Optima 8000
Optima 8000
Optima 8000
OPTIMA 8000
User Assistance
Perkin Elmer.
710 Bridgeport Avenue
Shelton, CT 06484-4794
U.S.A
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Contents
Customer Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
Safety and Regulatory Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Safety Information in the Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
FCC Compliance (United States) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Europe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Environment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Symbols Used on the Instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Warning Labels on the Instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
Labels on the front of the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
Warning labels on the back and side of the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Warning labels in the torch compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Using this Guide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
Documents to Help You . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
How this Guide is Organized . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
Using the Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
A Word on Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
Chapter 1: Safety Practices
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
Laboratory Guidelines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
General . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
Environmental Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Pollution Degree . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Handling of the Instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Laboratory Ventilation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Instrument Safety Practices . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
Safety Interlocks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
Radio Frequency Radiation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
Ultraviolet Radiation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
Electrical Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
High Temperatures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Contents
4
Contents
5
Contents
6
Contents
7
Contents
8
Contents
9
Contents
10
Customer Service
Company Name and Address:
PerkinElmer
710 Bridgeport Avenue
Shelton, Connecticut 06484-4794 USA
Tel: (800) 762-4000 or (203) 762-4000
www.perkinelmer.com/supplies
The most up-to-date information on part numbers, product brochures, spare parts and
application notes are located in the PerkinElmer website.
• If you are located within the U.S., call toll-free: (800) 762-4000, Monday -
Friday, 8:30 a.m. to 7 p.m. EST. Your order will be shipped promptly, usually
within 24 hours.
• If you are located outside the U.S., call your PerkinElmer sales office.
11
Safety and Regulatory Information
This manual contains important information regarding potential hazards that may
arise during the operation of the instrument. It is essential that this information is
read and thoroughly understood by all potential users of the instrument.
In this manual, the following graphic symbols and special text formats are used to
set apart important safety information.
12
FCC Compliance (United States)
This product is classified as Industrial, Scientific and Medical (ISM) equipment and
has been tested and found to comply with the limits specified for non-consumer
equipment, pursuant to Part 18 of the FCC Rules.
Europe
All information concerning EMC standards is in the Declaration of Conformity, and
these standards may change as the European Union adds new requirements.
This instrument has been designed and manufactured, having regard to the state of
the art, to ensure that
13
Environment
Operating Conditions
Explosive Atmosphere
! This instrument is not designed for operation in an explosive atmosphere.
Warning
Pollution Degree
Storage conditions:
• Ambient temperature –20 °C to +60 °C (–4 °F to +140 °F).
• Relative humidity 20% to 80%, without condensation.
• Altitude in the range 0 m to 12,000 m (sea level to 39,370 feet).
14
When you remove the instrument from storage, before unpacking or putting it into
operation, allow it to stand for at least a day under the approved operating conditions.
15
Indicates the ON position of the main power switch.
16
Warning Labels on the Instrument
Labels on the front of the instrument
17
Warning labels on the back and side of the instrument
Label #3 in Warning - Grounding circuit continuity is vital for the safe operation
Figure B. of this instrument. Grounding is accomplished by the use of an
IEC309 instrument power plug furnished by the factory and it is not
to be removed during or after installation.
Attention: La continuité de circuit par mettre a la terre est nécessaire pour
l’opération de cet instrument sans risque. L'usine fournit la fiche
d’instrument IEC309 qui mits à la terre l’instrument. N’enlève pas la fiche
pendant ou après l’installation.
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.
18
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.
19
3
4 5 6
Figure B. Location of warning labels on the back and side of the instrument.
20
Warning labels in the torch compartment
.
21
1
22
Using this Guide
This manual is your hardware guide to the Optima 8000 instrument. Main topics
include:
• safety practices
• preparing your laboratory
• a description of the system
• installation
• maintenance
• troubleshooting
• error messages
• Winlab32 Software Guide on the WinLab CD. 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.
23
How this Guide is Organized
Thoroughly read the Safety chapter before using the instrument. Consult the
appropriate reference materials listed at the end of the Safety chapter on page 46.
24
Using the Index
Use the index to look up information on the different hardware components. If you
need to find information on cleaning the nebulizer, for example, look up “nebulizer”
in the index. Also, use the index to look up information on the following topics:
• installation
• maintenance
• troubleshooting
A Word on Troubleshooting
We recommend that you consult the troubleshooting information included in this
manual before you call a PerkinElmer service engineer. The Troubleshooting
chapter contains suggestions to help you determine systematically whether
instrument problems are due to improper analytical techniques, improper selection
of instrument parameters, or malfunction of the instrument.
25
26
Safety Practices 1
28 Safety Practices
Introduction
This chapter describes general practices designed to aid you in safely operating the
spectrometer and accessories.
This advice is intended to supplement, not supersede, the normal safety codes in
the user's country. The information provided does not cover every safety procedure
that should be practiced. Ultimately, maintenance of a safe laboratory environment
is the responsibility of the analyst and the analyst's organization.
Please consult all manuals supplied with the spectrometer and accessories before
you start working with the instrument. Carefully read the safety information in this
chapter and in the other manuals supplied. When setting up the instrument or
performing analyses or maintenance procedures, strictly follow the instructions
provided.
Laboratory Guidelines
This section describes some general laboratory safety guidelines. For additional
information, we recommend The CRC Handbook of Laboratory Safety (1) and
Prudent Practices for Handling Hazardous Chemicals in Laboratories (2).
General
The protection provided by this equipment may be impaired if the
Caution equipment is used in a manner not specified by PerkinElmer.
Always wear safety glasses when using the instrument. Safety glasses with side
shields will provide an extra margin of safety as well as mechanical protection for
your eyes.
For safety reasons and to avoid contaminating samples, be sure that the instrument
and work area are kept scrupulously clean. This is especially important when
working with toxic elements or when measuring trace amounts of any element.
Clean up spilled chemicals immediately and dispose of them properly.
Laboratory Guidelines 29
Environmental Conditions
The instrument should be used indoors in a laboratory having the environmental
conditions as recommended in Environmental Conditions on page 49.
Pollution Degree
This product will operate safely in environments that contain nonconductive
foreign matter up to Pollution Degree 2 in EN/IEC 61010-1
Laboratory Ventilation
Toxic combustion products, metal vapor, and ozone can be generated by the
system, depending upon the type of analyses. Combustion products vary with the
type of sample analyzed. If the sample compartment door is opened, a maximum
of 0.9 liters of Argon may escape during the first minute. After that, 0.1 liters/
minute of Argon will continue to escape while the door is open.
An exhaust venting system is always required to remove those gases which are
generated during the normal operation of the instrument.
30 Safety Practices
Do not position the instrument so that it is difficult to operate the main power
switch which is the disconnecting device.
Safety Interlocks
The instrument has safety interlocks to protect the operator from radio frequency
(RF) radiation and ultraviolet radiation, and to prevent access to high voltage areas.
Do not attempt to defeat the safety interlocks. This would place the
! operator's safety at risk.
Warning
The following interlocks must be satisfied in order to ignite the plasma. If any of
these interlocks is interrupted while the plasma is on, the plasma will automatically
be shut down.
• The front door on the torch compartment must be closed before the plasma can
ignite.
• Argon pressures for the torch must be correct.
• Emergency Off Switch must be released.
• Cooling water must be flowing to the plasma induction plates and oscillator.
• Quick change torch must be installed.
• The shear gas must be flowing.
Instrument Safety Practices 31
Ultraviolet Radiation
The plasma generates high intensity ultraviolet radiation. A safety interlock is used
to automatically shut off the plasma if the sample compartment door is opened or
the torch is removed. The sample compartment has a viewing window for safely
viewing the plasma.
Electrical Safety
The instrument has been designed to protect the operator from potential electrical
hazards. This section describes some recommended electrical safety practices.
High Temperatures
The torch components remain hot for some time after the plasma has been shut off.
Allow sufficient time for these items to cool to room temperature before you handle
them.
A label with a crossed-out wheeled bin symbol and a rectangular bar indicates that
the product is covered by the Waste Electrical and Electronic Equipment (WEEE)
Directive and is not to be disposed of as unsorted municipal waste. Any products
marked with this symbol must be collected separately, according to the regulatory
guidelines in your area.
The objectives of this program are to preserve, protect and improve the quality of
the environment, protect human health, and utilize natural resources prudently and
rationally. Specific treatment of WEEE is indispensable in order to avoid the
dispersion of pollutants into the recycled material or waste stream. Such treatment
is the most effective means of protecting the customer's environment.
Requirements for waste collection reuse, recycling, and recovery programs vary by
regulatory authority at your location. Contact your local responsible body (e.g.,
your laboratory manager) or authorized representative for information regarding
applicable disposal regulations. Contact PerkinElmer at the web site listed below
for information specific to PerkinElmer products.
Web address:
http://las.perkinelmer.com/OneSource/Environmental-directives.htm
36 Safety Practices
For Customer Care telephone numbers select "Contact us" on the web page.
Products from other manufacturers may also form a part of your PerkinElmer
system. These other producers are directly responsible for the collection and
processing of their own waste products under the terms of the WEEE Directive.
Please contact these producers directly before discarding any of their products.
Consult the PerkinElmer web site (above) for producer names and web addresses.
