
Plasma Torch ............................................................................ 5-12
RF Coil ..................................................................................... 5-13
Removing the Scott Spray Chamber for
the Optima 5000 Series DV .................................................... 5-13
Removing the Injector .............................................................. 5-16
Removing and Disassembling the Torch .................................. 5-16
Cleaning the Torch .................................................................... 5-19
Cleaning the Spray Chamber .................................................... 5-21
Replacing the Torch .................................................................. 5-21
Replacing the Torch on the Mount ........................................... 5-26
Replacing the Spray Chamber ................................................. 5-29
Connecting the Nebulizer (NEB) Tubing ................................. 5-30
Torch Module for the Optima 5300V ............................................. 5-32
Plasma Torch ............................................................................ 5-32
Installing the Torch Module for the Optima 5300V ....................... 5-33
Installing the Torch Module Assembly .................................... 5-34
Removing the Torch Module Assembly ................................... 5-37
Cyclonic Spray Chamber for the Optima 5300V ............................ 5-38
Installing the Cyclonic Spray Chamber .................................... 5-39
Removing the Cyclonic Spray Chamber .................................. 5-43
RF Coil ...................................................................................... 5-43
Replacing the RF Coil ............................................................... 5-43
Purge Window/Tubes ..................................................................... 5-47
Removing and Cleaning the Purge Windows ........................... 5-47
Cleaning the Purge Windows ................................................... 5-47
Removing the Radial Purge Window Tube .............................. 5-48
Replacing the Radial Purge Window Tube ............................... 5-51
Removing the Axial Purge Window ......................................... 5-51
Removing the Purge Window for the Optima 5300V .............. 5-54
Removing the Ceramic Purge Window Holder for the Optima
5300V ........................................................................................ 5-56
Adjusting the Position of the Shear Gas Nozzle ............................. 5-57
Scott-Type Spray Chamber ............................................................ 5-60
Removing the Spray Chamber .................................................. 5-60
Removing the End Cap from the Spray Chamber .................... 5-60
 Contents ix

Cleaning the Scott-Type Spray Chamber ................................. 5-61

Cyclonic Spray Chamber for the Optima 5100, 5200 and 5300 DV .. 5-
62
Installing the Cyclonic Spray Chamber .................................... 5-62
Etching the Cyclonic Spray Chamber ....................................... 5-65
Cleaning the Cyclonic Spray Chamber ..................................... 5-66
Nebulizers ....................................................................................... 5-67
GemTip Cross-Flow Nebulizer ....................................................... 5-69
Removing the Nebulizer/End Cap ............................................ 5-69
Checking the Spray Pattern ....................................................... 5-70
Disassembling the Cross-Flow Nebulizer ................................ 5-71
Replacing the Nebulizer/End Cap ............................................. 5-80
GemCone Nebulizer ....................................................................... 5-81
Daily Cleaning of the Low-Flow GemCone Nebulizer ............ 5-81
Daily Cleaning of the High Solids GemCone Nebulizer .......... 5-81
Installing the GemCone Nebulizer on the Scott-Type Spray
Chamber .................................................................................... 5-82
Installing the GemCone Nebulizer on
the Cyclonic Spray Chamber ................................................... 5-83
Cleaning the GemCone Nebulizer ............................................ 5-84
GemCone Liquid Fitting Maintenance ..................................... 5-85
Installing the GemCone Nebulizer on the Cyclonic Spray Chamber
on the Optima 5300V ................................................................ 5-85
Cleaning the GemCone Nebulizer ........................................... 5-86
GemCone Liquid Fitting Maintenance ..................................... 5-87
Concentric Glass Nebulizer ........................................................... 5-87
Installing the Concentric Nebulizer .......................................... 5-87
Installing the Concentric Glass Nebulizer into
the Cyclonic Spray Chamber .................................................. 5-89
Cleaning Concentric Glass Nebulizer and
Cyclonic Spray Chamber ........................................................ 5-90
Cleaning the Concentric Glass Nebulizer ................................. 5-90
Mira Mist Nebulizer ........................................................................ 5-91
Sample Capillary Tubing .......................................................... 5-92
Gas Line .................................................................................... 5-92
Sample Introduction / Maximizing Stability ............................ 5-92
x Contents

Cleaning the Nebulizer ............................................................. 5-93

Peristaltic Pump .............................................................................. 5-93
Replacement Pump Tubing ....................................................... 5-93
Installing the Sample and Drain Tubing ................................... 5-94
Adjusting the Pump Tubing .................................................... 5-100
Cleaning the Pump .................................................................. 5-102
Drain ....................................................................................... 5-102
General System Maintenance ....................................................... 5-104
Cleaning the Instrument .......................................................... 5-104
Air Filters ............................................................................... 5-104
Changing the RF Generator Air Filter .................................... 5-104
Changing the Spectrometer Air Filter ..................................... 5-105
Fuses ....................................................................................... 5-106
Replacement Parts: General .................................................... 5-106

Chapter 6. Troubleshooting ................................................ 6-3

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 ............................... 6-9
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 6-20
Troubleshooting Form .............................................................. 6-20
General: ..................................................................................... 6-20
Sample Introduction Configuration: ......................................... 6-20
Operating Conditions: ............................................................... 6-20
Instrument Environment: .......................................................... 6-20
Troubleshooting Tasks Performed: ........................................... 6-21
Common Setup Problems: ........................................................ 6-21
 Contents xi

Chapter 7. Error Messages ................................................. 7-3

System Error (SYSERROR) Messages for Spectrometer ................ 7-4
Spectrometer Error Messages ........................................................... 7-5
System Error (SYSERROR) Messages for RF Generator .............. 7-25

Index .......................................................................................I-1
xii Contents
 Customer Service xiii

Customer Service
Company Name and Address:

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

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

PerkinElmer using the eight-digit part numbers provided in this manual. To place
an order for supplies and many replacement parts, request a free catalog, or ask for
information visit our website. Internet: www.perkinelmer.com

The most up-to-date information on part numbers, product brochures, spare parts
and application notes are located in the PerkinElmer website.

e-ssentials catalog service offers a full selection of high quality atomic

spectroscopy supplies. To place an order, request a free catalog, or ask for
information:

• If you are located within the U.S., call toll-free: (800) 762-4000, Monday -
Friday, 8:30 a.m. to 7 p.m. EST. Your order will be shipped promptly, usually
within 24 hours.

• If you are located outside the U.S., call your PerkinElmer sales office.
xiv

Safety and Regulatory Information

Safety Information in the Manual

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

Caution The protection provided by this equipment may be impaired if

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

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

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

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

In this manual, the following graphic symbols and special text formats are used to
set apart important safety information.

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.
 Safety and Regulatory Information xv

FCC Compliance (United States)

This product is classified as Industrial, Scientific and Medical (ISM) equipment
and has been tested and found to comply with the limits specified for non-consumer
equipment, pursuant to Part 18 of the FCC Rules.

These limits are designed to provide reasonable protection against harmful

interference in a non-residential installation.This equipment generates, uses, and
can radiate radio frequency energy and, if not installed and used in accordance with
the instructions, may cause harmful interference to radio communications.
However, there is no guarantee that interference will not occur in a particular
installation.

If this equipment does cause harmful interference to radio or television reception,

which, can be determined by turning the equipment on and off, the user is
encouraged to try to correct the interference by one or more of the following
measures:

• reorient or relocate the receiving antenna

• increase the separation between the equipment and the receiver

• connect the equipment into an outlet on a circuit different from that to

which the receiver is connected

• consult the dealer or an experienced RFI technician for assistance.

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

Environment
Operating Conditions

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

Pollution Degree

This equipment will operate safely in environments that contain non-conductive

foreign matter up to Pollution Degree 2 in EN/IEC 61010–1.
Recommended operating conditions:
• Indoors.
• The location must be free of smoke, dust, corrosive fumes, direct sunlight
and excessive vibration.
• Temperature +15 °C to +35 °C (+59 °F to +95 °F) with a maximum rate of
change of 2.8 °C (5 °F) per hour. For optimum instrument performance, the
room temperature should be controlled at 20° ± 2 °C. For optimum
instrument performance, the relative humidity should be between 35% and
50%.
• Relative humidity 20% to 80%, without condensation.
• Altitude in the range 0 m to 2,000 m (sea level to 6,562 feet) with a
maximum rate of change of 2.8 °C (5 °F) per hour. For optimum instrument
performance, the room temperature should be controlled at 20° ± 2 °C. For
optimum instrument performance, the room temperature should be
controlled at 20° ± 2 °C. For optimum instrument performance, the relative
humidity should be between 35% and 50%.

Safe operating conditions:

• Indoors
• Temperature +5 °C to +40 °C (+41 °F to +104 °F).
• Relative humidity 20% to 80%, without condensation.
• Altitude in the range 0 m to 2,000 m (sea level to 6,562 feet).
 Safety and Regulatory Information xvii

Storage conditions:
• Ambient temperature –20 °C to +60 °C (–4 °F to +140 °F).
• Relative humidity 20% to 80%, without condensation.
• Altitude in the range 0 m to 12,000 m (sea level to 39,370 feet).

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.

Symbols Used on the Instrument

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

This symbol indicates Caution, risk of electric shock.

AVERTISSEMENT: Risque de choc électrique.

This symbol indicates Caution, risk of danger.

Documentation must be consulted to determine the nature of the
potential hazard and any actions which have to be taken.
! AVERTISSEMENT: Risque de Danger: Réfère à la documentation
de déterminer la nature de l’hasard potentiel et aucunes actions qui
sont nécessaire de le réparer.

This symbol indicates Caution, hot surface.

AVERTISSEMENT: La surface est chaude.

xviii

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.

 Safety and Regulatory Information xix

Warning Labels on the Instrument

Safety Labels on the Front of the Instrument
The warning labels shown below appear in the locations described in the following
table and shown in Figure A. For more information on the Emergency Off Switch
see page 3-37 in this Hardware Guide.

Location of
Instructions for Safety
Warning Warning Label Hazard

On the front of the UV Radiation. Risk of eye Do not gaze into the
instrument above damage. The plasma may emitted light. Always wear
the Emergency emit UV radiation which can UV-absorbing safety
! Off Switch (Label damage your eyes. glasses when looking at the
#1 on Figure A) light from the plasma.
Rayonnement UV. Risque de
blessure des yeux. La plasma
peut émettre des UV qui peut
blesser les yeux. Ne regardez
pas fixement à la lumière
emis. Tourjours porter des
lunettes de protection
absorbant les UV pour
regarder le plasma.

On the front of the Hot gases are vented through Avoid this area of the
chimney (Label the chimney into the venting instrument when the
#2 on Figure A). system. plasma is on.
!
Les gaz chauds passent par la
cheminée dans l’installation
de ventilation.

The plasma generates high Do not view the plasma

intensity ultraviolet through the chimney.
radiation.

Le plasma crée des rayons

ultraviolets a haute intensité.
xx

1 2

Figure A. Warning labels located on front of the instrument.

 Safety and Regulatory Information xxi

Safety Labels on the Side of the Instrument

The warning label shown below appears on the side of the instrument (right hand
panel) in the locations indicated in Figure B (see label 1 on Figure B).

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

Location of Instructions for

Warning Warning Label Hazard Safety

Located beneath Proper gas Translations for the

the shear gas hook- instrument hook- word "air" in many
! ups (Label #2 on
Figure B).
ups. languages. See the
table on page xxii
for the translations.

The label (shown above) appears next to the Shear Gas Supply and the Coolant
connections label as shown in Figure B below (see label 2 on Figure B). The word
"air" is translated into many languages. The shear gas is typically compressed air;
however, nitrogen may also be used. The flow rate for the shear gas supply is
approximately 18 L/min (0.65 cubic feet/min) at a minimum of 550 kPa (80 psig).
xxii

Additional Label: The following label is located on the power line cord (see label
3 on Figure B):

SAFETY CODES REQUIRE

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

2
1
3

Figure B. Location of warning labels on the right hand panel of the instrument
and the power cord.
 Safety and Regulatory Information xxiii

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 ΑΕPΑΣ ΕΙΣΟΔΟΣ ΕΞΟΔΟΣ

Italian Aria Ingresso Uscita

Dutch Lucht In Uit

Norwegian Luft Inngang Avløp

Portuguese Ar Entrada Salída

Spanish Aire Entrada Salida

Swedish Luft In Ut
xxiv

Safety Labels on the Back of the Instrument

3 4
1 2

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).

CAUTION:
This unit contains protective circuitry.
! Contact PerkinElmer qualified personnel
before performing any AC line tests.
Attention: Cet appareil continent un circuit
protecteur. Contact le personnel qualifié de
PerkinElmer d’effectuer un quelconque
controle de circuit en courant alternatif.
 Safety and Regulatory Information xxv

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.
xxvi

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

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

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 filters.

To remove, slide filter

in this direction.

RF Generator Filter
Spectrometer Filter (Mesh side out)
(In front of fan)

Figure D. Location of the spectrometer and RF generator air filter on the

instrument.
 Safety and Regulatory Information xxvii

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.

Safety Labels in the Sample Compartment

Optima 5100DV, 5200DV, 5300DV

Front of Instrument
xxviii

Optima 5300V

DEFEAT IN TERLOCKS
WARNING - DO NOT

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

 Safety and Regulatory Information xxix

The warning labels shown below appears 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 La surface est the instrument
below the shear gas chaude. when the plasma is
assembly on the on.
transfer optics
radial snout. (Label
#2 on Figure B)
xxx

Safety Label in the Spray Chamber Compartment for the

Optima 5100DV, 5200DV and 5300DV

Instrument
Left Side
!
Spray Chamber Clip

The warning label shown below appears in the spray chamber compartment (see
the following page for the safety label).
 Using this Guide xxxi

WARNING – The spray chamber must

not be removed from the instrument
! during plasma operation.
Never view the plasma with the naked
eye. Damage to eyes will occur.

AVERTISSEMENT: Ne pas retirer la cab-

ine de pulvérisation de l’instrument pen-
dant le travail au plasma. Ne jamais
regarder le plasma a l’oeil nu, cela endom-
magerait l’oeil.

Using this Guide

This manual is your hardware guide to the Optima 5000 Series instrument. Main
topics include:
• safety practices
• a description of the system
• installation
• maintenance
• troubleshooting

Documents to Help You

This manual contains hardware information for Optima 5000 Series instruments.
The following documentation is also provided for Optima 5000 Series instruments.

• 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.
xxxii

How this Guide is Organized

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

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

1 Safety Practices Important safety information.

2 Preparing Your Laboratory The preparation of your laboratory
needed for the Optima 5000 series.
Environmental, electrical, space,
exhaust, gases, and cooling water
requirements are reviewed.
3 System Description The components of the instrument, how
the echelle 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.
 How this Guide is Organized xxxiii

Using the Index

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

• installation

• maintenance

• troubleshooting

A Word on Troubleshooting
We recommend that you consult the troubleshooting information included in this
manual before you call a PerkinElmer service engineer. The Troubleshooting
chapter contains suggestions to help you determine systematically whether
instrument problems are due to improper analytical techniques, improper selection
of instrument parameters, or malfunction of the instrument.
xxxiv
Chapter 1
 Safety Practices 1
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.

Laboratory Guidelines
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).

General
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.
1-4 Safety Practices

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.

Environmental Conditions
The instrument should be used indoors in a laboratory having the environmental
conditions as recommended in the Preparing Your Laboratory chapter
(Chapter 2).

This instrument is not designed for operation in an explosive

! environment.
Warning

Handling of the Instrument

Contact a PerkinElmer service engineer for assistance in installing or
evaluating the system after moving. The Optima 5000 weighs 193 kg (425
pounds), or 238 kg (525 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. Combustion products vary with the
type of sample analyzed. If the sample compartment door is opened, a maximum
of 0.9 liters of Argon may escape during the first minute. After that, 0.1 liters/
minute of Argon will continue to escape while the door is open.
 Instrument Safety Practices 1-5

An exhaust venting system is always required to remove those gases which are
generated during the normal operation of the instrument.

An efficient ventilation system must be provided for the instrument. Detailed

specifications for a recommended venting system are described in the section titled
Exhaust Vent Requirements in Preparing Your Laboratory (Chapter 2).

Instrument Safety Practices

This section describes potential hazards and recommended safety practices. You
should thoroughly review this information.

This equipment requires no specified inspection or preventive maintenance

to ensure the continuous functioning of its safety features.

Caution The protection provided by this equipment may be impaired if

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

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.

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.
1-6 Safety Practices

• Quick change torch must be installed.

• The shear gas must be flowing.

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

Electrical Safety
The instrument has been designed to protect the operator from potential electrical
hazards. This section describes some recommended electrical safety practices.
 Instrument Safety Practices 1-7

Lethal voltages are present at certain areas within the instrument.

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

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

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

Grounding circuit continuity is vital for safe operation of the

! equipment. Never operate equipment with grounding conductor
disconnected.
Warning

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

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

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.
1-8 Safety Practices

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

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

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

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

When working with the instrument:

• Connect the instrument to a correctly installed line power outlet that has a
protective conductor connection (earth ground).

• Do not operate the instrument with any covers or internal parts removed unless
required to do so.

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

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

in the manuals.

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

• Whenever it is possible that the instrument is no longer electrically safe for use,
make the instrument inoperative and secure it against any unauthorized or
unintentional operation. The electrical safety of the instrument is likely to be
impaired if, for example, the instrument shows visible damage; has been
subjected to prolonged storage under unfavorable conditions; or has been
subjected to severe stress during transportation.
 Instrument Safety Practices 1-9

High Temperatures
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.

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.

• 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.
1-10 Safety Practices

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

Dispose of waste in accordance with the regulations applicable to

! your locality, state, and/or country.
Warning

WEEE Instructions for PerkinElmer Products

A label with a crossed-out wheeled bin symbol and a rectangular bar indicates that
the product is covered by the Waste Electrical and Electronic Equipment (WEEE)
 Instrument Safety Practices 1-11

Directive and is not to be disposed of as unsorted municipal waste. Any products

marked with this symbol must be collected separately, according to the regulatory
guidelines in your area.

The objectives of this program are to preserve, protect and improve the quality of
the environment, protect human health, and utilize natural resources prudently and
rationally. Specific treatment of WEEE is indispensable in order to avoid the
dispersion of pollutants into the recycled material or waste stream. Such treatment
is the most effective means of protecting the customer's environment.

Requirements for waste collection, reuse, recycling, and recovery programs vary
by regulatory authority at your location. Contact your local responsible body (e.g.,
your laboratory manager) or authorized representative for information regarding
applicable disposal regulations. Contact PerkinElmer at the web site listed below
for information specific to PerkinElmer products.

Web address:

http://las.perkinelmer.com/OneSource/Environmental-directives.htm

For Customer Care telephone numbers select Contact us on the web page.

Products from other manufacturers may also form a part of your PerkinElmer
system. These other producers are directly responsible for the collection and
processing of their own waste products under the terms of the WEEE Directive.
Please contact these producers directly before discarding any of their products.

Consult the PerkinElmer web site (above) for producer names and web addresses.

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
1-12 Safety Practices

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.

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.
 Instrument Safety Practices 1-13

• 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 gas-pressure regulators, tubing, and hose connectors approved by an

appropriate regulatory agency.

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

• Do not refill 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.
1-14 Safety Practices

Hazardous Chemicals Warnings

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
Warning surrounding 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)

Responsible body: "Individual or group responsible for the use and maintenance
of equipment, and for ensuring that operators are adequately trained." [per EN/IEC
61010-1].

Operator: "Person operating equipment for its intended purpose." [per EN/IEC
61010-1].
 Instrument Safety Practices 1-15

Safe Use of Chemical Reagents

This section provides some general safety practices that should be observed when
working with any chemicals.

Give careful attention to the hazards associated with the chemical

! reagents being used. Refer to the safety data sheets provided by the
manufacturer, for example, Material Safety Data Sheets (MSDS) in
Warning the USA (for other names, see Reference 5).

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 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.
1-16 Safety Practices

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 1-17

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.
1-18 Safety Practices

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 1-19

• 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.
• Open the apparatus in a fume hood to vent the entrapped fumes safely.
1-20 Safety Practices

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 1-21

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.
1-22 Safety Practices
Chapter 2
 Preparing Your
Laboratory 2
Chapter Overview
The Optima 5000 Series is a complete system, with the exception of the following
items: suitable working area, exhaust vent, gases and regulators, cooling water, and
a computer table or bench. The items shown in the following checklist need to be
considered when preparing the laboratory for the instrument:
• Environmental Conditions
• Exhaust Vent Requirements
• Laboratory Space Requirements
• Cooling Water Requirements
• Electrical Requirements
• Pneumatic Requirements

Preparing the Laboratory

The following sections describe the laboratory requirements in detail for the
Optima 5000 Series.

Environmental Conditions
The laboratory in which the Optima 5000 Series Spectrometer system is located
must meet the following conditions:
2-4 Preparing Your Laboratory

• corrosive-free environment.

• Laboratory temperature between 15 and 35 °C (59 - 95 °F) with a maximum

rate of change of 2.8 °C (5 °F) per hour. For optimum instrument performance,
the room temperature should be controlled at 20° ± 2 °C. The instrument should
be located away from direct sources of heat and cold.

• The heat dissipated directly into the laboratory when the Optima 5000 Series
is properly vented, is approximately 9960 BTU/hour (3000 W). Most of this
heat is removed if the system is properly vented. Additionally, the chiller
dissipates about 3000 watts directly into the room air.

• 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 million 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. Failure to operate the instrument in a
relatively dust-free environment will necessitate more frequent maintenance
and could, eventually, damage the instrument. As a reference, a normal, clean
office environment would be 18 million to 36 million particles per cubic meter.

• Free of excessive vibration.

The Optima 5000 Series has been designed for indoor use. Do not use the
instrument in an area where explosion hazards may exist.

Exhaust Vent Requirements

The Optima 5000 Series has one vent. This exhaust vent for the ICP torch removes
combustion fumes and vapors from the torch compartment.

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.
 Preparing the Laboratory 2-5

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

• It removes dissipated heat produced from the ICP torch and RF 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) at 1500
watts of RF power. To withstand these temperatures stainless-steel tubing must be
used.

ICP torch vent required flow rate is 5660 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-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:

2-6 Preparing Your Laboratory

• Make sure duct casting 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. A
synthetic “smoke” can be generated by placing open bottles of hydrochloric
acid and ammonium in the proximity of the vent opening.

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

Vent Positions
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 the PerkinElmer Venting Kit by contacting your
PerkinElmer sales representative. 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 of 6 m (20 ft.) are also
provided. Figure 2-1 shows the location of the ICP torch exhaust vent.
 Preparing the Laboratory 2-7

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.)

28 cm (11 in.) from instrument

edge to chimney center

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

Laboratory Space Requirements

The Optima 5000 Series system includes the Optima 5000 Series instrument,
PolyScience 6105PE Chiller (or equivalent), a computer, and a printer. The Optima
5000 series 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 89 cm (35 in.).

Optima 5000 Instrument

The Optima instrument is 142-cm wide (56-in.), 80-cm deep (31.5-in.), and 74-cm
high (29-in.). The bottom of the ICP extraction vent must be a minimum of 7.5-cm
(3-in.) from the top of the torch compartment chimney. Figure 2-2 illustrates the
dimensions of the instrument. The Optima 5000 weighs 193 kg (425 pounds), or
270 kg (594 pounds) with the shipping container.
2-8 Preparing Your Laboratory

The Optima 5000 Series may be placed on a bench. A bench is available from
PerkinElmer (Part No. N077-3106).

The main cable length is 2.5 m (8.0 ft.) and the following hoses are supplied:

Argon and nitrogen hoses 2.5 m (8 ft)

Water hoses (2) 6.0 m (20 ft)
*Air hose for shear gas 3.7 m (12 ft)

*The air dryer filter should be located within the 3.7 m (12 ft) length of the air hose.

To provide access for servicing and space for ventilation, allow at least 45 cm (18
in.) of space between the instrument and the laboratory walls. Allow 71 cm (28 in.)
on the right end of the instrument to facilitate access.

80 cm
(31.5 in.)

74 cm
(29 in.)

142 cm
(56 in.)*

* NOTE: 159 cm (63 in.) wide

with the shipping handles.

