2000 HW
2000 HW
2000 HW
OPTIMA 2000
Hardware Guide
Release history
Any comments about the documentation for this product should be addressed to:
User Assistance
User Assistance
Perkin Elmer Ltd.
PerkinElmer Inc.
Chalfont Road
710 Bridgeport Avenue
Seer Green
Shelton, CT 06484-4794
Bucks, HP9 2FX
U.S.A.
United Kingdom
0993-6226
Contents
iv 0993-6226
Contents
Chapter 4:
Installation
Installation Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-3
Setting Up the Computer and Printer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-3
Moving the Instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-4
Connecting the Gases and Cooling Water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-5
Connecting the Gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-5
Connecting the PolyScience Chiller . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9
Filling the PolyScience Chiller . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-14
Starting Up the PolyScience Chiller . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-15
Connecting the System Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-17
Installing the Quick-Change Adjustable Torch Module . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-19
Installing the Quick-Change Adjustable Torch Module . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-19
Connecting the Nebulizer (NEB) Tubing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-22
Installing the Autosampler. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-24
Setting Up the Autosampler. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-26
To Fit the Sampling Probe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-26
Adjusting the Sampling Probe Height. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-27
Setting the Torch Viewing Position. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-29
Switching On the System. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-31
Setting Instrument Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-32
General parameter settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-32
Instrument Settings for Aqueous Solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-33
Instrument Settings for Organic Solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-33
Hardware Settings and Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-34
Shipping List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-35
Chapter 5:
Maintenance
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
Daily Checks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
Daily Cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
Argon Supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
Purge Gas Supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
Shear Gas Supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
Chiller . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
Vent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
Torch and RF Coil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
0993-6226 v
Contents
Nebulizer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-5
Peristaltic Pump and Drain . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-5
Periodic Checks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-5
Torch Assembly and RF Coil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-6
Purge Viewing Window/Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-6
Nebulizer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-6
Spray Chamber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-6
Peristaltic Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-7
Drains . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-7
General System Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-7
Torch Viewing Position Alignment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
Performance Checks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-8
Cleaning the Sample Introduction System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-9
Quick-Change Adjustable Torch Module . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-10
Plasma Torch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-10
RF Coil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-11
Removing the Scott Spray Chamber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-12
Removing the Injector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-12
Removing and Disassembling the Torch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-14
Cleaning the Torch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-16
Cleaning the Spray Chamber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-17
Replacing the Torch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-18
Replacing the Torch on the Mount . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-22
Replacing the Spray Chamber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-25
Connecting the Nebulizer (Neb) Tubing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-25
Replacing the RF Coil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-27
Windows . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-30
Removing and Cleaning the Windows . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-30
Removing the Windows . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-30
Cleaning the Windows . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-32
Replacing the Radial Window . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-32
Replacing the Axial Window . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-34
Replacing and Adjusting the Shear Gas Nozzle. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-35
Adjusting the Position of the Shear Gas Nozzle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-36
Scott-Type Spray Chamber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-37
Removing the Spray Chamber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-37
Removing the End Cap from the Spray Chamber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-37
vi 0993-6226
Contents
0993-6226 vii
Contents
Troubleshooting
A Word on 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 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-13
Plasma Ignition Problems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-13
Plasma Stability Problems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-14
Printing Problems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-15
Pump Problems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-16
Autosampler Problems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-17
RF Generator/Sample Introduction System Troubleshooting Form. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-18
Troubleshooting Form . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-18
General: . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-18
Sample Introduction Configuration: . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-18
Operating Conditions: . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-19
Instrument Environment: . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-19
Common Setup Problems: . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-20
Troubleshooting Tasks Performed: . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-21
Chapter 7:
Error Messages
System Error (SYSERROR) Messages for RF Generator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-3
Index
viii 0993-6226
Other Guides for the Optima 2000 DV
In addition to this guide, the following guides are also provided for the
Optima 2000 DV.
• Winlab32 Software Guide (Part No. 0993-6335). This guide contains basic
information on the ICP WinLab software, step-by-step procedures, and
comprehensive chapters that cover each of the software windows and parameters
for reference.
0993-6226 ix
Company Name and Addresses
U.S.A.:
PerkinElmer Instruments
710 Bridgeport Avenue
Shelton, Connecticut 06484-4794
U.S.A.
Phone: 800-762-4000 or
(+1) 203-762-4000
United Kingdom: PerkinElmer on the Internet:
PerkinElmer Ltd. http://www.perkinelmer.com
Chalfont Road Seer Green
Beaconsfield, Bucks, HP9 2FX
United Kingdom
x 0993-6226
Safety Information
1Safety Information
1
0993-6226 1-1
Safety Information
Safety conventions
The guide provided with the instrument contains information and warnings that
must be followed by the user to ensure safe operation and to maintain the
instrument in a safe condition. This advice is intended to supplement, not
supersede, the normal safety code of behavior prevailing in the country of
operation.
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 user and the user’s organization.
Possible hazards that could harm the user or result in damage to the instrument
are clearly stated at appropriate places throughout this guide. Any of the
following safety conventions can be used throughout this guide:
This symbol alerts you to situations that could result in personal injury to yourself
or other persons.
Details about these circumstances are in a box like this one.
This symbol alerts you to the risk of electric shock that could result in personal
injury to yourself or other persons.
Details about these circumstances are in a box like this one.
This symbol alerts you to the risk of hot surfaces that could cause personal
injury to yourself or other persons.
Details about these circumstances are in a box like this one.
This symbol alerts you to the risk of ultraviolet radiation that could cause
eye damage to yourself or other persons.
Details about these circumstances are in a box like this one.
Caution The term CAUTION alerts you to situations that could result in serious damage
to the instrument or other equipment.
Details about these circumstances are in a box like to this one.
0993-6226 1-3
Safety Information
Safety interlocks
PerkinElmer provides a number of safety interlocks to protect the user and other
persons from radio frequency (RF) radiation, ultraviolet radiation, high
temperatures, and high voltage areas.
• Do not attempt to defeat these interlocks; you may compromise your own, or
someone else’s, safety.
1-4 0993-6226
Safety Information
Electrical safety
W2.1
Warning: Electrical Hazard
Any interruption of the protective conductor inside or outside the instrument or
disconnection of the protective conductor (earth/ground) terminal is likely to
make the instrument dangerous.
Intentional interruption is prohibited.
Lethal voltages are present in the instrument
– Even with the power switch off, line power voltages can still be present within
the instrument.
– When the instrument is connected to line power, terminals may be live, and
opening covers or removing parts (except those to which access can be
gained without use of a tool) is likely to expose live parts.
– Capacitors inside the instrument may still be charged even if the instrument
has been disconnected from all voltage sources.
• To ensure satisfactory and safe operation of the instrument, the line power
cord must be connected to a correctly installed line power outlet that has a
protective conductor (earth/ground).
• Do not attempt to make internal adjustments or replacements except as
directed in the guide provided with the instrument.
• Do not operate the instrument with any covers or parts removed.
• 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 skilled person who is
aware of the hazard involved.
• Use only fuses with the required current rating and of the specified type for
replacement. Do not use makeshift fuses or short-circuit the fuse holders.
• Whenever it is likely that the instrument is no longer electrically safe for use,
make the instrument inoperative and secure it against any unauthorized or
unintentional operation. The instrument is likely to be electrically unsafe
when it:
– Shows visible damage, or has been subjected to severe transport stresses.
– Fails to perform the intended measurement.
– Has been subjected to prolonged storage under unfavorable conditions.
0993-6226 1-5
Safety Information
The instrument generates high levels of Radio Frequency (RF) energy, which is
potentially hazardous if allowed to escape.
W10.2
Warning: Radio Frequency Radiation – Risk of Burns
RF radiation can heat tissue, causing severe burns and internal injuries.
The instrument is designed to contain the RF energy within the shielded
enclosures. Safety interlocks prevent you from operating the instrument when
doors, shields, or covers are not in place.
• Never attempt to defeat the safety interlocks since this may expose you to
hazardous RF radiation.
FCC Compliance
This equipment has been tested and found to comply with the limits for a Class B
digital device, pursuant to Part 15 of the FCC Rules.These limits are designed to
provide reasonable protection against harmful interference when the equipment is
operated in a commercial environment. This equipment generates, uses, and can
radiate radio frequency energy and, if not installed and used in accordance with
the instruction manual, may cause harmful interference to radio communications.
Operation of this equipment in a residential area is likely to cause harmful
interference in which case the user will be required to correct the interference at
his or her own expense. Changes or modifications not expressly approved by the
manufacturer could void the user's authority to operate the equipment.
Ultraviolet radiation
The plasma generates high intensity ultraviolet radiation. The torch compartment
has a viewing window for safely viewing the plasma.
W3.6
Warning: UV Radiation – Risk of Eye Damage
The plasma generates high intensity UV radiation.
A safety interlock is used to automatically shut off the plasma if the torch
compartment door is opened.
• Never attempt to defeat the safety interlock and view the plasma directly.
This can cause permanent eye damage.
1-6 0993-6226
Safety Information
High temperatures
Operating conditions
W1.3
Warning: Explosive Atmosphere
This instrument is not designed for operation in an explosive atmosphere.
You can store the instrument safely under the following conditions:
• Ambient temperature –20 °C to +60 °C (–4 °F to +140 °F).
• Ambient relative humidity 20% to 80%, without condensation.
• Altitude in the range 0 m to 2000 m.
When you remove the instrument from storage and before you put it into
operation, allow it to stand for at least a day under the approved operating
conditions.
0993-6226 1-7
Safety Information
Laboratory hygiene
• Keep the work area scrupulously clean to avoid contaminating your samples
and to maintain a safe working environment. Clean up spilled chemicals
immediately and dispose of them properly.
• Do not allow smoking in the work area. Smoking is a source of significant
contamination and also a potential route for ingesting harmful chemicals.
• Do not store, handle, or consume food in the work area.
Laboratory ventilation
Toxic combustion products, metal vapor, ozone, etc., can be generated by the
system, depending on the type of analyses being performed. You must provide an
efficient laboratory ventilation system to remove toxic products generated during
instrument operation. Detailed specifications for a recommended venting system
are described in Chapter 2, Preparing Your Laboratory.
Waste disposal
The materials that you collect in waste containers may include small amounts of
the substances that were analyzed and other chemicals used in the analyses.
If these materials are toxic, corrosive, or contain organics you may have to treat
the collected effluent as hazardous waste. Refer to your local safety regulations
for proper disposal procedures.
1-8 0993-6226
Safety Information
The responsible body1 must take the necessary precautions to ensure that the
surrounding workplace is safe and that instrument operators are not exposed to
hazardous levels of toxic substances (chemical or biological) as defined in the
applicable national, state, and local health and safety regulations and laws.
Venting for fumes and disposal of wastes must be in accordance with all national,
state, and local health and safety regulations and laws.
• Use, store, and dispose of chemicals in accordance with the manufacturer’s
recommendations and the applicable national, state, and/or local regulations.
• Wear appropriate eye protection at all times while handling chemicals.
Depending on the types of chemicals you are handling, wear safety glasses
with side shields, or goggles, or a full-face shield.
• Wear suitable protective clothing, including gloves if necessary, resistant to
the chemicals you are handling.
• When preparing chemical solutions, always work in a fume hood that is
suitable for the chemicals you are using.
• Perform sample 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, away
from the instrument.
0993-6226 1-9
Safety Information
Identifying cylinders
• Legibly mark cylinders to clearly identify the contents and status (full, empty,
etc.). Use the chemical name or commercially accepted name for the gas.
Storing cylinders
• Store cylinders in accordance with the applicable national, state, and/or local
regulations and standards.
• When gas cylinders are stored in confined areas, such as a storage room, make
sure that ventilation is adequate to prevent toxic or explosive accumulations
of gas.