Gases commonly used with ICP instruments include argon and nitrogen. The major
hazard associated with these gases is suffocation. This can occur if the gas is
allowed to escape in an enclosed area and displaces the oxygen in the air. These
gases are neither explosive nor combustible.
Contact the gas supplier for a material safety data sheet (MSDS)
containing detailed information on the potential hazards associated
! with the gas.
Warning
Carefully use, store, and handle compressed gases in cylinders. Gas
cylinders can be hazardous if they are mishandled.
If liquid argon or nitrogen is used, the gas cylinder must be fitted with an over-
pressure regulator, which will vent the cylinder as necessary to prevent it from
becoming a safety hazard.
Listed below are some general safety practices for the proper identification,
storage, and handling of gas cylinders. Consult References 3 and 4 on page 46 for
more detailed information and additional guidelines.
Storing Cylinders
• When cylinders are stored indoors in storage rooms, the storage room should
be well ventilated and dry. Ensure that the ventilation is adequate to prevent
the formation of dangerous accumulations of gas. This is particularly important
in small or confined areas.
• Use and store cylinders away from exits and exit routes.
• Locate cylinders away from heat sources, including heat lamps. Compressed
gas cylinders should not be subjected to temperatures above 52 °C (126 °F).
• Do not allow ignition sources in the storage area and keep cylinders away from
readily ignitable substances such as gasoline or waste, or combustibles in bulk,
including oil.
Handling Cylinders
• Arrange gas hoses where they will not be damaged or stepped on, and where
objects will not be dropped on them.
• Check the condition of pipes, hoses, and connectors regularly. Perform gas
leak tests at all joints and seals of the gas system regularly, using an approved
gas leak detection solution.
• When the equipment is turned off, close all gas cylinder valves tightly at the
cylinder. Bleed the remainder of the line before turning the exhaust vent off.
Responsible body: "Individual or group responsible for the use and maintenance
of equipment, and for ensuring that operators are adequately trained." [per EN/IEC
61010-1].
Safe Handling of Gas Cylinders 39
Operator: "Person operating equipment for its intended purpose." [per EN/IEC
61010-1].
Protective Equipment
• Wear appropriate eye protection at all times while handling chemicals. Use
safety glasses with side shields, goggles, or full-face shields, according to the
types of chemicals being handled.
• Wear suitable protective clothing, including gloves specifically designed to
resist the chemicals being handled.
Sample Preparation
Sample preparation for ICP spectroscopy may require the handling of organic or
corrosive solutions. Dilution of samples and adding dilute acid to a liquid sample
is generally less hazardous than putting a solid sample into solution. This section
will deal specifically with the potential hazards associated with dissolving solid
samples, although the information can be applied to any sample handling situation.
Also, refer to the general precautions for handling chemicals described at the
beginning of this chapter.
Solid samples may be put into solution by dissolving the sample in an organic
solvent or acidic solution; digesting the sample; or reacting the sample with a
fusion mixture. Each of these techniques has certain hazards associated with it.
• Wear protective clothing and gloves. Some solvents are readily absorbed
through the skin.
Sample Preparation 41
Aliphatic hydrocarbons, ketones and esters, alcohols, and xylene, are the most
frequently used solvents. Make sure that all equipment that will come into
contact with the solvent is compatible with the solvent, e.g., tubing, sample
cups, storage and waste containers, etc.
Consult the data sheets provided by the manufacturer for information on health
hazards (see Reference 5 on page 46).
Using Acids
Acid Digestions
Acid digestions, either at atmospheric pressure or at increased pressure, require
special care. Spattering and foaming of the sample/acid mixture may expose the
user to a hazard, as well as compromise the sample integrity. A digested sample
containing concentrated acid will react violently with water.
Perchloric acid and hydrofluoric acid are particularly hazardous to work with.
Perchloric Acid
• Use hoods, ducts, and other devices for removing vapors specifically designed
to accommodate this kind of fume. There is a severe explosion hazard if a
normal hood is used, or if the hood is not properly used and maintained.
• Use goggles and face shields. Wear protective clothing and polyvinyl chloride
gloves. Do not use rubber gloves.
Hydrofluoric Acid
Hydrofluoric acid (HF) is also used for digestions. It is toxic and extremely
corrosive. Hydrofluoric acid will readily burn skin, and if the fumes are inhaled,
lung tissue. Burns may not be immediately painful or visible. Contact with eyes
could result in blindness.
Performing Digestions
• Use only the manufacturer's recommended amounts of sample and acid for the
type of sample you are preparing.
• Be sure the apparatus is in good condition and provides safe release of pressure
in the case of excess pressure buildup.
44 Safety Practices
Fusion Mixtures
Dissolving a sample by reacting with a fusion-flux mixture is generally chosen
when other techniques for sample dissolution fail. The fusion-flux mixture should
be carefully selected. Knowledge of fusion-flux mixture/crucible compatibility is
essential. Heating the sample-flux mixture may initiate a vigorous or explosive
reaction.
Caution The fusion matrix will deposit on and dissolve the quartz torch over time.
It is recommended to use the unslotted (0 slots) torch because the
slotted torches will dissolve much faster.
• Heat the mixture slowly and intermittently until the system is characterized.
• If you use a muffle furnace rather than a flame for heating, make a trial using
the standard amount of flux but with a smaller amount of sample.
• Most reacted fusion mixtures are dissolved in acidic solutions. Observe the
precautions described previously for handling acids.
Decontamination
Customers wishing to return instrumentation and/or associated materials to
PerkinElmer for repair, maintenance, warranty or trade-in purposes are advised
that all returned goods must be certified as clean and free from contamination.
Decontamination and Cleaning 45
http://las.perkinelmer.com/OneSource/decontamination.htm
If you do not have access to the internet and are located in the U.S., call toll free at
1-800-762-4000 or (+1) 203-925-4602, 8:30 a.m. - 7 p.m. EST and speak to
Customer Support.
If you are located outside of the United States or Canada, please call your local
PerkinElmer sales office for more information.
References
1. Furr, K., ed., CRC Handbook of Laboratory Safety, 5th ed., The Chemical
Rubber Co. Press, 2000.
4. Compressed Gas Association (USA), "The Inert Gases – Argon, Nitrogen and
Helium," pamphlet no. P-9, 2008.
7. Standard Methods for the Examination of Water and Wastewater, 17th ed,
American Public Health Association et al., USA, 2009.
10. Sax, N., ed., Dangerous Properties of Industrial Materials, 11th ed., Van
Nostrand Reinhold, New York, USA, 2004.
11. Bretherick, L., ed., Hazards in the Chemical Laboratory, 3rd ed., Royal
Society of Chemistry, London, UK, 1981.
Introduction
The items listed below need to be considered when preparing the laboratory for the
Optima 8000:
• Environmental Conditions
• Exhaust Vent Requirements
• Laboratory Space Requirements
• Cooling Water Requirements
• Electrical Requirements
• Pneumatic Requirements
Environmental Conditions
The laboratory in which the Optima 8000 Spectrometer system is located must meet
the following conditions:
• corrosive-free environment.
• The instrument will operate with a laboratory temperature between 15 and 35 °C
(59 - 95 °F). For optimum instrument performance, the room temperature should
be controlled at 20 ± 2 °C.
• The heat dissipated directly into the laboratory when the Optima 8000 is
properly vented is approximately 6600 BTU/hour (2200 W).
• Relative humidity between 20% and 80%, non-condensing. For optimum
instrument performance, the relative humidity should be between 35% and 50%.
• Dust levels not above 36 000 000 particles, 0.5 micron or larger, per cubic meter
of air. The environment should be relatively dust-free to avoid sample and
instrument contamination problems.
• Free of excessive vibration.
• Altitude: in the range -400 to 2,000 m (sea level to 6,562 feet)
The Optima 8000 has been designed for indoor use. Do not use the instrument in an
area where explosion hazards may exist.
Pollution Degree:
This product will operate safely in environments that contain nonconductive foreign
matter up to Pollution Degree 2 in EN/IEC 61010-1.
49
Preparing Your Laboratory
The Optima 8000 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 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 may be used instead of flexible stainless-steel
where flexibility is not required to reduce system friction loss or “drag.” If smooth
stainless steel is used, there must be a way to move the vent hood out of the way for
servicing. A length of smooth stainless-steel ducting has 20-30% less friction loss
50
Preparing Your Laboratory
• 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 (Part No. 03030447 Kit for 115
V or Part No. 03030448 Kit for 230 V) by contacting your PerkinElmer sales
representative. The minimum distance from the top of the instrument’s Torch
Compartment Chimney to the bottom of the extraction vent should be 7.5-12.5 cm.
(3-5 in.). Gas, water, and air lines of 6 m (20 ft.) are also provided. Figure 2-1 shows
the location of the ICP torch exhaust vent.
51
Preparing Your Laboratory
4
3
52
Preparing Your Laboratory
The Optima 8000 system includes the Optima 8000 instrument, a PolyScience
Recirculating Chiller (or equivalent), a computer, and a printer. The Optima 8000
instrument itself includes optics, electronics, a plasma torch, and an RF power
supply, all housed in a self-contained unit. The minimum door width must be 81 cm
(32 in.).