Figure 2-2. Outside Dimensions of the Optima 5000 series Instrument.

 Preparing the Laboratory 2-9

NOTE: For Optima 5300V, air for the shear gas is not required. Air or nitrogen is
required to the RF load coil.

Computer and Printer

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

PolyScience Chiller
The PolyScience 6106PE Chiller (or equivalent) is usually located on the floor, to
the right side of the instrument. Its dimensions are 36.5-cm (14.4 in.) wide, 67.3-
cm (26.5 in.) deep and 61-cm (24 in.) high. It weighs 80 kg (178 lbs.). The Chiller
has air intakes and exhausts that need to be unobstructed. The power is 2850 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 = 10 feet).

Drain Vessels
A drain vessel (0990-4991) and end cap (N069-0271) are supplied with the Optima
5000 systems. The vessel is made of plastic and used to gather the effluent from the
ICP torch. The drain vessel should be placed on the floor in front of the instrument.
The drain vessel should not be stored in an enclosed storage area. The system
should be checked regularly and replaced when necessary. Should it become
necessary to replace the drain vessel, it should be made from a material not likely
to be attacked by samples being analyzed. Glass or other brittle materials must not
be used.

Location
Typically, the Optima 5000 system is positioned with the computer and printer on
the bench. An optional table for the instrument is also available (N077-3106). The
computer and printer must not be placed on the instrument. The instrument must
be placed under the exhaust vent for the torch compartment and near electrical,
water, and gas supply points. Do not block the main power supply switch because
it functions as the disconnecting device for the instrument’s power.

A water supply is required to dissipate heat from the RF coil, oscillator, and the
detectors.
2-10 Preparing Your Laboratory

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

Cooling Capacity at 20 oC of 2850 watts

Temperature Stability ± 0.5 oC
Pump Rate 4.3 US gal/min. at 60 psi max. Pressure by pass set at 55 psi.

A PolyScience 6106PE Chiller meets these requirements and is recommended for

the instrument. The PolyScience 6106PE Chiller is available through PerkinElmer
in the following two configurations:

208/230V, 60 Hz PE Part No. N077-2026

220/230V, 50 Hz PE Part No. N077-2025

An additional 200-240V line is required for the chiller. A Hubbel No. 4560
receptacle (NEMA L6-15R configuration) is supplied with the chiller. For detailed
information on PolyScience 6106PE Chiller electrical requirements see the
following section, Electrical Requirements.

The PolyScience 6106PE Chiller comes with its own Instruction Manuals. The
headquarters for PolyScience Instruments is located at:

PolyScience Instruments, Inc.

6600 West Touhy Ave
Niles, Il 60714

USA: (800) 229-7569

Worldwide: (847) 647-0611

Fax: (847) 647-1155

 Preparing the Laboratory 2-11

Electrical Requirements
The following sections describe the power requirements for all the components that
make up the Optima 5000 series Spectrometer system.

Optima 5000 Series Instrument

A means of electrically grounding the instrument must be available at

! the customer’s facility.
Warning

The Optima 5000 Series instrument is supplied with a 2.5 m (98 in.) power cable
(Part No. N077-0164) that supplies both the spectrometer and the RF Generator
modules. The Optima 5000 Series requires a 200-240V, 50/60 Hz (± 1%) 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 5000 Series draws 12 Amps at 230V. The maximum power
consumption for the RF generator and the spectrometer is 2800 volt-amperes.

Note The instrument has a typical ground current of 8 mA. The use of a Ground
Fault Circuit Interruptor (GFCI) protected outlet with a trip point near this
value is not recommended.

The Optima 5000 Series 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). Alternative receptacles are Hubbell part No. C320R6W (20A, for US
and Canada) or Hubbell Part No. C316R6S (16 A, for Europe). A conduit box
(Hubbell Part No. SP20301, PerkinElmer Part No. 0994-0914 may also be required
in some regions. Both, a receptacle and a conduit box are shipped with the
instrument (PerkinElmer Part No. N077-0425).
2-12 Preparing Your Laboratory

Note Do not replace the IEC 309 instrument power plug.

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 a ±10% range 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 by the user 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
5000 Series.

PolyScience Chiller
The specific electrical requirements for the PolyScience 6106PE 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 PolyScience 6106PE Chiller 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
 Preparing the Laboratory 2-13

(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 PolyScience 6106PE Chiller 220/240 V, 50 Hz, 15A unit is
supplied with two detachable line cords.

Note NEMA: The National Electrical Manufacturer’s Association

Pneumatic Requirements

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

Argon
Liquid or gaseous argon can be used with the Optima 5000 Series 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 (0.04 - 1.0 cu. ft/min). The argon flow for the system (including the ICP)
may vary between 1 and 25 liters/min.

Caution Gas delivery lines from the argon tank should be contaminant-free and not
made of plastic. Teflon delivery lines are acceptable.
2-14 Preparing Your Laboratory

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

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

Caution Make sure that the required purity of the argon gas is 99.996% pure
otherwise the detector will be damaged.

Table 2-1. Argon and Nitrogen Quality Criteria

Purge Gas
Purging is required. Nitrogen or argon can be used to purge the Optima 5000 Series
spectrometer optics. nitrogen is the recommended purge gas due to its lower cost.
Normal purge gas usage is user selectable at either 1.0 L/min (low purge) or
5 L/min (high purge) for nitrogen (1.4 L/min or 7 L/min if argon is used) at 365
kPA (50 psig) pressure.

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

The purge gas should be 99.999% pure and is available from local suppliers.
 Preparing the Laboratory 2-15

Shear Gas

Caution Do not use Argon for shear gas. Use only air or nitrogen.

Air or nitrogen can be used as the plasma shear gas for the Optima 5000 Series
spectrometer optics.The Optima 5000 Series spectrometer typically consumes the
shear gas at a rate of 25 liters/min. Air or nitrogen is required to the RF load coil.

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

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

The Optima 5000 systems include an air dryer filter assembly. The air hoses are
supplied with 1/4-in. Swagelok fittings and the assembly mounts on the lab wall.
In humid environments, this may not be adequate to ensure that the compressed air
is dry. Additional filters or condensers may be a necessary part of the air supply
system.

Regulator
A pressure regulator for use with either argon or nitrogen is available from
PerkinElmer as Part No. N077-0507. The regulator can be used with CGA 580 or
CGA 590 fittings.

Note The responsible body must ensure that the type of connector used at the
outlet side of the gas-pressure regulator conforms to applicable national
requirements.
2-16 Preparing Your Laboratory
Chapter 3
System Description 3

Figure 3-1. The Optima 5000 Series of Inductively Coupled Plasma Optical
Emission Spectrometers (ICP-OES).

This chapter introduces you to the Optima 5000 Series Inductively Coupled Plasma
Optical Emission Spectrometer (ICP-OES). It includes the following sections.

Optima 5000 Series describes the family of Optima instruments, key instrument
features, and different plasma-viewing configurations.

The next section, Major Components, introduces you to the different modules of
the instrument and is followed by sections on the Spectrometer, RF Generator,
Sample Compartment, and Sample Introduction System.
3-4 System Description

System Initialization and Setup describes the safety interlocks, system initialization
sequences, and includes an overview of hardware control and optimization.

How the Echelle Spectrometer and SCD Work describes the fundamental principles
of the optical system.

In the next two sections, the Indicator Light and Main Switch and Connections to
Electrical, Gas, and Cooling Water Supplies are described.

Specifications contains power requirements, environmental requirements, and

other main specifications.

Optima 5000 Series Instruments

• The Optima 5100 DV, part of the Optima 5000 Series, has an extended UV
wavelength range from 165 to 403 nm.

• The Optima 5200 DV, part of the Optima 5000 Series, has an extended UV
wavelength range from 167 to 403 nm. In addition, the Optima 5200 optical
system has the ability to determine four wavelengths in the visible range (Sr II
at 421.552 nm, Li I at 610.362 nm and 670.784 nm and K I at 766.490 nm)
without having to employ a second detector.

• The Optima 5300 DV, part of the Optima 5000 Series, is a dual detector
systems. The UV detector covers an extended ultraviolet wavelength range
from 165 to 403 nm. The VIS detector covers the visible wavelength range
from 404 to 782 nm.

• The Optima 5300V, part of the Optima 5000 Series, is a dual detector systems.
The UV detector covers an extended ultraviolet wavelength range from 165 to
403 nm. The VIS detector covers the visible wavelength range from 404 to 782
nm. The Optima 5300V includes the vertical torch and radial view only.

Features of the Optima 5000 Series include:

• measurement of spectral background at the same time as the analyte line

• advanced 40 MHz, free-running solid-state RF generator

• easy access to sample compartment and torch assembly

 Optima 5000 Series Instruments 3-5

• ICP WinLab software, based on the familiar Microsoft Windows menus and
graphics, with easy-to-use graphics and familiar pull-down menus

Plasma Viewing Configurations

Dual View (DV) instruments can view the plasma either axially or radially. As
shown in the next two diagrams of the transfer optics on the Dual View instrument,
the torch is positioned horizontally in the sample compartment along the central
axis of the spectrometer optics. Changing from axial to radial viewing is a simple
software command and is accomplished by computer control of a mirror located in
the optical path.

Two toroidal mirrors image the plasma onto the entrance slit. The first mirror is
computer-controlled and allows selection of radial viewing or axial viewing mode.
For axial viewing, light emitted along the axis of the plasma is directed to the
spectrometer optics. For radial viewing, the computer-controlled mirror is rotated
slightly to capture light from the bottom of the plasma and direct it to the
spectrometer optics.

The computer-controlled mirror also adjusts plasma viewing in both the vertical
and horizontal planes.

Radial View (V) instruments use a radially viewed plasma. The torch is
positioned vertically in the sample compartment. Light emitted from the side if the
plasma is directed to the spectrometer optics. This may also be called "lateral" or
"side-on" viewing.

The observation zone of the plasma occurs in the central channel and is in the shape
of a vertical slit.

Two toroidal mirrors image the plasma onto the entrance slit. The first mirror is
computer controlled and can be rotated both vertically and horizontally to adjust
the viewing position.
3-6 System Description

Figure 3-2. Transfer optics on the Dual View instrument shown in Axial viewing
mode.
 Optima 5000 Series Instruments 3-7

Figure 3-3. Transfer optics on the Dual View instrument shown in Radial view-
ing mode.

A flow of shear gas (compressed air or nitrogen) is directed at the plasma to "shear"
off the tip of the plasma discharge. The shear gas minimizes the effects of self-
absorption by forcing cooler atoms from the tip of the plasma out of the optical
path. The shear gas also keeps the purge window cool. The shear gas flow is turned
on automatically when the plasma is ignited.
3-8 System Description

Figure 3-4. Transfer optics shown with the vertical torch.

Figure 3-5. Use of shear gas.

Major Components
The Optima 5000 consists of two major components: the spectrometer and the ICP
Source. For the Optima 5100 and 5200, the detector is a custom, two-dimensional
CCD array. The Optima 5300 consists of two detectors. The plasma source is a
dual-view (can be viewed either axially or radially) RF generator. The plasma
source for the Optima 5300V is radial view only.The sample introduction system
includes a built-in peristaltic pump and a "quick change" removable torch. The
 Optima 5000 Series Instruments 3-9

removable torch includes the nebulizer and spray chamber. The nebulizer and
spray chamber are located outside of the instrument for easy accessibility and to
avoid being heated by the RF generator. The entire sample introduction system is
adjustable from outside the torch box while the RF generator is running. The torch
pneumatics includes a mass flow based nebulizer gas, a closed-loop pressure
restrictor based AUX and plasma gases.

Features of the Optima 5000 include:

• improved analytical performance especially in the low UV spectra

• simultaneous background correction

• solid-state generator for improved reliability

• smaller and lighter bench top instrument when compared to earlier Optima
models.

The Spectrometer and the ICP Source is further divided into the assemblies
described below.

The Spectrometer consists of the following assemblies:

• Optical Tub assembly

(a) the Transfer Optics module
(b) the Input module
(c) the UV Detector module
(d) the VIS Detector module

• Spectrometer Electronics assembly

• Spectrometer Pneumatics assembly

The ICP Source consists of the following assemblies:

• RF Generator and Torch Compartment assemblies

• RF Control Electronics

• Torch Pneumatics assembly

3-10 System Description

In addition, the sample compartment (part of the ICP Source) contains a Quick-
Change Adjustable Torch Module, which can be easily removed in order to replace
the torch. Figure 3-6 shows the major components of the Optima 5000 Series.

Sample Introduction Spectrometer

Compartment with
Quick Change
Torch Module
Torch Compartment

Peristaltic Pump

Figure 3-6. Major components of the Optima 5000 Series instruments.

Spectrometer

Optical System
The Optima 5000 optical design combines an echelle polychromator with a solid-
state detector in an integrated system optimized for ICP-OES. The detector is a
custom, two-dimensional CCD array.The plasma source is a radial view or a dual-
view (can be viewed either axially or radially) RF generator.

The polychromator has an echelle grating designed to use multiple diffraction

orders. To separate the orders and create a two-dimensional diffraction pattern, the
 Spectrometer 3-11

echelle grating is combined with a cross-dispersing element. In the ultraviolet

range, a cross disperser is used. On the Optima 5300, a prism is used in the visible
range.

The Segmented-array, Charge-coupled-device Detector (SCD), patented by

PerkinElmer, is a solid-state imaging device. It provides simultaneous detection
with simultaneous background measurement.

The detector was designed to provide:

• high UV quantum efficiency.

• wide photometric dynamic range.

• random access data readout: subarrays are addressed individually and data is
read out sequentially using CCD (Charge-Coupled Device) transfer
techniques.

• low noise characteristics, including low dark current noise.

The slit width has three different settings: High, Normal, and Low. High resolution
uses the narrowest slit; low resolution uses the widest slit.

The way in which the detector is read varies when different slits are chosen. With
High resolution, each pixel is read as two separate half-pixels. With Normal and
Low resolution, each pixel in the detector subarray is read as a whole.

Optics Housing
The optics are sealed and insulated in a tub-like enclosure. The inside of the
enclosure is temperature-controlled by heating plates to a temperature of 380 C.
The optics are mounted on an optical bench which is mounted (a stress-free
mounting) to the inside of the tub-like enclosure.
3-12 System Description

Insulation Heaters

Optics Bench

Figure 3-7. Thermally regulated optics housing for Dual View only.
 Spectrometer 3-13

Insulation Heaters

Optics Bench

Figure 3-8. Thermally regulated optics housing for vertical (radial) view only.

Nitrogen is used to purge the optical system during operation to remove oxygen
and moisture and keep the environment dry. The nitrogen purge also improves
sensitivity for elements with wavelengths below 190 nm, particularly aluminum at
167 nm.

Detector Cooling and Purging

The detector is housed in an airtight enclosure and cooled to minus 40 0 C to

minimize dark current noise. The cooling system uses a solid-state thermoelectric
cooler with a water-cooled copper heat sink. A temperature sensor on the detector
monitors the temperature of the detector to make sure it is properly cooled. To
detect any water leaks, there is a drain well that is equipped with a sensor. If the
sensor detects that water is collecting, the cooling water is turned off and the
spectrometer automatically shuts down.
3-14 System Description

To avoid condensation on the detector, filtered argon is used to purge the detector
housing. A flow sensor on the argon input line monitors argon flows.

Caution Make sure that the required purity of the argon gas is 99.996% pure
otherwise the detector will be damaged.

ICP Source

RF Generator
The Optima 5000 series instruments use 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 5000 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 3-15

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 3-9. 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.
3-16 System Description

Sample Compartment
The sample compartment has a side door to provide easy access to the sample
introduction module for the Optima 5300V. 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.

Sample Introduction System

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 for the Optima 5300DV. This
module can be quickly removed from the sample compartment. This adjustable
mount allows the torch an adjustment of up to 5 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.The Optima 5300V offers
three slot torches: the standard alumina with 2.0 mm inner diameter, the 2.0 mm
(H.F.), and the 1.2 mm injector (oil).

Spray Chamber
A Ryton, double-pass Scott-type spray chamber and the GemTip Cross-Flow
pneumatic nebulizer are the standard components supplied with the 5300DV
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 spray chamber and Cross-Flow nebulizer or a Cyclonic spray
chamber/Concentric glass (Meinhard) nebulizer. Other combinations will also be
 Sample Introduction System 3-17

available. The 5300V instrument offers the Baffled Cyclonic and the HF resistant
Cyclonic.

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

Nebulizer end cap analysis of strong mineral acids (including
N068-0503 HF) and samples 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
(Conespray) high dissolved solids (up to 20%). Low Flow
Nebulizer GemCone permits lower nebulizer gas flow
High Solids: N069-0670 rates, useful for spectral lines with high
Low Flow: N077-0358 excitation energies and for providing a more
robust plasma. GemCone nebulizers require
an end cap (Part No. N068-0343).
Concentric Glass Provides excellent sensitivity and precision
Nebulizer for aqueous solutions and samples with few
(MEINHARD) dissolved 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
3-18 System Description

MEINHARD Type C Used for samples containing high dissolved

0047-2022 solids (up to 20%).
MEINHARD Type K Optimized for samples that require reduced
N068-1574 nebulizer gas flow rates, such as organic-
based samples.

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

Mira Mist Nebulizer The Mira Mist Nebulizer is recommended

N077-5330 for aqueous solutions. Organics will wet the
nebulizer tip and performance will
deteriorate.

Figure 3-10. GemTip Cross-Flow nebulizer and end cap N068-0503 (also shown
in cross-sectional view).
 Sample Introduction System 3-19

Figure 3-11. GemCone nebulizer and end cap N068-0504 (also shown in cross-
sectional view).
3-20 System Description

Figure 3-12. Concentric glass nebulizer and end cap N068-0504 (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 Compartment Heater (optional)

The nebulizer compartment 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 compartment 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 compartment heater temperature can be controlled via the software and
the spray chamber door must be closed for the heater to work properly. The heater
 Sample Introduction System 3-21

should always be on for inorganic analyses. The nebulizer compartment heater is

not available for the 5300V.

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 compartment
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 S10 Autosampler is available for automated sample handling.
This autosampler, available from PerkinElmer, will work with the Optima 5000
series. This autosampler consist of a sample table, a sample tray, and a motorized
sampling arm with an attached probe. Three sample trays are available covering a
variety of sample volume and total sample capacity requirements (see the
following table). All sample trays have one location for a wash vessel. See the S10
Autosampler User’s Guide (Part No. 0993-6788) for detailed information on
installing the autosampler.
3-22 System Description

S10 Sample Trays Number of Locations

Sample Tray E 200 total locations / 1 rinse locations

Sample Tray F 157 total locations / 1 rinse locations
Sample Tray G 62 sample locations / 1 rinse locations
Sample Tray H 140 sample locations / 1 rinse locations

System Initialization and Setup

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 must be connected.
• Emergency Plasma Off switch on front of instrument must be released.
Initialization Steps
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.
 How the Echelle Spectrometer and SCD Work 3-23

The spectrometer initialization is completed when the spectrometer sends a

"system ready" message to the computer.
Hardware Setup and Optimization
The following hardware settings are controlled by the software.
• RF Power: Power levels can be adjusted in 1-watt increments (range 750 to
1500 watts).
• 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 (range 0.0 to 20.0 L/min). Auxiliary argon is
adjustable in 0.1 L/min increments (range 0.0 to 2.0 L/min).
• Nebulizer argon flow rate: The flow rate is automatically controlled using a
mass flow controller in 0.01 L/min increments (range 0.0 to 2.0 L/min).
• 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
(range 0.0 to 5.0 L/min).
• Nitrogen purge rate: A high or normal flow rate can be specified. 1.0 L/min
(low purge) or 5.0 L/min (high purge).
• 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.

How the Echelle Spectrometer and SCD Work

Introduction
The Optima 5000 series optical design combines an echelle polychromator with a
solid-state detector in an integrated system optimized for ICP-OES. The echelle
polychromator produces a compact two-dimensional spectrum that is focused onto
the solid-state detector. The Segmented-array Charged-coupled device Detector
3-24 System Description

(SCD) simultaneously measures emission lines for the analytes and the spectral
background. On the silicon surface of the detector is a collection of linear detector
segments strategically located to measure the most important ICP emission lines.
Random access to data for individual emission lines ensures rapid analysis.

Depending on the instrument model, one or two detectors (SCDs) are used to cover
the wavelength range as follows:

• The Optima 5100 has one detector that covers an extended UV wavelength
range from 165 to 403 nm.

• The Optima 5200 has one detector that covers an extended UV wavelength
range from 165 to 403 nm and selected parts of the visible region (Sr II at
421.552 nm, Li I at 610.362 nm and 670.784 nm and K I at 766.490 nm).

• The Optima 5300 is a dual detector system. The UV detector covers an

extended ultraviolet wavelength range from 165 to 403 nm. The VIS detector
covers the visible wavelength range from 404 to 782 nm.

• The Optima 5300V, part of the Optima 5000 series, are dual detector systems.
The UV detector covers an extended ultraviolet wavelength range from 165 to
403 nm. The VIS detector covers the visible wavelength range from 404 to 782
nm. The Optima 5300V includes the vertical torch and radial view only.
Schematic representations of the optical systems for the Optima 5100DV, Optima
5200DV, Optima 5300DV and Optima 5300V instruments are shown in the next
four figures.
 How the Echelle Spectrometer and SCD Work 3-25

Figure 3-13. Schematic diagram of the Optima 5100 DV optical system.

3-26 System Description

UV Cutoff
Filter

Figure 3-14. Schematic diagram of the Optima 5200 DV optical system.

 How the Echelle Spectrometer and SCD Work 3-27

Figure 3-15. Schematic diagram of the Optima 5300 DV optical system.

3-28 System Description

Figure 3-16. Schematic diagram of the Optima 5300V optical system

The optical system consists of the transfer optics, input module, and UV module.
A Visible module is included on dual detector models, the Optima 5300DV and
Optima 5300V.
 How the Echelle Spectrometer and SCD Work 3-29

Transfer Optics
The torch emission is directed to the entrance slit by the transfer optics. A
computer-controlled toroidal mirror can be rotated both vertically and horizontally.
This computer-controlled movement allows the user to adjust the viewing height
and the viewing position. For more information on the transfer optics, see the
diagrams for radial and axial view, earlier in this chapter.

An automatic shutter mechanism (not shown in optical diagrams) minimizes the

UV exposure on the first mirror thus extending its useful lifetime. The shutter
mechanism also includes a mercury pen lamp. This pen lamp can be used to check
the wavelength calibration of the system.

Input Module
The input module consists of three components: the computer-controlled slit
mechanism, the parabolic collimator mirror and the echelle grating. The slit
mechanism contains three slit openings: the “High Resolution” slit, the “Normal
Resolution” slit, and the “Low” (High Energy) slit. After the light from the plasma
passes through the slit, it is collimated by the parabolic mirror and sent to the
echelle grating.

The echelle grating is a coarse grating with a ruling density of 79 lines/mm. It is

precisely ruled with broad flat grooves. The width of each groove is twice the
height. Because of this groove shape, this grating is often compared to a series of
steps, with diffraction occurring off the steep side of the steps. This produces
multiple, overlapping diffraction orders with very good efficiency in each of the
orders. By contrast, non-echelle-based spectrometers use an echellette grating,
which has a high ruling density. The echelle grating is optimized through the blaze
angle to have a maximum efficiency in one of its lower orders.
3-30 System Description

a b Diffracted
Ray

Incident
Incident Ray
and Diffracted
Rays

Figure 3-17. Echelle grating (a) and Echellette grating (b)

Another advantage of the echelle grating is that it has high dispersion
characteristics since it is used in the higher diffraction orders. This means that the
system has excellent resolution with a relatively short focal length. Also, since
multiple orders are used (higher orders in the UV and lower orders in the visible),
the resolution also changes as a function of wavelength (see figure below). Note
that the VIS detector is only used on dual detector models, the Optima 5300DV and
Optima 5300V.