• Do not store cylinders near exits and exit routes, elevators, gangways, or in
locations where heavy moving objects may strike or fall against them.
• Locate gas cylinders away from heat sources, including heat lamps.
Compressed gas cylinders should not be subjected to temperatures above
52 °C (125 °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 all gas cylinders only in a vertical position, with the valve cap in place,
and fastened securely to an immovable bulkhead or a permanent wall.
• If you store cylinders outdoors, store them above ground on a suitable floor
1-10 0993-6226
Safety Information
where they are protected against temperature extremes (including the direct
rays of the sun).
Handling cylinders
• Move cylinders with a suitable hand truck after making sure that the valve cap
is securely in place and that the cylinder is properly fastened to the hand truck.
• Use only approved regulators, tubing, and hose connectors. When you
connect fittings, keep in mind that left-hand thread fittings are used for fuel
gas connections (e.g., acetylene), whereas right-hand thread fittings are used
for oxidant and support gas connections (e.g., nitrous oxide, air).
• Arrange gas hoses where they will not be damaged or stepped on and where
things will not be dropped on them.
• Check the condition of pipes, hoses, and connectors regularly, and replace any
damaged parts.
• Do not attempt to refill gas cylinders.
• Perform periodic gas leak tests at all joints and seals of the gas system by
applying an approved gas leak detection solution.
0993-6226 1-11
Safety Information
1-12 0993-6226
Safety Information
This symbol indicates the off position of the main power switch or circuit
breaker. With the switch in this position, the instrument is disconnected entirely
from the line power supply.
This symbol indicates the on position of the main power switch or circuit
breaker. With the switch in this position, the instrument is connected to the line
power supply but is not necessarily switched on and operational.
0993-6226 1-13
Safety Information
1-14 0993-6226
Safety Information
Label #4 in Warning: All field wiring must have insulation suitable for at least 300 V.
Figure B. Avertissement: Le cablage a pied d’ouvre doit etre certifiés pour un
minimum de 300 V.
Label #5 in Warning: Disconnect supply before servicing.
Figure B. Avertissement: Couper l’alimentation avant l’entretien.
Label #6 in CAUTION: This unit contains protective circuitry. Contact PerkinElmer
Figure B. 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.
The instrument has AC line surge suppressing components which require
disconnection before testing. For safety reasons, testing and servicing
should be carried out only by a PerkinElmer service engineer or similarly
authorized and trained person.
0993-6226 1-15
Safety Information
1 2 3 4 5 6
Figure B. Location of warning labels on the back and side of the instrument.
1-16 0993-6226
Safety Information
0993-6226 1-17
Safety Information
Front of Instrument,
Sample Compartment
Door Open
1-18 0993-6226
Preparing Your
Laboratory 2
0993-6226
Preparing Your Laboratory
Introduction
The items listed below need to be considered when preparing the laboratory for the
Optima 2000 DV:
• Environmental Conditions
• Exhaust Vent Requirements
• Laboratory Space Requirements
• Cooling Water Requirements
• Electrical Requirements
• Pneumatic Requirements
Environmental Conditions
The laboratory in which the Optima 2000 DV Spectrometer system is located must
meet the following conditions:
• corrosive-free environment.
• The heat dissipated directly into the laboratory when properly vented by the
Optima 2000 DV is approximately 6600 BTU/hour (2200 W).
• Dust levels not above 36 000 000 particles, 0.5 micron or larger, per cubic meter
of air. The environment should be relatively dust-free to avoid sample and
instrument contamination problems.
The Optima 2000 DV has been designed for indoor use. Do not use the instrument
in an area where explosion hazards may exist.
0993-6226 2-3
Preparing Your Laboratory
The Optima 2000 DV requires an exhaust vent to remove 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.
• It helps to protect the instrument from corrosive vapors that may originate from
the sample(s).
• It removes dissipated heat produced from the torch and power supply.
The maximum temperature for the ICP torch vent system is 200 °C (392 °F). To
withstand these temperatures stainless-steel tubing must be used.
ICP torch vent required minimum flow rate is 5600 liters/min (200 cubic feet/min)
at the end of the venting hood.
Note Local electrical codes do not allow PerkinElmer Service Engineers to install the
blower and vent assembly.
The blower capacity depends on the duct length and number of elbows or bends used
to install the system. If an excessively long duct system or a system with many bends
is used, a stronger blower may be necessary to provide sufficient exhaust volume.
Alternatively, smooth stainless-steel tubing may be used instead of flexible stainless-
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
2-4 0993-6226
Preparing Your Laboratory
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.
• Make sure duct casing is installed using fireproof construction. Route ducts
away from sprinkler heads.
• Locate the blower as close to the discharge outlet as possible. All joints on the
discharge side should be airtight, especially if toxic vapors are being carried.
• Equip the outlet end of the system with a back draft damper and take the
necessary precautions to keep the exhaust outlet away from open windows or
inlet vents and to extend it above the roof of the building for proper dispersal of
the exhaust.
• Equip the exhaust end of the system with an exhaust stack to improve the overall
efficiency of the system.
• Make sure the length of the duct that enters into the blower is a straight length at
least ten times the duct diameter. An elbow entrance into the blower inlet causes
a loss in efficiency.
• Ensure that the system is drawing properly by using an air flow meter.
• Equip the blower with a pilot light located near the instrument to indicate to the
operator when the blower is on.
The venting system for the ICP torch should be positioned over the Torch
Compartment Chimney located on top of the sample compartment. For proper
instrument venting, order PerkinElmer Venting Kit # 0303-0406. The minimum
distance from the top of the instrument’s Torch Compartment Chimney to the bottom
of the extraction vent should be 7.5-12.5 cm. (3-5 in.). Gas, water, and air lines are
also provided. The gas line is 6 m (20 ft.) long. The water line is 1.4 m (4.5 ft.) long.
The air line is 3.6 m (12 ft.) long. Figure 2-1 shows the location of the ICP torch
exhaust vent. Figure 2-1 shows the location of the ICP torch exhaust vent.
0993-6226 2-5
Preparing Your Laboratory
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.)
2-6 0993-6226
Preparing Your Laboratory
To provide access for servicing and space for ventilation, allow at least 61 cm (24
in.) of space between the instrument and the laboratory walls.
0993-6226 2-7
Preparing Your Laboratory
81 cm
(32 in.)
76 cm
(30 in.)
132 cm
(52 in.)
PolyScience Chiller
The PolyScience 6105PE recirculating 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 61.0-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 = 1.4 meters or approximately 4 feet).
2-8 0993-6226
Preparing Your Laboratory
A water supply is required to dissipate heat from the RF coil and the oscillator.
Recirculating System
A recirculating system (Chiller) must be used. The requirements for the chiller are:
o
• Cooling Capacity at 20 C 950 watts
o
Temperature Stability ± 1 C
Pump Rate 1 US gal/min. at 55 psi max (45 psi min).
Coolant: distilled water
The PolyScience Chiller comes with its own Instruction Manuals. The headquarters
for PolyScience Instruments is located at:
0993-6226 2-9
Preparing Your Laboratory
Electrical Requirements
Optima 2000 DV
• The spectrometer requires a stable line power supply at 200-240 V, +6% –10%,
50/60 Hz ± 1%, rated for 15 A, that has a correctly wired protective earthing
system (ground connection) and a separate circuit breaker. Maximum power
consumption is 2800 VA. The line power supply must conform with local safety
regulations and be checked by a qualified electrician before you connect the
instrument to line power.
• The line power supply should be free of line transients in excess of 50 V peak.
If the electrical supply voltage produces large AC line voltage fluctuations, a
qualified electrician should install a voltage regulator between the electrical
outlet and the instrument.
• The Optima 2000 DV instrument is supplied with a 2.5 m (98 in.)line power cord
that supplies both the spectrometer and the RF Generator. The line power supply
point must be within 2.5 meters of the rear of the spectrometer.
• Connect the spectrometer, computer, printer, and any accessories to the same
phase of the line power supply and the same protective earth.
Note PerkinElmer instruments will normally operate within ± 10% of the specified voltage
and within ± 1 % of the specified frequency, unless otherwise noted. If the power line is
unstable, fluctuates in frequency or is subject to surges, additional control of the
incoming power may be required.
The Optima 2000 DV must not have a Ground Fault Circuit Interruptor (GFCI)
protected outlet. The instrument will trip the interruptor if this type of outlet protection
is used.
The Optima 2000 DV is equipped with an IEC 309 2 pole plus protective earth
connector, rated for 250 V 16/20A (Hubbell Part No. C320P6SVL, PerkinElmer Part
No. 0999-7530) that inserts into a receptacle (Hubbell Part No. C320R6SVL,
2-10 0993-6226
Preparing Your Laboratory
PerkinElmer Part No. 0999-7529). To order directly from Hubble you can also use
these two alternative Hubble part numbers.
• For the US/Canada (20A service) use Hubble Part No. C320R6W.
• For Europe (16A service) use Hubble Part No. C316R6S.
PolyScience Chiller
The specific electrical requirements for the PolyScience 6105PE 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.
0993-6226 2-11
Preparing Your Laboratory
Pneumatic Requirements
Argon
Liquid or gaseous argon can be used with the Optima 2000 DV system. The use of
liquid or gaseous argon tanks is determined primarily by the usage rate. Liquid argon
is usually less expensive per unit volume to purchase, but cannot be stored for
extended periods. If liquid argon is used, the tank should be fitted with an over-
pressure regulator for safety reasons. The over-pressure regulator vents the tank as
necessary to keep the argon cool enough to remain in its liquid state, thus preventing
the cylinder from exploding due to pressure build-up. A tank of liquid argon
containing 160 liters will typically last for 80 hours of continuous running time.
Gaseous argon tanks do not require venting and consequently can be stored for
longer periods without loss. A tank of gaseous argon will last 5 to 6 hours of running
time. The normal argon usage is 16-20 liters/min. with a maximum of 25 liters/min
(0.04 - 1.0 cu. ft/min). The argon flow for the system (including the ICP) may vary
between 1 and 25 L/min.
Caution Gas delivery lines from the argon tank should be contaminant-free and
not made of plastic. Teflon delivery lines are acceptable.
Available argon pressure should be between 550 to 825 kPa (5.5 to 8.25 bar or 80 to
120 psig ).
Argon can be purchased from local suppliers. The argon for use with ICP systems
should be 99.996% pure.
Purge Gas
Nitrogen or argon can be used to purge the Optima 2000 DV spectrometer optics.
The purge gas high flow is 5 L/min. The low gas flow is 1.0 L/min.
Caution Gas delivery lines from the purge gas tank should be contaminant-free and not
made of plastic. Teflon delivery lines are acceptable.
The available pressure should be between 275 and 825 kPa (2.75 to 8.25 bar or 40 to
120 psig).
The purge gas should be 99.999% pure and is available from local suppliers.
2-12 0993-6226
Preparing Your Laboratory
Shear Gas
Air or nitrogen can be used to shear the plasma for the Optima 2000 DV. The Optima
2000 DV RF generator typically consumes the shear gas at a rate of 25 L/min.
Available pressure should be between 550 and 825 (5.5 to 8.25 bar or 80 to 120 psig).
Regulator
A pressure regulator for use with either argon or nitrogen is available from
PerkinElmer as Part No. 0303-0264. To connect the regulator to the instrument gas
controls, use the 1/4-in. Swagelok connector. The gas tube provided has 1/4-in.
Swagelock fittings.
0993-6226 2-13
Preparing Your Laboratory
2-14 0993-6226
System Description 3
0993-6226
System Description
Introduction
0993-6226 3-3
System Description
Peristaltic Pump
3-4 0993-6226
System Description
Spectrometer
Introduction
The core of the optical system comprises a dual Echelle monochromator with a dual,
backside-illuminated, cooled, CCD detector. The system is specifically designed for
ICP-OES. Computer controlled transfer optics direct the radiation from the plasma
into the monochromator. The optics housing is sealed and continuously purged with
high purity nitrogen.