The Optima 8000 is 132-cm long (52-in.), 76-cm high (30-in.), and 81-cm deep (32-
in.). The bottom of the vent must be a minimum of 75-cm (3-in.) from the top of the
torch compartment chimney. Figure 2-2 illustrates the dimensions of the instrument.
The Optima 8000 weighs 146 kg (321 pounds), or 201 kg (442 pounds) with the
shipping container.
The Optima 8000 may be placed on a bench. The main power cable length is 2.4 m
(8.0 ft.).
To provide access for servicing and space for ventilation, allow at least 61 cm (24
in.) of space between the instrument and the laboratory walls.
Refer to the manuals supplied with your computer and printer for dimensions.
53
Preparing Your Laboratory
PolyScience Chiller
54
Preparing Your Laboratory
A water supply is required to dissipate heat from the plasma induction plates and the
oscillator.
Recirculating System
A recirculating system (Chiller) must be used. The requirements for the chiller are:
• Cooling Capacity at 20 °C is 2000 watts
Temperature Stability ±1 oC
Pump Rate 1 US gal/min. at 55 psi max (45 psi min).
Coolant: distilled water
55
Preparing Your Laboratory
Electrical Requirements
Optima 8000
• Optima 8000 requires an AC line voltage of 200 - 230 VAC +/-10% (180 - 253
VAC) 50/60 Hz. +/-1% under full instrument load, 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 8000 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 by the user may be required.
The Optima 8000 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 8000 is equipped with an IEC60309 250 V 16/20A 2 pole plus
protective earth plug (PerkinElmer Part No. 09997530) that inserts into an equivalent
IEC60309 series receptacle (Perkin Elmer part number 09290304 or 09290305
56
Preparing Your Laboratory
surface mount version) both of which are contained in the N0770425 conduit box kit
that ships with the instrument.
As an alternative you can use the following receptacle part numbers which can be
directly ordered from Hubble. For the US/Canada (20A service) use PerkinElmer
Part Number 09997529 Hubble Part No. C320R6SVL or C320R6W. For Europe
(16A service) use Hubble Part No. C316R6S. Also, Conduit Box-Cast Device Back
Box Hubble Part No. SP 20301 is available for the above Hubble versions.
Refer to the guides supplied with your computer and printer for electrical
requirements. The computer and printer must share a common earth ground with the
Optima 8000.
PolyScience Chiller
57
Preparing Your Laboratory
Pneumatic Requirements
Argon
Liquid or gaseous argon can be used with the Optima 8000 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 9-20 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 8000 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.
58
Preparing Your Laboratory
Shear Gas
Air or nitrogen can be used to shear the plasma for the Optima 8000. The Optima
8000 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. 0303-0284. 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.
59
Preparing Your Laboratory
60
System Description 3
System Description
Introduction
The Optima 8000 instrument consists of three major components: the spectrometer,
the ICP Source and the sample introduction system. Each component is further
divided into the different modules described below. This modular system design
facilitates system access, testing and servicing.
NOTE: All illustrations in this guide are based on the Optima 8000 instrument.
The spectrometer for the Optima 8000 consists of the following modules:
• Optics module
• Spectrometer electronics module
• Spectrometer pneumatics module
The ICP source for the Optima 8000 consists of three modules:
• RF generator module
• High voltage power supply module
• Plasma pneumatics module
63
System Description
1 4
3
64
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.
65
System Description
88
1 3
5
2
9 8
7
6
10 12 14
11
13
19
18 17
16
15
66
System Description
Item Description
4 Detector
5 Parabolic Collimators
6 Prism (internally reflective face)
7 Entrance Slit
8 Intermediate Slit (This is where the neon reference beam enters)
9 Torch
10 Axial View
11 Transfer Optics Mirrors
12 Echelle Grating
13 Detector
14 Parabolic Collimators
15 Prism (i internally reflective face)
16 Entrance Slit
17 Intermediate Slit (This is where the neon reference beam enters)
18 This mirror moves out of the optical path for Axial viewing.
19 Torch
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.
67
System Description
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.
68
System Description
3
4
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.
69
System Description
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.
1
2
3 4
6
5
7 8
70
System Description
Item Description
6 CCD Array
7 Output
8 Register for the reference measurement.
9 3 mm
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.
Photons of radiation from the analyte emission strike the photosensitive area of the
detector where photoelectrons are produced in each pixel of the detector. The
electrons are moved into the register where they accumulate as electric charge. The
charge is allowed to accumulate for the period selected for the integration time. At
the end of the integration time, the charge is transferred out of the register to the
signal processing electronics. The pixels in each vertical row are binned into the
register for the respective array. This use of an effective pixel length of 3 mm results
in the low noise performance typical of CCD devices.
71
System Description
2
3
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.
72
System Description
ICP Source
RF Generator
The Optima 8000 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 8000. 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.
73
System Description
1 3
2
5 6 4
74
System Description
Item Description
6 Power Measurement Signal
7 RF Power Control Loop
8 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 regulations regarding
radio frequency radiation.
In addition, adapters are available for special applications, such as the use of an
ultrasonic nebulizer or an external spray chamber.
75
System Description
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
Nebulizers
PerkinElmer offers these nebulizers for a wide variety of applications:
GemTip Cross-Flow Good general purpose nebulizer for the analysis of strong mineral acids
Nebulizer end cap (including HF) and samples with less than 5% dissolved solids. Uses
N0770546 GemTips made of sapphire and ruby in a Ryton end cap for maximum
chemical resistance.
GemCone (Conespray) High Solids GemCone is for samples with high dissolved solids (up to
Nebulizer 20%). Low Flow GemCone permits lower nebulizer gas flow rates, useful
High Solids: N0690670 for spectral lines with high excitation energies and for providing a more
Low Flow: N0690671 robust plasma. GemCone nebulizers require an end cap (Part No.
N0680343) for use with the Scott spray chambers.
Concentric Glass Provides excellent sensitivity and precision for aqueous solutions and
Nebulizer samples with few dissolved solids (less than 1%). Self-aspirating. Not to be
(MEINHARD) 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. N0680343) for use with the Scott spray chambers.
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.
76
System Description
MEINHARD Type C Used for samples containing high dissolved solids (up to 20%).
00472022
MEINHARD Type K Optimized for samples that require reduced nebulizer gas flow rates, such as
N0681574 organic-based samples.
U-6000AT+ Ultrasonic For samples with low analyte and low matrix concentrations. Typically
Nebulizer improves detection limits by a factor of 10 over conventional pneumatic
N0691709 (115 V) nebulizers.
N0691710 (230 V)
Mira Mist Nebulizer The Mira Mist Nebulizer is recommended for aqueous solutions. Organics
N0775330 will wet the nebulizer tip and performance will deteriorate.
Figure 3-7 GemTip Cross-Flow nebulizer and end cap N0680503 (also shown in
cross-sectional view).
77
System Description
Figure 3-8 GemCone nebulizer and end cap N0680343 (also shown in cross-sec-
tional view).
78
System Description
Figure 3-9 Concentric glass nebulizer and end cap N0680343 (also shown in
cross-sectional view).
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.
79
System Description
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.
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:
• The torch compartment door must be closed;
• the Emergency Off (EMO) switch on front of instrument must be released;
• the argon pressure for the torch must be correct;
• the cooling water must be flowing to the plasma induction plates and oscillator;
• the torch must be installed;
• the shear gas pressure must be correct.
80
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.)
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.
81
System Description
• 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.
82
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 N069275
Air / N2 Shear gas inlet for air or nitrogen. Use Air hose N0770348
Shear Gas included with Air Dryer Filter and regulator assembly.
Ar Argon inlet for torch. Use Argon hose N0690274.
H2O IN Cooling water inlet. Use hose N0770341 from the Chiller.
(Red Tie)
H2O OUT Cooling water outlet. Use hose N0770342 to the Chiller.
(White Tie)
83
System Description
2
3
7
8
4
9
6 5
10
11
12
13
Figure 3-11 Electrical, gas, and cooling water connections on the spectrometer
side of the instrument.
Item Description
1 Gas Connections
2 Ar Supply
3 Shear Gas Supply
84
System Description
Item Description
4 N2 Supply
5 Coolant IN
6 Coolant OUT
7 IEEE Computer Connection
8 Terminal strip (Part No. 09987900) for chiller remote operation
9 Power Switch
10 Instrument to 200-240 VAC, 16 AMP, IEC-309 Outlet
11 White Tie Wrap (Part No. N0770342)
12 Red Tie Wrap (Part No. N0770341)
13 Chiller
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.
85
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 (maximum)
Electrical Insulation: Class I
protection Pollution degree: 2
Safety See the Declaration of Conformity.
standards
86
System Description
Safety Interlocks: System checks water flow, shear gas flow, argon pressures,
emergency plasma off switch, 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.
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.
87
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 ° quartz. Spectral bandpass: 0.009 nm at 200 nm, 0.027 nm at 700 nm.
Transfer Optics: Computer-controlled toroidal mirrors. Adjustable viewing
position: ± 15mm along the plasma; ± 10 mm across the plasma.