0.03
Bandwidth FWHM (nm)

0.025

0.02

0.015

0.01

0.005

0
190 240 290 340 390 440 490 540 590
Wavelength

UV Detector VIS Detector

Figure 3-18. Comparison showing resolution for a sampling of data points at

different wavelengths.
 How the Echelle Spectrometer and SCD Work 3-31

UV Module
The UV module consists of a cross disperser, a camera sphere, a fold flat mirror, a
field flattener, and the detector module. On Optima 5100, and 5300 models, the
overlapping orders from the echelle grating are sent to a Schmidt cross disperser.
On Optima 5200 models, a patented PerkinElmer Cross Disperser is used.

Schmidt Cross Disperser (Optima 5100, and 5300 models)

The Schmidt Cross Disperser serves three purposes in the optical system. First, the
Schmidt cross disperser separates the light into the visible and UV channels. Light
reflecting off the surface of the Schmidt Cross Disperser is sent to the UV detector.
Light passing through the opening in the center of the optic becomes the visible
channel. On the dual detector model, the Optima 5300, the visible light is directed
to a VIS detector.

Second, the front surface of the Schmidt Cross Disperser is a coarse grating with a
ruling density of 374 lines/mm. This separates or “cross disperses” the overlapping
orders into the two-dimensional echelle pattern or echellogram (see figure below).
By using a grating instead of a prism for the cross disperser, optical throughput in
the UV is enhanced.
3-32 System Description

Diffraction Orders

782 nm

High
Dispersion

167 nm

Figure 3-19. Schematic representation of an echellogram.

Third, the surface of the Schmidt Cross Disperser has a small waveform on it. This
waveform corrects for the spherical aberrations generated by the camera sphere
mirror. By correcting for these spherical aberrations, the UV channel has excellent
optical throughput (f/2.5) and excellent resolution (0.006 nm at 200 nm). Without
this correction, the system would sacrifice either throughput or resolution.

Dual Density Cross Disperser (Optima 5200 model only)

The patented PerkinElmer Dual Density Cross Disperser is a grating that is ruled
with two different line densities. A computer-controlled mechanism allows
selection of either the UV or VIS region of the grating. In addition, Schmidt
correction is incorporated into the surface of the grating to eliminate spherical
aberration of the camera sphere.
 How the Echelle Spectrometer and SCD Work 3-33

Fold Flat Mirror (Optima 5100, 5200 and 5300 models)

The fold flat mirror deflects the UV light onto the detector. The fold flat mirror size
matches the size of the opening in the Schmidt Cross Disperser. Thus, the mirror
does not impact the optical throughput of the system. The field flattener is a lens
that provides good focus for the entire wavelength range on the UV detector.

Visible Module (5300 model only)

The VIS module is used on dual detector models, the Optima 5300. The
overlapping orders from the echelle grating are passed through the opening in the
Schmidt Cross Disperser to the visible prism. This prism separates the overlapping
orders into discrete orders. A two-dimensional pattern or echellogram is produced.
A compound lens directs the beam onto the solid-state detector for the visible
range.

Segmented-array Charge-coupled-device Detector (SCD)

The detector is a silicon chip with a surface area of 13 mm by 19 mm. On its
surface, the chip has a series of linear subarrays comprised of pixels. The pixels are
photosensitive areas of silicon that have an aspect ratio of approximately eight to
one. This aspect ratio matches the slit geometry of the instrument and ensures
excellent optical throughput. Also, unlike other charge-transfer device detectors,
the pixels have no UV-absorbing polysilicon electrodes over the detector surface.
Thus the quantum efficiency of the SCD is very good throughout the entire
wavelength range of the instrument.
3-34 System Description

Figure 3-20. Segmented-array Charge-coupled-device Detector (SCD).

The linear subarrays are positioned on the detector at x-y locations that correspond
to the locations of the desired emission lines generated by the echelle spectrometer.

The figure below shows a representation of the echelle pattern on the detector. The
diffraction orders are positioned along the x-axis and the emission lines are
positioned along the y-axis. The emission lines are detected by means of their
location on the chip.
 How the Echelle Spectrometer and SCD Work 3-35

Figure 3-21. Representation of echelle pattern on the detector (every tenth or-
der).

Each linear subarray contains from 8 to 40 pixels. Each pixel is 25µm wide and
approximately 100μm in height. The height of the pixels varies based on its
position on the detector and the width of the echelle order at that position. The
emission line for the analyte of interest falls on the subarray along with the spectral
information on each side of the peak. Thus the analyte peak and the spectral
background are measured simultaneously.

Electronic Processing of the Signal

On the Optima 5100 the detector consists of 182 subarrays. On the Optima 5200
the detector consists of 186 subarrays. On the Optima 5300 the detector consists of
235 subarrays. The number of subarrays that are used depends on the wavelength
range of the instrument. The subarray consists of three areas, the photosensitive
area, the storage register and the output register (see the next figure). Surrounding
this subarray is a “guard band” that prevents excessive charge from blooming onto
any other subarray. Next to each subarray are the output electronics and the
3-36 System Description

interface logic. Since the output electronics are next to the output register, the
capacitance is extremely small and thus the readout noise is very low (~13
electrons RMS). Since each subarray has its own interface logic, it can be
addressed and read out individually. All the address lines, output electronics, and
interface logic are covered by an opaque mask to block unwanted radiation.

Clock Lines
Interface Control Lines
Photosensitive Register
Logic
Address Lines

Storage Register
Output
Electronics

Guard
Band

Figure 3-22. Detector subarray pattern.

The next figure shows a cross-section of the detector. Photons strike the
photosensitive register and are immediately converted to photoelectrons. These
photoelectrons are pulled away from the surface and moved into the storage
register where they are stored as an electrical charge. The integration time is the
length of time that these photoelectrons are allowed to accumulate in the storage
register. When the integration is complete, the charge in the storage register is
transferred into the output register by a change in the electrical potential. The
charge in the output register is serially moved to the output electronics where it is
amplified and sent to the signal processing electronics.
 Indicator Light 3-37

Photons

- -
-
-

Photosensitive Storage Output

Register Register Register

Figure 3-23. Storage of photoelectrons during integration.

Indicator Light
The Optima 5000 series 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.)

Figure 3-24. Location of Red Emergency Plasma Off Switch.

3-38 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.

Note Shear Gas is not used for the Optima 5300V. Air or nitrogen is required to
cool the RF coil for the Optima 5300V.

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

Electrical (right side of Power cable Instrument to 200-

Connections instrument as viewed (attached to 240 VAC, 16 amp
from the front of the instrument) IEC-309 connector
instrument) outlet
Ethernet connection Ethernet cable Instrument to
(on left side of computer
instrument as viewed
from the front of the
instrument)
Gas Connections N2 Supply Nitrogen hose Nitrogen inlet to
N069-0275 nitrogen supply
Shear Gas Supply Air hose Require a supply of
0077-0348 air (typically) or
included with nitrogen for the
Air Dryer Filter shear gas.
and regulator
assembly
Ar Supply Argon hose Argon inlet to argon
N069-0274 supply
 Connections to Electrical, Gas, and Cooling Water Supplies 3-39

Cooling Water H2O IN Tubing Chiller or cooling

Connections (Red Tie Wrap) N077-0341 water supply
(spectrometer side
of instrument)
H2O OUT Tubing Chiller or cooling
(White Tie Wrap) N077-0342 water return
3-40 System Description

Customer Interface
Connections
Gas Connections
Shear Gas Supply
Ar Supply N2 Supply

Coolant IN
Coolant OUT (Red Tie Wrap)
(White Tie Wrap)

Power
Switch

Instrument to
200-240 VAC
16 AMP
IEC-309 Outlet

PolyScience 6106PE
Chiller

Line Cord Plug

Figure 3-25. Electrical, gas, and cooling water connections on the right side of
the instrument (as viewed from the front of the instrument).
 Connections to Electrical, Gas, and Cooling Water Supplies 3-41

TRIGGER
IN

ETHERNET

28 VDC MAX
100 mA @
RLY1

RLY2

CUSTOMER
INTERFACE

Figure 3-26. Remote chiller connections on the left side of the instrument (as
viewed from the front of the instrument).
3-42 System Description

Specifications

ICP System Specifications

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 requirements for RF emission.

Coil: 2-turn 3/16-in.copper 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
(PolyScience 6106PE 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 1.0 liter/minute
increments.The flow system is interlocked to prevent ignition without plasma gas
flowing.
 Specifications 3-43

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 0.00 and 2.00 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. The Optima 5100 DV, Optima 5200DV and Optima
5300DV require shear gas.

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 5.0 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.
3-44 System Description

User Plasma Viewing: The full plasma is viewed through a UV-blocking, low-
transmittance window located in the sample compartment door.
Spectrometer
Polychromator: The high energy (f/6.7) echelle-based polychromator is a
PerkinElmer design. The resolution of the system is 0.006 nm at 200 nm. The 80
by 160 mm echelle grating (manufactured by PerkinElmer) has 79 lines per mm
and a blaze angle of 63.4 degrees. On the Optima 5100 and 5300, the cross
disperser for the UV region is a grating (374 lines/mm) with Schmidt correction
incorporated into its surface. The Schmidt correction performs aberration
correction for the 400 mm radius camera sphere. On the Optima 5200, a patented
PerkinElmer Dual Density Cross Disperser grating (374 and 187 lines/mm) is used
(U.S. Patent No. 5,565,983) with Schmidt correction incorporated into its surface.
The cross disperser for the visible region on dual detector model, Optima 5300, is
a 60-degree prism.
The entire optical system is enclosed in a purged and thermostated optical
enclosure.
Thermostating: The polychromator is thermostated to 38 °C. The thermostating
includes the transfer optics along with the polychromator.
Plasma Viewing: The Optima 5000 series offers Dual View (U.S. Patent No.
5,483,337). The viewing position can be optimized by the software with all
configurations.

Shutter and Mercury Recalibration System: The computer-controlled

pneumatically operated shutter automatically opens and closes for each sample. By
closing the shutter between each sample, the first transfer mirror is protected from
long exposures to the intense UV radiation of the plasma thus extending the useful
lifetime of the mirror. A mercury lamp is built into the entrance shutter mechanism
and can be viewed when the shutter is closed to monitor the mercury emission line
at 253 nm and automatically update the system wavelength calibration. Frequency
of the automatic recalibration is user selectable between 0 and 1000 minutes and
can be varied during an autosampler analysis.
Detector: The patented PerkinElmer Segmented-array Charge-coupled-device

Detector (SCD) (U.S. Patent No. 4,820,048).

Electronics: Correlated double sampling data acquisition electronics reduce
electronic noise.
Chapter 4
 Installation 4
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:

• Installation Summary

• Moving the Instrument

• Connecting the Gases and Cooling Water

• Connecting the System Components

• Installing the Quick-Change Adjustable Torch Module

• Installing the Torch Module for the Optima 5300V

• Installing the Autosampler and Printer

• Instrument Start-up

• Automatically Aligning the Torch Viewing Position

• Shipping List
4-4 Installation

Installation Summary
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 the Torch Module for the Optima 5300V

• 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

Caution If moving the Optima 5000 series 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.
 Connecting the Gases and Cooling Water 4-5

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

• Remove the 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. 0993-6391).

• 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 torch module, the chiller, any accessories,
gas and water lines, the computer and the printer; see the procedures later in
this chapter.

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.
4-6 Installation

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 the following figure.

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

N2/Air Shear Gas

and RF Coil Cooling

(White Tie Wrap) (Red Tie Wrap)

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

4-8 Installation

Connecting the Argon Supply

Caution Make sure that the required purity of the argon gas is 99.996% pure
otherwise the detector will be damaged.

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.
PerkinElmer recommends copper lines.

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 RF Coil Cooling Gas

Air or nitrogen is required to cool the RF coil for the Optima 5300V. The Optima
5300V spectrometer typically consumes the RF coil cooling gas at a rate of 25
liters/min.

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 Installation kit (Part No.
N077-0432).

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

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

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 Installation kit (Part No. N077-0432). The
 Connecting the Gases and Cooling Water 4-9

following procedure describes how to connect the PerkinElmer air compressor,

filter and regulator.

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 Installation kit (Part
No. N077-0432). 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 Installation kit (Part No. N077-0432). 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.

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.
4-10 Installation

Setting the Shear Gas or RF Coil Cooling Pressure

The following procedure describes how to set the shear or RF coil cooling gas
pressure for the Optima 5000 Series instruments 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. 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 or the RF coil cooling fitting on the side of the spectrometer.

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

 Connecting the Gases and Cooling Water 4-11

Connecting the PolyScience Chiller

The PolyScience 6106PE Chiller must be used to supply cooling water to the
instrument. This chiller requires a single wall receptacle. The PolyScience 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 PolyScience 6106PE chiller.

The PolyScience 6106PE is available through PerkinElmer in the following two

configurations:

208/230V, 60 Hz PerkinElmer Part No. N812-2026

220/240V, 50 Hz PerkinElmer Part No. N812-2025 (For Europe the
PerkinElmer Part No. is ED00-0097)

Connecting the Chiller to the Instrument

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

Connect the instrument to the chiller with hoses. The direction of the flow through
the system can be controlled by the way the hoses are connected to the chiller. The
"INLET" port will draw liquid into the chiller; the "OUTLET" port will pump
liquid out. See the following figure for the location of the cables.

1. Locate the instrument Return/Output coolant line (Part No. N077-0342) and
connect to the chiller "INLET" fitting. 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. The following figure shows the
water supply connections at the instrument.

2. Locate the instrument Input coolant line (Part No. N077-0341, uses 3/8-in.
Swagelok fittings) and connect to the chiller "OUTLET" fitting. Use 3/8-in.
space collars (Part No. 0992-0584) at the instrument. The following figure
4-12 Installation

shows the chiller connections. Figure 4-3 shows the water supply connections
at the instrument.

3. Make sure that the hoses and fittings are tight and that there are no bends or
crimps in the hoses.

Remote Chiller Connections

The chiller can be turned on or off via the software. Your service engineer will
connect the cable from the chiller to the Optima 5000 so that the chiller can be
operated remotely. See the following figure for the location of the cable
connections.

To connect the remote chiller cable to the instrument see the next two figures and
follow these steps.

1. Attach the plug end of the remote cable to the external chiller.

2. Take the other end of the cable and locate the Customer Interface connections
on the left side of the instrument (as viewed from the front of the instrument).

3. Attach the red wire to the position #5 of the External Customer Interface
connections.

4. Attach the black wire to the position #7 of the External Customer Interface
connections.

5. Attach the grey wire to the position #8 of the External Customer Interface
connections.
 Connecting the Gases and Cooling Water 4-13

Customer Interface
Connections

Coolant OUT
Remote Cable
3/8-in.Space Collars (Part No. N077-0175)
(Part No. 0992-0584)

Coolant Drain Hose

(White Tie Wrap)
(Part No. N077-0342)

Coolant IN
From OPTIMA
"OUT"

To OPTIMA
"IN"

Coolant Supply Hose

(Red Tie Wrap)
(Part No. N077-0341)

PolyScience 6106PE
Chiller

Line Cord Plug

Figure 4-2. Remote chiller connections on the right side of the instrument (as
viewed from the front).
4-14 Installation

TRIGGER
IN

ETHERNET

28 VDC MAX
100 mA @
RLY1

RLY2

CUSTOMER
INTERFACE

Figure 4-3. Remote chiller connections on the left side of the instrument (as
viewed from the front).

Remote Chiller Operations

The remote chiller will automatically be on when the Optima 5000 Spectrometer is
warming up. The warming up period includes just being turned on, coming out of
Sleep mode or Standby mode.

If the instrument has just been turned on, starting WinLab32 will automatically
begin warm up. Initiating Winlab32 will have no effect on the chiller if the chiller
is already on.

If the Optima 5000 Spectrometer is in Sleep or Standby mode and the instrument
is still ignited, the chiller will remain on. If the instrument is not ignited in Sleep or
Standby mode the chiller will turn itself off.
 Connecting the Gases and Cooling Water 4-15

Note The plasma should never be ignited if the chiller is off.

Customer Interface
Connections

3/8-in.Space Collars
(Part No. 0992-0584)

Coolant OUT
(White Tie Wrap)

Coolant IN
(Red Tie Wrap)

PolyScience 6106PE
Chiller

Line Cord Plug

Figure 4-4. Water flow diagram with the chiller.

4-16 Installation

Filling the PolyScience Chiller

Use the following procedure to fill the Chiller.

Caution Do not use deionized water in the chiller reservoir.Deionized

water is considered corrosive and will react with the copper in the
chiller.

1. Unscrew the two screws and remove the Reservoir Access Panel. Refer to the
following figure.

2. Turn the filler cap count clockwise and lift the cap off

3. Fill the reservoir up with the coolant fluid (Part No. N077-6099). The chiller
reservoir has a capacity of 7 liters (2 US gallons). Part No. N077-6099 is five
one half gallon bottles (8.75 liters or 2.5 gallons of this mixture).

4. Keep some coolant fluid beside the unit and proceed to Starting Up the
PolyScience Chiller. The reservoir tank may need to be topped off once the
unit has been started.
 Connecting the Gases and Cooling Water 4-17

Reservoir Access Panel

Reservoir Plug

Figure 4-5. Filling the chiller.

Starting Up the PolyScience Chiller

Check the following before starting up the chiller:
• All plumbing connections are tight.
• The chiller reservoir is full.
• The chiller power cord is plugged in.
1. Turn the On/Off switch, located in the rear of the chiller, to the On position.
Press the On button located on the front of the chiller and the refrigeration
system and the recirculation pump will start.
4-18 Installation

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

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

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 two figures):
• Ethernet cable from the computer to the instrument.
• Centronics Parallel cable from the computer to the printer.
• The Optima 5000 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). A conduit box (Hubbell Part No. SP20301,
PerkinElmer Part No. 0994-0914 may also be required in some regions. Both,
a receptacle and a conduit box are shipped with the instrument (PerkinElmer
Part No. N077-0425).
To order directly from Hubbell you can also use these two alternative Hubble
part numbers.
For the US/Canada (20A service) use Hubbell Part No. C320R6W.
For Europe (16A service) use Hubbell 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.
 Connecting the System Components 4-19

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

Cable from
Computer to
Autosampler

Figure 4-6. System component connections on the right side of the instrument
(as viewed from the front of the instrument).
4-20 Installation

TRIGGER
IN

ETHERNET

28 VDC MAX
100 mA @
RLY1

RLY2

CUSTOMER
INTERFACE

Figure 4-7. System component connections on the left side of the instrument
(as viewed from the front of the instrument).

Note The 12-pin instrument 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 4-21

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 on the Optima

5100, 5200 and 5300 DV
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.

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. Wear latex, rubber or cotton gloves when handling the
glassware. To remove the alkali, wipe the glassware clean with cotton
wool dipped in alcohol.

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

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
4-22 Installation

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.

Torch Positions
For typical applications the following torch positions are recommended:

Analysis System Torch Position

Scott-Cross Flow Sample -3
Introduction System
Cyclonic/Concentric -2
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.
 Installing the Quick-Change Adjustable Torch Module 4-23

Caution If you are having problems with the torch prematurely devitrifying,
increase the gas flow up to 20 L/min. Also 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. Wear latex,
rubber or cotton gloves when handling the glassware. To remove the
alkali, wipe the glassware clean with cotton wool dipped in alcohol.

To determine the best torch position for your analyses start with our suggestions in
the previous chart as a guideline. Any modifications from these recommended
values should be done in small increments.

As a general rule, the more volatile the solution the closer the torch should be to
the plasma to insure greater sensitivity. The closer the torch is to the plasma more
deposits will accumulate on the injector. The injector will have to be cleaned more
often (see Chapter 5, Maintenance for the cleaning procedures). For less volatile
solutions the torch can be further from the plasma. Keep in mind that the further
the torch is from the plasma the less stable the plasma is.
To successfully determine torch position always duplicate the conditions you will
be running your samples. For example, have the sample compartment door closed
when running aqueous samples and open when running organic solutions.
See Setting Instrument Parameters later in this chapter for more information on
plasma parameters.
4-24 Installation

Figure 4-8. 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 4-25

O-Ring
(Part No. 0990-2045)

Bonnet
(Part No. N077-5289)
Copper Foil Torch
Ignitor Contact (Part No.
(Part No. N077-5297) RF Coil N077-0338)

Ground
Pointer
Front of Instrument,
Torch Compartment
Door Open

Ignitor
Contact
Finger

Figure 4-9. 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.
4-26 Installation

6. Firmly push the spray chamber/nebulizer 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.

Caution When installing the spray chamber/nebulizer end cap make sure that the
end cap screws are not perpendicular to the door. The door will not close
properly unless the screws are rotated so that they are at a slight angle to
the door.

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

8. To the spray chamber drain connect the barbed fitting (Part No. 0992-0267).

9. Attach the Solvent Flex tubing (Part No. 0998-5735) to the barbed fitting.
Attach the other end of the Solvent Flex tubing to the tubing coupler (Part No.
0992-0186).

10. Use the other end of the tubing coupler (Part No. 0992-0186) 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.(If you need, at some point, to release
the NEB tubing from the quick connect, push on the quick disconnect to
disconnect the NEB tubing.)

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.

 Installing the Quick-Change Adjustable Torch Module 4-27

For instructions on connecting tubing to the peristaltic pump see the section on the
Peristaltic Pump, in Chapter 5, Maintenance.

Nebulizer (NEB)
Argon Tubing
Quick Disconnect

Quick Disconnect

Nebulizer (NEB)
Drain Tubing Argon Tubing

Sample
Capillary
Tubing
Waste
Vessel

Figure 4-10. Nebulizer (NEB) connections to torch and nebulizer end cap.
4-28 Installation

Installing the Torch Module for the Optima 5300V

The Torch Module for the Optima 5300V is shipped pre-assembled in a separate
box. The vertical torch, injector, torch mount and the dovetail mount come pre-
assembled. The cyclonic spray chamber, cyclonic spray chamber spring clip and
low flow gemcone nebulizer will come as separate items in the same box.

Before installing the 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.

Note During shipment the bonnet will be secured to the RF coil with a tie wrap.
Remove the tie wrap before you begin the torch module installation
procedure

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. Wear latex, rubber or cotton gloves when handling the
glassware. To remove the alkali, wipe the glassware clean with cotton
wool dipped in alcohol.

To install the torch module follow these steps and see the following figure:

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.
 Installing the Torch Module for the Optima 5300V 4-29

Installing the Torch Module Assembly

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

2. Carefully remove the torch module assembly from its box.

3. Holding the torch assembly securely with one hand 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. Make sure
that the bonnet securely rest on the coil and top of the torch.

4. Still holding on to the torch assembly with one hand use your other hand to set
the height adjustment to -3 on the scale located on the dovetail mount (as
shown in the following figure).

5. While still holding on to the torch assembly with one hand use your other hand
to tighten the side knurled nut located on the dovetail mount.

6. The unit is know security in place and you can proceed to attach the quick
disconnect fittings.

7. Connect the Auxiliary Gas Quick Disconnect Fitting by pushing the fitting on
to the bottom glass arm of the torch.

8. Connect the Plasma Gas Quick Disconnect Fitting (with the ignitor pin in it)
by pushing the fitting on to the top glass arm of the torch.

9. You have completed the torch assembly procedure and you need to now attach
the cyclonic spray assembly.
4-30 Installation

Ground
Pointer

Plasma Gas
Quick Torch
Disconnect
Aux Gas
Quick RF Coil
Disconnect
Top Thumb
Screw
Scale
Bottom Thumb
Screw

Figure 4-11. Installing the torch into the sample compartment of the
Optima 5300V.
 Installing the Torch Module for the Optima 5300V 4-31

Installing the Cyclonic Spray Chamber Assembly

1. Remove the The cyclonic spray chamber, cyclonic spray chamber spring clip
and low flow GemCone nebulizer from the box.
2. Install the drain capillary to the bottom of the cyclonic spray chamber.
3. Install the GemCone nebulizer into the cyclonic spray chamber. See the
following figure.
4. 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.
5. 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.

