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PerkinElmer
710 Bridgeport Avenue
Shelton, CT 06484-4794
U.S.A.
Notices
The information contained in this document is subject to change without notice.
Except as specifically set forth in its terms and conditions of sale, PerkinElmer makes no warranty of any kind with
regard to this document, including, but not limited to, the implied warranties of merchantability and fitness for a partic-
ular purpose.
PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in connection with fur-
nishing, performance or use of this material.
Copyright Information
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All rights are reserved. No part of this publication may be reproduced in any form whatsoever or translated into any
language without the prior, written permission of PerkinElmer, Inc.
Trademarks
Registered names, trademarks, etc. used in this document, even when not specifically marked as such, are protected by
law.
Introduction
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.
Any of the following safety conventions can be used throughout this guide:
This symbol alerts you to the risk of electric shock that could result in personal
injury to yourself or other persons.
Details about these circumstances are in a box like this one.
xiv
This symbol alerts you to the risk of hot surfaces that could cause personal
injury to yourself or other persons.
Details about these circumstances are in a box like this one.
This symbol alerts you to the risk of ultraviolet radiation that could cause
eye damage to yourself or other persons.
Details about these circumstances are in a box like this one.
This symbol alerts you to the risk of strong magnetic fields that could cause
injury to persons wearing a heart pacemaker or having metallic implants.
Details about these circumstances are in a box like this one.
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.
All eight digit numbers are PerkinElmer part numbers unless stated otherwise.
Software Help
This manual contains hardware information for PinAAcle 900 Series instruments.
For information on the software for the PinAAcle 900 Series, see the following
help file.
This advice is intended to supplement, not supersede, the normal safety codes in
the user's country. It is also a supplement to the PerkinElmer standard Safety and
Health Policy. The information provided does not cover every safety procedure
that should be practiced. Ultimately, maintenance of a safe laboratory environment
is the responsibility of the analyst and the analyst's organization.
Please consult all manuals supplied with the PinAAcle Series and accessories
before you start working with the instrument. Carefully read the safety information
in this chapter and in the other manuals supplied. When setting up the instrument
or performing analyses or maintenance procedures, strictly follow the instructions
provided.
Precautions
The following precautions must be observed when using the PinAAcle Series:
• Be sure that the voltage of the PinAAcle Series corresponds to the voltage
used in your laboratory.
• Never remove the side panels of the PinAAcle Series without shutting
down the instrument and disconnecting the instrument power cord from
line power.
• Only high quality purge gases should be used with the PinAAcle Series.
Minimum purity of 99.9% is recommended. A high quality filter-dryer
Environmental Conditions 3
accessory is recommended for the removal of any moisture from the purge
gases.
• Before the instrument is installed, the area around, under and behind the
instrument's planned location is to be cleared of any dirt and dust to
prevent their entry into the instrument's interior which could cause a
negative effect on performance.
• When you remove the instrument from storage and before you put it into
operation, allow it to stand for at least a day under the approved operating
conditions.
Environmental Conditions
The instrument will operate correctly under the following conditions:
• Indoors.
You can store the instrument safely under the following conditions:
• Ambient temperature: -20 C to +60 C (-4 F to +140 F).
• Ambient relative humidity: 20% to 80%, without condensation.
• Altitude: in the range -400 m to 12 000 m (-1300 to 39 000 feet).
When you remove the instrument from storage and before you put it into operation,
allow it to stand for at least a day under the approved operating conditions.
Electrical Safety
The instrument has been designed to protect the operator from potential electrical
hazards. This section describes some recommended electrical safety practices.
Note Make sure that your laboratory has a matching receptacle for the IEC
60309 power plug.
The product is designed and manufactured, having regard to the state of the art, to
ensure that:
• the electromagnetic disturbance generated does not exceed the level above
which radio and telecommunications equipment or other equipment
cannot operate as intended;
Use of this product in residential areas may cause interference and such use should
be avoided unless special measures are taken by the user to restrict emissions to a
level that allows the reception of broadcast emissions.
• Connect the instrument to a correctly installed line power outlet that has a
protective conductor connection (earth ground).
• Do not operate the instrument with any covers or internal parts removed.
• Disconnect the instrument from all voltage sources before opening it for
any adjustment, replacement, maintenance, or repair. If afterwards, the
opened instrument must be operated for further adjustment, maintenance,
or repair, this must only be done by a PerkinElmer Service engineer or a
similarly trained and authorized person.
Fuses
Use only fuses with the required current rating and of the specified type for
replacement.
EMC Compliance
Europe
All information concerning EMC standards is in the Declaration of Conformity,
and these standards may change as the European Union adds new requirements.