Detector: Dual, backside-illuminated, cooled, CCD detector. Cooling to between -
7 and -8 °C with integrated Peltier cooler. Detector area: approximately 3 x 5 mm
split into a reference and an analyte array with separate read-out registers. Reference
array: 64 x 192 pixels of 18 x 32 m. Analyte array: 64 x 192 pixels of 18 x 56 m.
Read-out noise: 30 electrons. Dark current: 150 electrons/pixel/second. Read-out
time: 64 s. Full well capacity: 1.1 million electrons. Charge transfer efficiency:
0.99995.
Wavelength correction: Temperature and pressure sensors for the optics housing.
Spectrum from a neon discharge lamp is collected with each analytical
wavelength measurement and acts as a wavelength scale to enable active
wavelength correction.
88
Installation 4
Installation
Installation Summary
A PerkinElmer service engineer should install your system for the first time or help
you in moving the system. This chapter is provided for your reference should you
need information on moving the system, or reinstalling accessories. In conjunction
with this material, be sure to consult the Safety Practices chapter beginning on page
27and Preparing Your Laboratory chapter beginning on page 47. The following
sections are included in this chapter:
91
Installation
To install the ICP WinLab software, computer, and printer, refer to Winlab32
Software Installation and Administration Guide (Part No. 09936397).
Moving the Instrument
Caution If moving the Optima 8000 will subject the instrument to any freezing temperatures
you must contact a PerkinElmer service engineer to assist you in the move. The
PerkinElmer service engineer will flush all traces of cooling water from the RF
generator to prevent freezing of RF generator components.
If you must move the instrument any great distance, especially if the instrument may
be subject to vibration or jolts contact a PerkinElmer service engineer to assist
you in moving your system.
If you are only moving the instrument within the lab or to a laboratory nearby you
may use the following procedure.
• Remove the Quick-Change Torch module.
• Remove the chiller.
• Remove any accessories, for example an autosampler.
• Disconnect all gas and water lines.
• Remove the computer and printer.
• Attach the handles.
• Lift the instrument onto a movable table or put it in the wooden platform
originally shipped with the instrument. See the Unpacking Instructions (Part
No. 09931013).
• Lift into position at the new location. Make sure that the new location
complies with the laboratory requirements; see Laboratory Space
Requirements on page 53.
• Remove the handles.
• At the new location reconnect the Quick-Change Torch module, the chiller,
any accessories, gas and water lines, the computer and the printer; see the
92
Installation
After the instrument has been moved into its position, it can be connected to the
various services in the laboratory.
Note All gas hose connections use 1/4 inch Swagelok fittings.
Use two wrenches when making Swagelok connections. Use a space collar (Part No.
09920125, 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.
N0690275, uses 1/4-in. Swagelok fitting) using a 1/4-in. space collar (Part No.
09920125) 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.
93
Installation
1 2 3
4 5 6
3 N2 Supply
94
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.
N0690274, uses a 1/4-in. Swagelok fitting) using a 1/4-in. space collar (Part No.
09920125) 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. N0775325) and is included in the Installation kit (Part No.
N0770432). For more information on the requirements for the shear gas supply, refer
to Pneumatic Requirements on page 58.
An air hose (Part No. N0770348) 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 also
included. The following procedure describes how to connect the PerkinElmer air
compressor, filter and regulator.
Note All If you are using house air, it must be clean and dry. The instrument
includes an air dryer assembly (Part No. N0775325). 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. N0770348, uses 1/4-in. Swagelok fittings at each
end). Connect the air hose from the air compressor to the AIR IN fitting on the
95
Installation
Air Dryer Filter using a 1/4-in. space collar at both ends. Make sure the air flow
is in the proper direction, as indicated by arrows on top of the filters.
3. Locate the second air hose (Part No. N0770348, 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.
96
Installation
Note A qualified electrician must install the single wall receptacle for the
PolyScience® WhisperCoolTM chiller.
208/230V, 60 Hz
220/240V, 50 Hz
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. N0770342 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. 09920584) at the instrument. The following figure shows the water
supply connections at the instrument.
2. Locate the instrument Input coolant lines (Part No. N0770341, uses 3/8-in
Swagelock fittings) and connect to the chiller “OUTLET” fitting. Use a 3/8-in.
space collars (Part No. 09920584) at the instrument. The following figure shows
the chiller connections. Figure 4-3 on page 101shows 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.
97
Installation
98
Installation
3
2 4
7 8
11
10
99
Installation
Item Description
5 Coolant Drain Hose (Part No. N0770342) White Tie Wrap
6 From Optima Out
7 Coolant In
8 To Optima In
9 Coolant Supply Hose (Part No. N0770341) Red Tie Wrap
10 Line Cord Plug
11 Chiller
The remote chiller will automatically be on when the Optima 8000 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 8000 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.
100
Installation
6 7
101
Installation
Item Description
5 Coolant In (Part No. N0770341) Red Tie Wrap
6 Line Cord Plug
7 Chiller
Use the following procedure to fill the PolyScience® WhisperCoolTM Chiller, and
refer to the following figure.
1. Turn the filler cap counter clockwise and lift the cap off.
2. Fill the reservoir with the coolant fluid (Part No. N0776099). The chiller
reservoir has a capacity of 4.2 liters (1.1 US gallons).
3. 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.
102
Installation
103
Installation
1. Turn the On/Off switch to the On position. The refrigeration system and the
recirculation pump will start.
2. With the chiller running, top off the reservoir tank and screw in the reservoir
plug.
3. Install the reservoir access panel and secure it with its screws.
! Electrical Hazard
Warning To prevent potential injury to yourself and damage to the instrument, switch
OFF all instruments in the system and disconnect them from the line power
supply before you perform the procedures described below.
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 8000 is equipped with an IEC 309 250 V 16/20A 2 pole plus
protective earth plug (PerkinElmer Part No. 09997530) that inserts into an
equivalent IEC 309 series receptacle (see Section 2, Electrical
Requirements).
• 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.
104
Installation
105
Installation
4
5
6
7
106
Installation
Item Description
4 IEEE Cable Part No. 09991355 Computer to Instrument
5 Autosampler
6 IEEE Cable Part No. 09991355 Computer to Autosampler
7 Printer
8 AC Outlet
Note If the torch is not supplied with the copper foil ignitor in place on the torch
glassware. You must put a piece of copper foil ignitor tape (Part No.
N0781097) over the ignitor hole in the torch.
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.
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Installation
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.
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.
108
Installation
3
9
4 7
6
5
8
109
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 plasma induction
plates.
3 4
6
2 5
110
Installation
2. For more detailed instructions on connecting the tubing, see Table 5-7 on
page 213.
111
Installation
1
2
6
8
Figure 4-8 Nebulizer (NEB) connections to torch and nebulizer end cap.
Item Description
1 Nebulizer (NEB) Argon Tubing (Detail)
2 Quick Disconnect (Detail)
3 Left Side of Instrument
4 Quick Disconnect
112
Installation
Item Description
5 Nebulizer (NEB) Argon Tubing
6 Sample Capillary Tubing
7 Drain Tubing
8 Waste Vessel
The instrument can be used with the PerkinElmer S10 Autosamplers. The following
procedures describe the electrical connections necessary to install the PerkinElmer
autosamplers.
After the autosampler is installed, the software must be configured for the type of
autosampler you are using. This can be done during the software installation or, in
the ICP WinLab software, by selecting the Configure Autosampler command from
the System menu. See the S10 Autosampler User’s Guide (Part No. 09936788) for
detailed information on installing the autosampler.
113
Installation
Figure 4-9 Electrical connectors and switches located on the underside of the
autosampler.
114
Installation
2
1
5 4
Figure 4-10 Electrical connection for the S10 autosampler to the Optima spec-
trometer.
Item Description
1 Instrument
2 Serial Communication Cable (Part No. 09290259)
3 Autosampler
4 Com 1
5 Power
6 Plug-In Power Supply
115
Installation
4. Connect the autosampler to the line power supply using the plug-in power
supply provided.
The plug-in power supply uses a wide-range input of 100-240 VAC, 50-60 Hz.
Plug the power cord into the power supply, then plug the other end of the power cord
into the power source.
5. Connect the spectrometer and other components in the system to the line power
supply.
6. Switch on all components of the system, following the routine in the manual for
your spectrometer.
116
Installation
Caution When you fit the sampling probe, take care not to press forcefully
in any direction on the autosampler arm since this can damage the
arm.
1. If not already done, carefully insert the sampling probe guide from above into
the sampling probe holder on the autosampler arm and push it down fully, as
shown in the following figure.
2. Carefully insert the sampling probe from above into the probe guide.
3. Push the sampling probe down until about 20 mm protrudes from the bottom end
of the probe guide, then position the O-ring on the probe to set this position, as
shown in the following figure.
This is not the final position for the sampling probe. The probe can be adjusted
when the rinsing port has been set up. See the following procedure, Adjusting
the Sampling Probe Height on page 119.
117
Installation
Note The standard sampling probe is a PTFE-lined epoxy polymer tube. This
polymer is resistant to the acids, alkalis and organic solvents normally used
in atomic spectroscopy. If your samples contain an organic solvent that
attacks this polymer, a PTFE-lined stainless steel sampling probe is
offered as an option (B3000152).
7 2
3
5
6
4
118
Installation
Note The procedure described below assumes that you are using a spectrometer
operated via ICP WinLab software. If you are using an AA or ICP-MS
instrument, please refer to the information on operating an autosampler in
the online help for the respective instrument.