Capillary
Tubing
(Part No.
0990-8265)

Teflon
Tubing (1 in.)
(Part No.
0998-5708)

GemCone
Nebulizer
Assembly
Cyclonic
Spray Chamber

Nebulizer Gas Fitting

Figure 4-12. Installing the GemCone nebulizer into the cyclonic spray chamber.
4-32 Installation

6. Install the sample capillary tubing into the nebulizer.

7. Attach the nebulizer gas fitting and finger tight (do not use a wrench).

8. Then place the cyclonic spray chamber assembly at the base of the
compartment.

9. Secure the cyclonic spray chamber clip to the base of the cyclonic spray
chamber (see the following figure).

10. Feed the drain and sample tubing through the side of the instrument
compartment.

for more information on installing the GemCone nebulizer into the Cyclonic spray
see Chapter 5, Maintenance, Installing the GemCone Nebulizer in the Cyclonic
Spray Chamber.
 Installing the Torch Module for the Optima 5300V 4-33

Ground
Pointer

Torch

Drain RF Coil
Tubing

Sample
Tubing

Spring
Clip
Cyclonic
Spray
Chamber

Figure 4-13. The torch and cyclonic spray chamber.

4-34 Installation

Connecting the Nebulizer (NEB) Tubing to the Optima 5300V

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 fitting.

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 Autosampler

The instrument can be used with the PerkinElmer S10 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 S10 Autosampler User’s Guide (Part No. 0993-6788)
for detailed information on installing the autosamper.

To connect the S10 Autosampler follow this procedure:

1. Switch off the spectrometer and other components in the system and
disconnect them from the line power supply.

2. Locate the connectors on the underside of the autosampler as shown in

following figure.
 Installing The Autosampler 4-35

Figure 4-14. Electrical connectors and switches located on the underside of the
autosampler.

3. Place the autosampler either adjacent to the spectrometer or on top of the

spectrometer.

When used alone, the autosampler is connected directly to the nebulizer's

sample tube. Since the length of the sample tube has an influence on the
aspiration rate of the nebulizer, you should position the autosampler as close to
the spectrometer as possible. See the following figure.
4-36 Installation

Figure 4-15. Electrical connection for the S10 autosampler to the Optima spec-
trometer.

4. Connect the RS232/serial communication cable provided, between the Com 1

port on the underside of the autosampler (as shown in Figure 4-14) and one of
the Com ports on the PC.

5. Connect the autosampler to the line power supply using the plug-in power
supply provided.

The plug-in power supply uses a wide-range input of 100-240 VAC, 50-60 Hz.
 Fitting and Connecting the Autosampler Sampling Probe 4-37

Plug the power cord into the power supply, then plug the other end of the power
cord into the power source.

6. Connect the spectrometer and other components in the system to the line power
supply.

Note To avoid problems of interference caused by earth loops, always connect

the spectrometer, computer, printer and other components to the same
phase of the line power supply. The most convenient method is to use a
multisocket outlet.

7. Switch on all components of the system, following the routine in the manual
for your spectrometer.

Fitting and Connecting the Autosampler Sampling Probe

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 as this will damage it, and reassembly is not
possible.

Never attempt to move the sampling probe holder along the

autosampler arm by hand. The autosampler may be damaged if the
tower is moved by hand when it is under system control.

Disconnect the power supply to the autosampler if you need to

manually move the tower
4-38 Installation

Fitting the Sampling Probe

1. If not already done, carefully insert the sampling probe guide from above into
the sampling probe holder on the autosampler arm and push it down fully, as
shown in the following figure.

2. Carefully insert the sampling probe from above into the probe guide.
3. Push the sampling probe down until about 20 mm protrudes from the bottom
end of the probe guide, then position the O-ring on the probe to set this
position, as shown in the following figure.

This is not the final position for the sampling probe. The probe can be adjusted
when the rinsing port has been set up. See the following procedure, Adjusting
the Sampling Probe Height.

Note The standard sampling probe is a PTFE-lined epoxy polymer tube. This
polymer is resistant to the acids, alkalis and organic solvents normally used
in atomic spectroscopy. If your samples contain an organic solvent that
attacks this polymer, a PTFE-lined stainless steel sampling probe is
offered as an option (B3000152).

Figure 4-16. Inserting the sampling probe.

 Fitting and Connecting the Autosampler Sampling Probe 4-39

Adjusting the Sampling Probe Height

Note The procedure described below assumes that you are using a spectrometer
operated via ICP WinLab software. If you are using an AA or ICP-MS
instrument, please refer to the information on operating an autosampler in
the online help for the respective instrument.

1. Install the rinsing-port rack on the autosampler.

See the procedure Assembling Sample Racks starting on page 46 in the S10
Autosamplers User’s Guide (Part No. 0993-6788) for more information.

2. Place the rinsing port in the rinse location in the sample rack.

See the procedure Installing the Rinsing Port on the Rack starting on page 43
in the S10 Autosamplers User’s Guide (Part No. 0993-6788) for more
information.

3. In the ICP WinLab software, from the main menu make the following
selections:

4. Select Analysis->AutoSampler->Go to Wash.

5. Carefully push the sampling probe down until it bottoms in the rinsing port.
Then pull the sampling probe up by about 5mm as shown in the following
figure. Use the O-ring on the probe to prevent it from slipping down. The
sampling probe is now in the correct height.

6. To remove the sample rack, first select Analysis->AutoSampler->Load

Autosampler Tray to raise the sampling probe, then remove the rack.
4-40 Installation

Figure 4-17. Inserting the sampling probe.

This completes installation of the sampling probe. For detailed information on

adjusting the sample probe height and connecting the sample tube between the
sample probe and the spectrometer’s sample input system see the S10
Autosamplers User’s Guide (Part No. 0993-6788).
 Instrument Start-up 4-41

Instrument Start-up
First turn on the gases and water chiller. Then use the Main Instrument switch to
turn on the spectrometer. Once the plasma has been ignited, you should wait one
half hour for the system to stabilize before running samples.

It is recommended to leave the main power switch to the Optima 5000 in

Note the ON position to maintain spectrometer thermal equilibrium.

Do not block the main power switch because it functions as the

disconnecting device for the instrument's power.

If the Optima 5000 is turned off (via the power switch) for more than 24
hours the instrument will require, once it is turned on, three to four hours
to initialize and an additional two hours for thermal stabilization before
the instrument can operate at peak performance.

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.

4-42 Installation

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 for the 5X00 DV. Select Radial for the 5300V. 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.

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.

 Automatically Aligning the Torch Viewing Position 4-43

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.

Detector Calibration
Detector calibration is the process of collecting and processing the detector signal
bias and dark current data needed to quantify signals from the detectors properly.

The plasma does not need to be on for this procedure.

To perform detector calibration:

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

The Spectrometer Control window appears.

2. Click on Detector Calibration in the Spectrometer Control window.

The system automatically closes the shutter to measure signal bias and dark
current. The detector calibration routine may take up to twenty minutes.

Wavelength Calibration for all Optima 5000 Series Models

The UV and VIS channel calibration gathers data for UV and VIS emission lines
to compensate for slight variations in optical alignment. At the end of the UV and
VIS wavelength calibration, the system determines the wavelength offset of an
emission line from the internal mercury lamp and records the slit position as a
reference point for future mercury realignments.

Note Since spectrometers are sensitive to thermal effects, it is important that the
instrument be operated with the plasma on for at least one-half hour before
initiating wavelength calibration.

Wavelength calibration is performed in the following steps:

• UV channel calibration
4-44 Installation

• VIS channel calibration (for instruments with a second detector that covers the
visible wavelength range)
Solutions you'll need for wavelength calibration include:
• Calmix 3 solution (Part No. N058-2152) available through PerkinElmer, which
contains 100 mg/L of P, K, S; and 20 mg/L of As, La, Li, Mn, Mo, Ni, Sc, Na.
• VIS Wavecal mix (Part No. N930-2946) available through PerkinElmer, which
contains 1 mg/mL Ba, Ca; and 10 mg/L of La, Li, Mn, Na, Sr; and 50 mg/L of
K.
• Rinse solution.

To initiate a wavelength calibration:

1. Make sure that the plasma is lit and has been on for at least one hour.

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

The Spectrometer Control window appears.

To perform UV channel wavelength calibration:

1. Aspirate the Calmix 3 solution (Part No. N058-2152).

Note On Dual View (DV) instruments, the spectrometer will automatically

change to radial viewing to prevent saturation of the detector.

2. Select UV, then click on Wavelength Calibration in the Spectrometer Control

window.

The UV calibration may take several minutes. You may view the spectra used
for calibration by clicking on Spectra in the toolbar. When the UV calibration
is complete, the UV coefficients and RMS (Root Means Square) value will be
displayed in the Results window. These values should meet the following
specifications:

UV Coefficients and RMS Specification

First Coefficient absolute value < 2.0
Second Coefficient absolute value < 2.0
 Automatically Aligning the Torch Viewing Position 4-45

Third Coefficient absolute value < 8.0

RMS < 2.0
(measures variability of
wavelength offsets)

If these specifications are not met, repeat the wavelength calibration and make sure
all peaks can be seen in the Spectra Display window. If these specifications are still
not met, a complete optical alignment may be required. Contact a PerkinElmer
service engineer.

To perform VIS channel wavelength calibration:

1. Aspirate VIS Wavecal mix (Part No. N930-2946).

2. Select VIS, then click on Wavelength Calibration in the Spectrometer

Control window.

The VIS calibration may take several minutes. You may view the spectra used for
calibration by clicking on Spectra in the toolbar. When the VIS calibration is
complete, the VIS coefficients and RMS (Root Means Square) value will be
displayed in the Results window. These values should meet the following
specifications.

VIS Coefficients and RMS Specification

First Coefficient absolute value < 3.0
Second Coefficient absolute value < 3.0
Third Coefficient absolute value < 12.0
RMS < 2.0
(measures variability of
wavelength offsets)

If these specifications are not met, repeat the wavelength calibration and make sure
all peaks can be seen in the Spectra Display window. If these specifications are still
not met, a complete optical alignment may be required. Contact a PerkinElmer
service engineer.
4-46 Installation

Setting Instrument Parameters

Aqueous Setting Instrument Parameters

Use the ICP WinLab software to set up the instrument parameters. For optimal
performance the following settings are recommended.

Plasma Parameters

Parameter Baffled Cyclonic Spray Chamber/

Low Flow GemCone Nebulizer
Aqueous Organics
RF power: 1500 watts 1500 watts
Nebulizer Flow: 0.6 L/min 0.4-0.5 L/min
(for Cross-Flow
Nebulizer)
Auxiliary Flow: 0.2 L/min 1.0-1.5 L/min
Plasma Flow: 15 L/min 15 L/min
Sample Flow 1.5 to 2.5 mL/min 3.0 mL/min
Rate:
Equilibration 15 sec 15 sec
Time:
Torch Position -3 -2 to -1
 Setting Instrument Parameters 4-47

Organic Setting Instrument Parameters

Use the ICP WinLab software to set up the instrument parameters. For optimal
performance the following settings are recommended.

Plasma Parameters

Baffled Cyclonic Spray Chamber/

Parameter
Low Flow GemCone Nebulizer

RF power: 1500 watts

Nebulizer Flow: 0.60 L/min
(for Cross-Flow
Nebulizer)
Auxiliary Flow: 1.0 L/min
Plasma Flow: 15 L/min
Sample Flow Rate: 0.8 to 1.0 mL/min
Equilibration Time: 30 sec
Torch Position -3

The long torch (Part No. N077-0343) is another torch that can be ordered. This is
the best torch to use for axial viewing for samples with organics or high dissolved
solids. Using the long torch will extend the torch life since the long torch does not
have a slot.

For more information on the above parameters, refer to the Winlab32 Software
Guide (Part No. 0993-6335) and the Baffled Cyclonic Spray Chamber Kit
Instruction Sheet (0993-6506).
4-48 Installation

High Dissolved Solids Setting Instrument Parameters

Use the ICP WinLab software to set up the instrument parameters. For optimal
performance the following settings are recommended.

Plasma Parameters

Scotts Spray Chamber/Low Flow

Parameter
GemCone Nebulizer (2.0mm Qtz. injector)

RF power: 1500 watts

Nebulizer Flow: 0.80 L/min
Auxiliary Flow: 1.0 L/min
Plasma Flow: 15 L/min
Sample Flow Rate: 1.5 mL/min
Equilibration Time: 30 sec
Torch Position -1

The long torch (Part No. N077-0343) is another torch that can be ordered. This is
the best torch to use for axial viewing for samples with organics or high dissolved
solids. Using the long torch will extend the torch life since the long torch does not
have a slot.
For more information on the above parameters, refer to the Winlab32 Software
Guide (Part No. 0993-6335).

Torch Positions
For typical applications the following torch positions are recommended:

Analysis System Torch Position

Scott-Cross Flow Sample -3
Introduction System
Cyclonic/Concentric -2
High Dissolved Solids* -1
Organics* -3
 Setting Instrument Parameters 4-49

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

To determine the best torch position for your analyses start with our suggestions in
the previous chart as a guideline. Any modifications from these recommended
values should be done in small increments.
As a general rule, the more volatile the solution the closer the torch should be to
the plasma to insure greater sensitivity. The closer the torch is to the plasma more
deposits will accumulate on the injector. The injector will have to be cleaned more
often (see Chapter 5, Maintenance for the cleaning procedures). For less volatile
solutions the torch can be further from the plasma. Keep in mind that the further
the torch is from the plasma the less stable the plasma is.

To successfully determine torch position always duplicate the conditions you will
be running your samples. For example, have the sample compartment door closed
when running aqueous samples and open when running organic solutions.

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 Dual View (DV) instruments. Optimum
conditions will depend on the type of analyses being performed; however, in
general, the following considerations are important for axial viewing.
Settings are given for the Scott-type spray chamber and cross-flow nebulizer.
The following parameters are set in the method:
• Auto integration times are recommended, using the following settings:

Auto Int Samp Time: Min: 10 sec, Max: 50 sec

(Auto Integration Sampling Time)

Note A Max time of 100 seconds may be required for the ultimate detection limit
work.
4-50 Installation

• Normal resolution is recommended.

• 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.

The following parameter is set in the hardware.ini file:

Auto Integration Threshold: 2.0 sec recommended (default setting)

The Auto Integration Threshold sets a level for the integration. When the
software does a "snapshot" (called a pre-shot) for each solution, it will
determine the sampling time and adjust it based on the threshold. If the time is
greater than or equal to the threshold, the maximum sampling time will be
used. If it is less than the threshold, the minimum sampling time will be used.

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 4-51

Shipping List
Table 4-2. Items Shipped with Instruments (Optima 5100, 5200
and 5300 DV)
Part No. Description
0993-6391 Unpacking Instructions

N077-0400 Instrument

N077-0600 Torch Module-Dual View

N077-0432 Installation Kit

N077-0433 Spares Kit

N077-0439 Spares Kit DV (periscope)

N077-5289 Bonnet

0993-6762 Optima 5000 Series Hardware Guide

Table 4-3. Items Shipped with Spares Kit DV (Periscope)

Part No. Description

0990-2143 O-Ring (0.551 ID, 0.070 WD)

0992-0064 2 O-Rings (0.674 ID, 0.103 WD)

N077-0944 Tube Assembly for DV radial window

N077-1116 Axial Window

0990-7917 Hex Key Wrench

4-52 Installation

Table 4-4. Items Shipped with Instruments (Optima 5300V)

Part No. Description
0993-6391 Unpacking Instructions

N077-0407 Instrument

N077-0910 or Torch Assy 4300/5300 Vertical (OIL)

N077-0911 Torch Assy 4300/5300 Vertical (HFR)

N077-0432 Installation/Spares Kit

N077-0917 Spares Kit

N077-5289 Load Coil Bonnet

0993-6762 Optima 5000 Series Hardware Guide

Table 4-5. Items Included in Installation for the Optima 5100, 5200
and 5300DV

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 Sample Compartment

0990-4845 Cooling Water Filter (for the cooling sys-

tem)

0990-4991 Drain Bottle

N069-1538 Drain Kit Flow Diagram

 Shipping List 4-53

Table 4-5. Items Included in Installation for the Optima 5100, 5200
and 5300DV

0990-8265 Polyethylene Tubing, Sample Capillary

0990-8585 PVC Pump Tubing, 1.14 mm i.d. (drain

tubing)

0990-8587 PVC Pump Tubing, 0.76 mm i.d. (sample

tubing)

0993-6225 ICP-OES Instrument Maintenance Log

Table 4-6. Spare Parts Available for the Optima 5100, 5200 and
5300 DV

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 Spray Chamber with Cap for Aque-

ous Solutions

N077-0612 Wide Baffled (8 mm) Cyclonic Spray Cham-

ber with Cap
4-54 Installation

Table 4-6. Spare Parts Available for the Optima 5100, 5200 and
5300 DV

N077-6090 Narrow Baffled (4mm) Cyclonic Spray

Chamber with Cap
N077-0614 Cap for either the Baffled or Unbaffled
Cyclonic Spray Chamber

N069-0288 Axial Drain Assembly Kit

N077-0338 Quartz Torch (Tulip)

N077-0343 Long Torch (for organics and high dissolved

solids)

N077-5289 Quartz Bonnet

N077-0357 Ryton Scott Spray Chamber

N077-6052 Cyclonic Spray Chamber Assembly

N077-5300 RF Load Coil

0940-1066 Card-PCI GPIB/WIN NT Driver

N069-1870 CD-ROM ICP Winlab32

N077-5227 Alumina Injector, 0.8 mm i.d, 141 mm LG

N077-5228 Alumina Injector, 1.2 mm i.d, 141 mm LG

N077-5177 Alumina Injector, 2.0 mm i.d., 141 mm LG

(Standard Injector)

N077-5247 Sapphire Injector, 2.0 mm i.d, 141 mm LG

N077-5225 Quartz Injector, 0.8 mm i.d., 141 mm LG

 Shipping List 4-55

Table 4-6. Spare Parts Available for the Optima 5100, 5200 and
5300 DV

N077-5226 Quartz Injector, 1.2 mm i.d., 141 mm LG

N077-5223 Quartz Injector, 1.6 mm i.d., 141 mm LG

N077-5014 Quartz Injector, 2.0 mm i.d., 141 mm LG

0992-1045 Small O-Ring for Gem Tips

N077-0358 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)

0998-5735 Solvent Flex Tubing, 1.5 mm i.d. for Spray

Chamber Drain (before pump tubing)

0250-6241 Tubing for Drain Connection to Sample Bot-

tle

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

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

tubing)

0998-5708 Teflon Tubing Piece, Nebulizer

4-56 Installation

Table 4-6. Spare Parts Available for the Optima 5100, 5200 and
5300 DV

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)

N077-1116 Purge Window, Axial Viewing

N077-0944 Purge Window Tube, Radial Viewing

0990-7917 2 mm Hex Key for Purge Window

0990-2143 O-Ring, Axial Purge Window

0920-0064 2 O-Rings, Radial Purge Window Tube

0990-2155 O-Ring for Axial Window Holder

N812-0160 O-Rings for Cyclonic Spray Chamber,

10 included

An Installation Parts Kit is available and the Part Number is N077-0432.

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

 Shipping List 4-57

Table 4-7. Items Included in Installation Kit for the Optima 5300V

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 Sample Compartment

0990-4845 Cooling Water Filter (for the cooling sys-

tem)

0990-4991 Drain Bottle

N069-1538 Drain Kit Flow Diagram

0990-8265 Polyethylene Tubing, Sample Capillary

0990-8585 PVC Pump Tubing, 1.14 mm i.d. (drain

tubing)

0990-8587 PVC Pump Tubing, 0.76 mm i.d. (sample

tubing)

0993-6225 ICP-OES Instrument Maintenance Log

Table 4-8. Spare Parts Available for the Optima 5300V

Part No. Description

N069-0676 Cross-Flow Nebulizer GemTip Kit

N077-0437 Torch Glassware O-Ring Kit

4-58 Installation

Table 4-8. Spare Parts Available for the Optima 5300V

N077-0438 Injector Adapter O-Ring Kit

N077-0910 or Torch Assy 4300/5300 Vertical (OIL)

N077-0911 Torch Assy 4300/5300 Vertical (HFR)

N077-0602 Injector Positioning Tool Kit

N077-0603 Torch Injector Assembly

N077-0604 Adjustable Torch Holder Assembly

N077-0605 Cyclonic Spray Chamber with Cap for

Aqueous Solutions

N077-0612 Wide Baffled (8 mm) Cyclonic Spray

Chamber with Cap

N077-6090 Narrow Baffled (4mm) Cyclonic Spray

Chamber with Cap
N077-0614 Cap for either the Baffled or Unbaffled
Cyclonic Spray Chamber

N069-0288 Axial Drain Assembly Kit

N077-1500 Tube Assy-4300V/5300V Quartz

N077-5289 Quartz Bonnet

N077-6052 Cyclonic Spray Chamber Assembly

N077-5300 RF Load Coil

0940-1066 Card-PCI GPIB/WIN NT Driver

N069-1870 CD-ROM ICP Winlab32

 Shipping List 4-59

Table 4-8. Spare Parts Available for the Optima 5300V

N077-1531 Alumina Injector, 1.2 mm i.d., 83 mm LG

(Standard with N077-0910 OILS Torch)

N69-5362 Alumina Injector, 2.0 mm i.d., 83 mm LG

(Standard with N077-0911 HRF Torch)

0992-1045 Small O-Ring for Gem Tips

N077-0358 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)

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

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

tubing)

0998-5708 Teflon Tubing Piece, Nebulizer

0999-5098 Air Filter for Spectrometer Fan

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

4-60 Installation

Table 4-8. Spare Parts Available for the Optima 5300V

0998-5735 Solvent Flex Tubing, 0.11 mm i.d. (PVC

tubing)

0047-3550 Solvent Flex Pump Tubing, 0.76 mm

(PVC sample tubing)

N058-1497 Radial Purge Window

N058-1455 Ceramic Purge Extension

N069-5258 O-Ring, Radial Purge Window

N812-0160 O-Rings for Cyclonic Spray Chamber,

10 included

An Installation Parts Kit is available and the Part Number is N077-0432.

A Spares Parts Kit is available and the Part Number is N077-0917.
Chapter 5
 Maintenance 5
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 PerkinElmer, the responsible bodies should
check with PerkinElmer that the proposed method will not damage
the equipment.

Note The responsible body has the responsibility for carrying out appropriate
decontamination if hazardous material is spilled on or inside the
equipment.
5-4 Maintenance

Note Decontamination
If the instrument or an accessory requires decontamination before
repair, maintenance, warranty or trade-in purposes at PerkinElmer the responsible
body should read the procedure and complete the certificate which is available on
the PerkinElmer public website:http://las.perkinelmer.com/OneSource/
decontamination.htm.

Follow the “Decontamination of Instrumentation and Associated Sub-

assemblies” procedure and complete the “Certificate of Decontamination.” The
certificate is used to certify the decontamination process was completed before
equipment can be returned to PerkinElmer.”.

This equipment requires no specified inspection or preventive

Note maintenance to ensure the continuous functioning of its safety features.

Daily Checks
The following maintenance procedures should be done on a daily basis. Make sure
to inspect and replace any hoses which show signs of wear because their failure
could cause a hazard.

Exterior of Instrument Cleaning

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

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.
 Daily Checks 5-5

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.

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

Caution Make sure that the required purity of the argon gas is 99.996% pure
otherwise the detector will be damaged.

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 4X00 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)

5-6 Maintenance

RF Coil Cooling Gas

The Optima 5300V requires air or nitrogen to cool the RF coil. Make sure that an
adequate supply of air or nitrogen is available and connected to the system. Check
that the supply has sufficient pressure, and that a spare cylinder is ready if
necessary.

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

Chiller
Fill the reservoir up with the coolant fluid (Part No. N077-6099). The chiller
reservoir has a capacity of 7 liters (2 US gallons). Part No. N077-6099 is five one
half gallon bottles (8.75 liters or 2.5 gallons of this mixture).

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.
 Periodic Checks 5-7

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.

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
5-8 Maintenance

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. Wear latex or rubber gloves when handling the glassware.
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. Contact your PerkinElmer Service
Representative to 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.

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.
 Periodic Checks 5-9

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 air filters. Clean or replace the spectrometer and generator air
filters as necessary.

Note It is recommended to leave the main power switch to the Optima 5000 in
the ON position to maintain spectrometer thermal equilibrium. If the
Optima 5000 is turned off (via the power switch) for more than 24 hours
the instrument will require, once it is turned on, three to four hours to
initialize and an additional two hours for thermal stabilization before the
instrument can operate at peak performance

Wavelength Calibration
A wavelength calibration is necessary when the system is first installed, when it is
moved to a new location or when the system has been shut down for an extended
time. Wavelength calibration is described in Chapter 4, Installation. Do the
wavelength calibration only after the instrument has had the power on for several
hours and is completely warmed up. The software also has a mercury recalibration
function. See the ICP WinLab Software Guide for more information.
5-10 Maintenance

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.