Signals at the required analytical wavelengths are measured using a scanning CCD
(charged coupled device) based technology, with simultaneous measurement of the
background emission and a neon spectrum for active wavelength correction.
Transfer Optics
The computer controlled transfer optics are used to select either radial or axial
viewing of the plasma and to direct the radiation from the plasma onto the entrance
slit of the monochromator. The exact viewing position, horizontal and vertical
position, can be selected in the software.
0993-6226 3-5
System Description
Echelle Grating
Parabolic
Collimators
Transfer Optics
Mirrors
Torch Prism
Detector
Radial View Entrance Slit
(Internally
reflective face)
Intermediate Slit
(This is where the neon reference beam enters.)
Echelle Grating
Parabolic
Collimators
Transfer Optics
Mirrors
Axial View
Torch Prism
Detector
(This mirror moves out of the (Internally
optical path for Axial viewing.)
Entrance Slit reflective face)
Intermediate Slit
(This is where the neon reference beam enters.)
3-6 0993-6226
System Description
Monochromator
In the dual echelle monochromator, the prism monochromator acts as a preselection
system to select the required wavelength range to pass on to the echelle
monochromator. Optimally positioned slits and baffles result in very low stray light
levels reaching the echelle monochromator. The prism and echelle dispersion
systems use Littrow configurations, designed to eliminate astigmatism, with
identical, 300 mm focal length, 10° off-axis, parabolic, collimating and focusing
mirrors.
The echelle grating has 79 lines/mm with a blaze angle of 63.4°. The grating is used
in the higher orders, where the high efficiency and high dispersion allow a relatively
short focal length resulting in a compact optical system.
The dual monochromator system enables relatively high slits to be used with no loss
of image quality, which contributes to the high optical throughput. In addition, part
of the slit height is used for the simultaneous measurement of a neon reference
spectrum for wavelength correction.
Two slit width settings are available, optimized for UV and visible wavelengths. The
system automatically selects the correct slit for each analytical measurement.
0993-6226 3-7
System Description
Detector
The detector is a two-dimensional CCD device containing approximately 25,600
pixels. The photosensitive area is separated into two differently sized arrays that are
used for separate reference and analytical measurements. The analytical signal is
measured in the larger, lower array.
The rear of the actual detector area is thinned to a few micrometers to allow
illumination from the rear. This prevents the absorption of radiation by components
other than the detector pixels and maximizes the quantum efficiency without the use
of a fluorescent coating.
3-8 0993-6226
System Description
2 mm CCD array
3 mm
l
At 240 nm the array covers a wavelength range of approximately 0.52 nm, and at 850
nm, approximately 25 nm. Thus the emission line for the analyte of interest and
emission on each side of the analytical line fall simultaneously on the array. This
allows simultaneous measurement of the analyte and background signals.
To improve performance and reduce noise levels, the CCD detector is cooled
between –7 and –8 °C with an integrated Peltier cooler. The entire CCD is
hermetically sealed and the housing filled with dry nitrogen.
0993-6226 3-9
System Description
register for the respective array. This use of an effective pixel length of 3 mm results
in the low noise performance typical of CCD devices.
Photons
e- e-
e-
e-
Photosensitive Register
Register
Wavelength Correction
The optical system uses a two-component, active wavelength stabilizing system. The
overall stability is controlled by temperature and pressure sensors in the optics
housing.
3-10 0993-6226
System Description
ICP Source
RF Generator
The Optima 2000 DV uses a 40-MHz free-running solid state RF generator. The RF
power from the solid state oscillator is used to ionize the argon in the torch and excite
the atoms of the liquid sample so that they emit energy at their atomic wavelength in
the form of photons. The photons from the torch are detected optically and measured
electronically in the spectrometer section of the Optima 2000 DV. It is displayed in
terms of wavelength and intensity, which are converted to sample concentration.
The RF generator provides a power output of 750 to 1500 watts. The power output
levels are computer-controlled and may be adjusted in one-watt steps for different
sample matrices.
The RF generator is designed with RF Power Control (RFPC), using a power control
loop which maintains the plasma setting regardless of line voltage fluctuations and
changes in the plasma.
0993-6226 3-11
System Description
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
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.
3-12 0993-6226
System Description
In addition, adapters are available for special applications, such as the use of an
ultrasonic nebulizer or an external spray chamber.
Torch
The torch has a standard alumina injector with a 2.0 mm inner diameter. Other
injectors available include alumina injectors in different sizes for optimum sample
flow rate, and quartz injectors for different sample types.
Spray Chamber
Depending on the instrument configuration ordered the instrument may include a
Scott-type spray chamber or GemTip Cross-Flow pneumatic nebulizer and a
cyclonic spray chamber. Other combinations are also be available. A Ryton, double-
pass Scott-type spray chamber and the GemTip Cross-Flow pneumatic nebulizer are
one of the standard configurations. This rugged combination provides the best results
for a variety of elements and sample types.
0993-6226 3-13
System Description
Nebulizers
PerkinElmer offers these nebulizers for a wide variety of applications:
GemTip Cross-Flow Good general purpose nebulizer for the analysis of strong mineral
Nebulizer end cap acids (including HF) and samples with less than 5% dissolved solids.
N068-0503 Uses GemTips made of sapphire and ruby in a Ryton end cap for
maximum chemical resistance.
GemCone High Solids GemCone is for samples with high dissolved solids (up
(Conespray) to 20%). Low Flow GemCone permits lower nebulizer gas flow
Nebulizer rates, useful for spectral lines with high excitation energies and for
High Solids: N069-0670 providing a more robust plasma. GemCone nebulizers require an end
Low Flow: N069-0671 cap (Part No. N068-0343).
Concentric Glass Provides excellent sensitivity and precision for aqueous solutions and
Nebulizer samples with few dissolved solids (less than 1%). Self-aspirating.
(MEINHARD) 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).
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.
MEINHARD Type A General purpose Meinhard nebulizer.
0047-2020
MEINHARD Type C Used for samples containing high dissolved solids (up to 20%).
0047-2022
MEINHARD Type K Optimized for samples that require reduced nebulizer gas flow rates,
N068-1574 such as organic-based samples.
U-6000AT+ Ultrasonic For samples with low analyte and low matrix concentrations.
Nebulizer Typically improves detection limits by a factor of 10 over
N069-1709 (115 V) conventional pneumatic nebulizers.
N069-1710 (230 V)
3-14 0993-6226
System Description
Figure 3-7 GemTip Cross-Flow nebulizer and end cap N068-0503 (also shown in
cross-sectional view).
Figure 3-8 GemCone nebulizer and end cap N068-0343 (also shown in cross-sec-
tional view).
Figure 3-9 Concentric glass nebulizer and end cap N068-0343 (also shown in
cross-sectional view).
0993-6226 3-15
System Description
Nebulizer Heater
The nebulizer heater allows you to set the temperature of the spray chamber
enclosure to provide a constant temperature for the spray chamber. The nebulizer
heater ensures maximum long-term stability even as room temperature varies.
The use of the nebulizer heater also ensures that the sample aerosol is uniformly
maintained with respect to temperature and aerosol droplet size. The heater can be
used with the cyclonic and the Scott-type spray chamber. The nebulizer heater
temperature can be controlled via the software and the spray chamber door must be
closed for the heater to work properly. The heater should always be on for inorganic
analyses.
For organic, high solids or salt analyses the spray chamber should be as cool as
possible, therefore we recommend that you do not use the heater to achieve the best
performance. We also recommend that you leave the sample compartment door open
when running organic analyses. Also do not use the nebulizer heater when using an
ultrasonic nebulizer.
Peristaltic Pump
The peristaltic pump is fully computer-controlled. As an added feature, the pump
speed can be programmed to run at a fast speed for the read or rinse cycle. The
TubingSaver mode is a feature for extending the life span of pump tubing.
Autosampler
PerkinElmer offers autosamplers for automated sample handling. These
autosamplers consist of a sample table, a sample tray, and a motorized sampling arm
with an attached probe. Different sample trays are available for each autosampler,
covering a variety of sample volume and total sample capacity requirements. All
sample trays have one location for a 150-mL wash vessel.
3-16 0993-6226
System Description
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. Before you can ignite the plasma:
0993-6226 3-17
System Description
EMO Switch
The EMO switch, Emergency Off Switch, is the illuminated red switch on the front of
the instrument. 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.)
3-18 0993-6226
System Description
Software Controls
Many of the hardware settings are controlled by the software.
• Plasma and auxiliary argon flow rates: Flow rates can be automated during the
analysis with specific flow rates for each element if desired. Plasma argon is
adjustable in 1 L/min increments. Auxiliary argon is adjustable in 0.1 L/min
increments.
• Nebulizer argon flow rate: The flow rate is automatically controlled using a
mass flow controller in 0.01 L/min increments.
• Pump rate: By specifying the desired flow rate (adjustable in 0.1 mL/min
increments) and the tubing diameter, the software calculates the pump speed.
• 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.
0993-6226 3-19
System Description
Marking Function
O I Main power switch.
Connections for remote control of accessories. Do not exceed the stated
voltage and current:
Umax = 30 V AC, Imax = 0.5 A AC
Umax = 30 V DC, Imax= 2 A DC
IEEE 488.2 IEEE-488 cable 0999-1355 to connect instrument to the computer.
Line power cord, permanently attached with an IEC 309 connector. Connect
to 200-240 VAC, 15 A, IEC-309 line power outlet.
N2 Purge gas inlet for nitrogen (or argon). Use hose N069-0275
Air / N2 Shear gas inlet for air or nitrogen. Use Air hose 0077-0348
Shear Gas included with Air Dryer Filter and regulator assembly.
Ar Argon inlet for torch. Use Argon hose N069-0274.
H2O IN Cooling water inlet. Use hose N077-0341 from the Chiller.
(Red Tie)
H2O OUT Cooling water outlet. Use hose N077-0342 to the Chiller .
(White Tie)
3-20 0993-6226
System Description
Gas Connections
Shear Gas Supply
Ar Supply N2 Supply
Coolant IN
Coolant OUT
Instrument
Power to 200-240 VAC
Switch 16 AMP
Computer IEC-309 Outlet
Connection
INLET
OUTLET
Filter
Neslab CFT-75
Chiller
Figure 3-11 Electrical, gas, and cooling water connections on the spectrometer
side of the instrument.
0993-6226 3-21
System Description
System Initialization
1. The peltier cooling system for the detector starts to cool the detector.
2. The system sets up all the motors for the optics at the default positions for the
axial viewing mode.
3. The system has been continuously monitoring the detector temperature. When
the temperature is stable at about -8 °C, the system continues with the
initialization.
4. The system performs a dark current measurement; this takes about 30 seconds.
5. The system switches on the neon reference lamp and measures the intensity. If
the energy is too low, the system displays an error message. When the measured
intensity is above the lower limit, the system is ready for use.
3-22 0993-6226
System Description
Technical Data
General
Principle Inductively coupled plasma optical emission spectrometer.
Computer controlled, using a special application program running
under a graphical user interface.
Power 200 ° to 240 V AC ~, 50/60 Hz
requirements Power consumption 2800 VA
Electrical As defined in EN 61010-1-1993 (IEC 1010-1) and IEC 664:
protection Insulation: Class I
Insulation category (transient overvoltage): II
Pollution degree: 2
Safety As defined in EN 61010-1-1993 (IEC 1010-1: 1990 + A1 + A2)
standards and EN 61010-2-061:1996.
EMC Complies with the generic EMC standard EN 61326-1:1997
standards Electrical equipment for measurement, control, and laboratory
use – EMC requirements – General requirements. Meets the
requirements of the EU Directives 89/336/EEC and 92/31/EEC.