See the procedure Assembling Sample Racks starting on page 46 in the S10
Autosamplers User’s Guide (Part No. 09936788) for more information.
2. Place the rinsing port in the rinse location in the sample rack.
See the procedure Installing the Rinsing Port on the Rack starting on page 43 in
the S10 Autosamplers User’s Guide (Part No. 09936788) for more
information.
3. In the ICP WinLab software, from the main menu make the following selections:
5. Carefully push the sampling probe down until it bottoms in the rinsing port. Then
pull the sampling probe up by about 15mm as shown in the following figure. Use
the O-ring on the probe to prevent it from slipping down. The sampling probe is
now in the correct height.
119
Installation
120
Installation
This procedure adjusts the torch viewing position for the highest signal intensity.
Perform this procedure when:
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:
121
Installation
-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.
Note If you switch off the spectrometer or turn off the purge gas, air slowly
diffuses into the spectrometer optics. To make sure that the instrument is
always ready for use, especially when you intend to make measurements
at wavelengths below 190 nm, always leave the main switch of the
spectrometer in the On position and leave the purge gas turned on.
122
Installation
Read Parameters
Time: Auto: Min: 2 sec, Max: 10 sec
123
Installation
Aqueous Organics
RF power: 1500 watts 1500 watts
Nebulizer Flow: 0.6 L/min 0.4-0.5 L/min
(for Cross-Flow Nebulizer)
Auxiliary Flow: 0.2 L/min 1.0-1.5 L/min
Plasma Flow: 15 L/min 15 L/min
Sample Flow Rate: 1.5 to 2.5 mL/min 3.0 mL/min
Equilibration Time: 8 sec 15 sec
Torch Position -3 -2 to -1
*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 (09936506).
124
Installation
For the analysis of organics it may be necessary to open the sample compartment
door while the instrument is in operation
• Make sure you use solvent resistant tubing for organic solvents. See Table 5-
7 on page 213.
• 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 removing the window that are given in Removing and
Cleaning the Windows on page 168.
• PerkinElmer offers different types of nebulizers for a wide variety of
applications. For descriptions of the nebulizers and their different uses and
advantages, see Nebulizers on page 76.
125
Installation
Shipping List
Every day you count on PerkinElmer to provide you with solutions that deliver
reliable performance, control operating costs and maximize operational time. Our
complete portfolio of consumables, parts, supplies, training and service helps you
meet both routine and demanding measurement challenges. We invest heavily in
testing and validating our products to ensure you receive guaranteed compatibility
and performance - on-time, every time, for every instrument in your laboratory.
126
Installation
127
Installation
128
Installation
129
Installation
Software:
09923037 Solvent Flex Pump Tubing, 1.14mm ID, Red/Red (Drain tub-
ing)
130
Installation
131
Installation
N0776090 Narrow Baffled (4mm baffle) Cyclonic Spray Chamber for Oil
or Organics Analysis
N0770614 Cap for either the Baffled or Unbaffled Cyclonic Spray Cham-
ber
132
Installation
133
Installation
134
Installation
Filters
Kits
135
Installation
Miscellaneous
09401056 PCB-PCI/GPIB
N0770434 Fresh Air Inlet Kit (which includes the Flex Hose and Hose
Clamp)
136
Maintenance 5
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. 09936225). If additional maintenance is required, contact a PerkinElmer service
engineer. This instrument requires no specified inspection or preventive
maintenance to ensure the continuous functioning of its safety features.
Daily Checks
The following maintenance procedures should be done on a daily basis. Make sure
to inspect and replace any hoses which show signs of wear because their failure
could cause a hazard.
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.
139
Maintenance
The purge gas should be 99.999% pure and is available from local suppliers.
Nitrogen output pressure: 275-825 kPa (40-120 psig)
Chiller
Fill the reservoir up with the coolant fluid (Part No. N0776099). The chiller reservoir
has a capacity of 4.2 liters (1.1 US gallons).
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.
140
Maintenance
Caution When the humidity in your lab is high, water can condense on the plasma
induction plates when the torch is not in operation. To prevent damage to
the plasma induction plates, use a soft dry cloth to gently dry the
plasma induction plates before igniting the torch. Be careful not to
change the position of the plasma induction plates.
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. If you are planning to leave the pressure plate
clamped overnight, we recommended that you use the TubingSaver feature.
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.
141
Maintenance
Periodic Checks
The frequency of maintenance required will be determined by the amount of use the
system receives, the cleanliness of the environment, and the number and nature of
the samples being analyzed. You should consider the usage of your spectrometer and
establish a suitable maintenance schedule, with particular emphasis on the following
areas of the system.
The plasma induction plates must be kept clean to prevent arcing across the plasma
induction plates. Inspect the plasma induction plates for any deformations or carbon
buildup. Contact your PerkinElmer Service Representative to replace the plasma
induction plates if there are any signs of pitting. Pitting causes weakness in the
plasma induction plates which can result in a hole in the plasma induction plates and
a gas leak.
Nebulizer
Check the nebulizer spray pattern with deionized water. Clean or replace the
nebulizer as necessary.
142
Maintenance
Spray Chamber
Check for leaks around the nebulizer and drain fitting. Inspect the spray chamber for
deposits and check the condition of the O-rings.
Peristaltic Pump
Check that the pump rollers are clean, not scored, free from deposits due to spills,
and move freely. Remove and clean the pump head if necessary. Replace the pump
rollers if necessary.
Periodically observe the drain tubing. Liquid should drain smoothly from the spray
chamber. If not, adjust the pump tension on the pump tubing.
Drains
Check the spray chamber drain fittings, tubing and connections and replace if
necessary.
Caution Do not use deionized or tap water in the chiller. Do not use an
algaecide other than that specified above.
143
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.
144
Maintenance
145
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. 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.
146
Maintenance
If your lab has high humidity, check the plasma induction plates to make sure it is
dry. Use a soft dry cloth to dry the plasma induction plates if necessary. To replace
147
Maintenance
and adjust the plasma induction plates refer to the procedure, see Replacing the
Plasma Induction Plates on page 166.
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.
148
Maintenance
5 6
4
9 7
149
Maintenance
Item Description
5 Clamp
6-7 Torch Coupler
8 Injector Lock
9 Injector
If the plasma has been on, the torch glass will be very hot and can
! cause serious burns. Wait five minutes after turning off the plasma
before you begin these maintenance procedures.
Warning
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
plasma induction plates. The torch coupler and torch are now separated from the
instrument. See the following figure.
150
Maintenance
1 4
2
7 5
Figure 5-3 Removing the torch coupler from the torch mount.
Item Description
1 Spray Chamber Clamp
2 Nebulizer
3 Torch Coupler
4 Torch Glass
5 Torch Mount
6 Torch Holder
7 Spray Chamber
4. Pull open the clamp that holds the spray chamber in place. The action of opening
the clamp will partially push the spray chamber out.
5. Firmly hold onto the spray chamber and lift it all the way out of the spray
chamber mounting block, which will disconnect it from the injector adaptor.
6. Press in the injector lock on the torch coupler and remove the injector. See
Figure 5-2 for a view of the injector lock.
Inspect the O-rings on the injector adapter for cracks and wear. If the O-rings
need to be removed, carefully remove them using a small paper clip with a hook
151
Maintenance
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 Adapter O-ring kit is available from PerkinElmer (Part No. N0770438).
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. N0780131).
Warning Remove the knurled nut, sleeve and washers on the torch mounting shaft
to make sure that all glass fragments are removed.
7. Loosen the knurled nut on the torch holder and carefully remove the torch.
Inspect the torch, if it is cracked replace with a new one (Part No. N0780131). If
the torch needs to be cleaned see the next section Cleaning the Torch on page
153 for more information.
8. Inspect the O-rings on the torch mounting shaft for cracks and wear (see Figure
5-4). 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.
152
Maintenance
2
3
After installation, you will need to perform the Torch Viewing Position Alignment
Procedure described in Chapter 4, Installation.
153
Maintenance
Caution The copper foil ignitor (Part No. N0781097) contact must be removed
from the torch glassware before it is cleaned in acid. Replace a new piece
of copper foil tape over the ignitor hole in the torch after the glass is clean
and dry.
If you have been analyzing aqueous solutions, the torch glassware and injector tube
should be cleaned in an acid bath. An ultrasonic bath may be used. Start with a
solution of 5% nitric acid or aqua regia and, if deposits persist, increase the acid
concentration, up to 20% if necessary. Acid solutions must be used with care.
Observe all of the manufacturer's safety recommendations. These recommendations
are normally provided in a material safety data sheet (MSDS) supplied with the
chemical.
If you have been analyzing organic solutions, the 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.
154
Maintenance
mark on the torch mount and the guide pin on the torch coupler. Firmly tighten
the knurled nut. See the following figure.
1
2
4
5
6 7
12
9
8
10 13
14
11
155
Maintenance
Item Description
4 Knurled Nut (Part No. N0776027)
5 Washer (Part No. N0776028)
6 O-Ring (Part No. 09902223)
7 Spacer (Part No. N0776029)
8 O-Ring (Part No. 09921061)
9 O-Ring (Part No. 09921062)
10 O-Ring (Part No. 09902131)
11 Torch Coupler
12 Stripe on Torch
13 Index Mark on Torch Holder
14 Guide Pin
Note If the torch glass does break, discard the broken torch and replace (Part No.