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 5-20% aqua
Bonnet regia; use an ultrasonic cleaner if available.
Injector For more detailed information, see Cleaning
Spray Chamber the Torch later in this chapter.
O-Rings Clean with soap and water, rinse thoroughly.
 Periodic Checks 5-11

Table 5-1. Recommended Cleaning Procedure (Continued)

GemTips for Clean with soap and water, rinse thoroughly;

Cross-Flow or 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.
Mira Mist For the longest life and best performance,
Nebulizer wash your nebulizer by simply running water
as a sample for 10 minutes at the end of the
day before shutting down the plasma. Any
other form of washing is usually unnecessary.
Please DO NOT wash your nebulizer in acid
or solvents to 'prevent salt build up'. DO NOT
use surfactants as they will destroy the surface
tension at the tip and performance. The tip is
very easily damaged and should NEVER be
touched with fingers, tissues, or anything
else.
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.
5-12 Maintenance

Quick-Change Torch Module for the Optima 5000 Series DV

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.
 Quick-Change Torch Module for the Optima 5000 Series DV 5-13

.
Torch RF Coil

Bonnet

Slot
(To secure bonnet during
O-Ring torch installation, removal,
or adjustment)

Figure 5-1. Quartz torch (O-ring Part No. N077-0437).

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. Contact your PerkinElmer Service Representative
to replace and adjust the RF coil.

Removing the Scott Spray Chamber for the Optima 5000 Series DV
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.

5-14 Maintenance

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.
 Quick-Change Torch Module for the Optima 5000 Series DV 5-15

Figure 5-2. Removing the spray chamber assembly.

5-16 Maintenance

Once the above steps have been done, you can if needed, follow the steps for the
procedure Removing and Disassembling the Torch.

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.

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.
 Quick-Change Torch Module for the Optima 5000 Series DV 5-17

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.

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 5-3 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).
5-18 Maintenance

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
Warning No. N077-0338). Remove the knurled nut, sleeve and 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 Torch Module for the Optima 5000 Series DV 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.
5-20 Maintenance

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.

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 5% 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. Wear latex or rubber gloves when handling the glassware.
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 Torch Module for the Optima 5000 Series DV 5-21

Cleaning the Spray Chamber

See Cleaning the Scott-type Spray Chamber later in this chapter.

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.
5-22 Maintenance

Copper Foil
(Part No.
N077-5297) Torch Glass
(Part No.
N077-0338)

Torch Cutout Knurled Nut

(Part No.
N077-6027)

Washer
(Part No.
N077-6028)

O-Ring Spacer
(Part No. (Part No.
0990-2223) N077-6029)

Stripe on Torch
O-Ring
(Part No.
0992-1062)
O-Ring
(Part No.
0992-1061) O-Ring
(Part No.
0990-2131) Index Mark
on Torch Holder

Torch
Coupler

Guide Pin

Figure 5-5. Replacing the torch. (Part Number for O Ring Kit is N077-0437.)
 Quick-Change Torch Module for the Optima 5000 Series DV 5-23

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. See step two
above, on how to use this feature. The other end can be inserted
into the torch holder to remove O-rings (Part No. 0992-1028 for
the larger O-rings or N077-6024 for the smaller O-rings) or
Injector Seal Nut (Part No. N077-6036) 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.

Note For a complete set of spare Injector Adapter O-rings order Kit Part
No. N077-0438.
5-24 Maintenance

Injector
Positioning
Tool
(Part No.
N077-0602)
Injector
Seal Nut
(Part No.
N077-6036)

Injector Seal
Washer (open side up)
(Part No. (Part No.
N077-6014) 0992-3509)

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

 Quick-Change Torch Module for the Optima 5000 Series DV 5-25

Torch Coupler
Spray Chamber Clamp
(Part No. N077-6031)

Injector
(Part No.
N077-5177)

Knurled Nut

Lock Collar Injector Lock

Injector O-Ring (Part No.
O-Rings Adaptor (Part No. N077-6025)
(Part No. (Part No. 0990-2207)
0992-1028) N077-6024)
Washer
(Part No.
N077-6014)
Injector
Injector Positioning
Positioning
Tool
Tool (Part No.
(Part No. N077-0602)
N077-0602)
Injector
Seal Nut
(Part No.
N077-6036)
Injector
(1 ½ mm set Injector Seal
below inner glass) Washer (open side up)
(Part No. (Part No.
N077-6014) 0992-3509)

Figure 5-7. Inserting the injector.

5-26 Maintenance

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.
 Quick-Change Torch Module for the Optima 5000 Series DV 5-27

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.
5-28 Maintenance

O-Ring
(Part No. 0990-2045)

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 torch compartment.

 Quick-Change Torch Module for the Optima 5000 Series DV 5-29

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 Figure 5-10.

Caution When installing the spray chamber/nebulizer end cap make sure that the
end cap screws are not perpendicular to the door. The door will not close
properly unless the screws are rotated so that they are at a slight angle to
the door.

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.
5-30 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.(If you need, at some point, to release
the NEB tubing from the quick connect, push on the quick disconnect to
disconnect the NEB tubing.)

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 Torch Module for the Optima 5000 Series DV 5-31

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.
5-32 Maintenance

Torch Module for the Optima 5300V

The torch module for the Optima 5300V consists of a vertical torch assembly,
cyclonic spray chamber, and low flow gemcone nebulizer. These components can
be 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 vertical 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 1.2 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 is mounted vertically
and has one or more slots. 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. two vertical torch
assemblies are available. Once assembly is for the analysis of oils and the other
assembly is Hf resistant.
 Installing the Torch Module for the Optima 5300V 5-33

Installing the Torch Module for the Optima 5300V

Follow this procedure to replace the torch module in the Optima 5300V.

Before installing the 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.

Note During shipment the bonnet will be secured to the RF coil with a tie wrap.
Remove the tie wrap before you begin the torch module installation
procedure

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. Wear latex, rubber or cotton gloves when handling the
glassware. To remove the alkali, wipe the glassware clean with cotton
wool dipped in alcohol.
5-34 Maintenance

To install the torch module follow these steps and see the following figure:

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.

Installing the Torch Module Assembly

1. Turn off the plasma if it is on.

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

3. 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

4. Carefully remove the torch module assembly from its box.

5. Holding the torch assembly securely with one hand 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. Make sure
that the bonnet securely rest on the coil and top of the torch.

6. Still holding on to the torch assembly with one hand use your other hand to set
the height adjustment to -3 on the scale located on the dovetail mount (as
shown in the following figure).

7. While still holding on to the torch assembly with one hand use your other hand
to tighten the side knurled nut located on the dovetail mount.

8. The unit is now securely in place and you can proceed to attach the quick
disconnect fittings.
 Installing the Torch Module for the Optima 5300V 5-35

9. Connect the Auxiliary Gas Quick Disconnect Fitting by pushing the fitting on
to the bottom glass arm of the torch.

10. Connect the Plasma Gas Quick Disconnect Fitting (with the ignitor pin in it)
by pushing the fitting on to the top glass arm of the torch.

11. You have completed the torch assembly procedure and you need to now attach
the cyclonic spray assembly.
5-36 Maintenance

Ground
Pointer

Plasma Gas
Quick Torch
Disconnect
Aux Gas
Quick RF Coil
Disconnect
Top Thumb
Screw
Scale
Bottom Thumb
Screw

Figure 5-11. Installing the torch into the sample compartment of the
Optima 5300V.
 Installing the Torch Module for the Optima 5300V 5-37

Slot

RF Coil

Torch

Figure 5-12. Quartz torch (O-ring Part No. N077-0437).

Removing the Torch Module Assembly

You may need to remove the torch module assembly to inspect it and replace it.
Follow this procedure and refer to the previous two figures.

1. Turn off the plasma if it is on.

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

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

When removing the torch module in the next steps, do so

! carefully so you will avoid breaking the torch and risking
possible injury.
Warning
5-38 Maintenance

4. Holding the cyclonic spray chamber assembly carefully disconnect the

cyclonic spray chamber clip and lay the spray chamber assembly (including the
GemCone nebulizer) at the bottom of the instrument compartment. If you need
to remove the spray chamber assembly see the procedure Removing the
Cyclonic Spray Chamber later in this chapter.

5. Disconnect the Plasma Gas Quick Disconnect Fitting (with the ignitor pin in
it) from the top glass arm of the torch. Disconnect the Auxiliary Gas Quick
Disconnect Fitting from the bottom glass arm of the torch.

6. Holding on to the torch assembly with one hand use your other hand to loosen
the side knurled nut located on the dovetail mount.

7. Still holding the torch assembly securely with one hand carefully slide the
torch out from under the RF coil and bonnet. Make sure that the bonnet is still
securely resting on the RF coil.

Take the torch assembly and lay it down in a flat, safe location. Once a month
inspect the torch and o-rings for signs of wear (brittle or discolored) and replace if
damaged. Use an allen wrench to remove the screws from the bottom of the plastic
torch clamp to check O-rings and replace if the O-rings show signs of wear.

Cyclonic Spray Chamber for the Optima 5300V

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. the cyclonic spray chamber is the only spray chamber used
with the vertical torch.

Three cyclonic spray chamber options are available. You can use a large baffled
(8mm) cyclonic spray chamber (Part No. N077-6053) for aqueous solutions that
cause the plasma to become unstable or extinguishes frequently. You can use a
cyclonic spray chamber without a baffle (Part No. N077-6052) for aqueous
solutions analysis. Lastly you can use a narrow baffled (4mm) cyclonic spray
chamber (Part No. N077-6090) for organics.
 Cyclonic Spray Chamber for the Optima 5300V 5-39

Installing the Cyclonic Spray Chamber

The following procedure describes how to install the cyclonic spray chamber. the
vertical torch uses either a baffled cyclonic spray chamber (Part No. N077-1501)
which is used for oils analysis or and unbaffled a cyclonic spray chamber (Part No.
N077-1543). See the following figure.

The l baffled and unbaffled cyclonic spray chamber can be order

Note with or without the cap. The narrow baffled (4mm) cyclonic
spray chamber assembly (Part No. N077-6053) does not come
with a cap. You must order this cap separately as needed. A cap
(Part No. N077-6052) does not have to be ordered with every
replacement cyclonic spray chamber. Caps can be reused for
either the baffled or unbaffled cyclonic spray chambers.

See Table 4-4 in the Installation chapter or Table 5-4 and Table
5-14 later in this chapter for part numbers.

1. Remove the The cyclonic spray chamber, cyclonic spray chamber spring clip
and low flow gemcone nebulizer from the box.

2. Turn off the plasma if it is on.

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

4. Install the drain capillary to the bottom of the cyclonic spray chamber.

5. Install the GemCone nebulizer into the cyclonic spray chamber. See the
following figure.
5-40 Maintenance

Capillary
Tubing
(Part No.
0990-8265)

Teflon
Tubing (1 in.)
(Part No.
0998-5708)

GemCone
Nebulizer
Assembly
Cyclonic
Spray Chamber

Nebulizer Gas Fitting

Figure 5-13. Installing the GemCone nebulizer into the cyclonic spray chamber.

6. Install the sample capillary tubing into the nebulizer.

7. Attach the nebulizer gas fitting and finger tight (do not use a wrench).

8. Then place the cyclonic spray chamber assembly at the base of the
compartment.

9. Secure the cyclonic spray chamber clip to the base of the cyclonic spray
chamber (see the following figure).

10. Feed the drain and sample tubing through the side of the instrument
compartment.
 Cyclonic Spray Chamber for the Optima 5300V 5-41

Ground
Pointer

Torch

Drain RF Coil
Tubing

Sample
Tubing

Spring
Clip
Cyclonic
Spray
Chamber

Figure 5-14. The torch and cynic spray chamber.

5-42 Maintenance

Torch
Bracket

Torch
Mount

Spring
Clip

Cyclonic
Spray
Chamber

Figure 5-15. Quartz torch (O-ring Part No. N077-0437).

 Cyclonic Spray Chamber for the Optima 5300V 5-43

Removing the Cyclonic Spray Chamber

You may need, on occasion, to remove the cyclonic spray chamber. Following this
procedure and refer to the previous two illustration.

1. Turn off the plasma if it is on.

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

3. Disconnect the drain and sample tubing from the cyclonic spray chamber
assembly.

4. Disconnect the argon gas fitting and the capillary tubing from the GemCone
nebulizer assembly.

5. Carefully holding on to the cyclonic spray chamber remove the cyclonic spray
chamber clip. Place the clip in a safe location.

6. Remove the cyclonic spray chamber and the GemCone nebulizer from the
instrument.

Inspect the spray chamber and nebulizer for wear. If the spray chamber is broken
or shows signs of wear replace.

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. Contact your PerkinElmer Service Representative
to replace and adjust the RF coil.

Replacing the RF Coil

The RF coil may need to be replaced occasionally as a result of overheating,
pitting, or arcing. Contact your Perkin Elmer Service Representative to replace the
RF coil Replace with a new RF coil and tighten the Brass Swagelok nuts until hand-
tight then tighten an additional 1/4 turn.
5-44 Maintenance

Table 5-2. Replacement Parts: Torch Assembly

OPTIMA 5000 Series Dual View Instruments

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
N077-0343 Long Torch
N077-5289 Quartz Bonnet
N077-5227 Alumina Injector, 0.8 mm i.d., 141 mm LG
N077-5228 Alumina Injector, 1.2 mm i.d., 141 mm LG
N077-5177 Alumina Injector, 2.0 mm i.d., 141 mm LG
(standard injector)
N077-5225 Quartz Injector, 0.8 mm i.d., 141 mm LG
N077-5226 Quartz Injector, 1.2 mm i.d., 141 mm LG
N077-5223 Quartz Injector, 1.6 mm i.d., 141 mm LG
N077-5014 Quartz Injector, 2.0 mm i.d., 141 mm LG
N077-5247 Sapphire Injector, 2.0 mm i.d., 141 mm LG

N077-6027 Knurled Nut

N077-0604 Torch Holder Assembly

 Cyclonic Spray Chamber for the Optima 5300V 5-45

Table 5-2. Replacement Parts: Torch Assembly

OPTIMA 5000 Series Dual View Instruments

Part No. Description

N077-0603 Injector Adapter Assembly

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

N077-6036 Injector Seal Nut

N077-0438 Injector Adapter O-Ring Kit

N077-0437 Torch Glassware O-Ring Kit

N077-0602 Injector Positioning Tool Kit

Table 5-3. Replacement Parts: Torch Assembly

OPTIMA 5300V Instrument

Part No. Description

N077-0910 Torch Assembly- OIL (includes torch, glass-

ware, injector (Alumina Injector, 1.2mm i.d.),
Baffled Cyclonic Spray Chamber & Low
Flow GemCone Nebulizer
N077-0911 Torch Assembly - HFR (includes torch,
glassware, injector (Alumina Injector, 2.0mm
i.d.), HFR Spray Chamber - TC44 Cyclonic
& Highs Solids Nebulizer
N077-1500 Quartz Torch
N077-5289 Quartz Bonnet
N077-1531 Alumina Injector, 1.2 mm i.d., 83 mm LG
(Standard with N077-0910 OILS Torch)
5-46 Maintenance

Table 5-3. Replacement Parts: Torch Assembly

OPTIMA 5300V Instrument

Part No. Description

N069-5362 Alumina Injector, 2.0 mm i.d., 83 mm LG

(Standard with N077-0911 HRF Torch)
N077-0358 Low Flow GemCone Nebulizer
N069-0670 High Solids Nebulizer
N077-0336 Quick Disconnect Tubing Assembly (for
High Solids Nebulizer)
N077-1501 Baffled Cyclonic Spray Chamber
N077-1550 HF Resist Spray Chamber - TC44 Cyclonic
N077-1526 Injector Support Fitting (bottom half)
N077-1527 Injector Support Fitting (top half)
0990-2155 O-Ring (for Torch Clamp)
0990-2207 O-Ring (for Torch Injector Fittings bottom &
top-2 required)
0990-2247 O-Ring (for Torch Glassware seal-2 required)
0992-6070 O-Ring (for Spray Chamber Ball Mount)
0921-0005 Locking Set Screw for Torch Height Adjust-
ment
N077-1509 Torch Clamp
N077-1518 Block
 Purge Window/Tubes 5-47

Purge Window/Tubes
It may become necessary to remove and clean the radial purge window tube or the
axial purge window. If the purge windows crack, it will be necessary to replace
them.

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 need 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.

Cleaning the Purge Windows

If you have been analyzing aqueous solutions, the glassware 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 manufacturers
safety recommendations. These recommendations are normally provided in a
material safety data sheet (MSDS) supplied with the chemical.

Note Avoid getting fingerprints on the purge windows.

5-48 Maintenance

If you have been analyzing organic solutions, the glassware can be cleaned using a
solvent or diluted soap solution. Be sure to inspect the glassware often for carbon
buildup.

Rinse glassware and O-rings with deionized water.

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

O-rings may be cleaned with soap and water. An ultrasonic bath may be used.
Replace if cracked or worn. Part numbers are located in a table later in this section.

Removing the Radial Purge Window Tube

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.

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 procedures.
Warning

2. Open the front door to the sample compartment.

 Purge Window/Tubes 5-49

3. Remove the torch.

Caution If a spill occurs in the sample compartment, clean off the spill from the
radial purge window and remove. Complete the cleaning process away
from the instrument. This will protect and prevent contamination of the
focusing mirror, which is below this window.

4. See the following figure. Carefully grasp the radial purge window and gently
lift it off the tube plug.
5-50 Maintenance

Instrument
Left Side

Axial Purge
Window
(Part No. N077-1116)

Radial Purge
Window
(Part No. N077-0944)

O-Rings
(Part No. 0920-0064)

Tube Plug

Figure 5-16. Location of the purge windows on the Optima 5100, 5200
and 5300 DV.
 Purge Window/Tubes 5-51

5. Clean the window (as described earlier) or replace.

6. The radial purge window assembly has two O-rings. Inspect the O-rings and
either clean them (as described earlier) or replace them.

7. Then reinstall the window according to the next procedure.

Replacing the Radial Purge Window Tube

Refer to the previous figure when performing the steps below.

1. If needed put the new O-rings (Part Number 0920-0064) in the groves of the
tube plug.

2. Gently push down the radial purge window tube (Part No. N077-0944), as far
as it will go, into the tube plug and over the O-rings. Take care not to get
fingerprints on the face of the viewing window.

Note When adjusting the radial purge window tube note that the closer the tube
is to the torch the better the UV performance will be. In this higher position
the glass will get more coated and wear out more quickly than if it is in a
lower position relative to the torch.

Removing the Axial Purge Window

The axial purge window is located inside the axial purge window assembly on the
dual view casting. Refer to the previous figure for the location of the axial purge
window.

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 procedures.
Warning
5-52 Maintenance

2. Open the front door to the torch compartment.

3. Remove the torch.

4. Twist the axial purge window assembly (which consists of the axial window
cap and the axial window holder) counter clockwise so that it unlocks from the
shoulder screws which are part of the axial window mount (Part No. N077-
3086) and pull it out of the mount. Remove the axial purge window assembly
from the torch box and place it on a table where you can disassemble it.

Mount
Shoulder Screw (2)
0991-9740

2mm Hex Key

0990-7917 O-Ring
0990-2143

Window
N077-1116

O-Ring, 0990-2155

Flat Head Screw (2)

0991-9791
Purge Tubing
Axial Window Holder, N077-3090 from Spectrometer

Axial WindowCap
N077-3084

Figure 5-17. Axial purge window.

5. Use the 2 mm hex key (Part No. 0990-7917) to unscrew one flat head screw
(Part No. 0991-9791) and loosen the other screw so that the two halves of the
assembly that secure the axial window cap to the axial window holder can be
twisted apart.

6. Remove the purge window (Part No.N077-1116) and the O-ring from the axial
window holder.

7. Clean the purge window as described earlier.

 Purge Window/Tubes 5-53

8. If needed place a new O-ring (Part No. 0990-2143)in the recessed bore of the
axial window holder (see the following figure). Place the cleaned purge
window in the recessed bore on top of the O-ring. Also the O-ring (Part No.
0990-2155) located in the groove on the back of the axial window holder may
need to be replaced.

9. Place the axial window cap in front of the axial window holder (with the
cleaned purge window and new O-ring) and reattach the two flat head screws.

10. Orient the axial purge window assembly so that the notch on the axial window
holder lines up with the purge tube fitting. See the following figure.

"O" Ring
Notch

Purge Tube Fitting

Screw

Figure 5-18. Axial window holder alignment.

11. Push the assembly into the mount and twist the axial purge window assembly
(which consists of the axial window cap and the axial window holder)
clockwise so that it locks with the shoulder screws which are part of the axial
window mount.
5-54 Maintenance

Table 5-4. Replacement Parts: Purge Components

Part No. Description

N077-0944 Radial Purge Quartz Window Tube (long)

for DV instruments

0920-0064 O-rings, Radial Purge Window Tube

for DV instruments

N077-1116 Axial Purge Quartz Window

for DV instruments

0990-2143 O-ring, Axial Purge Window

for DV instruments

0990-7917 2 mm Hex Key for Purge Window

Removing the Purge Window for the Optima 5300V

The purge window is mounted in the ceramic purge window holder. Refer to the
next figure for the location of the purge window.

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 procedures.
Warning

2. Open the front door to the torch compartment.

3. Carefully lift up and remove the purge window from the ceramic purge
window holder.
 Purge Window/Tubes 5-55

4. Clean or replace the window by following the procedures earlier in this chapter
and return the window to the holder.

Ceramic Purge
Window Holder

Figure 5-19. Location of the purge window on the Optima 5300V.

5-56 Maintenance

Removing the Ceramic Purge Window Holder for the Optima 5300V
The ceramic purge window holder can be removed if you suspect a leak and need
to check the O-ring. Refer to the previous figure for the location of the ceramic
purge window holder.

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 procedures.
Warning

2. Open the front door to the torch compartment.

3. Carefully lift up and remove the purge window from the ceramic purge
window holder.

4. Unscrew the knurled nut that holds the ceramic purge window holder in place.

5. Examine the O-rings if it shows signs of wear replace it.

Table 5-5. Replacement Parts: Purge Components

Part No. Description

N058-1497 Purge Window for the Optima 5300V in-

struments

N058-1455 Ceramic Purge Window Holder

N069-5146 Purge Window Nut

N069-5258 O-ring
 Adjusting the Position of the Shear Gas Nozzle 5-57

Adjusting the Position of the Shear Gas Nozzle

The position of the shear gas nozzle is important to prevent the degradation of the
purge interface from hot plasma exhaust gases. See the following figure for the
location of the shear gas nozzle.

If the plasma has been on, the torch and dual view parts will
! be very hot and can cause serious burns. Wait five minutes
after turning off the plasma before you begin this procedure.
Warning

The nozzle should be positioned as shown in the next figure. Line up a straight edge
with the front of the axial purge window assembly and measure the distance
between the straight edge and the slit in the shear gas nozzle. This should be
approximately 6 mm (1/4-in.).
5-58 Maintenance

Instrument
Left Side

Shear Gas
Nozzle

Figure 5-20. Location of the shear gas nozzle.

 Adjusting the Position of the Shear Gas Nozzle 5-59

To adjust the position of the shear gas nozzle:

1. Loosen the thumbscrews securing the nozzle.

2. Reposition the nozzle as necessary.

3. Tighten the thumbscrews.

6 mm

Shear Gas Axial Purge

Nozzle Window
Radial Purge
Window

Thumbscrews

Figure 5-21. Adjusting the position of the shear gas nozzle.

Note The shear gas nozzle should be positioned so that shear gas is
directed at a 90-degree angle to the torch. If necessary, adjust the
nozzle using the clearance in the holes around the thumbscrews.
5-60 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 5-61

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 5-22. Spray chamber, end cap, and associated parts. (Illustration shows
cross-flow nebulizer end cap assembly, Part No. N058-0613.)