This symbol indicates that there is a potential hazard and that the user must look
in the guide for an explanation of the hazard and how to avoid it.
This symbol indicates that there is a potential hazard due to a strong magnetic
field and that persons wearing heart pacemakers should remain at least 0.6 m
away from the furnace.
8 Safety Practices
This symbol indicates the off position of the main power switch or circuit
breaker. With the switch in this position, the instrument is disconnected entirely
from the line power supply.
This symbol indicates the on position of the main power switch or circuit breaker.
With the switch in this position, the instrument is connected to the line power
supply but is not necessarily switched on and operational.
1
3
Item Description
1 Warning-Hot Surface (the PinAAcle 900H)
10 Safety Practices
Item Description
1 Press button to unlock the lever
Warning Labels on the Instrument 11
1
2
Item Description
1 Warning-Hot Surface
2 Warning-UV Light Hazard. Avoid looking directly at flame
3 Warning-Not to open the door-Chemical Hazard
12 Safety Practices
4
1
2
3
Item Description
1 Warning-To reduce the chance of electric shock do not remove
covers that require tool access. No user serviceable parts are
inside. Refer servicing to qualified service personnel.
2 Warning-Ground circuit continuity is vital for safe operation of this
instrument. Grounding is accomplished by use of an IEC 60309
instrument power plug furnished by the factory. The plug is not to
be removed during or after installation.
3 Warning-For protection against fire hazard, replace with only same
type and rating of fuse.
4 Warning-Furnace gases minimum and maximum pressures.
Warning Labels on the Instrument 13
Item Description
1 Caution-Do not restrict air intake or exhaust
14 Safety Practices
Item Description
1 Caution-Do not restrict air intake or exhaust
Do not use an air filter. This is an air exhaust.
Some chemicals used with this PinAAcle 900 Series instrument may be
! hazardous or may become hazardous after completion of an analysis. The
responsible body (for example, the Lab Manager) must take the necessary
Warning precautions to insure that the instrument operators and the surrounding
workspace are not exposed to hazardous levels of toxic substances
(chemical and biological) as defined in the applicable Material Safety
Data Sheets (MSDS) or OSHA or ACGIH or COSHH documents.
Venting for fumes and disposal of waste must be accordance with all
national, state and local health and safety regulations and laws.
Responsible body Individual or group responsible for the use and maintenance of equipment, and
for ensuring that operators are adequately trained. [per IEC 61010-1].
Operator Person operating equipment for its intended purpose [per IEC 61010-1]
OSHA Occupational Safety and Health Administration (United States)
ACGIH American Conference of Governmental Industrial Hygienists
COSHH Control of Substances Hazardous to Health (United Kingdom)
Pollution Degree
This product will operate safely in environments that contain nonconductive
foreign matter up to Pollution Degree 2 in EN/IEC 61010-1.
Waste Disposal
If these materials are toxic, corrosive, or contain organics you may have to treat the
collected effluent as hazardous waste. Refer to your local safety regulations for
proper disposal procedures.
In addition, hollow cathode lamps and deuterium lamps are maintained under
reduced pressure. Handle and dispose of them correctly to minimize the implosion
risk.
For EDLs, the quantity of analyte material used is much less than the quantities
used in HCLs. Typically, only several milligrams of material are placed in the EDL
bulb. No PerkinElmer EDLs (System 1 or 2) contain more than 0.05 g of analyte
material.
18 Safety Practices
UV Radiation
You should be aware of the health hazard presented by UV radiation.
• When the instrument is on, do not remove any covers unless specifically
instructed to do so in the guide or you may be exposed to potentially hazardous
UV radiation.
• Always wear UV-absorbing eye protection when viewing any of these sources:
• The flame, especially the nitrous oxide/acetylene flame.
• The graphite furnace when it is heated to incandescence.
• Hollow cathode or electrodeless discharge lamps.
• The deuterium background correction lamp.
Magnetic Field
Warning - No Pacemakers
There is a potential hazard due to a strong magnetic field and persons
wearing heart pacemakers or other metallic implants should remain at
Warning least 0.6 m away from the furnace.
High Temperatures 19
High Temperatures
Burner System
The flame can generate temperatures of up to 2800 °C.
• Do not touch the burner head until it has cooled to room temperature.
Graphite Furnace
The THGA graphite furnace can generate temperatures of up to 2600 °C.
20 Safety Practices
• Do not attempt to inject a sample into the graphite tube when the furnace is hot.
You may be subjected to fumes from the sudden vaporization of the sample,
and may damage the pipette.
• Do not touch any part of the heating mantle (electrically heated systems), or
the cell holder (flame-heated systems), or the QTA-cell until they have cooled
to room temperature.