N0780131). Remove the knurled nut, sleeve and washers and make sure
that you remove all glass fragments.
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. N0770602) 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 the following figure.
The Injector Positioning tool (Part No. N0770602) has a dual purpose. One end
is used to position the injector. See step two above, on how to use this feature.
After removing the torch glassware, the other end of the torch positioning tool
can be inserted into the torch holder to loosen or remove the injector seal nut
(Part No. N0776036) 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 seal nut to make it easier to slide the injector out. See the following two
figures.
156
Maintenance
Note For a complete set of spare Injector Adapter O-rings order Kit (Part No.
N0770438).
3
4
157
Maintenance
1
2
3
10
9
8
5 6 7
4
11
12 15
16
14 17
13
18
19
158
Maintenance
Item Description
4 O-Rings (Part No. 09921028)
5 Injector Adapter (Part No. N0776024)
6 O-Rings (Part No. 09902207)
7 Washer (Part No. N0770602)
8 Locking Collar (Part No. N0776025)
9 Injector Lock
10 Knurled Nut
11 Use this end to remove O-Rings
12 Injector Positioning tool (Part No. N0770602)
13 Torch
14 Injector (1 1/2 mm set below the inner glass)
15 Injector Positioning tool (Part No. N0770602)
16 Injector Seal Nut (Part No. N0776014)
17 Use this end to remove Injector Seal Nut
18 Injector Seal-open side up (Part No. 09923509)
19 Washer (Part No. N0776014)
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.
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.
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Maintenance
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.
160
Maintenance
3 6 7 10
5 8
4 9
161
Maintenance
Item Description
6 Locking Lug
7-9 Channels
10 Torch Mount
4. Carefully slide the torch through the plasma induction plates. 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.
162
Maintenance
3
5
6 2
5. Check that the injector is flush or slightly below the inner glass tube of the torch.
If the injector tube is not seated properly an air leak could occur or sample could
drip into the torch.
163
Maintenance
2. Check the condition of the two O-rings (Part No. 09921028) 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 the end of the nebulizer (NEB) argon tubing to the nebulizer end cap
and the other end to the quick disconnect by pushing the male quick connect
fitting into 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.
164
Maintenance
1
2
6 8
Figure 5-10 Nebulizer (NEB) connections to torch and nebulizer end cap.
Item Description
1 Nebulizer (NEB) Argon Tubing
2 Quick Disconnect Detail
3 Instrument Left Side
165
Maintenance
Item Description
4 Quick Disconnect
5 Nebulizer (NEB) Argon Tubing
6 Drain Tubing
7 Waste Vessel
8 Sample Capillary Tubing
Regularly inspect the plasma induction plates. It should not show any signs of
deforming or pitting.
If your lab has high humidity, check the plasma induction plates to make sure it is
dry. Use a soft dry cloth to dry the plasma induction plates if necessary. Contact your
Perkin Elmer Service Representative to replace and adjust the plasma induction
plates.
166
Maintenance
167
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 procedures.
Warning
Gradually, deposits may accumulate on the windows, for example, metallic oxides,
and the windows may become etched. You must remove the windows to clean or
replace them.
If you notice a drop in UV performance the purge windows may needed to be cleaned
or replaced even if the windows still look clear. Clean the windows first, if the UV
performance does not improve replace the windows.
The axial window mount is also the purge outlet for the spectrometer. The radial
window is a cylinder with one closed end; this end being the actual window.
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 Removing and Disassembling the Torch on page
150.
168
Maintenance
2. Remove the two screws that hold the shear gas nozzle assembly in
position and move the assembly carefully to one side. See the following
figure.
5
4
169
Maintenance
4. Remove the O-ring that holds the axial window in the mount and remove the
window.
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.
Note Do not rub the surfaces of the windows before you have cleaned them as
described below. The more you rub the surface of the windows, the more
chance there is of scratching them. You must discard scratched windows.
Allow to dry completely before reinstalling. If there is any moisture on the
inside of the window it can degrade the UV performance and/or damage
the optics.
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.
170
Maintenance
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.
171
Maintenance
Note Do not leave fingermarks on the window. Use an optical cloth to handle
the window.
1. Hold the axial window with an optical-quality cloth and refit the window in the
mount.
4. Screw the axial window mount onto the axial snout — handtighten firmly, do not
overtighten.
172
Maintenance
3
6
4
5
7
173
Maintenance
Caution Risk of heat damage to the axial window. Never set the nozzle slit behind
the front edge of the axial window mount.
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 Pozi Drive
Head 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 on page 154
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.
174
Maintenance
Caution Risk of heat damage to the axial window. Never set the nozzle slit behind
the front edge of the axial window mount.
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 Pozi Drive Head screws that hold the shear gas nozzle assembly
in position.
2. Slide the assembly to the position you require, then tighten the screws.
175
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.
176
Maintenance
3
4
5
1
Figure 5-14 Spray chamber, end cap, and associated parts. (Illustration shows
cross-flow nebulizer end cap assembly, Part No. N0770546.)
Item Description
1 Spray Chamber (Part No. N0770357)
2 O-Ring (Part No. 09902033)
3 End Cap Ring (Part No. 00473543)
4 End Cap (Part No. N0681688 not complete assembly)
5 Knurled Screw (2) (Part No. 00473539)
177
Maintenance
if necessary. Acid solutions must be used with care. Observe all of the
manufacturer's safety recommendations. These recommendations are normally
provided in a material safety data sheet (MSDS) supplied with the chemical.
If you have been analyzing organic solutions, the spray chamber can be cleaned
using a solvent or diluted soap solution. Be sure to inspect the torch and injector daily
for carbon buildup.
O-rings may be cleaned with soap and water. An ultrasonic bath may be used.
Replace if cracked or worn. A torch O-ring kit is available. See the list of
replacement parts at the end of this chapter.
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. N0776053) for aqueous solutions that cause
the plasma to become unstable or extinguishes frequently. You can use a cyclonic
spray chamber without a baffle (Part No. N0776052) for aqueous solutions analysis.
Lastly you can use a narrow baffled (4mm) cyclonic spray chamber (Part No.
N0776090) for organics.
178
Maintenance
Note The large baffled (8 mm) and unbaffled cyclonic spray chamber can be
ordered with or without a cap. The narrow baffled (4 mm) cyclonic spray
chamber assembly (Part No. N0776090) does not come with a cap. You
must order this cap separately as needed. A cap (Part No. N0770614) does
not have to be ordered with every replacement cyclonic spray chamber.
Caps can be reused for either the baffled or unbaffled cyclonic spray
chambers.
See Table 4-3 on page 127 in the Installation chapter or Table 5-4 on page 184 and
Table 5-13 on page 232 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.
179
Maintenance
Figure 5-15 Installing the cyclonic spray chamber into the cyclonic spray chamber
cap.
Item Description
1 Cyclonic Spray Chamber
180
Maintenance
Item Description
2 Cyclonic Spray Chamber Cap (opened position)
3 Cyclonic Spray Chamber (seated in cap)
4 Cyclonic Spray Chamber Cap (closed position)
3. Slide the chamber onto 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
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.
02506516). To the other end of the Tygon tubing attach the tubing coupler (Part
No. 09920186). See the following figure.
181
Maintenance
4
3
182
Maintenance
5. To the open end of the tubing coupler (Part No. 09920186) connect the drain
tubing to the peristaltic pump tubing. See the procedure Installing the Drain
Tubing on page 221 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 on page 204, 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.
4. At first, you will see beads of water inside the cyclonic spray chamber, then after
approximately 30 seconds, the beads will begin to disappear.
183
Maintenance
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.
184
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.
185
Maintenance
186
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.
187
Maintenance
When checking the spray pattern of the nebulizer pump only use
! deionized water. Do not use any other solution.
Warning
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
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.
188
Maintenance
1
2
Figure 5-17 The nebulizer/end cap assembly removed from the spray chamber. Il-
lustration shows cross-flow nebulizer end cap assembly.
Item Description
1 Cross-Flow GemTip Nebulizer End Cap Assembly (Part No.
N0770546)
2 Knurled Screw (Part No. 00473539)
3 Knurled Screw (Part No. 00473539)
4 Spray Chamber (Part No. N0770357)
4. To check the spray pattern, leave the sample capillary tubing and the nebulizer
argon tubing connected. Then refer to the next procedure.
189
Maintenance
When checking the spray pattern of the nebulizer pump only use
! deionized water. Do not use any other solution.
Warning
2. Place the sample capillary tubing in a beaker of deionized water and start the
pump at a rate of 1.0 mL/min.
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.
190
Maintenance
2
3
1
1. If you have not already done so, remove the nebulizer/end cap assembly from
the spray chamber.
191
Maintenance
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.
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. N0690676). They are not
available separately.
192
Maintenance
2
3
Figure 5-19 Clear GemTip for sample inlet and associated parts for Cross-Flow
End Cap, N0770546.