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.
5-62 Maintenance

Cyclonic Spray Chamber for the Optima 5100, 5200 and 5300 DV
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.

Three cyclonic spray chamber options are available. You can use a large baffled
(8mm) cyclonic spray chamber (Part No. N077-6053) for aqueous solutions that
cause the plasma to become unstable or extinguishes frequently. You can use a
cyclonic spray chamber without a baffle (Part No. N077-6052) for aqueous
solutions analysis. Lastly you can use a narrow baffled (4mm) cyclonic spray
chamber (Part No. N077-6090) for organics.

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), a
large baffled (8mm) cyclonic spray chamber assembly (Part No. N077-6053) or a
narrow baffled (4mm) cyclonic spray chamber assembly (Part No. N077-6090).
See the following two figures.

The large baffled (8 mm) and unbaffled cyclonic spray chamber

Note can be order with or without the cap. The narrow baffled (4mm)
cyclonic spray chamber assembly (Part No. N077-6090) does
not come with a cap. You must order this cap separately as
needed. A cap (Part No. N077-0614) does not have to be ordered
with every replacement cyclonic spray chamber. Caps can be
reused for either the baffled or unbaffled cyclonic spray
chambers.

See Table 4-3 in the Installation chapter or Table 5-4 and Table
5-14 later in this chapter for part numbers.

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 (Part No. N077-0614). Insert the
cyclonic spray chamber into the cyclonic spray chamber cap. Slide the cap
closed. See the following figure.
 Cyclonic Spray Chamber for the Optima 5100, 5200 and 5300 DV 5-63

Cyclonic Spray Chamber

Cyclonic Spray
Chamber Cap
(opened position)

Cyclonic Spray Chamber

(seated in cap)

Cyclonic Spray
Chamber Cap
(closed position)

Figure 5-23. Installing the cyclonic spray chamber into the cyclonic spray cham-
ber cap.
3. Slide the chamber into the injector adapter. 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
downward angle of the cyclonic spray chamber. The cyclonic spray chamber
must point in a downward direction to allow the spray to flow away from the
nebulizer. This angle will remain locked even if you later remove the cyclonic
5-64 Maintenance

spray chamber from the instrument. Future installations will not require any
readjustments.
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. 0992-0186). See the following figure.

Nebulizer
Adapter
(Part No.
N077-6006)

O-Rings
(Part No.
N077-6007)

Tubing Coupler
(Part No.
0992-0865)

Tygon Tubing
(Part No.
0250-6516)

Figure 5-24. Installing the cyclonic spray chamber.

 Cyclonic Spray Chamber for the Optima 5100, 5200 and 5300 DV 5-65

5. To the open end of the tubing coupler (Part No. 0992-0186) 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,
Warning storage and disposal. These recommendations are 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.

5-66 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 5-6. Replacement Parts: Spray Chambers

Part No. Description

N077-0357 Ryton Double-Pass Scott-Type Spray Chamber

N077-6052 Cyclonic Spray Chamber for aqueous solutions
N077-6053 Wide Baffled (8 mm) Cyclonic Spray Chamber
N077-0605 Cyclonic Spray Chamber with Cap for Aqueous
Solutions
N077-0612 Wide Baffled (8 mm) Baffled Cyclonic Spray
Chamber with Cap
N077-6090 Narrow Baffled (4 mm) Cyclonic Spray Chamber
N077-0608 External Spray Chamber Mount
For use with high-volatility organic solutions.
N077-0614 Cap for either the Baffled or Unbaffled Cyclonic
Spray Chamber.
 Nebulizers 5-67

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 5-7. 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
Mira Mist 1 L/min 1 L/min
5-68 Maintenance

Table 5-8. Replacement Parts: Nebulizers and End Caps

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

N069-0676 GemTip Replacement Nebulizer Tips for GemTip Cross-Flow Neb-

ulizer

N069-0670 High Solids GemCone Nebulizer

N077-0358 Low-Flow GemCone Nebulizer

N068-0504 Scott-Type Spray Chamber End Cap for GemCone and concentric
glass nebulizers

N077-6006 Nebulizer Adapter

N077-6007 O-Rings for Nebulizer Adapter

N077-0621 Concentric Glass Nebulizer, MEINHARD Type A

N077-0622 Concentric Glass Nebulizer, MEINHARD Type C

N077-0623 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

N077-5330 Mira Mist Nebulizer

 GemTip Cross-Flow Nebulizer 5-69

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.

5-70 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 5-25. The nebulizer/end cap assembly removed from the spray chamber.
Illustration 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 5-71

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.
5-72 Maintenance

Red GemTip
Argon
Clear GemTip Inlet

Sample
Inlet

Figure 5-26. 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 5-73

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.

5-74 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 5-27. Clear GemTip for sample inlet and associated parts for Cross-Flow
End Cap, N077-0546.
 GemTip Cross-Flow Nebulizer 5-75

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 5-28. 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.
5-76 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 5-77

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 5-29. 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. 0998-5723). 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. 0998-5723).

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.
5-78 Maintenance

Ferrule (Part No. 0992-0515)

Nut (Part No. 0992-0545)

1/8-in. O.D. Tubing

(Part No. 0998-5723)

Figure 5-30. 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. 0998-5723) through the nut (Part No. 0992-0545) and
attach the ferrule on the end of the tubing. See the previous 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 sample introduction
system. See the following figure.
 GemTip Cross-Flow Nebulizer 5-79

Ferrule (Part No. 0992-0515)

Nut (Part No. 0992-0545) Quick Disconnect-Male (Part No. N077-5206)

1/8-in. Tubing
(Part No. 0998-5723)

Quick Disconnect-Female
(Part No. 0992-00861)

Instrument
Left Side
Nut (Part No. 0992-0545)

Ferrule (Part No. 0992-0515)

Figure 5-31. Connecting the nebulizer argon tubing. Cross-Flow End Cap,
N077-0546.

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.
5-80 Maintenance

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.

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.
 GemCone Nebulizer 5-81

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.
5-82 Maintenance

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. N068-0504) 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. N068-0504) to the spray chamber with
a twisting action.Alternately 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.

 GemCone Nebulizer 5-83

Figure 5-32. 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.
5-84 Maintenance

3. Insert the nebulizer into the cyclonic spray chamber as shown in the next
figure. The nebulizer may be inserted to its fullest extent.

Capillary
Tubing
(Part No.
0990-8265)

Teflon
Tubing (1 in.)
(Part No.
0998-5708)

Torch Coupler
GemCone
Nebulizer
Assembly
Cyclonic
Spray Chamber

Argon Gas Fitting

Figure 5-33. 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.
 GemCone Nebulizer 5-85

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 a minimum

of 5 to a maximum of 30 minutes depending on the type of deposit.

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

Installing the GemCone Nebulizer on the Cyclonic Spray Chamber on

the Optima 5300V
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.

3. Install the GemCone nebulizer into the cyclonic spray chamber. See the
following figure.
5-86 Maintenance

Capillary
Tubing
(Part No.
0990-8265)

Teflon
Tubing (1 in.)
(Part No.
0998-5708)

GemCone
Nebulizer
Assembly
Cyclonic
Spray Chamber

Nebulizer Gas Fitting

Figure 5-34. Installing the GemCone nebulizer into the cyclonic spray chamber.

4. Install the sample capillary tubing into the nebulizer.

5. Attach the nebulizer gas fitting and finger tight (do not use a wrench).

6. Then place the cyclonic spray chamber assembly at the base of the
compartment.

7. Secure the cyclonic spray chamber clip to the base of the cyclonic spray
chamber (see the following figure).

8. Feed the drain and sample tubing through the side of the instrument
compartment.

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).
 Concentric Glass Nebulizer 5-87

2. Disconnect the argon gas fitting and the capillary tube connection from the
nebulizer.

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 a minimum

of 5 to a maximum of 30 minutes depending on the type of deposit.

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

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 (Part No. 0992-3512). Insert this tubing as far into the
concentric nebulizer as possible.
5-88 Maintenance

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.

Concentric Nebulizer Viton Black-Black Tubing

Capillary Tubing

Clamp

Argon Line

Figure 5-35. 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 5-89

End Cap Assembly

Part No. N068-0504

Meinhard
Concentric Nebulizer

Figure 5-36. Installation of the Concentric Glass Nebulizer in the End Cap.

Installing the Concentric Glass Nebulizer into the Cyclonic Spray

Chamber
In the analysis of organics the best results are achieved when the concentric glass
nebulizer is with the cyclonic spray chamber.

1. Insert the cyclonic spray chamber into the cyclonic spray chamber cap. See
Figure 5-18.

2. Install the cyclonic spray chamber onto the torch coupler. See Figure 5-18.

3. Insert the tapered end of the concentric glass nebulizer, as far as it will go,
through the opening in the cyclonic spray chamber.
5-90 Maintenance

Cleaning Concentric Glass Nebulizer and Cyclonic Spray Chamber

When analyzing organics the concentric glass nebulizer needs to be cleaned on a
daily basis due to carbon buildup. Two methods are available:

• Place the concentric glass nebulizer in a muffle furnace for approximately two
hours. -Or-

• Place the concentric glass nebulizer in an acid wash which should be heated up
(but not boiling) for approximately two hours. The acid wash is Aqua Regia
which is a 3:1 solution of HCL and HNO3.

After running organics rinse out the cyclonic spray chamber. Drain tubing should
be replaced when the tubing becomes hard and brittle. The torch can crack when
there is too much carbon build up. It can be cleaned using the same procedures as
listed above for the concentric glass nebulizer.

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: http://www.meinhard.com

The following table summarizes the cleaning procedures for the MEINHARD
Concentric Glass nebulizer.
 Mira Mist Nebulizer 5-91

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 5-37. Cleaning Strategy for the MEINHARD Nebulizer.

(Reprinted with the permission of JE Meinhard Assoc., Inc.)

Mira Mist Nebulizer

This device operates on compressed gases. Appropriate care

must be taken. If in doubt about correct operating procedures, call
! an experienced operator. Burgener Mira Mist Nebulizers require
45 - 55 psi to have a 1 liter per minute of Argon gas flow, so the
Warning operating pressures are in the range of 25 - 45 psi, depending on
the torch optimum flow rate.

Mira Mist nebulizers will pulse if the pump can not deliver
constant sample flow: Change your pump tubing often, or use a
surgless pump if possible.

Caution The gas orifice is at the very tip of the nebulizer. It is made of Teflon which
is VERY SOFT. This tip is very easily damaged and should NEVER be
touched with fingers, tissues, or anything else. If the tip is accidentally
touched, and the nebulizer continues to operate, then it is still functional,
and its use can be safely continued.
5-92 Maintenance

Sample Capillary Tubing

Note The PEEK Mira Mist body has 10/32 threads for the gas and capillary
fittings. Gently tighten until snug for the sample line. For the gas line, if
there seems to be any leakage, then tighten HARD. PEEK is very strong.

The capillary tubing is attached with UpChurch® 10/32 chromatographic fittings.

We supply.043" OD X.017" ID Poly Capillary tubing, but you may use any other
tubing that fits an UpChurch 10/32 fitting. We recommend that you use a 0.017"
ID or smaller ID capillary tube for the sample feed. This should catch any particles
before they get into the nebulizer. It is much safer & easier to replace the capillary
tubing than to clean the nebulizer.
The Mira Mist Nebulizer body is PEEK, the inner capillaries are Teflon. Generally
it will not break. If it is dropped such that the tip is deformed, then it will be
irreparably damaged. If it continues to operate after being dropped, then it has not
been affected, and its use can be safely continued.

Gas Line
The gas line is attached with UpChurch® 10/32 chromatographic fittings. We
supply 2 mm OD X.039" ID Teflon tubing. A gas line filter is NOT included in the
nebulizer. Any particles from the gas line will destroy the nebulizer. We have
found this is one of the main causes of blockage of our nebulizers, so please ensure
that the gas line to the nebulizer is clean of any particles.
The gas line terminates in the standard Optima 5000 and 2000 Series quick
disconnect. It is a direct replacement for typical concentric nebulizers.

Sample Introduction / Maximizing Stability

The Mira Mist does not have any suction, so it requires a pump to supply the
sample solution. The pump speed and the quality of the pump tubing have a large
effect on the performance of the nebulizer. Try to select a pump tubing size that
allows running the pump at a higher speed (If you use the standard black-black
tubing you may need to use a higher pump rate: for example 1.5 mL/min). So for
low sample flow, use orange green or orange blue pump tubing. Generally the
pump tubing should be changed Every Day for maximum stability and lowest %
RSD.
 Peristaltic Pump 5-93

Cleaning the Nebulizer

Caution The gas orifice is at the very tip of the nebulizer. It is made of Teflon which
is VERY SOFT. This tip is very easily damaged and should NEVER be
touched with fingers, tissues, or anything else. If the tip is accidentally
touched, and the nebulizer continues to operate, then it is still functional,
and its use can be safely continued.

For the longest life and best performance, wash your nebulizer by simply running
water as a sample for 10 minutes at the end of the day before shutting down the
plasma. Any other form of washing is usually unnecessary. DO NOT wash your
nebulizer in acid or solvents to "prevent salt build up". DO NOT use surfactants as
they will destroy the surface tension at the tip and performance.

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 up.The following table gives part numbers for pump tubing for the sample and
drain.
5-94 Maintenance

Table 5-9. 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 0992-3512
Xylene 0.89 mm (0.035 in.)
not MIBK.* Drain: Yellow-Yellow 0992-3511
1.40 mm (0.056 in.)

*Silicone tubing is not recommended for use with kerosene or xylene.

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.
 Peristaltic Pump 5-95

From
Spray Chamber

To Drain Bottle
To Nebulizer

From Sample
Container

Figure 5-38. 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 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.
5-96 Maintenance

Cover Door
Spray Chamber

Lip

Peristaltic
Pump Tubing

Figure 5-39. 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.

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.
 Peristaltic Pump 5-97

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 5-40. 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.
5-98 Maintenance

Table 5-10. Spray Chamber Drain Spare Parts

Part No. Drain Spare Part

0992-0267 Barbed Fitting

0998-5735 Solvent Flex Tubing, 0.11 mm i.d. (PVC tubing)
N069-5415 Sleeve
N069-5414 Adapter
0992-0186 Tubing Coupler
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. 0998-5735)
to the barbed fitting (Part No. 0992-0267).
2. Cut the 1 mm i.d. tubing at an angle and insert it into the 1.5 mm tubing.

The External Drain Kit Part Number is N077-0613.

Connecting the Drain Tubing Assembly

To connect the drain tubing assembly, use the following steps and refer to the next
figure.

1. Connect the sleeve (Part No. N069-5415) and adapter (Part No. N069-5414) to
the spray chamber drain. Thread the barbed fitting (Part No. 0992-0267) into
the coupler and adapter.

2. Attach the Solvent Flex (PVC) tubing (Part No.0998-5729) to the barbed
fitting. Attach the other end of the Solvent Flex (PVC) tubing to the tubing
coupler (Part No. 0992-0186). See the following figure.

3. Use the other end of the tubing coupler (Part No. 0992-0186) to connect the
drain tubing to the peristaltic pump tubing. See the following figure.
 Peristaltic Pump 5-99

Spray Chamber

Coupler
Sleeve PVC Tubing, 1.5 mm i.d. (Part No.
(Part No. N069-5415) (Part No. 0998-5735) 0992-0186)

Adapter
(Part No. N069-5414)
Spray Chamber Drain Tubing Parts:
Barbed Fitting Adapter, Barbed Fittings, and Tubing
(Part No. 0992-0267)

Teflon Tubing Pump Tubing 1.14 mm i.d.

1 mm i.d.
(Part No. N822-1152)

Drain Bottle

Figure 5-41. 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.

5-100 Maintenance

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 5-35. 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 5-36 in the Drain section later in this
chapter.

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.
 Peristaltic Pump 5-101

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.

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.

5-102 Maintenance

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 5000 series. 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.
 Peristaltic Pump 5-103

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.

Solvent Flex
Tubing, 1.5 mm i.d. Coupler
(Part No. 0998-5735) (Part No. 0992-0186)

Figure 5-42. Tubing connections to the drain bottle.

5-104 Maintenance

Table 5-11. 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

Cleaning the Instrument

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

Air Filters
To ensure that the electrical components in the spectrometer and the RF generator
are properly cooled, check the air filters regularly. There are two air filters on the
instrument as shown in the figure below. One filter is for the generator and one
filter is for the spectrometer.

Changing the RF Generator Air Filter

Two generator air filters are provided with the instrument. Refer to the following
figure.

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.
 General System Maintenance 5-105

To remove, slide filter

in this direction.

RF Generator Filter
Spectrometer Filter (Mesh side out)
(In front of fan) Part No. N077-5220
Part No. 0999-5098

Figure 5-43. Location of the spectrometer and RF generator air filters on the
instrument.

Changing the Spectrometer Air Filter

The filter for the spectrometer cooling is inside the snap-on plastic grid. Two
spectrometer air filters are provided with the instrument. Refer to the following
figure.
1. Shut down and switch off the spectrometer.
2. To remove the spectrometer air filter, carefully pull off the snap-on plastic grid
that holds the air filter in place (see the following figure).
3. Clean or replace the filter (Part No. 0999-5098). The filter may be washed with
water, but replace it with the other filter. This insures that a completely dry
filter is in the instrument.
4. Carefully push the plastic grid onto the ventilator.
5. Power up the instrument.
Replacement filters (Part No. 0999-5098) are included in the spares kit.
5-106 Maintenance

Figure 5-44. Removing the spectrometer air filter.

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 5-12. Filters

Part No. Description

N077-5220 Air Filter for Generator

0999-5098 Air Filter for Spectrometer
0990-4845 Cooling Water Filter
0990-4846 Cooling Water Filter Cartridge,
replacement for Water Filter 0990-4845
 General System Maintenance 5-107

Table 5-13. Solutions

Part No. Description

N058-2152 Calmix 3 Test mix (for wavelength calibration)

N930-2946 VIS Wavelength Calibration Test Mix
N077-6099 Solution for Chiller

Table 5-14. Gas and Water Supply Connections

Part No. Description

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

0999-5098 Air filter-Spectrometer

0992-0125 Space Collar for 1/4-in. Swagelok fittings

5-108 Maintenance

Table 5-15. 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

Table 5-16. Organic Sample Introduction Kit (Part No. N077-0420)

Part No. Description

09902207 O-ring

0992-1028 O-ring metric

N077-6014 Washer for the injector adapter

N077-6025 Nut for the injector adapter

N077-6090 Narrow Baffled (4mm) Cyclonic Spray

Chamber

N077-0614 Spray Chamber Cap

N077-6091 Injector Adapter (1.2 ID)

N077-6093 Alumina Injector (1.2mm)

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

PerkinElmer using the eight-digit part numbers provided in this manual.
 General System Maintenance 5-109

e-ssentials, 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 visit out website
www.perkinelmer.com or call:

• If you are located within the U.S., call toll free 1-800-762-4000, 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.
5-110 Maintenance
Chapter 6
 Troubleshooting 6
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

results. Verifying Performance
in the WinLab32
Software Guide or
Performance Problems:
Troubleshooting Table in
this chapter.
You cannot ignite the plasma, or the Plasma Ignition and
plasma is unstable. Stability Problems in this
chapter.
A red fault icon appears in the Operating Status
Instrument Diagnostics window or the Problems in the
system is not ready. WinLab32 Software
Guide.
6-4 Troubleshooting

Problem Refer to section

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.

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.

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.

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.
 Sodium Bullet Test 6-5

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
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:
6-6 Troubleshooting

• 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.

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?

 Performance Problems 6-7

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?

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.
6-8 Troubleshooting

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.

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
 Performance Problems: Troubleshooting Table 6-9

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 (HF), you should be

thoroughly familiar with its hazards and safe handling
! practices. When handling HF always wear gloves. Observe the
Warning manufacturer's recommendations for use, storage and disposal.

Bonnet

Is the bonnet cloudy or dirty?

Remove the bonnet and clean in a 20% nitric acid solution. Rinse well.

Performance Problems: Troubleshooting Table

Table 6-17. 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.
6-10 Troubleshooting

Table 6-17. Performance Problems: Troubleshooting Table

Problem Possible Cause(s) Corrective Action

Does the sample have a high Try increasing the integration time.
viscosity or high percentage Refer to the Winlab32 Software Guide
of dissolved solids? for details.
For high dissolved solids, try the cone
spray nebulizer. For more information
see Chapter 4, Installation, Setting
Instrument Parameters section.
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 6-17. Performance Problems: Troubleshooting Table

Problem Possible Cause(s) Corrective Action

Cannot obtain You may not be comparing Refer to the Winlab32 Software Guide
suggested BEC value the appropriate BEC value for for details.
the 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
may need to be optimized. mode) 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 Chapter 5, Maintenance, the
require cleaning. section on Purge Windows/Tubes for
the instructions for removing and
cleaning the purge windows for your
instrument.
6-12 Troubleshooting

Table 6-17. Performance Problems: Troubleshooting Table

Problem Possible Cause(s) Corrective Action

Results Corrections may not have Aspirate a blank and rerun standards
erroneously been made for the reagent and samples.
high blank.
Standard solutions may have Restandardize with a proven standard.
deteriorated or may have been
improperly made.
Background emission may be Use background correction.
present.
Results Standard solutions may have Rerun proven standards.
erroneously low been improperly made.
Blank solution may be Remake the blank solution. Acidify
contaminated or not matrix- the blank if the sample matrix is
matched to the standards. acidified.
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 Check the placement of background
being used? correction points. Refer to the
Winlab32 Software Guide for details.
Are you analyzing aluminum Run a high nitrogen purge for one
at 167 nm? hour before starting the analysis.
Refer to the Winlab32 Software Guide
for details.
 Performance Problems: Troubleshooting Table 6-13

Table 6-17. Performance Problems: Troubleshooting Table

Problem Possible Cause(s) Corrective Action

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 Clean the spray chamber if necessary.
may need cleaning.
Cannot get The sample introduction Refer to Chapter 4, Maintenance.
suggested detection system may not be set up
limits 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 completely. Refer to the Winlab32
to 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.
6-14 Troubleshooting

Table 6-17. Performance Problems: Troubleshooting Table

Problem Possible Cause(s) Corrective Action

Cannot get The standard may have too The standard should be 100 times the
suggested detection high a concentration. estimated detection limit.
limits
(continued)
You may not be comparing Confirm that you are using the
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 problems such See the section Checking the Sample
performance as poor precision or loss of Introduction System earlier in this
problems signal can often be traced to chapter.
the setup and condition of the
sample introduction system.

You are having difficulty Use a sapphire injector.

getting values for silicon in
samples with HF.
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.

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 contact finger is making contact with the
tape on the bottom of the torch glassware. Also, check the ignitor ground. If
 Plasma Ignition and Stability Problems 6-15

necessary, use a brush to clean it. Refer to chapter 4, Installation, to Figure 4-

9 for an illustration on the location of the ignitor contact finger and the ignitor
ground.

• 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, 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.
6-16 Troubleshooting

• 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.

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, 2.0 mm i.d., is recommended for typical
organic analyses. The alumina injector, 1.6 mm i.d., should be used with
volatile organic solvents, for example, methanol.
 Printing Problems 6-17

• Try increasing the RF power, using less solvent, slowing down the pump
speed, or adjusting the torch height.

Printing Problems

Table 6-18. Printing Problems

Problem Possible Cause(s) Corrective Action

Printer does not The correct printer driver may Check the printer drivers in Windows.
print or does not not be installed or selected in Check the website of your printers
print correctly Windows. Make sure you are manufacturer for the most current
using the most current printer driver. For more information, also see
driver for your printer. the 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 6-19. 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 The tension on the pump Use the adjustment screw to adjust the
flowing 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 6-20. Autosampler Problems

Problem Possible Cause(s) Corrective Action

Autosampler does There may be a GPIB Use the Instrument Diagnostics

not respond communication problem. window to reset the autosampler.
The software may not be In the System menu, click on
configured for the Configure Autosampler. In the
autosampler 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 pins on the autosampler Check the connector. If the pins are
cable connector may be broken, order a replacement cable.
broken.
Autosampler does The software may not be In the System menu, click on
not go to the correct configured for the correct Configure Autosampler. In the
location. autosampler tray. dialog, select the appropriate tray.
6-20 Troubleshooting

RF Generator/Sample Introduction System Troubleshooting Form

Fill out the following form before you contact PerkinElmer service.