Complies with Part 18 of the FCC rules and EN 55011 Class B
Group 2.
Environmental Ambient temperature: +15 °C to +35 °C (59 °F to 95 °F)
requirements 20–80% relative humidity; non-condensing
Altitude in the range 0 m to 2000 m.
Dimensions Width: 1320 mm, 52 inches
Height: 760 mm, 30 inches
Depth: 810 mm, 32 inches
Mass 141 kg, 310 lb. Spectrometer alone, not including the computer,
(weight) autosampler, and chiller.
0993-6226 3-23
System Description
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.
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.
3-24 0993-6226
System Description
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.
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.
User Plasma Viewing: The full plasma is viewed through a UV-blocking, low-
transmittance window located in the sample compartment door.
0993-6226 3-25
System Description
Optical system
Monochromator: Wavelength range: 165 nm – 800 nm. High throughput, f/6, dual
echelle monochromator. Echelle grating: 79 line/mm, blaze angle: 63.8 °. Dispersing
prism: 30 ° calcium fluoride. Spectral bandpass: 0.009 nm at 200 nm, 0.027 nm at
700 nm.
Wavelength correction: Temperature and pressure sensors for the optics housing.
Spectrum from a neon discharge lamp is collected with each analytical
wavelength measurement and acts as a wavelength scale to enable active
wavelength correction.
3-26 0993-6226
Installation 4
0993-6226
Installation
Installation Summary
A PerkinElmer service engineer should install your system for the first time or help
you in moving the system. This chapter is provided for your reference should you
need information on moving the system, or reinstalling accessories. In conjunction
with this material, be sure to consult the Safety Practices chapter and Preparing Your
Laboratory chapter in this manual. The following sections are included in this
chapter:
• Instrument Start-up
To install the ICP WinLab software, computer, and printer, refer to Winlab32
Software Installation and Administration Guide (Part No. 0993-6397).
0993-6226 4-3
Installation
Caution If moving the Optima 2000 will subject the instrument to any freezing temperatures
you must contact a PerkinElmer service engineer to assist you in the move. The
PerkinElmer service engineer will flush all traces of cooling water from the RF
generator to prevent freezing of RF generator components.
If you must move the instrument any great distance, especially if the instrument may
be subject to vibration or jolts contact a PerkinElmer service engineer to assist
you in moving your system.
If you are only moving the instrument within the lab or to a laboratory nearby you
may use the following procedure.
• Lift the instrument onto a movable table or put it in the wooden platform
originally shipped with the instrument. See the Unpacking Instructions (Part No.
0993-6390).
• Lift into position at the new location. Make sure that the new location complies
with the laboratory requirements; see Chapter 2, Preparing Your Laboratory.
• At the new location reconnect the Quick-Change Torch module, the chiller, any
accessories, gas and water lines, the computer and the printer; see the procedures
later in this chapter.
4-4 0993-6226
Installation
After the instrument has been moved into its position, it can be connected to the
various services in the laboratory.
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.
1. Connect the instrument to the nitrogen supply using the nitrogen hose (Part No.
N069-0275, uses 1/4-in. Swagelok fitting) using a 1/4-in. space collar (Part No.
0992-0125) on both ends of the tubing. Refer to Figure 4-1.
2. Set the nitrogen supply regulator between 275 kPa and 825 kPa (2.75 to 8.25 bar
or 40-120 psig).
3. Check for leaks using a proprietary leak testing fluid for high purity gas lines.
0993-6226 4-5
Installation
4-6 0993-6226
Installation
Caution Gas delivery lines from the argon tank must be contaminant-free and not made of
plastic, although PTFE lines are acceptable.
1. Connect the instrument to the argon supply using the argon hose (Part No. N069-
0274, uses a 1/4-in. Swagelok fitting) using a 1/4-in. space collar (Part No. 0992-
0125) on both ends of the tubing.
2. Set the argon supply regulator between 550 kPa and 825 kPa (5.5 to 8.25 bar or
80-120 psig).
3. Check for leaks using a proprietary leak testing fluid for high purity gas lines.
The shear gas used is typically compressed air; however, nitrogen may also be used.
The shear gas must be clean and dry, so the instrument includes an air dryer filter
assembly (Part No. N077-0198) and is included in the Pre-Installation kit (Part No.
N077-0431). For more information on the requirements for the shear gas supply,
refer to Pneumatic Requirements in the Preparing Your Laboratory, Chapter 2.
An air hose with 1/4-in. Swagelok fittings at each end is supplied in the hose kit that
is shipped with the instrument. A second air hose is included with the PerkinElmer
Air Dryer Filter in the Pre-Installation kit (Part No. N077-0431). The following
procedure describes how to connect the PerkinElmer air compressor, filter and
regulator.
Note: If you are using house air, it must be clean and dry. The instrument includes an air
dryer assembly (Part No. N077-0198). Refer to Connecting the Shear Gas Supply
later in this chapter.
1. Install the Air Dryer Filter as described in the instructions that are included with
the filter.
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.
0993-6226 4-7
Installation
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.
! 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
Warning kPa (150 psig) at 50 °C
(125 °F). At a higher pressure, the filter bowls can be blown off and cause injury.
The following procedure describes how to set the shear gas pressure when using the
PerkinElmer Air Dryer Filter.
1. Make sure the shut-off valve on the Air Dryer Filter is closed (knob turned fully
clockwise), then set the air pressure on the air compressor to between 550 kPa
and 825 kPa (5.5 to 8.25 bar or 80-120 psig).
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 on the side of the spectrometer.
4-8 0993-6226
Installation
Note: A qualified electrician must install the single wall receptacle for the PolyScience
6105PE chiller.
Connect the instrument to the chiller inlet using coolant drain hose. 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 lines (Part No. N077-0342, uses 3/8-in
Swagelock fittings) and connect to the chiller “OUTLET” fitting. Use a 3/8-in.
space collars (Part No. 0992-0584) at the instrument. The following figure
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.
0993-6226 4-9
Installation
The chiller can be turned on or off via the software. Your service engineer will
connect the cable from the chiller to the Optima 2000 so that the chiller can be
operated remotely. See the following figure for the location of the cable connections.
4-10 0993-6226
Installation
Remote Cable
Coolant OUT (Part No.
N077-0341)
3/8-in.Space Collars
(Part No. 0992-0584)
Coolant Supply
(White Tie Wrap)
Hose (Part No.
N077-0342)
Coolant IN
From OPTIMA
"OUT"
To OPTIMA
"IN"
PolyScience 6105PE
Chiller
0993-6226 4-11
Installation
the remote chiller will automatically be on when the Optima 2000 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 WinLab 32 will have no effect on the chiller if the chiller is
already on.
If the Optima 2000 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.
Note: The plasma should never be ignited if the chiller is off.
4-12 0993-6226
Installation
3/8-in.Space Collars
(Part No. 0992-0584)
Coolant OUT
Coolant IN
PolyScience 6105PE
Chiller
0993-6226 4-13
Installation
1. Unscrew the two screws and remove the Reservoir Access Panel. Refer to the
following figure.
2. Turn the filler cap counter clockwise and lift the cap off.
3. Fill the reservoir up with the coolant fluid (Part No. N077-6060). The chiller
reservoir has a capacity of 7 liters (2 US gallons). Part N0. N077-6060 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.
4-14 0993-6226
Installation
Reservoir Plug
1. Turn the On/Off switch to the On position. The refrigeration system and the
recirculation pump will start.
2. With the chiller running, top off the Reservoir Tank and screw in the Reservoir
Plug.
0993-6226 4-15
Installation
3. Install the Reservoir Access Panel and secure it with its screws.
4-16 0993-6226
Installation
W2.3
Electrical Hazard
! To prevent potential injury to yourself and damage to the instrument, switch OFF all
Warning instruments in the system and disconnect them from the line power supply before
you perform the procedures described below.
The system component connections are as follows (see the following figure):
• IEEE cable from the computer to the instrument IEEE connector on the
spectrometer side of the instrument. IEEE cable from an optional autosampler to
the instrument IEEE connector.
Note: Extending IEEE cables by making tandem connections will compromise instrument
communication.
• The Optima 2000 DV is equipped with an IEC 309 250 V 16/20A 2 pole plus
protective earth (Hubbell Part No. C320P6SVL, PerkinElmer Part No. 0999-
7530) that inserts into a receptacle (Hubbell Part No. C320R6SVL, PerkinElmer
Part No. 0999-7529). A conduit box, Hubbel PN SP20301, PerkinElmer PN
0994-0914 is not provided with the instrument. These two parts can be ordered
through PerkinElmer Express. To order directly from Hubble you can also use
these two alternative Hubble part numbers.
• For the US/Canada (20A service) use Hubble Part No. C320R6W.
• For Europe (16A service) use Hubble Part No. C316R6S.
• Connect the computer and printer to electrical power as described in the guides
provided with these items.
Note: Make sure that the computer and printer share a common ground with the
instrument.
0993-6226 4-17
Installation
Instrument to 200-240
VAC
16 AMP (EUROPE)
20 AMP (US)
IEC-309 Outlet
4-18 0993-6226
Installation
! 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 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.
0993-6226 4-19
Installation
4. 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.
Note: For recommended torch positions, see page 4-32 later in this chapter.
4-20 0993-6226
Installation
5. 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.
O-Ring
Bonnet
Copper Foil Torch
Ignitor Contact RF Coil
Ground
Pointer
Front of Instrument,
Torch Compartment
Door Open
Ignitor
Contact
Finger
6. Slide the bonnet into position around the torch. Angle the bonnet so that it will
not touch the radial window.
0993-6226 4-21
Installation
2. For more detailed instructions on connecting the tubing, see page 5-66 .
4-22 0993-6226
Installation
Nebulizer (NEB)
Argon Tubing
Quick Disconnect
Quick Disconnect
Nebulizer (NEB)
Drain Tubing Argon Tubing
Sample
Capillary
Tubing
Waste
Vessel
Figure 4-8 Nebulizer (Neb) connections to torch and nebulizer end cap.
0993-6226 4-23
Installation
The instrument can be used with the PerkinElmer AS-90, AS-91 or 90 plus
Autosamplers. The following procedures describe the electrical connections
necessary to install the PerkinElmer autosamplers.
After the autosampler is installed, the software must be configured for the type of
autosampler you are using. This can be done during the software installation or, in
the ICP WinLab software, by selecting the Configure Autosampler command from
the System menu. See the AS-90 Series Autosampler Users Guide (Part No. 0993-
5264) for detailed information on installing the autosampler.
To connect the AS-90, AS-91 or 90 plus Autosampler via the IEEE-488 interface:
1. Connect the IEEE-488 cable supplied with the autosampler from the
autosampler to the instrument as follows:
a. Connect one end of the cable to the receptacle on the rear panel of the
autosampler labeled IEEE-488.
b. Connect the other end of the cable to the receptacle on the rear panel of the
computer or the rear panel of the instrument labeled IEEE-488. The IEEE
cables can be stacked.
3. Check that the voltage selector on the rear panel of the autosampler is set to the
correct operating voltage.
4-24 0993-6226
Installation
Instrument to 200-240
VAC
16 AMP (EUROPE)
20 AMP (US)
IEC-309 Outlet
0993-6226 4-25
Installation
Caution Never move the sampling probe holder by hand. You may damage the
autosampler if you move the sampling arm tower by hand when it is under system
control.
Turn off the power to the autosampler if you need to move the tower manually
(Unplug the plug-in power supply or disconnect the autosampler from the
spectrometer.)
When you fit the sampling probe, take care not to press forcefully in any direction
on the autosampler arm since this can damage the arm.
The sampling probe is a complete assembly. Do not attempt to take the probe apart
since this can damage it; reassembly is not possible.