Item Description
1 O-Ring (Part No. 09921045)
2 Clear GemTip Nebulizer (Sample Inlet Available in GemTip
Kit Part No. N0690676)
3 Ferrule (Part No. 09920518)
193
Maintenance
Item Description
4 Nut (Part No. 09920546)
5 1/16 inch O.D. teflon Tubing Piece (Part No. 09985708)
6 Sample Capillary Tubing
5. Check the condition of the tubing piece (Part No. 09985708). If the tubing is
worn, replace it as follows:
• Obtain a new piece of 1/16-in. O.D. teflon tubing (Part No. 09985708).
• Using a razor blade, make a straight cut on one end of the tubing.
• Insert a nut (Part No. 09920546) and ferrule (Part No. 09920518) on the
newly cut end of the tubing with the ferrule oriented as shown in the figure
below.
1
2
3
Figure 5-20 Installing new tubing for the sample inlet. Cross-Flow End Cap,
N0770546.
Item Description
1 Ferrule (Part No. 09920515)
2 Nut (Part No. 09920545)
3 1/8 inch O.D. Tubing (Part No. 09985723)
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.
194
Maintenance
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. 09908265). Using a razor blade, bevel the tubing
by cutting it at an angle. Insert the sample capillary tubing into the tubing piece.
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. N0690676). They are not available
separately.
195
Maintenance
2
3
4
5
Figure 5-21 Red GemTip for argon inlet and associated parts for Cross-Flow End
Cap (Part No. N0770546).
Item Description
1 End Cap O-Ring (par No. 09902033)
2 O-Ring (Part No. 09921045)
3 Red GemTip Nebulizer -Argon Inlet (Part No. N0690676)
4 Ferrule (Part No. 09920515)
5 Nut (Part No. 09920545)
6 1/8 inch O.D. Tubing (Part No. 09985723)
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.
196
Maintenance
6. Check the condition of the argon inlet tubing (Part No. 09985723). 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. 09985723).
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. 09920545) and ferrule (Part No. 09920515) on the newly
cut end of the tubing, with the ferrule oriented as shown in the figure below.
1
2
3
Figure 5-22 Installing new tubing for the argon inlet. Cross-Flow End Cap,
N0770546.
Item Description
1 Ferrule (Part No. 09920515)
2 Nut (Part No. 09920545)
3 1/8 inch O.D. Tubing (Part No. 09985723)
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 .
197
Maintenance
2. Insert the ferrule with the tubing and nut to the Male Quick Disconnect (Part No.
N0775206). Connect the entire Quick Disconnect to the sample introduction
system. See the following 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. 09903128), rear ferrule, front ferrule, and
tubing insert onto the tubing as shown in the figure below.
4. Connect the nebulizer argon tubing to the NEB connection. Using a wrench,
tighten the 1/8-in. nut an additional 3/4 turn.
198
Maintenance
4
3 5
2
1
8 7
Figure 5-23 Connecting the nebulizer argon tubing. Cross-Flow End Cap (Part No.
N0770546).
Item Description
1 Instrument Left Side
2 1/8 inch O.D. Tubing (Part No. 09985723)
3 Nut (Part No. 09920545)
199
Maintenance
Item Description
4 Ferrule (Part No. 09920515)
5 Quick Disconnect-Male (Part No. N0775206)
6 Quick Disconnect-Female (Part No. N09920861)
7 Nut (Part No. 09920545)
8 Ferrule (Part No. 09920515)
• Check the end cap O-ring (Part No. 09902033) 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 on page 189.
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.
200
Maintenance
GemCone Nebulizer
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.
201
Maintenance
1. Remove the existing nebulizer/end cap assembly (if the wrong one is installed)
by loosening the knurled nuts 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. N0680504) to the spray chamber with a
twisting action.Alternately hand-tighten the knurled screws until the end cap
ring is pulled snugly against the end cap.
3. Before inserting the GemCone nebulizer into the cap, connect the argon gas
fitting to the threads on the nebulizer where shown in the next figure. First,
tighten the gas fitting by hand. Tighten the fitting another 1/8 of a turn using a 9/
16-in. open-end wrench. Support the nebulizer with a back-up wrench when
tightening or loosening fittings. Do not overtighten the fitting as this may cause
leaking and poor ICP performance.
4. Connect the capillary tubing to the nebulizer. Be sure not to crimp or bend the
tubing as you insert it. Crimps may reduce flow to the tip of the nebulizer or may
cause air to enter the liquid stream during operation.
5. Insert the nebulizer as far as it will go through the opening in the end cap.
202
Maintenance
4
1
3
2
5
203
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.
204
Maintenance
6
1
5 2
3
4
Figure 5-25 Connecting the GemCone nebulizer to the cyclonic spray chamber.
Item Description
1 Torch Coupler
2 Cyclonic Spray Chamber
3 Tubing Assembly for the GemCone Nebulizer (Part No.
0770336)
4 Argon Gas Fitting
5 GemCone Nebulizer Assembly
6 Teflon Tubing-1 inch (Part No. 09985708)
7 Capillary Tubing (Part No. 09908265)
205
Maintenance
1. Remove the nebulizer from the end cap (loosen both thumbscrews).
2. Disconnect the argon gas fitting and the capillary tube connection from the
nebulizer.
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.
206
Maintenance
1. Wet the outside of a short length of tubing cut from pump tubing (Part No.
00473550 or 09908587). 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. 09908265) inside this short piece of peristaltic pump tubing.
3. Connect the supplied Tygon tubing (Part No. 02506515) 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.
1 2
3
207
Maintenance
Item Description
4 2.54 cm or 1 inch
5 Clamp
6 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.
208
Maintenance
Figure 5-27 Installation of the Concentric Glass Nebulizer in the End Cap.
Item Description
1 End Cap (Part No. N0680504)
2 Meinhard Concentric Nebulizer
209
Maintenance
(714) 250-3332
Internet address: http://www.meinhard.com
The following table summarizes the cleaning procedures for the MEINHARD
Concentric Glass nebulizer.
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.
210
Maintenance
Mira Mist nebulizers will pulse if the pump can not deliver
constant sample flow: Change your pump tubing often, or use a
surgeless pump if possible.
Caution The gas orifice is at the very tip of the nebulizer. It is made of Teflon which
is VERY SOFT. This tip is very easily damaged and should NEVER be
touched with fingers, tissues, or anything else. If the tip is accidentally
touched, and the nebulizer continues to operate, then it is still functional,
and its use can be safely continued.
Note The PEEK Mira Mist body has 10/32 threads for the gas and capillary
fittings. Gently tighten until snug for the sample line. For the gas line, if
there seems to be any leakage, then tighten HARD. PEEK is very strong.
The Mira Mist Nebulizer body is PEEK, the inner capillaries are Teflon. Generally
it will not break. If it is dropped such that the tip is deformed, then it will be
211
Maintenance
irreparably damaged. If it continues to operate after being dropped, then it has not
been affected, and its use can be safely continued.
Gas Line
The gas line is attached with UpChurch® 10/32 chromatographic fittings. We supply
2 mm OD X 0.039 ID Teflon tubing. A gas line filter is NOT included in the
nebulizer. Any particles from the gas line will destroy the nebulizer. We have found
this is one of the main causes of blockage of our nebulizers, so please ensure that the
gas line to the nebulizer is clean of any particles.
The gas line terminates in the Optima 8000 quick disconnect. It is a direct
replacement for typical concentric nebulizers.
Caution The gas orifice is at the very tip of the nebulizer. It is made of Teflon which
is VERY SOFT. This tip is very easily damaged and should NEVER be
touched with fingers, tissues, or anything else. If the tip is accidentally
touched, and the nebulizer continues to operate, then it is still functional,
and its use can be safely continued
For the longest life and best performance, wash your nebulizer by simply running
water as a sample for 10 minutes at the end of the day before shutting down the
plasma. Any other form of washing is usually unnecessary. DO NOT wash your
nebulizer in acid or solvents to "prevent salt build up". DO NOT use surfactants as
they will destroy the surface tension at the tip and performance.
212
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.
213
Maintenance
Figure 5-29 Tubing installed on pump for sample and drain (side view).
Item Description
1 From Spray Chamber
2 To Nebulizer
3 To Drain Bottle
4 From Sample Container
214
Maintenance
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.
215
Maintenance
216
Maintenance
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.
09908265), one for the sample capillary and one for the nebulizer capillary.
Using a razor blade, bevel one end of each piece of capillary tubing by cutting it
at an angle. See the next figure.
5. Insert the beveled end of the sample capillary tubing into one end of the pump
tubing. Lead the capillary tubing to the sample bottle.
4
2
217
Maintenance
Item Description
3 Pump Tubing 0.76 mm i.d. (different part numbers available)
4 Polyethylene tubing (including with the Nebulizer, 0.58 mm
i.d. Part No. 09908265)
5 To Sample Inlet
6. Insert the beveled end of the nebulizer capillary tubing into the other end of the
pump tubing.
To connect the drain tubing assembly, use the following steps and refer to the next
figure.
1. Connect the sleeve (Part No. N0695415) and adapter (Part No. N0695414) to the
spray chamber drain. Thread the barbed fitting (Part No. 09920267) into the
coupler and adapter.