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
 RF Generator/Sample Introduction System Troubleshooting Form 6-21

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
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
6-22 Troubleshooting

The following illustrations show various torch positions. Figure 6-1 and 6-2 show
the correct position of the injector for normal plasma conditions. The dotted line
represents the center of the hex nut and its relationship to the position of the
injector. Figure 6-3 through 6-8 illustrated incorrectly positioned injectors or other
faulty conditions that produce an incorrect plasma flow.

Figure 6-1. Normal plasma conditions at 0 torch position.

Figure 6-2. Normal plasma at -3mm position.

 RF Generator/Sample Introduction System Troubleshooting Form 6-23

Figure 6-3. Rounded Plasma due to sample or air getting around the outside
(typically subtle air leak).

Figure 6-4. Aux Gas too high, air leak, or spray chamber temperature too high.

Figure 6-5. Injector too far forward.

6-24 Troubleshooting

Figure 6-6. No Aux Gas (torch may be glowing).

Figure 6-7. Air leak or spray chamber temperature too high.

Figure 6-8. Thin plasma due to leak in plasma gas line.

Chapter 7
 Error Messages 7
This section describes the error messages for the system and their meaning. Where
possible, corrective actions are suggested.
7-4 Error Messages

System Error (SYSERROR) Messages for Spectrometer

In the following chart, the first column lists the error code. The second column lists
the error messages that appear in the 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.

System error messages for the spectrometer appear in two formats. The first format
indicates the command sent (from the computer to the spectrometer) and the error
code that resulted, followed by a brief message:

The command sent (2 letters) and error code (2 letters or two numbers) should be
recorded. If the problem persists contact a PerkinElmer service engineer to aid in
the diagnosis of the problem.

• TA “Warning” means that you can continue to run the instrument; however,
your data may be affected in some cases. There is no risk of damaging the
instrument.

• In “Fatal Mode,” the instrument cannot be operated until the problem is fixed.
In this state, the argon, cooling water, detectors, and thermoelectric cooler
power supply (for the detectors) are turned off. This is done to protect the
instrument from potential damage. For example, if the chiller was turned off,
the instrument would go into fatal mode and turn off power to the detectors to
protect them from being damaged.

The following error messages are all listed alphanumerically by error code.
 Spectrometer Error Messages 7-5

Spectrometer Error Messages

Error Code Error Meaning Corrective Action
Messages

00 No Error There is no error. No corrective action is needed.

01 Invalid A command was Contact PerkinElmer Service.
Command issued that was not
recognized. This error
is not likely to occur
and would indicate an
Optima application or
diagnostic software
problem.
02 Invalid A number or Contact PerkinElmer Service.
Number/ parameter that
Type of follows a command
Parameter was not
recognized.This error
is not likely to occur
and would indicate an
Optima application or
diagnostic software
problem.
03 Not Last A command was Contact PerkinElmer Service.
Command issued that was not in
the correct order. The
software normally
checks this order.
This error is not likely
to occur and would
indicate an Optima
application or
diagnostic software
problem.
7-6 Error Messages

Error Code Error Meaning Corrective Action

Messages

04 No Data An attempt to transfer Contact PerkinElmer Service.

Available data was made that
was not preceded by a
read. This error is not
likely to occur and
would indicate an
Optima application or
diagnostic software
problem.
05 Wrong The block which a Contact PerkinElmer Service.
Block group of data in the
Number detector read
sequence was
specified incorrectly.
This error is not likely
to occur and would
indicate an Optima
application or
diagnostic software
problem.
06 Wrong The subarray address Contact PerkinElmer Service.
Subarray on the detector was
Number specified incorrectly.
This error is not likely
to occur and would
indicate an Optima
application or
diagnostic software
problem.
 Spectrometer Error Messages 7-7

Error Code Error Meaning Corrective Action

Messages

07 Invalid The parameter Contact PerkinElmer Service.

Parameter specified for a
command did not
follow the correct
format. This error is
not likely to occur
and would indicate an
Optima application or
diagnostic software
problem.
09 Slit Motor Spectrometer slit Turn off the power to the spectrometer and
Error motor problem wait a few minutes. Turn the spectrometer
detected. The system back on and start the software again. If the
has detected a problem goes away, monitor the system and
problem with the if the problem reappears contact PerkinElmer
motor that moves the Service.
spectrometer slit.
10 View X Problem detected See error code 09.
Motor Error with the spectrometer
plasma-view
positioning motor.
11 View Y Problem detected See error code 09.
Motor Error with the spectrometer
plasma-view
positioning motor.
12 Detector The system is unable See error code 09.
Read Error to read the
spectrometer
detector.
18 BRAM The values read on Contact PerkinElmer Service.
Data the BRAM failed.
Fitness
Error
7-8 Error Messages

Error Code Error Meaning Corrective Action

Messages

23 Transient Transient Signal is Turn the spectrometer off and on, and retry FIAS
Signal Read FIAS mode. Too read. If the problem still exists, contact PerkinElmer
Overflow much data was service to determine if there are detector or controller
Error collected during a board problems.
read.
24 Detector Incorrect number of Turn the spectrometer off and on, and retry read. If
Pixel Read pixels read from the the problem still exists, contact PerkinElmer service
Error detector. to determine if there are detector or controller board
problems.
71 to 79 Invalid One of the parameters Contact PerkinElmer Service.
Parameter specified for a
#1 through command did not
#9 follow the correct
format. This error is
not likely to occur
and would indicate an
Optima application or
diagnostic software
problem.
7A to 7F Invalid One of the parameters Contact PerkinElmer Service.
Parameter specified for a
#10 through command did not
#15 follow the correct
format. This error is
not likely to occur
and would indicate an
Optima application or
diagnostic software
problem.
AC ABORT Indicated that the No corrective action needed.
Command ABORT commands
was issued to stop a
detector read
sequence.
 Spectrometer Error Messages 7-9

Error Code Error Meaning Corrective Action

Messages

AF Spectro- The argon is not Check that there is sufficient argon. The input
meter flowing to the pressure should be between 550-825 kPa (80-120
Argon Flow spectrometer. Argon psig). Check the pressure on the argon supply
Error is needed by the and the connections between the supply and the
(Fatal) spectrometer to spectrometer. After the argon supply is restored
protect the detector. click on the Initialize button on the Spectrometer
page of the Diagnostics window to begin the
warm-up. The warm-up will require 15 to
75 minutes depending on the length of time the
spectrometer was disabled. If this does not solve
the problem, contact PerkinElmer Service.
AO Argon Flow The argon flow has No corrective action needed.
OK restarted.
BF Error The firmware is In this software it is unlikely that this error
Buffer Full generating error message would be produced. Contact
codes faster than they PerkinElmer Service if this message appears.
can be read, so the
data capacity of the
firmware buffer was
exceeded. The buffer
is automatically
cleared for new
messages.
7-10 Error Messages

Error Code Error Meaning Corrective Action

Messages

CF Casting The casting Check the external cooling water supply and water
Warm Up temperature did not filter. Make sure that the chiller is on and sufficiently
Failed stabilize correctly. filled. Make sure the laboratory temperature is
(Fatal) between 10 °C to 35 °C. Make sure that there
are no heat emitting devices near the spectrometer.
Make sure there are no cooling devices such as
an air conditioner vent near the spectrometer.
Before calling service, turn off the power to the
spectrometer and wait a few minutes. Turn the
spectrometer back on and restart the software.
If the problem goes away, monitor the system and if
the problem reappears contact PerkinElmer
Service.
D1 High UV High dark current was Allow the system to warm up for at least one hour.
Dark measured on the Then click on the Detector Calibration button in
Current. detector in the the Spectrometer Control window and calibrate the
(Warning) ultraviolet (UV) detector. Before calling service, turn off the power
range. to the spectrometer and wait a few minutes. Turn
the spectrometer back on and restart the software
and click on the Detector Calibration button. If the
problem goes away, monitor the system and if the
problem reappears contact PerkinElmer Service.
Analytical results may be affected. Also check the
external cooling water supply and water filter. Make
sure that the chiller is on and sufficiently filled.
High dark current is usually caused by the detector
not being sufficiently cooled. Also see error codes
U1, U2,U3, U4, U5, V1, V2, V3, V4, and V5. If
this does not solve the problem, contact Service.
D2 High VIS High dark current was See Code D1.
Dark measured on the
Current. detector in the visible
(Warning) (VIS) wavelength
range.
 Spectrometer Error Messages 7-11

Error Code Error Meaning Corrective Action

Messages

D3 High UV High dark current was See Code D1.

and VIS measured on both
Dark detectors.
Current.
(Warning)
DO Detector The system tried to This error usually occurs during a read command
Power Off read the detector and when the spectrometer has not been fully initialized.
(Warning) the detector is off. Fully initialize the system.
DP Detector Detector power is on. No corrective action needed.
Power On
(Warning)
FO Fan The temperature in No corrective action needed.
Tempera- the laboratory is OK.
ture OK
FH Fan The temperature of Make sure the laboratory temperature is between
Tempera- the air entering the 10 °C to 35 °C. Make sure that there are no heat
ture High spectrometer is out of emitting devices near the spectrometer. Make
(Warning) range. sure there are no cooling devices such as an air
conditioner vent near the spectrometer. Before
calling service, turn off the power to the
spectrometer and wait a few minutes. Turn the
spectrometer back on and restart the software.
If the problem goes away, monitor the system and
if the problem reappears contact Service.
FL Fan The temperature of See Code FH.
Tempera- the air entering the
ture Low spectrometer is out of
(Warning) range.
FM Invalid
Command
During
Fatal Mode
7-12 Error Messages

Error Code Error Meaning Corrective Action

Messages

L1 No UV The mercury line was Before calling service, turn off the power to the
mercury not detected. The spectrometer and wait a few minutes. Turn the
line system was unable to spectrometer back on and restart the software.
(Warning) detect one of the If the problem goes away, monitor the system
mercury lines used and if the problem reappears contact PerkinElmer
for wavelength Service.
calibration.
L2 No VIS The mercury line was See Code L1.
mercury not detected. The
line system was unable to
(Warning) detect one of the
mercury lines used
for wavelength
calibration.
L3 No UV and The mercury line was See Code L1.
VIS not detected. The
mercury system was unable to
line detect one of the
(Warning) mercury lines used
for wavelength
calibration.
LE Motor A problem has Contact PerkinElmer Service.
Problem occurred with the Slit,
Looker View X, or View Y
Error motors. The system
(Fatal) was not able to set
one of the motors to
the correct position.
 Spectrometer Error Messages 7-13

Error Code Error Meaning Corrective Action

Messages

NF Nitrogen Spectrometer Check the nitrogen supply and make sure it is

Flow Error nitrogen purge gas adequate. Make sure that the connection between
(Warning) flow was interrupted. the supply and the spectrometer is correct and that
the nitrogen supply is set between 200 and
825gkPA (30 to 80 psig). After the nitrogen flow
has been restored, you may have to wait for the
system to again be purged particularly if you
plan to measure wavelengths below 250 nm.
NO Nitrogen The nitrogen flow is No corrective action needed.
Flow OK OK.
P1 24-Volt The 24-volt power Contact PerkinElmer Service.
Power supply provides
Supply power to the
Minimum spectrometer’s
(Fatal) motors and
pneumatic systems. If
the voltage has
exceeded the
minimum or
maximum levels, the
system is shut down.
P2 24-Volt Power supply is low. Contact PerkinElmer Service.
Power
Supply
Low
P3 24-Volt Power supply is high. Contact PerkinElmer Service.
Power
Supply
High
7-14 Error Messages

Error Code Error Meaning Corrective Action

Messages

P4 24-Volt Power supply has Contact PerkinElmer Service.

Power exceeded the
Supply maximum level.
Maximum
(Fatal)
P5 24-Volt OK response to codes No corrective action needed.
Power P1, P2, P3 or P4.
Supply OK
S0 Slit Motor The system has Before calling service, turn off the power to the
Looker detected a problem spectrometer and wait a few minutes. Turn the
Error with the motor that spectrometer back on and restart the software.
(Warning moves the If the problem goes away, monitor the system
or Fatal) spectrometer slit. and if the problem reappears contact Service.
S1 Slit Motor The system has See Error Code S0.
Home Error detected a problem
(Warning with the motor that
or Fatal) moves the
spectrometer slit.
S2 Slit Motor The system has See error message S0.
Limit Error detected a problem
(Warning with the motor that
or Fatal) moves the
spectrometer slit.
S3 Slit Motor The system has See error message S0.
Total Steps detected a problem
Error with the motor that
(Warning moves the
or Fatal) spectrometer slit.
S4 UV Shutter Problem with the See error message S0.
Failure spectrometer shutter
(Warning) detected.
 Spectrometer Error Messages 7-15

Error Code Error Meaning Corrective Action

Messages

S5 VIS Shutter Problem with the See error message S0.

Failure spectrometer shutter
(Warning) detected.
S6 UV and Problem with the See error message S0.
VIS Shutter spectrometer shutter
Failure detected.
(Warning)
T0 Top Plate The top plate sensor Contact PerkinElmer Service.
Sensor Not in the optics is not
Working working properly.
T1 Bottom The bottom plate Contact PerkinElmer Service.
Plate sensor in the optics is
Sensor Not not working properly.
Working
T2 Fin Sensor The fin sensor in the Contact PerkinElmer Service.
Not optics is not working
Working properly.
T3 Tub Sensor The tub sensor in the Contact PerkinElmer Service.
Not optics is not working
Working properly.
T4 Fin Not a fatal error but Contact PerkinElmer Service.
Tempera- the optics is not at an
ture Below optimal setting.
Setpoint
Range
T5 Fin Not a fatal error but Contact PerkinElmer Service.
Tempera- the optics is not at an
ture Above optimal setting.
Setpoint
Range
7-16 Error Messages

Error Code Error Meaning Corrective Action

Messages

T6 Tub Not a fatal error but Contact PerkinElmer Service.

Tempera- the optics is not at an
ture Below optimal setting.
Setpoint
Range
T7 Tub Not a fatal error but Contact PerkinElmer Service.
Tempera- the optics is not at an
ture Above optimal setting.
Setpoint
Range
T8 Bottom Not a fatal error but Contact PerkinElmer Service.
Plate the optics is not at an
Tempera- optimal setting.
ture Over
Maximum
T9 Tub Not a fatal error but Contact PerkinElmer Service.
Tempera- the optics is not at an
ture more optimal setting.
than 5
Degrees
Above
Setpoint
TA Top Plate Not a fatal error but Contact PerkinElmer Service.
Tempera- the optics is not at an
ture over optimal setting.
Maximum
TB Fin Not a fatal error but Contact PerkinElmer Service.
Tempera- the optics is not at an
ture more optimal setting.
than 5
Degrees
Above
Setpoint
 Spectrometer Error Messages 7-17

Error Code Error Meaning Corrective Action

Messages

TC Warning Top, Tub, and Fin Turn the spectrometer off and on. If the problem still
sensors not working; exists, contact PerkinElmer service since it is
therefore, Top plate possible that the connector to the sensors is
heater turned off. disconnected or a sensor is defective. PerkinElmer
service must replace the sensor or connector if
defective.
TD Warning Bottom and Tub Turn the spectrometer off and on. If the problem still
sensors not working; exists, contact PerkinElmer service since it is
therefore, Bottom possible that the connector to the sensors is
plate heater turned disconnected or a sensor is defective. PerkinElmer
off. service must replace the sensor or connector if
defective.
TH Time This can occur during This message should be preceded by CT (Casting
count-down system initialization Temperature Warm-Up Time Exceeded). When
on hold. if the spectrometer this error is received, the time countdown is held at
(Fatal) temperature does not approximately 15 minutes. If this problem persists,
reach the required contact PerkinElmer Service.
temperature within
one hour.
U0 UV OK response to error No corrective action needed.
Detector codes U1, U2, and
Cooler U3.
Voltage OK
7-18 Error Messages

Error Code Error Meaning Corrective Action

Messages

U1 UV Problem with the The cooling system for the spectrometer detector
Detector spectrometer detector was not able to cool or maintain the detector at the
Cooler cooling system. correct temperature. Make sure there is an adequate
Voltage supply of cooling water temperature below 25 °C and
Minimum filled with water coolant. Make sure the laboratory
(Fatal) temperature is between 10 °C to 35 °C. Make sure
that there are no heat emitting devices near the
spectrometer. Make sure there are no cooling devices
such as an air conditioner vent near the spectrometer.
Click on the Initialize button on the Spectrometer
page of the Diagnostics window to begin a warm up.
Warm up requires 15 to 75 minutes. Before calling
service, turn off the power to the spectrometer and
wait a few minutes. Turn the spectrometer back on
and restart the software.
If the problem goes away, monitor the system and if
the problem reappears contact PerkinElmer Service.
U2 UV Problem with the See Error Code U1.
Detector spectrometer detector
Cooler cooling system.
Voltage
Low
(Warning)
U3 UV Problem with the See Error Code U1.
Detector spectrometer detector
Cooler cooling system.
Voltage
Maximum
(Fatal)
 Spectrometer Error Messages 7-19

Error Code Error Meaning Corrective Action

Messages

U5 UV Problem with the See Error Code U1.

Detector spectrometer detector
Cooler cooling system.
Tempera-
ture
Maximum
(Fatal)
U6 UV Problem with the See Error Code U1.
Detector spectrometer detector
Tempera- cooling system.
ture High
U7 UV OK response to Error No corrective action needed.
Detector Codes U4, U5, or U6.
Tempera-
ture is OK
U8 UV Detector temperature Before calling service, turn off the power to the
Detector sensor problem spectrometer and wait a few minutes. Turn the
Minimum detected. spectrometer back on and restart the software.
Tempera- If the problem goes away, monitor the system
ture error and if the problem reappears contact PerkinElmer
Service.
7-20 Error Messages

Error Code Error Meaning Corrective Action

Messages

U9 UV Detector temperature The system has detected a problem with the UV

Detector sensor problem detector that may be due to a bad sensor or may
Heating detected. be due to cooling system problems. Make sure
error there is an adequate supply of cooling water
temperature below 25 °C and filled with water
coolant. Make sure the laboratory temperature is
between
10 °C to 35 °C. Make sure that there are no heat
emitting devices near the spectrometer. Make sure
there are no cooling devices such as an air
conditioner vent near
the spectrometer. Click on the Initialize button on the
Spectrometer page of the Diagnostics window to
begin a warm up. Warm up requires 15 to 75 minutes.
Before calling service, turn off the power to the
spectrometer and wait a few minutes. Turn the
spectrometer back on and restart the software. If

V0 VIS Detector Indicates that the No corrective action needed.

Cooler temperature did rise but
Voltage OK only a warning was
given. The problem has
been corrected and the
temperature is now in
an acceptable range.
 Spectrometer Error Messages 7-21

Error Code Error Meaning Corrective Action

Messages

V1 VIS Problem with the Make sure there is an adequate supply of cooling
Detector spectrometer detector water temperature below 25 °C and filled with water
Cooler cooling system. coolant. Make sure the laboratory temperature is
Voltage between 10 °C to 35 °C. Make sure that there are
Minimum no heat emitting devices near the spectrometer.
(Fatal) Make sure there are no cooling devices such as an
air conditioner vent near the spectrometer. Click on
the Initialize button on the Spectrometer page of the
Diagnostics window to begin a warm up. Warm up
requires 15 to 75 minutes. Before calling service,
turn off the power to the spectrometer and wait a
few minutes. Turn the spectrometer back on and
restart the software. If the problem goes away,
monitor the system and if the problem reappears
contact PerkinElmer Service.
V2 VIS Problem with the See Error Code V1.
Detector spectrometer detector
Cooler cooling system.
Voltage
LOW
(Warning)
V3 VIS Problem with the See Error Code V1.
Detector spectrometer detector
Cooler cooling system.
Tempera-
ture MAXI-
MUM
(Fatal)
V5 VIS Problem with the See Error Code V1.
Detector spectrometer detector
Tempera- cooling system.
ture
Maximum
(Fatal)
7-22 Error Messages

Error Code Error Meaning Corrective Action

Messages

V6 VIS Problem with the See Error Code V1.

Detector spectrometer detector
Tempera- cooling system.
ture High
V7 VIS Indicates that the No corrective action needed.
Detector temperature did rise
Tempera- but only a warning
ture OK was given. The
problem has been
corrected and the
temperature is now in
an acceptable range.
V8 VIS Visible range detector The system has detected a problem with the
Detector temperature sensor temperature sensor for the visible detector. Check
Tempera- problem detected. out the chiller and water supply. The supply lines
ture Low could be clogged or the water could be contaminated.
Before calling service, turn off the power to the
spectrometer and wait a few minutes. Turn the
spectrometer back on and restart the software. If
the problem goes away, monitor the system and
if the problem reappears contact PerkinElmer
Service.
 Spectrometer Error Messages 7-23

Error Code Error Meaning Corrective Action

Messages

V9 UV Visible range detector Check out the chiller and water supply. The
Detector temperature sensor supply lines could be clogged or the water could
Heating problem detected. be contaminated. Make sure there is an adequate
error supply of cooling water temperature below 25 °C
and filled with water coolant. Make sure the
laboratory temperature is between 10 °C to 35 °C.
Make sure that there are no heat emitting devices
near the spectrometer. Make sure there are no cooling
devices such as an air conditioner vent near the
spectrometer. Click on the Initialize button on the
Spectrometer page of the Diagnostics window to
begin a warm up. Warm up requires 15 to 75 minutes.
Before calling service, turn off the power to the
spectrometer and wait a few minutes. Turn the
spectrometer back on and restart the software. If
the problem goes away, monitor the system and if the
problem reappears contact PerkinElmer Service.
W0 No Water Water leak OK. No corrective action needed.
Leak
Detected
WL Water Leak The spectrometer has Shut off the water supply and power to the
(FATAL) an internal water leak. spectrometer. Contact PerkinElmer Service.
X0 View X Problem detected Before calling service, turn off the power to the
Motor with the spectrometer spectrometer and wait a few minutes. Turn the
Looker plasma view spectrometer back on and restart the software. If
Error positioning motor in the problem goes away, monitor the system and if
(Warning the X-direction. the problem reappears contact PerkinElmer Service.
or Fatal)
X1 View X Problem detected See Error Code X0.
Motor with the spectrometer
Home Error plasma view
(Warning positioning motor in
or Fatal) the X-direction.
7-24 Error Messages

Error Code Error Meaning Corrective Action

Messages

X2 View X Problem detected See Error Code X0.

Motor with the spectrometer
Limit Error plasma view
(Warning positioning motor in
or Fatal) the X-direction.
X3 View X Problem detected See Error Code X0.
Motor Total with the spectrometer
Steps Error plasma view
(Warning positioning motor in
or Fatal) the X-direction.
Y0 View Y Problem detected Before calling service, turn off the power to the
Motor with the spectrometer spectrometer and wait a few minutes. Turn the
Looker plasma view spectrometer back on and restart the software.
Error positioning motor in If the problem goes away, monitor the system
(Warning the Y-direction. and if the problem reappears contact PerkinElmer
or Fatal) Service.
Y1 View Y Problem detected See Error Code Y0.
Motor with the spectrometer
Home Error plasma view
(Warning positioning motor in
or Fatal) the Y-direction.
Y2 View Y Problem detected See Error Code Y0.
Motor with the spectrometer
Limit Error plasma view
(Warning positioning motor in
or Fatal) the Y-direction.
Y3 View Y Problem detected See Error Code Y0.
Motor Total with the spectrometer
Steps Error plasma view
positioning motor in
the Y-direction.
 System Error (SYSERROR) Messages for RF Generator 7-25

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 messages for the RF generator are displayed
in the following format:
7-26 Error Messages

Error Error Mes- Meaning Corrective Action

Code sage
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.
 System Error (SYSERROR) Messages for RF Generator 7-27

Error Error Mes- Meaning Corrective Action

Code sage
04 Ignition Instrument failed Ignition failure may be caused by incorrect
Failure ignition sequence. argon flows, air leaks, weak/no ignition spark,
cracked or 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 coil.Check the proper
flows of argon in the plasma and auxiliary
lines; excessive argon pressure can “blow” a
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
window power FET transistor forms properly but extinguishes right away,
1 is out of the level 2 check the argon flows, torch condition, and test
Tolerance window. for air leaks. It 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.
7-28 Error Messages

Error Error Mes- Meaning Corrective Action

Code sage
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.
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 set Failed to set power to Contact PerkinElmer Service.
power to a value specified in
specified the Plasma Controls
level Dialog window.
 System Error (SYSERROR) Messages for RF Generator 7-29

Error Error Mes- Meaning Corrective Action

Code sage
12 Failed to set Failed to set AUX to a Check argon supply, argon pressure, AUX
AUX flow to value specified in the flow tubing and connections. If this does not
specified AUX Setting Flow correct the problem, contact PerkinElmer
level Controls window. Service.