After you have completed the installation and electrical connections of the
autosampler, fit the sampling probe as follows and see the next figure:
1. If not already done, carefully insert the sampling probe arm and push it down
fully.
2. Carefully insert the sampling probe from above into the probe guide. Push the
sampling probe down until about 20 mm protrude from the bottom end of the
probe guide. Use the O-ring on the probe to prevent it from slipping.
Note: The standard probe is a PTFE-lined epoxy polymer tube. This polymer is resistant to
the acids, alkalis and organic solvents normally used in analysis. If your samples
contain an organic solvent that attacks this polymer, a PTFE-lined stainless steel
sampling probe is offered as an option (Part No. B300-0152).
4-26 0993-6226
Installation
2. Holding the sample tray so that the location for the wash beaker (location 0) is
at the rear left, place the tray on the autosampler.
5. Carefully push the sampling probe down until the tip is about 5 mm above the
bottom of the beaker. The sampling probe is now at the correct height.
6. To remove the sample tray, first click on Load Tray to raise the sampling probe,
then remove the tray.
This completes the installation of the sampling probe. See the AS-90 Series
Autosampler Users Guide (Part No. 0993-5264) for detailed information on
connecting the sample tube between the sample probe and the spectrometer’s sample
input system.
0993-6226 4-27
Installation
O-Ring
Holder
Sampling
Probe Guide
Sampling
Probe
4-28 0993-6226
Installation
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
4. In the Options menu, click on Autosampler, and make sure that the software is
configured for the autosampler 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.
8. Select Axial or Radial. We recommend that you first do the alignment in one
viewing mode, then select the other viewing mode and repeat the procedure.
9. To view spectra collected during the procedure, open the Spectra Display
window.
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:
0993-6226 4-29
Installation
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.
When using radial viewing, the system adjusts the lateral viewing position only.
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.
4-30 0993-6226
Installation
3. Make sure that the torch is correctly installed, the torch compartment door is
shut, and the EMO switch is released.
8. In the Tools menu, click on Plasma Control and ignite the plasma.
Allow the torch to warm up for 30 minutes before you start making
measurements.
0993-6226 4-31
Installation
Read Parameters
Time: Auto: Min: 2 sec, Max: 10 sec
• Make sure that the read delay, wash time, and rinse times are sufficient.
• Re-check the Interelement Corrections (IECs) if you make any changes to the
ionization or excitation characteristics of the plasma after collecting IEC data.
This would include changing the source conditions or changing the nebulizer or
the torch.
4-32 0993-6226
Installation
*For the analysis of high solids, set the torch to -1 and switch the nebulizer heater off.
For more information refer to the Baffled Cyclonic Spray Chamber Kit Instruction
Sheet (0993-6506).
For the analysis of organics it may be necessary to open the sample compartment
door while the instrument is in operation
0993-6226 4-33
Installation
• Make sure you use solvent resistant tubing for organic solvents. See the table of
tubing types on page 5-66 .
• 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.
• Make sure that the spray chamber is being drained properly to avoid solution
filling the torch.
• For radial viewing, two different windows are available. If you intend to make
measurements near the detection limit, use the longer window. Instructions for
replacing the window are given on page 5-30.
4-34 0993-6226
Installation
Shipping List
0993-6226 4-35
Installation
4-36 0993-6226
Installation
0993-6226 4-37
Installation
4-38 0993-6226
Maintenance 5
0993-6226
Maintenance
Introduction
This chapter describes the routine maintenance procedures required to keep your
instrument in proper working condition and to ensure the highest possible level of
performance. It includes maintenance checks that should be done on a daily basis and
maintenance procedures that should be done periodically depending on instrument
use. This chapter is divided into several sections, each section covering maintenance
procedures for a particular component of the system.
You should perform only the maintenance procedures described in this chapter.
Record your daily maintenance procedures in the ICP-OES Maintenance Log (Part.
No. 0993-6225). If additional maintenance is required, contact a PerkinElmer service
engineer.
Caution Before using any cleaning or decontamination methods except those specified by
the manufacturer, users should check with the manufacturer that the proposed
method will not damage the equipment.
Daily Checks
Daily Cleaning
At the end of each working day, it is recommended that you flush out the sample
introduction system for five minutes with the plasma on. After analyzing aqueous
solutions, flush with deionized water or a 2% nitric acid solution, followed by
deionized water. After analyzing organic solutions, flush the system using clean
solvent. Also clean the spectrometer housing using a mild lab detergent.
Argon Supply
Make sure that an adequate supply of argon is available and connected to the system.
Check that the argon tank(s) have sufficient pressure, and that a spare tank is ready
if necessary. Argon can be purchased from local suppliers. The argon for use with
ICP systems should be 99.996% pure.
0993-6226 5-3
Maintenance
The purge gas should be 99.999% pure and is available from local suppliers.
Chiller
Fill the reservoir up with the coolant fluid (Part No. N077-6060). The chiller
reservoir has a capacity of 7 liters (2 US gallons). Part N0. N077-6060 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.
5-4 0993-6226
Maintenance
Caution To extend the life and aid in preventing devitrification of glassware, it is necessary
to remove all traces of alkali on glassware caused by handling it with bare hands.
To remove the alkali, wipe the glassware clean with cotton wool dipped in alcohol.
Caution When the humidity in your lab is high, water can condense on the RF coil when the
torch is not in operation. To prevent damage to the coil, use a soft dry cloth to
gently dry the coil before igniting the torch. Be careful not to change the position
of the coil.
Nebulizer
Check that the nebulizer is not clogged and that the sample capillary tubing is clean
and in good condition. Flush the nebulizer daily with deionized water.
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
0993-6226 5-5
Maintenance
the samples being analyzed. You should consider the usage of your spectrometer and
establish a suitable maintenance schedule, with particular emphasis on the following
areas of the system.
Caution To extend the life and aid in preventing devitrification of glassware, it is necessary
to remove all traces of alkali on glassware caused by handling it with bare hands.
To remove the alkali, wipe the glassware clean with cotton wool dipped in alcohol.
The RF coil must be kept clean to prevent arcing across the coils. Inspect the RF coil
for any deformations or carbon buildup. Replace the RF coil if there are any signs of
pitting. Pitting causes weakness in the coil which can result in a hole in the coil and
a water leak.
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.
5-6 0993-6226
Maintenance
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.
• Neslab Chiller: Flush out the chiller every 6 months. Inspect the water filter
(Part No. 0990-4845) installed on the chiller and replace the water filter element
(Part No. 0990-4846) every 3 months or as needed. To fill the chiller, use only
distilled water with an addition of Chloramine-T, one gram per gallon, as an
algaecide. The chiller reservoir has a capacity of 6.8 liters (1.8 US gallons). This
would require 1.8 grams of Chloramine-T to be added to the distilled water.
Caution Do not use deionized or tap water in the chiller. Do not use an algaecide other
than that specified above.
0993-6226 5-7
Maintenance
Performance Checks
Several checks should be done periodically to check instrument performance. These
include the sodium bullet test to check the nebulizer argon flow, the Background
Equivalent Correction (BEC) test, and Coefficient of Variation (CV) test. These tests
are described in Chapter 6, Troubleshooting.
5-8 0993-6226
Maintenance
0993-6226 5-9
Maintenance
The Quick-Change Adjustable Torch Module consists of the torch assembly, spray
chamber, and nebulizer. These components are easily removed from the system for
regular inspection and maintenance. Normal wear on these components is shown by
metal or salt deposits on the quartzware or injector, glazed or devitrified quartz, worn
O-rings, or clogged nebulizer tips.
All the O-rings in the sample introduction system must be in place and be in good
condition. Otherwise, pressure leaks may occur, which can cause difficulties in
igniting the plasma and poor performance.
It is good practice to have spare parts available before removing any of the parts of
this module, particularly the torch, since it may be accidentally broken. Replacement
parts are listed at the end of this chapter.
Plasma Torch
The plasma torch assembly is comprised of a quartz torch with an inner quartz tube,
injector, and adapter for securing the injector into an inlet in the spray chamber. The
injector supplied is an alumina injector with a 2.0 mm inner diameter. Other injectors
available include alumina injectors of different inner diameter for varying sample
flow rate, quartz injectors for different sample types and sapphire injectors for silicon
applications. For more volatile solvents, use a smaller diameter injector.
Regularly inspect the torch glassware and aerosol injector tube. The glassware
should be clean, with no traces of deposits or signs of melting. Give particular
attention to the inner quartz tube. Before removing the torch for cleaning, be sure to
have a spare torch available, in case it should break.
The quartz torch is shown in the next figure. The quartz torch has one slot and a glass
bonnet. The torch glassware is slotted so the plasma is viewed optically through the
slot and not the quartz, for best performance while maintaining optimum shielding
of the plasma from entrained air.
5-10 0993-6226
Maintenance
RF Coil
Regularly inspect the RF coil. It should not show any signs of deforming or pitting.
If your lab has high humidity, check the coil to make sure it is dry. Use a soft dry
cloth to dry the coil if necessary. To replace and adjust the RF coil refer to the
procedure, Replacing the RF Coil discussed later in this chapter.
0993-6226 5-11
Maintenance
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.
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.
1. Push and hold the injector lock with your right thumb while holding the base of
the injector adapter with your left hand.
2. Firmly pull the injector adapter out with your left hand.
Note: If the injector adapter pulls off the injector, remove the glassware and grab the
injector and push through. The injector adapter can be pulled off the injector if the
nut on the injector adapter is not tight or the O-rings on the adapter and the base of
the torch are worn.
5-12 0993-6226
Maintenance
Instrument
Left Side
Front of
Instrument
C la m p
Torch
Spray C h a m b e r C o u p ler
D rain Tubing
Torch
Injector C o u p ler
Injector Lock
0993-6226 5-13
Maintenance
! 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
Warning maintenance procedures.
3. With two hands firmly grasping the torch coupler turn in a counterclockwise
direction. Allow the two locking lugs, located on the side of the torch coupler
and guide pin to pass through the torch coupler channels and out. The torch is
mounted on an assembly that slides out. Carefully slide the torch out of the RF
coil. The torch coupler and torch are now separated from the instrument. See the
following figure.
Torch Coupler
Nebulizer
Spray Chamber
Clamp Torch Glass
Torch Holder
Torch Mount
Spray
Chamber
Figure 5-3 Removing the torch coupler from the torch mount.
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.
5-14 0993-6226
Maintenance
5. Firmly hold onto the spray chamber and lift it all the way out of the spray
chamber mounting block, which will disconnect it from the injector adaptor.
6. Press in the injector lock on the torch coupler and remove the injector. See
Figure 5-2 for a view of the injector lock.
Inspect the O-rings on the injector adapter for cracks and wear. If the O-rings
need to be removed, carefully remove them using a small paper clip with a hook
bent on one end or a mico-spatula. Do not use a knife blade because the blade
will cut the O-rings and damage the O-ring seats. Replace with new O-rings. An
injector O-ring kit is available from PerkinElmer (Part No. N077-0438).
In the next step, be sure to carefully remove the torch so you will avoid breaking the
! glassware and risking possible injury. If the torch does break, discard the broken
torch and replace (Part No. N077-0338). Remove the knurled nut, sleeve and
Warning washers on the torch mounting shaft to make sure that all glass fragments are
removed.
7. Loosen the knurled nut on the torch holder and carefully remove the torch.
Inspect the torch, if it is cracked replace with a new one (Part No. N077-0338).
If the torch needs to be cleaned see the next section Cleaning The Torch for
more information.
8. Inspect the O-rings on the torch mounting shaft for cracks and wear. If the O-
rings need to be removed, carefully remove them using a small paper clip with a
hook bent on one end or a mico-spatula. Do not use a knife blade because the
blade will cut the O-rings and damage the O-ring seats. Replace with new O-
rings. A torch O-ring kit is available from PerkinElmer (Part No. N077-0437).