2. Attach the Solvent Flex (PVC) tubing (Part No. 09985735) to the barbed fitting.
Attach the other end of the Solvent Flex (PVC) tubing to the tubing coupler (Part
No. 09920186).
218
Maintenance
3. Use the other end of the tubing coupler (Part No. 09920186) 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. 09985729)
to the barbed fitting (Part No. 09920267).
2. Cut the 1 mm i.d. tubing at an angle and insert it into the 1.5 mm tubing.
219
Maintenance
5 6
2
7
8
220
Maintenance
Item Description
5 PVC Tubing 1.5 mm i.d. (Part No. 09985735)
6 Coupler (Part No. 09920186)
7 Pump Tube 1.14 mm i.d.
8 Teflon Tubing 1 mm i.d. (Part No. 09985708)
9 Drain bottle
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. 09985708). 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 5-33.
221
Maintenance
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).
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.
222
Maintenance
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. A
replacement stainless-steel pump head is available (Part No. N0690360).
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.
223
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 8000. 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.
224
Maintenance
2 1
3 4
5 6
225
Maintenance
Item Description
5 Drain Tubing Piece 1.6 mm i.d. (Part No. 02506241)
6 Teflon Tubing 1 mm i.d. (Part No. 09985708)
7 Pump Tubing 1.14 mm i.d.
8 Peristaltic Pump
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 5-34. 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 RF generator air filters (Part No. N0775220) are included in the spares
kit.
226
Maintenance
3. Remove the filter and insert a new one (Part No. 09995098).
3 4
Figure 5-34 Location of the air filters on the back of the instrument.
Item Description
1 Access Panel for Neon Lamps
2 Spectrometer Air Filters (Part No. 09995098)
3 RF Generator Filter (Part No. N0775220)
4 To remove, slide filter in this direction.
227
Maintenance
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. B0810144) onto the tub
using the metal plates on the tub as guides. Tighten the large screw securely.
Fill the chiller reservoir with the coolant fluid (Part No. N0776099). The chiller
reservoir has a capacity of 7 liters (2 US gallons). Refer to Connecting the
PolyScience Chiller on page 97 for more information on filling the chiller.
Caution Do not use deionized or tap water in the chiller. Only use the coolant
fluid (Part No. N0776099) recommended above.
228
Maintenance
Fuses
Fuses may only be replaced by a PerkinElmer service engineer.
229
Maintenance
Every day you count on PerkinElmer to provide you with solutions that deliver
reliable performance, control operating costs and maximize operational time. Our
complete portfolio of consumables, parts, supplies, training and service helps you
meet both routine and demanding measurement challenges. We invest heavily in
testing and validating our products to ensure you receive guaranteed compatibility
and performance - on-time, every time, for every instrument in your laboratory.
The following replacement parts are required for general system maintenance. For
other replacement parts, refer to the appropriate sections earlier in this chapter.
230
Maintenance
231
Maintenance
232
Maintenance
09401056 PCB-PCI/GPIB
233
Maintenance
234
Maintenance
09923037 Solvent Flex Pump Tubing, 1.14mm ID, Red/Red (Drain Tub-
ing)
235
Maintenance
236
Maintenance
N0770434 Fresh Air Inlet Kit (which includes the Flex Hose and Hose
Clamp)
237
Maintenance
N0770614 Cap for either the Baffled or Unbaffled Cyclonic Spray Cham-
ber
238
Maintenance
239
Maintenance
N0776090 Narrow Baffled (4mm baffle) Cyclonic Spray Chamber for Oil
or Organics Analysis
240
Maintenance
241
Maintenance
242
Troubleshooting 6
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 on the WinLab
CD or Performance Problems:
Troubleshooting Table in this chapter.
You cannot ignite the plasma, or Plasma Ignition and
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 on the WinLab CD.
or the system is not ready.
There is a software error. Software Troubleshooting in the Winlab32
Software Guide on the WinLab CD.
The printer is not working. See Printing Problems on page 257
Problems in this chapter.
The pump is not working. Pump Problems on page 258 in this chapter.
245
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 on
the WinLab CD 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 on the WinLab CD for
details.
246
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 Quick-Change
Adjustable Torch Module on page 146.
247
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
on the WinLab CD 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 Replacement Parts:
General on page 230.
Refer to the adjustment procedure in Adjusting the Pump Tubing on page 222.
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
Removing the Pump Head on the Peristaltic Pump on page 224.
Capillary Tubing
Are the nebulizer and sample capillary tubing properly connected? Is the tubing
discolored or clogged? Is tubing crimped or pinched?
248
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 O
ring may need to be replaced. Check the drain fitting and tubing to be sure the spray
chamber is being properly drained. Check that the waste is being pumped in the
proper direction.
Check the nebulizer spray pattern: run deionized water for several minutes, then
remove the nebulizer end cap. Is the nebulizer spray sputtering or uneven?
If the spray pattern is uneven, the nebulizer tips may be clogged or worn.
Disassemble the nebulizer and clean or replace the GemTips. See GemTip Cross-
Flow Nebulizer on page 187.
Torch Assembly
Check for deposits, particularly if running organics, alloys, or samples with high
dissolved solids. See Cleaning the Torch on page 153.
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 Removing the Injector on page 148.
If the torch requires disassembly, check the O-rings. Are they cracked or worn? Is
the injector adapter discolored?
249
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.
250
Troubleshooting
251
Troubleshooting
252
Troubleshooting
253
Troubleshooting
254
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 plasma induction plates. Check the
plasma induction plates for condensation, particularly in labs with high
humidity. Dry the plasma induction plates 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 Removing the Injector on page 148.
In addition, try pumping solutions with the Nebulizer, Auxiliary, and Plasma gas
255
Troubleshooting
flows on for approximately two minutes. Then turn off the pump and try to
reignite the plasma again.
• Optics Interlock. Check that the optics is centered over the torch. Problems
with ignition may be due to the optics having been bumped out of the correct
position. If this has happened carefully move the optics to the correct position.
• Nebulizer End Cap and Fittings. Check that it is tightly secured to the spray
chamber.
• 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.
256
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
257
Troubleshooting
Pump Problems
258
Troubleshooting
Autosampler Problems
259
Troubleshooting
Fill out the following form before you contact PerkinElmer service.
Troubleshooting Form
General:
Instrument Serial Number:
Site:
Date:
260
Troubleshooting
Operating Conditions:
RF Power:W
Torch Position:mm
Instrument Environment:
Lab Temperature:C C
Line Voltage:V
Line FrequencyHz
261
Troubleshooting
Injector Dry:Yes/No
262
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 the
following figures.
263
Troubleshooting
Figure 6-3 Rounded Plasma due to sample or air getting around the outside (typ-
ically subtle air leak)
264
Troubleshooting
Figure 6-4 Aux Gas too high, Air Leak, or Spray Chamber Temperature too high
265
Troubleshooting
266
Error Messages 7
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.
269
Error Messages
270
Error Messages
271
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 5-10 on page 165. 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.
272
Error Messages
273
Error Messages
274
Error Messages
275
Error Messages
276
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.
277
Error Messages
278
Error Messages
279
Error Messages
69 Fiber Optic The firmware cannot Check that the fiber optics is in line with the
not detect the plasma plasma induction pl ates. If the problem
detecting after ignition. The persists contact 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.
280
Index
A coolant recommended 102
Acid Digestions 42 daily checks 140
Adjusting the Sampling Probe Height 119 electrical requirements 57
Air Filters filling 102, 103
general maintenance 226 filters 228
maintenance 226 requirements 54
periodic checks 143 starting 103
RF generator, changing 226 Coil, RF
spectrometer, changing 227 see RF Coil 142
Alignment Computer
torch viewing position 121 configuration and setup 92
Argon Connections
checking 255 cooling water 93
Argon Supply cooling water supplies 83
connecting, instructions 83, 95 electrical 83
daily checks 139 gases 83, 93
requirements 58 Cooling Water
Autosampler connections at back of instrument 94
connecting to computer 114, 115 remote chiller connectionsr 99
description 80 Cyclonic Spray Chamber
inserting sampling probe 118, 120 cleaning 184
installing 113 etching 183
setting up sampling probe 117 installing 178
troubleshooting problems with 259 maintenance 178
Axial Window D
replacing 172 Daily Cleaning 139
C Dark Current
Capillary Tubing measuring 82
inspecting 248 Detector 69
Chemical Reagents 39 Digestions
Chiller at elevated pressure 43
connecting 97 performing 43
connections at back of instrument 99
0993-6226 281
Index
282
Index
283
Index
284
Index
285
Index
286
Index
Torch Module
part numbers 166
Torch Viewing Position Alignment Procedure
121, 144
Transfer Optics 67
Troubleshooting
autosampler problems 259
general information 245
performance problems 248
performance problems, table 251
plasma ignition problems 255
plasma stability problems 255
printing problems 257
pump problems 258
U
Ultraviolet Radiation
safety practices 31
V
Viewing 121
W
Warnings
symbols used on instrument 15
Waste Disposal Procedures 34
Water Filter
general maintenance 228
Water Supply
replacement parts 230
Wavelength Correction 72
287
PerkinElmer, Inc.
710 Bridgeport Avenue
Shelton, CT 06484-4794, U.S.A.
Internet: http://www.perkinelmer.com
email: [email protected]