13 Failed to set Failed to set Plasma Check the argon supply, argon pressure,
Plasma flow flow to a value plasma flow tubing, and connections. If this
to specified specified in the Flow does not correct the problem, contact
level Controls window. PerkinElmer Service.

14 Failed to set Failed to set Neb flow Check the nebulizer tips for blockage.
Neb flow to to a value specified in
specified the Flow Controls Check the argon supply, argon pressure, neb
level window. flow tubing and connections. If this does not
correct the problem contact PerkinElmer
Service.
15 The EMO Attempted ignition Reset the EMO button to correct this error
button is still sequence with the message.
pressed EMO button pressed.
If resetting the EMO button does not clear
the error message, check the operation of the
switch.
16 EMO switch The EMO switch has Release and reset the EMO button to correct
pressed been pressed. this error message.

If resetting the EMO button does not clear

the error message, check the operation of the
switch.
7-30 Error Messages

Error Error Mes- Meaning Corrective Action

Code sage
17 EMO switch Reset the EMO button to correct this error
latched message.

If resetting the EMO button 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
sensed closed. message.

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.
21 Shear not Shear gas is not Check the shear gas flow.
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.
 System Error (SYSERROR) Messages for RF Generator 7-31

Error Error Mes- Meaning Corrective Action

Code sage
22 Failed to The instrument has Verify that the NEB Quick-Disconnect fitting
maintain Neb failed to maintain or is correctly mated. Examine the nebulizer tips
flow attain the nebulizer for blockage. Check the argon lines from
flow. Pneumatics 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
maintain failed to maintain or does not correct the problem contact
AUX flow attain the AUX flow. PerkinElmer Service.
24 Failed to The instrument has Check the argon lines for crimping. If this
maintain failed to maintain or does not correct the problem, contact
Plasma flow attain the plasma PerkinElmer Service.
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 limits cooling water is temperature. Check the water lines (and water
detected. The RF filter, if installed). If this does not correct the
generator will be shut problem, contact PerkinElmer Service.
down when the
temperature is out of
limits.
26 +24V supply This warning Contact PerkinElmer Service.
out of range message will appear
(Warning) if the RF Control
Electronics Supply is
+/-10% out of range.
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.
7-32 Error Messages

Error Error Mes- Meaning Corrective Action

Code sage
29 Fiber optic The firmware expects Contact PerkinElmer Service.
not detecting the plasma to be on
plasma but the plasma is not
on. The fiber optic
will do a hardware
shutdown.
31 Neb Pressure In this hardware Verify that the NEB Quick-Disconnect fitting
out of range failure the nebulizer is correctly mated. Examine the nebulizer tips
back pressure is out for blockage. If this does not correct the
of the acceptable problem, contact PerkinElmer Service.
range of 0 to 65 psi.
32 Ids 1 higher Drain to source Contact PerkinElmer Service.
than level 1 current across the
power FET transistor
1 is a non-zero
current. This
transistor should be
off but current is still
going through it.
33 Ids 2 higher Drain to source Contact PerkinElmer Service.
than level 1 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 not In the Plasma Control The Shear Control must be turned on. If this
enabled Dialog window the does not correct the problem, contact
Shear Control is off. PerkinElmer Service.
35 Water still May indicate Check the operation of the water flow
flowing hardware failure. solenoid in the RF generator.
 System Error (SYSERROR) Messages for RF Generator 7-33

Error Error
Meaning Corrective Action
Code Message

36 Shear still May indicate Check the operation of the shear gas solenoid
flowing hardware failure. on the Pneumatics PC board.
37 Interlocks set The interlocks are not Check that the torch door access door is
satisfied. closed and the torch is in position.
38 Ids The current in one Contact PerkinElmer Service.
imbalance transistor is larger
than the other
transistor. Both
transistors should
have an equal current
within tolerance
limits.
39 +24 V This fatal message Contact PerkinElmer Service.
Supply out of will appear if the 24 V
range (Fatal) Supply is 10% out of
range (24V +/-2.4 V).
40 +DC Supply This fatal message Contact PerkinElmer Service.
out of range will appear if the DC
(Fatal) Supply is 10% out of
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 Contact PerkinElmer Service.
detecting fiber optic is
plasma detecting the plasma
but the plasma is not
on.
7-34 Error Messages

Error Error
Meaning Corrective Action
Code Message

43 Ids1 not 0 Drain to source Contact PerkinElmer Service.

current across the
power FET transistor
1 is turned off but
current is still flowing
this transistor.
44 Ids2 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.
45 Watchdog A hardware/firmware Contact PerkinElmer Service.
not working failure. The safety
timer that protects the
instrument in case the
firmware fails is not
working.
46 Plasma flow The Flow Controls Check inlet pressure and the output regulators
low (<10 l/m) Setting in the Plasma and that there is enough pressure into the
Control Dialog instruments. If this does not solve the
window is too low, or problem, contact PerkinElmer Service.
not enough inlet
pressure and flow to
sustain the plasma gas
flow.
47 Neb flow not The Neb flow should Something is wrong with the Neb flow control.
zero be zero but the Check that the Neb tubing is properly
hardware detects a connected to the Quick Disconnect to allow
flow. for flow. If this does not solve the problem,
contact PerkinElmer Service.
 System Error (SYSERROR) Messages for RF Generator 7-35

Error Error
Meaning Corrective Action
Code Message

48 Plasma flow Flow control setting The ignite flow must be at least 10 LPM. See
< 10 while is below 10 LPM. Error Message 46.
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/min. See
too low to Setting for AUX in Error Message 46.
ignite (0.5 L/ the Plasma Controls
Min) Dialog window is <
0.5 LPM.
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 Plasma The Plasma Contact PerkinElmer Service.
checksum calibration table has
error been corrupted,
relearn Plasma gas.
7-36 Error Messages

Error Error
Meaning Corrective Action
Code Message

55 Parameter This warning This warning indicates that an error occurred

validation message indicates earlier 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 log The Lifetime log has Data is lost.
checksum been corrupted.
error
57 Manufac- The Manufacturing Data is lost.
turing log log has been
checksum corrupted.
error
58 Vds too high The supply voltage Contact PerkinElmer Service.
for ignition should be closer to
(>5 volts) zero.
59 Shear gas Check the shear gas valve.
stuck on
60 Water flow Check the water valve. The valve maybe
stuck on frozen 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 reading Parameters for the Contact PerkinElmer Service.
post-ignite ignite command for
power setting the power setting are
invalid.
62 Error reading Parameters for the Contact PerkinElmer Service.
post-ignite ignite command for
AUX flow the AUX flow are
invalid.
 System Error (SYSERROR) Messages for RF Generator 7-37

Error Error
Meaning Corrective Action
Code Message

63 Error reading Parameters for the Contact PerkinElmer Service.

post-ignite ignite command for
neb flow the neb flow are
invalid.
64 Error reading Parameters for the Contact PerkinElmer Service.
post-ignite ignite command for
plasma flow the plasma flow are
invalid.
65 Learn AUX There is a fault in the Contact PerkinElmer Service.
failed range pneumatics system.
checking
66 Learn Plasma There is a fault in the Contact PerkinElmer Service.
failed range pneumatics system
checking
67 Learn AUX The system calculates Verify that the AUX gas is turned on.
failed slope a slope to verify that Otherwise the plasma will not ignite.
checking the AUX flows are
actually increasing.
68 Learn Plasma The system calculates Verify that the plasma is turned on.
failed slope a slope to verify that Otherwise the plasma will not ignite.
checking the Plasma flows are
actually increasing.
69 Plasma went Check the sample introduction system.
out
unexpectedly
70 Neb back- The nebulizer has Check and correct any leaks in the sample
pressure >60 been shut off once the introduction system. Check that all fittings
psi (413 kPa) nebulizer are engaged. Check the spray pattern and
& shut off backpressure has disconnect the nebulizer to check if there is
neb fallen below 60 psi flow.
(413 kPa).
7-38 Error Messages

Error Error
Meaning Corrective Action
Code Message

71 Neb heater The nebulizer Call PerkinElmer Service.

sensor is not compartment heater
working- sensor is not working
heater off properly and the
heater is now off.
72 Ids 1 out of Call PerkinElmer Service.
window, no
plasma
detected
73 Ids 2 out of Call PerkinElmer Service.
window, no
plasma
detected
74 Plasma The plasma sensor Check that all sample introduction tubing is
impedenance has failed to sense the properly connected. Check and perform
(Plasma-Z) extinguished plasma. maintenance on the entire sample introduction
exceeds system (including the torch, injector, injector
working adapter and nebulizer). Check for wear and
range replace all O-rings where needed. Change
the method to reduce sample or vapor loading
to improve analytical performance. If you
still get this error message after performing
all these corrective actions call PerkinElmer
Service.
 Index
A B
Acid Digestions 1-17 Bonnet
Adjusting the Sampling Probe Height 4- inspecting 6-9
39 C
Air Filters Calibration
general maintenance 5-104 detector 4-43
maintenance 5-104 wavelength 4-43
periodic checks 5-9 Capillary Tubing
RF generator, changing 5-104 inspecting 6-7
spectrometer, changing 5-105 Chemical Reagents 1-15
Alignment Chiller
torch viewing position 4-41 connecting 4-11
Aqueous Instrument Parameters 4-46 connections at back of instrument 4-
Argon 15
checking 6-15 coolant recommended 4-16
Argon Supply daily checks 5-6
connecting, instructions 3-23, 4-8 electrical requirements 2-12
daily checks 5-5 filling 4-16, 4-17
requirements 2-13 remote connections 4-12
Autosampler remote operations 4-14
connecting to computer 4-35, 4-36 space requirements 2-9
description 3-21 starting 4-17
inserting sampling probe 4-38, 4-40 Cleaning 5-4
installing 4-34 Coil, RF
setting up sampling probe 4-37 see RF Coil 5-8
troubleshooting problems with 6-19
I-2 Index: D

Computer using acids 1-17

configuration and setup 4-20 Drain
Concentric Glass Nebulizer daily checks 5-7, 6-15
cleaning 5-90 periodic checks 5-9
organics 5-89 safety practices 1-9
Connections tubing, connecting 5-102
cooling water 3-38, 4-5 Drain Tubing
cooling water supplies 3-23 adjusting 5-101
electrical 3-23, 3-38 connecting 5-98
gas 3-38 installing 5-94, 5-99
gases 3-23, 4-5 Drain Vessels 2-9
Cooling Water Dual Density Cross Disperser 3-32
connections at back of instrument 3-40, Dual View (DV) Instruments 3-5
3-41, 4-7 recommendations 4-49
flow diagram with chiller 4-15 E
Cyclonic Spray Chamber Echelle Grating
cleaning 5-66, 5-90 comparison with echellette 3-29
etching 5-65 description 3-29
installing 5-62 Echelle Spectrometer
installing 4300V 5-39 operating principles 3-23
maintenance 5-38, 5-62 Echellogram
organics 5-89 schematic representation of 3-32
removing Optima 4300V 5-43 Electrical Connections 3-38
Cyclonic Spray Chamber Assembly 4300V at back of instrument 3-40, 3-41
4-31 Electrical Requirements
D chiller 2-12
Daily Cleaning 5-4 laboratory preparation 2-11
Dark Current Electrical Safety
measuring 3-23 safety practices 1-6
Detector Emergency Off Switch 3-37
cooling 3-13 End Cap
purging 3-13 removing from Scott spray chamber 5-
Detector Calibration 4-43 60
Digestions replacement parts 5-68
at elevated pressure 1-19 replacing 5-80
performing 1-19 Environment i-xiv
Dissolving Solid Samples Environmental Conditions
in organics 1-16 laboratory preparation 2-3
 Index: F I-3

Error Messages ters 4-48

spectrometer 7-4 High Temperatures
Exhaust Vent safety practices 1-9
checking 6-15 Hoses, Gas and Water
daily checks 5-6 part numbers 5-107, 5-108
requirements, laboratory preparation 2- Hot Exhaust Gases
4 safety practices 1-9
F Hydrofluoric Acid 1-18
Filters I
air 5-104 ICP Source
part numbers 5-106, 5-107 RF control electronics 3-15
replacement parts 5-106 RF generator 3-14
Fitting the Sampling Probe 4-38 Ignitor
Fold Flat Mirror 3-33 checking cable 6-14
Fuses Indicator Lights
maintenance 5-106 illustration 3-37
Fusion Mixtures 1-20 Initialization of Instrument
G initialization steps 3-22
Gas Connections 3-38 interlocks 3-22
at back of instrument 3-40, 3-41 Initialization of instrument 3-22
Gas Cylinders Injector
handling 1-13 checking 6-15
identification 1-12 removing 5-16
storing 1-12 Input Module
Gas Supply description 3-29
replacement parts 5-107, 5-108 Installation
Gases autosampler 4-34
connecting, instructions 4-6 connecting cooling water 4-5
connections at back of instrument 4-7 connecting gases 4-5
GemCone Nebulizer connecting the system components 4-
Cleaning Optima 4300 V 5-86 18
Optima 4300 V 5-85 general information 4-3
H moving the instrument 4-4
Hardware Settings Quick-Change Adjustable Torch Mod-
controlled by software 3-23 ule 4-21
Hazards shipping list 4-51, 4-57
ultraviolet radiation 1-6 summary 4-4
High Dissolved Solids Instrument Parame-
I-4 Index: L

Installation Kit cyclonic spray chamber, installing 5-62

items included 4-51, 4-57 cyclonic spray chamber, installing 4300
Instrument V 5-39
calibration 4-41 cyclonic spray chamber, removing Op-
setup 4-41 tima 4300 V 5-43
Instrument Handling 1-4 daily checks 5-4
Instrument Location 2-9 end cap, removing 5-60
Instrument Parameters end cap, replacing 5-80
aqueous 4-46 fuses 5-106
high dissolver solids 4-48 GemCone nebulizer 5-81
organic 4-47 GemCone nebulizer, cleaning 5-81
plasma parameters 4-46, 4-47, 4-48 GemTip Cross-Flow nebulizer 5-69
setting 4-46 nebulizer 5-67
Interlocks periodic checks 5-8, 5-9
description 3-22 peristaltic pump 5-93
L purge windows on DV instruments 5-
Labels on the Instrument i-xv 47
three different types i-xv replacement parts 5-106
Laboratory Guidelines 1-3 RF coil 5-43
Laboratory Preparation 2-3 Scott spray chamber, cleaning 5-61
argon supply 2-13 spray chamber 5-13, 5-21
electrical requirements 2-11 spray chamber, replacing 5-29
environmental conditions 2-3 spray chamber,removing 5-60
exhaust vent requirements 2-4 torch, cleaning 5-19
laboratory space requirements 2-7 torch, removing 5-16
Laboratory Requirements torch, replacing 5-21
pneumatic requirements 2-13 Meinhard Nebulizer
purge gas 2-14 cleaning 5-90
shear gas supply 2-15 maintenance 5-87
Laboratory Ventilation 1-4 organics 5-89
M Mira Mist Nebulizer 5-91
Maintenance Nebulizer, Mira Mist 5-91
air filters 5-104 Moving
cleaning procedures 5-10 instrument 4-4
concentric glass nebulizer 5-87, 5-90 N
cyclonic spray chamber 5-38, 5-62 Nebulizer
cyclonic spray chamber, cleaning 5-66 argon flow rate 3-23
cyclonic spray chamber, etching 5-65 argon tubing, connecting 5-78
 Index: O I-5

argon tubing, replacing 5-79 Nebulizer Tubing

comparison of different types 3-17 connecting 4-26, 4-34
concentric glass nebulizer, maintenance Nitrogen Purge Rate 3-23
5-87 Nitrogen Supply
concentric glass, cleaning 5-90 connecting, instructions 3-23, 4-6
concentric glass, installing 5-87 O
Cross-Flow nebulizer argon tip, remov- Optical System
ing 5-76 description 3-10
Cross-Flow nebulizer sample tip, re- illustration 3-25, 3-27
moving 5-73 input module 3-29
Cross-Flow nebulizer spray pattern, optical housing 3-11, 3-12
checking 5-70 SCD 3-33
Cross-Flow nebulizer, disassembling 5- transfer optics 3-29
71 UV module 3-31
daily checks 5-7 visible channel 3-33
end cap, removing 5-69 Optics Interlock
GemCone liquid fitting, maintenance 5- checking 6-15
85, 5-87 Optima 3000 Series
GemCone nebulizer, cleaning 5-84, 5- specifications 3-42
86 Optima 4000 Series
GemCone nebulizer, installing on cy- features 3-4
clonic spray chamber 5-83 major components 3-8
GemCone nebulizer, installing on Scott Optima 4300V Torch Installation 4-28, 5-
spray chamber 5-82 33
GemCone, maintenance 5-81 Optimization 3-23
GemTip Cross-Flow, maintenance 5-69 Organic Instrument Parameters 4-47
High Solids GemCone nebulizer, clean- Organic Vapors
ing 5-81 checking 6-16
inspecting 6-7 Organics
low-flow GemCone nebulizer, cleaning and plasma stability 6-16
5-81 checking 6-16
maintenance 5-67 cleaning 5-90
periodic checks 5-8 Concentric Glass Nebulizer 5-89
replacement parts 5-68 P
tubing, connecting 5-30 Perchloric Acid 1-18
Nebulizer Compartment Heater 3-20 Performance Checks
Nebulizer End Cap periodic checks 5-10
checking 6-16
I-6 Index: Q

Peristaltic Pump laboratory requirements 2-14

cleaning 5-102 Purge Window
daily checks 5-7 axial, removing 5-51
description 3-21 axial, replacing 5-51
flow rate 3-23 inspecting 6-8
inspecting 6-6 periodic checks 5-8
maintenance 5-93 radial, removal 5-48
part numbers 5-104 radial, replacing 5-51
periodic checks 5-9 removal Optima 4300 V 5-54
pump head, removing 5-102 replacement parts 5-54, 5-56
replacement parts 5-104 Purge Window Holder
troubleshooting problems with 6-18 removal Optima 4300V 5-56
TubingSaver 3-23 Purge Windows
Peristaltic Pump Tubing cleaning 5-47
inspecting 6-6 maintenance on DV instruments 5-47
replacing 5-93 replacement parts on DV instruments 5-
Plasma 54, 5-56
troubleshooting ignition problems 6-14 Q
troubleshooting stability problems 6-14 Quick-Change Adjustable Torch Module
Plasma Argon Flow Rates 3-23 installation 4-21
Plasma Parameters 4-46, 4-47, 4-48 periodic maintenance 5-12
recommendations 4-46, 4-47, 4-48 Quick-Change Torch Module 3-16
Plasma Torch description 3-16
periodic maintenance 5-12, 5-32 R
Plasma Viewing Regulator
configurations 3-5 requirements 2-15
Pneumatic 2-13 Replacement Parts
Pneumatic Requirements peristaltic pump 5-104
laboratory requirements 2-13 purge windows 5-54, 5-56
Printer solutions 5-107
configuration and setup 4-20 torch module 5-44
troubleshooting problems with 6-17 Resolution
Pump Tubing table of settings for 3-11
adjusting 5-100 RF Coil
Pump, Peristaltic daily checks 5-6
maintenance 5-93 inspecting 6-15
Purge Gas periodic checks 5-8
daily checks 5-5 periodic maintenance 5-13, 5-43
 Index: S I-7

replacing 5-43 waste disposal procedures 1-10

RF Coil Cooling Sample Capillary
daily checks 5-6 checking 6-16
RF Control Electronics 3-15 Sample Compartment
RF Generator 3-14 description 3-16
RF Power 3-23 Sample Introduction System
RF Radiation autosampler 3-21
safety practices 1-6 cleaning 5-10
S description 3-16
Safety Information inspection of 6-6
environment i-xiv nebulizer 3-17
Safety Interlocks 1-5 peristaltic pump 3-21
burner system 1-6 Quick-Change Torch Module 3-16
Safety Practices spray chamber 3-16
acid digestions 1-17 torch 3-16
chemical reagents 1-15 Sample Preparation 1-16
digestions 1-19 Sample Tubing
dissolving solid samples in organics 1- adjusting 5-100
16 installing 5-94
dissolving solid samples using acids 1- SCD
17 and echelle pattern 3-35
drain system 1-9 cooling and purging 3-13
electrical safety 1-6 description 3-11, 3-33
environmental conditions 1-4 electronic processing of signal 3-35
fusion mixtures 1-20 operating principles 3-23
general practices 1-3 photo 3-34
hazardous chemicals warnings 1-14 storage of photoelectrons 3-37
high temperatures 1-9 subarray pattern 3-36
hot exhaust gases 1-9 Schmidt Cross Disperser 3-31
hydrofluoric acid 1-18 Shear Gas
instrument handling 1-4 adjusting nozzle 5-57
laboratory guidelines 1-3 connecting, instructions 3-23, 4-9
laboratory ventilation 1-4 connection at back of instrument 4-7
perchloric acid 1-18 daily checks 5-5
RF radiation 1-6 purpose 3-7
safety interlocks 1-5 requirements 2-15
sample preparation 1-16 setting pressure 4-10
ultraviolet radiation 1-6
I-8 Index: T

Shipping List 4-57 Spray Chamber, Scott

Shipping List, DV Spares kit 4-51 cleaning 5-61
Space Collar illustration 5-61
used in gas connections 4-6 maintenance 5-60
Spares Kit, Dual View replacing 5-29
items included 4-51, 4-57 Switch 3-37
Specifications 3-42 illustration 3-37
argon flow controls 3-42 Symbols
ICP system 3-42 graphics on the instrument i-xv
sample introduction system 3-43 used on the instrument i-xv
spectrometer 3-44 warnings on the instrument i-xv
Spectrometer T
description 3-10 Test Solutions 5-107
detector cooling and purging 3-13 Torch
Dual Density Cross Disperser 3-32 alignment 4-41
fold flat mirror 3-33 cleaning 5-19
input module 3-29 daily checks 5-6
SCD detector 3-33 description 3-16
Schmidt Cross Disperser 3-31 disassembling 5-16
specifications 3-44 inspecting 6-8
transfer optics 3-29 inspecting glassware 6-15
UV module 3-31 long 4-47, 4-48
Visible Module 3-33 periodic checks 5-8
Spray Chamber removing 5-16
checking 6-16 replacing 5-21
cleaning 5-21, 5-61 Torch Connections
description 3-16 checking 6-15
end cap, removing 5-60 Torch Module
inspecting 6-7 part numbers 5-44
maintenance 5-60 Torch Module Assembly 4300V 4-29
periodic checks 5-8 installing 5-34
removing 5-13, 5-60 removing 5-37
replacement parts 5-66 Torch Positions 4-22, 4-48
replacing 5-29 Torch Viewing Position Alignment Proce-
spare parts 5-97 dure 4-41, 5-10
Spray Chamber, Cyclonic Transfer Optics
maintenance 5-38, 5-62 description 3-29
 Index: U I-9

Troubleshooting
autosampler problems 6-19
general information 6-3
performance problems 6-6
performance problems, table 6-9
plasma ignition problems 6-14
plasma stability problems 6-14
printing problems 6-17
pump problems 6-18
U
Ultraviolet Radiation
safety practices 1-6
UV Module
description 3-31
V
Vent Positions 2-6
Viewing 4-41
Visible Channel
description 3-33
W
Warnings
symbols used on instrument i-xv
Waste Disposal Procedures 1-10
Water Connections 3-38
Water Supply
replacement parts 5-107, 5-108
Wavelength Calibration 4-43, 5-9
I-10 Index: W