Caution When the torch glassware is removed from the coil, the bonnet may be on the coil
with nothing securing it. Be careful not to knock it off and break it. There is an O-ring
that can be used to secure the bonnet. (Included with O-ring kit, Part No. N077-
0437.)
Inspect the bonnet, if it is cracked replace with a new one (Part No. N077-5289).
0993-6226 5-15
Maintenance
After installation, you will need to perform the Torch Viewing Position Alignment
Procedure described in Chapter 4, Installation.
Caution The copper foil ignitor (Part No. N077-5297) contact must be removed from the
torch glassware before it is cleaned in acid. Replace a new piece of copper foil tape
over the ignitor hole in the torch after the glass is clean and dry.
5-16 0993-6226
Maintenance
If you have been analyzing aqueous solutions, the torch glassware and injector tube
should be cleaned in an acid bath. An ultrasonic bath may be used. Start with a
solution of 5% nitric acid or aqua regia and, if deposits persist, increase the acid
concentration, up to 20% if necessary. Acid solutions must be used with care.
Observe all of the manufacturer's safety recommendations. These recommendations
are normally provided in a material safety data sheet (MSDS) supplied with the
chemical.
Caution To extend the life and aid in preventing devitrification of glassware, it is necessary
to remove all traces of alkali on glassware caused by handling it with bare hands.
To remove the alkali, wipe the glassware clean with cotton wool dipped in alcohol.
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.
0993-6226 5-17
Maintenance
5-18 0993-6226
Maintenance
Copper Foil
(Part No.
N077-5297) Torch Glass
(Part No.
N077-0338)
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
Note: If the torch glass does break, discard the broken torch and replace (Part No. N077-
0338). Remove the knurled nut, sleeve and washers and make sure that you remove
all glass fragments.
0993-6226 5-19
Maintenance
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.
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 N0.
0992-1028 for the larger O-rings or N077-6024 fore the smaller O-rings) or
iInjector 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).
5-20 0993-6226
Maintenance
Torch Coupler
Spray Chamber Clamp
(Part No. N077-6031)
Injector
(Part No.
N077-5177)
Knurled Nut
0993-6226 5-21
Maintenance
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.
3. For proper ignition, turn the torch coupler fully clockwise and continue an
additional 2 mm from where you want to go. For example, if you want the torch
set in the -3 position, turn clockwise to -5 position and then return the torch
coupler to -3 position. Then lock the torch coupler to set the hard stop for the -3
position.
If in the future you remove the torch coupler and then return it to the instrument
you will not have to reset it. The torch coupler will return to the locked position
that you set earlier.
5-22 0993-6226
Maintenance
4. 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.
5. Slide the bonnet into position around the coil and torch. Angle the bonnet so that
it will not touch the radial window.
0993-6226 5-23
Maintenance
O-Ring
Bonnet
Copper Foil Torch
Ignitor Contact RF Coil
Ground
Pointer
Front of Instrument,
Torch Compartment
Door Open
Ignitor
Contact
Finger
6. 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.
5-24 0993-6226
Maintenance
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.
1. Connect one end of the nebulizer (NEB) argon tubing to the nebulizer end cap
and the other end to the quick disconnect.
2. Make sure that the teflon tubing is in good condition. Replace the tubing if
necessary. Connect the sample capillary tubing to the nebulizer sample inlet.
For instructions on connecting tubing to the peristaltic pump see the section on the
Peristaltic Pump, later in this chapter.
0993-6226 5-25
Maintenance
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.
5-26 0993-6226
Maintenance
! If the plasma has been on, the torch will be very hot and can cause serious burns.
Wait five minutes after turning off the plasma before you begin these maintenance
Warning procedures.
Caution Use a backing wrench on the stationary part of the Swagelok fitting when removing
or installing the load coil. This will prevent any excess pressure from being exerted
on the load coil which could damage the load coil.
Do not overtighten the Brass Swagelok nuts when replacing the RF Coil since this
can damage the coil.
If you cannot align the RF coil with the torch and bonnet contact a PerkinElmer
Service Engineer.
6. Place paper towels below the load coil to absorb any water that is spilled.
7. Loosen the two 1/2-inch Brass Swagelok nuts that hold the RF coil in place.
8. Replace with a new RF coil (Part No. N077-5299) and tighten the Brass
Swagelok nuts until hand-tight then tighten an additional 1/4 turn.
0993-6226 5-27
Maintenance
Emergency
Of f Switch
RF Coil
Micro
Switches
(Torch Door
Interlock)
1/2-inch
Swagelok Nuts
5-28 0993-6226
Maintenance
0993-6226 5-29
Maintenance
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
Warning procedures.
Gradually, deposits may accumulate on the windows, for example, metallic oxides,
and the windows may become etched. You must remove the windows to clean or
replace them.
If you notice a drop in UV performance the purge windows may needed to be cleaned
or replaced even if the windows still look clear. Clean the windows first, if the UV
performance does not improve replace the windows.
The axial window mount is also the purge outlet for the spectrometer. The radial
window is a cylinder with one closed end; this end being the actual window.
Caution 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.
Normally you should remove the axial window before you remove the radial
window. This releases the pressure in the spectrometer and helps avoid objects or
contamination falling into the radial snout.
1. Remove the torch assembly; see the section Removing and Disassembling the
Torch earlier in this chapter.
5-30 0993-6226
Maintenance
2. Remove the two Torx-head screws that hold the shear gas nozzle
assembly in position and move the assembly carefully to one side. See the
following figure.
Axial Window
to Purge Extension
Shear Gas
Nozzle
Radial Window
Torch
Torx Screws
Retaining Ring
3. Carefully unscrew the axial window mount.You may need to use the key
provided.
4. Remove the O-ring that holds the axial window in the mount and remove the
window.
5. Unscrew and remove the radial window retaining ring. You may need to use the
key provided.
6. Lift the radial window and O-ring out of the mount — take care if the
spectrometer purge is set to high and you have not removed the axial window,
the pressure inside the spectrometer may force out the radial window.
0993-6226 5-31
Maintenance
4. If the windows are scratched or badly etched, discard them and install new ones.
Caution Do not leave fingermarks on the window. Use an optical cloth to handle the window.
Normally you should install the radial window before the axial window. This helps
avoid objects or contamination falling into the radial snout. If the axial window is
already installed, and the spectrometer purge is set to high, the pressure inside the
spectrometer may lift the radial purge window unless you hold it in place until you
have tightened the retaining ring.
3. Hold the radial window with an optical-quality cloth. Carefully push the open
end of the cylinder through the O-ring right to the base of the mount. The closed
end must be at the top.
4. Screw the radial window retaining ring onto the mount — handtighten firmly.
Do not overtighten. Hold the radial window with an optical-quality cloth and
push the window through the O-ring right to the base of the mount.
5-32 0993-6226
Maintenance
Radial Window
O-Ring
0993-6226 5-33
Maintenance
1. Hold the axial window with an optical-quality cloth and refit the window in the
mount.
4. Screw the axial window mount onto the axial snout — handtighten firmly, do not
overtighten.
Axial Snout
Radial Window
Purge Outlet
O-Ring
Radial Window
Mount Axial Window
5-34 0993-6226
Maintenance
The basic shear gas nozzle position is with a 1 to 2 mm gap between the nozzle slit
and the front edge of the axial window mount. For some special analyses you may
want to move the nozzle, for example, for samples containing organics or salts, set
the nozzle slit 4 mm in front of the front edge of the axial window mount.
1. Place the shear gas assembly back into position and insert the two Torx screws.
Slide the shear gas nozzle to the required position, then tighten the screws.
2. Reinstall the torch assembly; see the section Replacing the Torch earlier in this
chapter.
3. Align the torch and perform an axial and radial alignment refer to chapter 4,
Installation.
Note: Before you perform an analysis at wavelengths below 190 nm, purge the optics
overnight on high purge. For other analyses, purge the system until you obtain a
steady signal.
0993-6226 5-35
Maintenance
The basic shear gas nozzle position is with a 1 to 2 mm gap between the nozzle slit
and the front edge of the axial window mount. For some special analyses you may
want to move the nozzle, for example, for samples containing organics or salts, set
the nozzle slit 4 mm in front of the front edge of the axial window mount.
1. Loosen the two Torx-head screws that hold the shear gas nozzle assembly in
position.
2. Slide the assembly to the position you require, then tighten the screws.
5-36 0993-6226
Maintenance
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.
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.
0993-6226 5-37
Maintenance
Spray Chamber
O-Ring
(Part No. 0990-2033)
Figure 5-15 Spray chamber, end cap, and associated parts. (Illustration shows
cross-flow nebulizer end cap assembly, Part No. N077-0546.)
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.
5-38 0993-6226
Maintenance
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 (8
mm) cyclonic spray chamber (part No. N077-6053) for aqueous solutions that cause
the plasma to become unstable or extinquish frequently. You can use a cyclonic
spray chamber without a baffle (Part No. N077-6052) for aqueous solutions analysis
organic solvent analysis. Lastly you can use a narrow baffled (4mm) cyclonic spray
chamber (Part No. N077-6090) for organics.
See Table 4-3 in the Installation chapter or Table 5-4 and Table 5-13 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. Insert the cyclonic spray chamber
into the cyclonic spray chamber cap. Slide the cap closed. See the following
figure.
0993-6226 5-39
Maintenance
Cyclonic Spray
Chamber Cap
(opened position)
Cyclonic Spray
Chamber Cap
(closed position)
Figure 5-16 Installing the cyclonic spray chamber into the cyclonic spray chamber
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
5-40 0993-6226
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. 0992-0865). See the following figure.
0993-6226 5-41
Maintenance
5. To the open end of the tubing coupler (Part No. 0992-0865) connect the drain
tubing to the peristaltic pump tubing. See the procedure Installing the Drain
Tubing later in this chapter for information on connecting the drain tubing to the
drain bottle.
6. After you install the cyclonic spray chamber, install the concentric glass or
GemCone nebulizer. See the procedure, Installing the GemCone Nebulizer on
the Cyclonic Spray Chamber, later in this chapter. Insert the nebulizer, as far
as it will go, through the O-rings of the spray chamber.
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.
At first, you will see beads of water inside the cyclonic spray chamber, then after
approximately 30 seconds, the beads will begin to disappear.
5-42 0993-6226
Maintenance
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.
0993-6226 5-43
Maintenance
Nebulizers
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.
5-44 0993-6226
Maintenance
0993-6226 5-45
Maintenance
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 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:
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.
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
5-46 0993-6226
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.
Knurled Screw
Spray Chamber
Knurled Screw
Figure 5-18 The nebulizer/end cap assembly removed from the spray chamber. Il-
lustration shows cross-flow nebulizer end cap assembly.
4. To check the spray pattern, leave the sample capillary tubing and the nebulizer
argon tubing connected. Then refer to the next procedure.
2. Place the sample capillary tubing in a beaker of deionized water and start the
pump at a rate of 1.0 mL/min.
0993-6226 5-47
Maintenance
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.
5-48 0993-6226
Maintenance
Red GemTip
Argon
Clear GemTip Inlet
Sample
Inlet
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.
0993-6226 5-49
Maintenance
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.
5-50 0993-6226
Maintenance
O-Ring
(Part No. 0992-1045)
Nut
(Part No. 0992-0546)
1/16" O.D.
Teflon Tubing Piece
(Part No. 0998-5708)
Sample
Capillary
Tubing
Figure 5-20 Clear GemTip for sample inlet and associated parts for Cross-Flow
End Cap, N077-0546.
0993-6226 5-51
Maintenance
5. Check the condition of the tubing piece (Part No. 0998-5708). If the tubing is
worn, replace it as follows:
- Obtain a new piece of 1/16-in. O.D. teflon tubing (Part No. 0998-5708).
- Using a razor blade, make a straight cut on one end of the tubing.
- 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.
Figure 5-21 Installing new tubing for the sample inlet. Cross-Flow End Cap, N077-
0546.
6. To reassemble the nebulizer make sure that the O-ring is completely seated on
the base of the sample tip, then insert the sample tip into the sample inlet.
7. With the tubing and ferrule assembled as shown in the previous figure, screw the
nut into the sample inlet making a finger-tight connection. Do not use any tools
to tighten the nut.
8. Examine the two GemTips in the end cap. These tips should almost butt up to
each other at an angle of 90 °.
9. If you have installed new 1/16-in. tubing, cut the tubing so that it extends
approximately 1/2 in. beyond the nut.
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.
5-52 0993-6226
Maintenance
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.
0993-6226 5-53
Maintenance
O-Ring
(Part No. 0992-1045)
Figure 5-22 Red GemTip for argon inlet and associated parts for Cross-Flow End
Cap, N077-0546.
5. To reassemble the nebulizer make sure that the O-ring is completely seated on
the base of the argon tip, then insert the argon tip into the argon inlet.
6. Check the condition of the argon inlet tubing (Part No. 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.
5-54 0993-6226
Maintenance
Figure 5-23 Installing new tubing for the argon inlet. Cross-Flow End Cap, N077-
0546.
7. With the tubing and ferrule assembled as shown in the figure above, screw the
nut into the argon inlet making a finger-tight connection. Do not use any tools to
tighten the nut.
8. Examine the two GemTips in the end cap. These tips should almost butt up to
each other at an angle of 90 °.
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 following figure.
2. Insert the ferrule with the tubing and nut to the Quick Disconnect (Part No.
N077-5206). Connect the entire Quick Disconnect to the sample introduction
system. See the following figure.
If you replace the argon tubing with new tubing, you will need to replace the
Swagelok nut as follows. See the previous figure.
1. Using a razor blade, make a straight cut on one end of the tubing. Wire cutters
or scissors do not make acceptable cuts.
2. Put the 1/8-in. Swagelok nut (Part No. 0990-3128), rear ferrule, front ferrule, and
tubing insert onto the tubing as shown in the figure below.
0993-6226 5-55
Maintenance
4. Connect the nebulizer argon tubing to the NEB connection. Using a wrench,
tighten the 1/8-in. nut an additional 3/4 turn.
1/8-in. Tubing
(Part No. 0998-5723)
Instrument
Left Side
Nut (Part No. 0992-0545)
Figure 5-24 Connecting the nebulizer argon tubing. Cross-Flow End Cap, N077-
0546.
5-56 0993-6226
Maintenance
• 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.
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
0993-6226 5-57
Maintenance
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.
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.
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.
1. Remove the existing nebulizer/end cap assembly (if the wrong one is installed)
by loosening the knurled screws on the end cap. Use a gentle twisting action to
remove the assembly from the spray chamber.
2. Assemble the correct end cap (Part No. N077-0546) to the spray chamber with
a twisting 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.
5-58 0993-6226
Maintenance
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.
0993-6226 5-59
Maintenance
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. 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
Figure 5-26 Connecting the GemCone nebulizer to the cyclonic spray chamber.
1. Remove the nebulizer from the end cap (loosen both thumbscrews).
5-60 0993-6226
Maintenance
2. Disconnect the argon gas fitting and the capillary tube connection from the
nebulizer.
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.
0993-6226 5-61
Maintenance
Handle the concentric nebulizer carefully to avoid breaking the glassware and
! possible injury.
Warning
1. Wet the outside of a short length of Viton Orange-Orange I.D. 0.89 mm (0.036
in.) pump tubing (Cole Parmer Part No. P-07606-26). Insert this tubing as far
into the concentric nebulizer as possible.
2. After you have inserted this Viton Orange-Orange tubing, cut the tubing so that
one inch extends out from the nebulizer. Insert a section of capillary tubing (Part
No. 0990-8265) inside this short piece of peristaltic pump tubing.
3. Connect the supplied Tygon tubing (Part No. 0250-6515) to the argon inlet of
the nebulizer. Secure this tubing to the nebulizer by using the snap clamp
provided with the nebulizer. Cut the tubing to a sufficient length using a razor
blade.
5-62 0993-6226
Maintenance
Clamp
Argon Line
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.
0993-6226 5-63
Maintenance
Meinhard
Concentric Nebulizer
Figure 5-28 Installation of the Concentric Glass Nebulizer in the End Cap.
5-64 0993-6226
Maintenance
The following table summarizes the cleaning procedures for the MEINHARD
Concentric Glass nebulizer.
1. Disengage nebulizer
Examine visually (20 - 30X)
Caution When cleaning the concentric glass nebulizer, do not use ultrasonic cleaning. This
can adversely affect nebulizer performance.
Do not attempt to clean out the concentric nebulizer with any wire instrument. This
can cause irreparable damage to the nebulizer.
0993-6226 5-65
Maintenance
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.
5-66 0993-6226
Maintenance
From
Spray Chamber
To Drain Bottle
To Nebulizer
From Sample
Container
Figure 5-30 Tubing installed on pump for sample and drain (side view).
To install the sample tubing refer to the instructions below and the next two figures:
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.
0993-6226 5-67
Maintenance
Cover Door
Spray Chamber
Lip
Peristaltic
Pump Tubing
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. Using a
razor blade, bevel one end of each piece of capillary tubing by cutting it at an
angle. See the next figure.
5-68 0993-6226
Maintenance
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
Polyethylene Tubing
(Included with Nebulizer),
0.58 mm i.d.
(Part No. 0990-8265)
To Sample Inlet
6. Insert the beveled end of the nebulizer capillary tubing into the other end of the
pump tubing.
0993-6226 5-69
Maintenance
N069-5415 Sleeve
N069-5414 Adapter
0990-0267 Barbed Fitting
0998-5729 Solvent Flex Tubing
0992-0186 Tubing Coupler
0998-5729 PVC Tubing
N822-1152 Teflon Tubing
To connect the drain tubing assembly, use the following steps and refer to the next
figure.
1. Connect the coupling (Part No. N069-5415) and adapter (Part No. N069-5414)
to the spray chamber drain. Thread the barbed fitting (Part No. 0990-0267) 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. 0992-0865).
3. Use the other end of the tubing coupler (Part No. 0992-0865) to connect the drain
tubing to the peristaltic pump.
Drain tubing with 1 mm i.d. (0.04 in.) can also be used by following these steps:
1. Attach a small piece of 1.5 mm (0.06 in.) i.d. PVC tubing (Part No. 0998-5729)
to the barbed fitting (Part No. 0992-0528).
2. Cut the 1 mm i.d. tubing at an angle and insert it into the 1.5 mm tubing.
5-70 0993-6226
Maintenance
Spray Chamber
Adapter
N069-5414
Barbed Fitting
0990-0267
Drain Bottle
Install the drain tubing on an open channel of the peristaltic pump as follows:
0993-6226 5-71
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 5-33. If the tubing is installed
in the wrong direction, the spray chamber will flood.
4. For the tubing that leads to the drain bottle, use one piece of 1.07 mm i.d. (0.042
in.) teflon tubing (Part No. N822-1152). Bevel one end by cutting it at an angle.
5. Insert the teflon tubing into the other side of the pump tubing. Lead this tubing
to the drain bottle. Refer to Figure 5-34 in the Drain section.
1. Make sure the sample tubing is centered in the channel, then place the clamp
around the tubing and swing back the cam lever.
3. Set the pump speed to 1.5 mL/min and start the pump.
4. Dip the tubing in DI water a few times to let bubbles form. As you watch the
bubbles form loosen the adjustment screw in a counterclockwise direction until
the bubbles stop or do not flow smoothly.
5. Tighten the adjustment screw slowly (turn clockwise) until droplets just start
forming at the end of the SAMPLE OUT side of the sample tubing.
6. Tighten the adjustment screw until you see a smooth flow of bubbles (about 1/2
to 1 turn more on the peristaltic pump).
5-72 0993-6226
Maintenance
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.
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.
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).
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.
0993-6226 5-73
Maintenance
2. Unscrew the large screw in the center of the pump head. Place the screw and
washer in a secure place.
3. Lift the pump head off. To clean the pump head, use water or a mild solvent and
dry thoroughly.
4. Return the pump head to the pump. Orient the pump head by aligning the notch
on the bottom of the pump head with the pin on the shaft. The pump head must
click in this slot for a proper fit. Replace the washer and tighten the screw.
Drain
One drain is used on the Optima 2000 DV. This pumped drain leads from the spray
chamber.
To connect the drain to the drain bottle, refer to the next figure and follow the steps
below:
1. Connect the drain tubing leading from below the sample compartment to one of
the large fittings on the drain bottle.
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.
5-74 0993-6226
Maintenance
0993-6226 5-75
Maintenance
Air Filters
To ensure that the electrical components in the spectrometer and the RF generator
are properly cooled, check the air filters regularly to see if they are clogged or dirty.
There are two air filters on the instrument as shown in Figure 5-35. The one filter is
for the RF generator and the other for the spectrometer.
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.
3. Remove the filter and insert a new one (Part No. B051-1305).
5-76 0993-6226
Maintenance
Figure 5-35 Location of the air filters on the back of the instrument.
2. Remove the screw that secures the access panel on the right-hand side of the
spectrometer and remove the panel. Place the screw in a secure location.
3. The neon lamp assembly is the metal box that is visible inside the access hole.
Loosen the large screw on the metal box inside the access panel and pull the
metal box off the side of the optics tub.
4. Carefully slide a new neon lamp assembly (Part No. B081-0144) onto the tub
using the metal plates on the tub as guides. Tighten the large screw securely.
0993-6226 5-77
Maintenance
To fill the chiller, use only distilled water with an addition of Chloramine-T, one
gram per US gallon, as an algaecide. The chiller reservoir has a capacity of 6.8 liters
(1.8 US gallons). This would require 1.8 grams of Chloramine-T to be added to the
distilled water. Refer to Chapter 4, Installation for more information on filling the
chiller.
Caution Do not use deionized or tap water in the chiller. Do not use an algaecide other
than that specified above.
Fuses
Fuses may only be replaced by a PerkinElmer service engineer.
5-78 0993-6226
Maintenance
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
0990-2207 O-ring
0992-1028 O-ring metric
N077-6014 Washer for the injector adaptor
0993-6226 5-79
Maintenance
• If you are located outside of the U.S., call your local PerkinElmer sales office.
5-80 0993-6226
Troubleshooting 6
0993-6226
Troubleshooting
A Word on Troubleshooting
If after using the troubleshooting techniques in this chapter your instrument is still
not performing properly fill out the form at the end of this chapter and contact
PerkinElmer service.
Use the following table to guide you to the appropriate section or manual.
You are not getting the desired Optimizing and Verifying Performance in the
results. WinLab32 Software Guide or Performance
Problems: Troubleshooting Table in this
chapter.
You cannot ignite the plasma, Plasma Ignition and
or the plasma is unstable. Stability Problems in this chapter.
A red fault icon appears in the Operating Status Problems in the WinLab32
Instrument Diagnostics window Software Guide.
or the system is not ready.
There is a software error. Software Troubleshooting in the Winlab32
Software Guide.
The printer is not working. Printer Problems in this chapter.
The pump is not working. Pump Problems in this chapter.
0993-6226 6-3
Troubleshooting
The tests in this section allow the operator to measure performance aspects of the
instrument. If you are experiencing problems with your results, these tests can
pinpoint the cause of the problem.
• Sodium Bullet Test: 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.
• Precision Test: This test indicates the Relative Standard Deviation (RSD) of the
instrument's analyte emission intensity or concentration measurements. The
RSD may also be referred to as the CV (Coefficient of Variation). A high RSD
or CV is usually indicative of a problem with the sample introduction system
such as improper drainage, leaks, improper tension on the pump tubing, worn
pump tubing, or nebulizer problems. Refer to the Winlab32 Software Guide for
details.
• Detection Limit Test: This test measures the baseline signal for a blank solution
to give an indication of the lowest concentration of an element which can be
measured. The detection limit is calculated as three times the standard deviation
of the blank. Refer to the Winlab32 Software Guide for details.
6-4 0993-6226
Troubleshooting
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.
If the above checks fail to make an improvement, turn off the plasma, then check the
following:
• Check that the nebulizer end cap is connected tightly.
• Check the nebulizer spray pattern: run deionized water for several minutes, then
remove the nebulizer end cap. If the nebulizer spray is sputtering or uneven,
inspect the nebulizer tips for clogging and clean or replace them as necessary.
If the plasma has been on, allow one minute for the Quick-Change Torch Module to
! cool and an additional two minutes for the torch to cool before checking the
following.
Warning
• Check that the injector is not clogged. You will need to remove the Quick-
Change Torch Module and disassemble the torch as described in Chapter 5,
Maintenance.
0993-6226 6-5
Troubleshooting
Performance Problems
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.
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.
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?
6-6 0993-6226
Troubleshooting
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 Oring
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.
Torch Assembly
Check for deposits, particularly if running organics, alloys, or samples with high
dissolved solids. See Chapter 5, Maintenance for cleaning procedures.
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?
0993-6226 6-7
Troubleshooting
Purge Window
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.
Even if the purge windows look clean a drop in UV performance indicates that the
windows should be cleaned or replaced. First rinse with deionized water and dry with
a soft cloth. If the UV performance does not improve replace the purge windows. Do
not touch the window. If oils from the skin are deposited on the window, this can
cause inaccurate results. A 10% solution of hydrofluoric acid may be used to clean
the window. Observe the following warning statement. Soak the window briefly,
then rinse thoroughly.
Bonnet
Remove the bonnet and clean in a 20% nitric acid solution. Rinse well.
6-8 0993-6226
Troubleshooting
0993-6226 6-9
Troubleshooting
6-10 0993-6226
Troubleshooting
0993-6226 6-11
Troubleshooting
6-12 0993-6226
Troubleshooting
• If the plasma will not light check the ignitor. Open the door to the sample
compartment. Check that the ignitor finger is making contact with the tape on
the bottom of the torch glassware. Also, check the ignitor ground. If necessary,
use a brush to clean it.
• If the plasma is unstable check the exhaust vent. Be certain that your exhaust
vent is operating properly and is not blocked. Operation of the exhaust vent is
required to establish proper argon gas flow patterns as well as for safety reasons.
• Torch Connections. Verify that all gas fittings to the torch are finger-tight.
Leakage of air into any part of the torch, nebulizer or spray chamber will cause
ignition problems. The torch should be clean and in good condition. Do not use
tools to tighten, the nebulizer fittings may be damaged.
• If the plasma will not light check the RF coil. Check the RF coil for
condensation, particularly in labs with high humidity. Dry the RF coil with a soft
cloth if necessary.
• 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
0993-6226 6-13
Troubleshooting
for approximately two minutes. Then turn off the pump and try to reignite the
plasma again.
• Optics Interlock. Check that the optics is centered over the torch. Problems
with ignition may be due to the optics having been bumped out of the correct
position. If this has happened carefully move the optics to the correct position.
• Nebulizer End Cap and Fittings. Check that it is tightly secured to the spray
chamber.
• 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.
• 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.
• 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.
6-14 0993-6226
Troubleshooting
• Be sure that the injector you are using is recommended for the types of solvents
you are using. The quartz injector, 1.2 mm i.d., is recommended for typical
organic analyses. The alumina injector, 0.85 mm i.d., should be used with
volatile organic solvents, for example, methanol.
• Try increasing the RF power, using less solvent, slowing down the pump speed,
or adjusting the torch height.
Printing Problems
0993-6226 6-15
Troubleshooting
Pump Problems
6-16 0993-6226
Troubleshooting
Autosampler Problems
0993-6226 6-17
Troubleshooting
Fill out the following form before you contact PerkinElmer service.
Troubleshooting Form
General:
Instrument Serial Number:
Site:
Date:
6-18 0993-6226
Troubleshooting
Operating Conditions:
RF Power:W
Torch Position:mm
Instrument Environment:
Lab Temperature:°C± °C
Line Voltage:V
Line FrequencyHz
0993-6226 6-19
Troubleshooting
Injector Dry:Yes/No
6-20 0993-6226
Troubleshooting
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
Referring to the figures on the following pages, the plasma looked like FIGURE:
0993-6226 6-21
Troubleshooting
Figure 6-3 Rounded Plasma due to sample or air getting around the outside (typ-
ically subtle air leak)
Figure 6-4 Aux Gas too high, Air Leak, or Spray Chamber Temperature too high
6-22 0993-6226
Troubleshooting
0993-6226 6-23
Troubleshooting
6-24 0993-6226
Error Messages 7
0993-6226
Error Messages
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.
0993-6226 7-3
Error Messages
7-4 0993-6226
Error Messages
0993-6226 7-5
Error Messages
13 Failed to Failed to set Plasma Check the argon supply, argon pressure,
set Plasma flow to a value plasma flow tubing, and connections. If this
flow to specified in the Flow does not correct the problem, contact
specified Controls window. PerkinElmer Service.
level
14 Failed to Failed to set Neb Check the nebulizer tips for blockage.
set Neb flow to a value Check the argon supply, argon pressure, neb
flow to specified in the Flow flow tubing, and connections. Verify that the
specified Controls window. Nebulizer Quick Disconnect fitting is
level connected. See Figure 5-11. If this does not
correct the problem, contact PerkinElmer
Service.
15 The Attempted ignition Reset the Emergency Off Switch to correct
Emergency sequence with the this error message.
Off Switch Emergency Off If resetting the Emergency Off Switch does
is still Switch pressed. not clear the error message, check the
pressed operation of the switch.
16 Emergency Release and reset the Emergency Off Switch
Off Switch to correct this error message.
pressed If resetting the Emergency Off Switch does
not clear the error message, check the
operation of the switch.
17 Emergency Reset the Emergency Off Switch to correct
Off Switch this error message.
latched If resetting the Emergency Off Switch does
not clear the error message, check the
operation of the switch.
18 Torch not Torch interlock Contact PerkinElmer Service.
installed switch not satisfied.
19 Door open Door ajar or not Close the RF door to correct this error
sensed closed. message.
If closing the door does not clear this error
message, contact PerkinElmer Service.
7-6 0993-6226
Error Messages
0993-6226 7-7
Error Messages
7-8 0993-6226
Error Messages
0993-6226 7-9
Error Messages
7-10 0993-6226
Error Messages
46 Plasma The Flow Controls Check inlet pressure and the output
flow low Setting in the Plasma regulators and that there is enough pressure
(<10 L/m) Control Dialog into the 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 The Neb flow should Something is wrong with the Neb flow
not zero be zero but the control. Check that the Neb tubing is
hardware detects a properly connected to the Quick Disconnect
flow. to allow for flow. If this does not solve the
problem, contact PerkinElmer Service.
48 Plasma Flow control setting The ignite flow must be at least 10 L/m. See
flow < 10 is below 10 L/m. Error Message 46.
while
plasma lit
49 FLASH The Flash has been Contact PerkinElmer Service.
Checksum corrupted,
error redownload the
software.
50 AUX flow The Flow Controls The ignite flow must be at least 0.5 L/m. See
too low to Setting for AUX in Error Message 46.
ignite (0.5 the Plasma Controls
L/m) Dialog window is
< 0.5 L/m.
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.
0993-6226 7-11
Error Messages
7-12 0993-6226
Error Messages
0993-6226 7-13
Error Messages
69 Fiber Optic The firmware cannot Check that the fiber optics is in line with the
not detect the plasma load coil. If the problem persists contact
detecting after ignition. The PerkinElmer Service.
plasma in fiber optic will do a
the monitor hardware shutdown.
70 Neb back- The nebulizer has Check the sample introduction system for
pressure been shut off once the leaks and blockage and correct. Check that
>60 psi nebulizer back- all the fittings are tight and check if the
(413 kPa) pressure has fallen nebulizer spray pattern is correct. If the
& shut off below 60 psi (413 problem persists contact PerkinElmer
neb kPa). Service.
71 Neb heater The nebulizer If there is a large variance in room
sensor is compartment heater temperature you might experience instrument
not sensor is not working drift if the nebulizer compartment heater is
working- properly and the off. Otherwise the instrument is fully
heater off heater is now off. functional.
Contact PerkinElmer Service to have the
nebulizer compartment heater repaired.
7-14 0993-6226
Index
A C
Air Filters Capillary Tubing
general maintenance 5-76 inspecting 6-6
maintenance 5-76 Chiller
periodic checks 5-7 connecting 4-9
RF generator, changing 5-76 connections at back of instrument 4-11
spectrometer, changing 5-76 coolant recommended 4-14
Alignment daily checks 5-4
torch viewing position 4-29 electrical requirements 2-11
Argon filling 4-14, 4-15
checking 6-13 filters 5-78
Argon Supply requirements 2-8
connecting, instructions 3-20, 4-7 starting 4-15
daily checks 5-3 Coil, RF
requirements 2-12 see RF Coil 5-6
Autosampler compressed gases
connecting to computer 4-25 safety 1-10
description 3-16 Computer
DIP switch settings, IEEE 4-24 configuration and setup 4-3
inserting sampling probe 4-28 Connections
installing 4-24 cooling water 4-5
sampling probe fit 4-26 cooling water supplies 3-20
sampling probe height adjustment 4-27 electrical 3-20
setting up 4-26 gases 3-20, 4-5
troubleshooting problems with 6-17 Cooling Water
Axial Window connections at back of instrument 4-6
replacing 5-34 remote chiller connectionsr 4-11
B correct use of the instrument 1-4
Bonnet Cyclonic Spray Chamber
inspecting 6-8 cleaning 5-43
burner system etching 5-42
drain system 1-9 installing 5-39
maintenance 5-39
0993-6226 1
Index
D G
Daily Cleaning 5-3 Gas Supply
Dark Current replacement parts 5-79
measuring 3-19 Gases
Detector 3-8 connecting, instructions 4-5
Drain connections at back of instrument 4-6
daily checks 5-5, 6-13 H
periodic checks 5-7 Hardware Settings
tubing, connecting 5-74 controlled by software 3-19
drain system 1-9 High Temperatures
Drain Tubing safety practices 1-7
adjusting 5-73 Hoses, Gas and Water
connecting 5-70 part numbers 5-79
installing 5-67, 5-71 Hot Exhaust Gases
E safety practices 1-7
electrical protection 3-23 hygiene 1-8
Electrical Requirements I
laboratory preparations 2-10 ICP Source
electrical safety 1-5 RF control electronics 3-12
Emergency Off Switch 3-18 RF generator 3-11
End Cap Ignitor
removing from Scott spray chamber 5-37 checking cable 6-13
replacement parts 5-45 Initialization of Instrument 3-17
replacing 5-56 initialization steps 3-17
Environmental Conditions interlocks 3-17
laboratory requirements 2-3 Injector
Exhaust Vent checking 6-13
checking 6-13 removing 5-12
daily checks 5-4 Installation
requirements 2-4 autosampler 4-24
F connecting cooling water 4-5
Filters connecting gases 4-5
air 5-76 connecting the system components 4-17
part numbers 5-78 general information 4-3
replacement parts 5-78 moving the instrument 4-4
water 5-78 Quick-Change Adjustable Torch Module 4-
Fuses 19
maintenance 5-78 shipping list 4-35
summary 4-3
2 0993-6226
Index
0993-6226 3
Index
4 0993-6226
Index
0993-6226 5
Index
6 0993-6226