Note The responsible body must ensure that the type of connector used at the
outlet side of the gas-pressure regulator conforms to applicable national
requirements.
Note The responsible body is responsible for the correct collection and disposal
of waste materials. This includes the necessity for a suitably sized waste
container of appropriately resistant material for the collection of organic
solvent waste and provision for the removal into an appropriate exhaust
system of any gases or vapors which may be produced in hazardous
concentrations.
Note The responsible body must carry out appropriate leakage tests necessary
for safety on those gas and liquid connections which the operator is
directed to assemble during installation, normal use, or maintenance.
Handling Compressed Gases 21
Note The permanent installation of gas supplies is the responsibility of the user
and should conform to local safety and building regulations.
Spontaneous Decomposition
Gas Suffocation Explosion
or Combustion
Air - - -
Argon x - -
Nitrogen x - -
Acetylene (ethyne, C2H2) x x x
Contact the gas supplier for a material safety data sheet (MSDS) containing
detailed information on the potential hazards associated with the gas.
Identifying Cylinders
• Legibly mark cylinders to clearly identify the contents and status (full, empty,
etc.). Use the chemical name or commercially accepted name for the gas.
Combustion products may vary with the analysis of each sample. Acetylene (less
than 1 liter) is released during the bleeding of the gas box prior to shutdown. An
exhaust venting system is always required to remove those gases which are
generated during the normal operation of the instrument.
Contact the gas supplier for a material safety data sheet (MSDS)
containing detailed information on the potential hazards associated
! with the gas. Carefully use, store, and handle compressed gases in
cylinders. Gas cylinders can be hazardous if they are mishandled.
Warning
Note The permanent installation of gas supplies is the responsibility of the user
and should conform to local safety and building codes.
Listed below are some general safety practices for the proper identification,
storage, and handling of gas cylinders. Consult the following references for more
detailed information and additional guidelines.
Storing Cylinders
Review the following precautions with the customer to ensure the safe use and
storage of gas cylinders.
• Cylinders should be stored in accordance with the regulations and standards
applicable to the customers locality, state, and country.
• Flammable gases must be stored separately from the non-flammable gases and
oxidizing gases stored separately from the non-oxidizing gases.
• When cylinders are stored indoors in storage rooms, the storage room should
be well ventilated and dry. Ensure that the ventilation is adequate to prevent
the formation of dangerous accumulations of gas. This is particularly important
in small or confined areas.
• Do not store cylinders near elevators, gangways, or in locations where heavy
moving objects may strike or fall against them.
• Use and store cylinders away from exits and exit routes.
• Locate cylinders away from heat sources, including heat lamps. Compressed
gas cylinders should not be subjected to temperatures above 52 °C (126 °F).
• Do not allow ignition sources in the storage area and keep cylinders away from
readily ignitable substances such as gasoline or waste, or combustibles in bulk,
including oil.
• Store cylinders standing upright, fastened securely to an immovable bulkhead
or permanent wall.
• When storing cylinders outdoors, they should be stored above ground on a
suitable floor and protected against temperature extremes (including the direct
rays of the sun).
• Mark gas cylinders clearly to identify the contents and status (full, empty, etc.).
• Do not attempt to refill gas cylinders.
24 Safety Practices
Handling Cylinders
Review the following precautions to ensure the safe use and handling of gas
cylinders.
• If it becomes necessary to move cylinders, do so with a suitable hand truck
after insuring that the container cap is secured and the cylinder is properly
fastened to the hand truck.
• Use only regulators, tubing and hose connectors approved by an appropriate
regulatory agency.
• Arrange gas hoses where they will not be damaged or stepped on and where
objects will not be dropped on them.
• Do not refill cylinders.
• Check the condition of pipes, hoses and connectors regularly. Perform gas leak
tests at all joints and seals of the gas system regularly, using an approved gas
leak detection system.
• When the equipment is turned off, close all gas cylinder valves tightly at the
cylinder. Bleed the remainder of the line before turning the exhaust vent off.
Safety Interlocks
PerkinElmer provides a number of safety interlocks on the burner system to
monitor gas pressure and check for the proper setup of the burner head, nebulizer,
and drain system. In addition a flame sensor checks that the flame is burning.
• Do not attempt to defeat these interlocks; you may compromise your own,
or someone else's, safety.
• Regularly check for leaks at joints and seals using an approved leak test
solution.
• When you perform any maintenance or installation procedures, follow the
instructions in the guide exactly.
• Do not attempt to service the gas control system yourself. A PerkinElmer
service engineer, or similarly authorized and trained person, must perform
the work.
• When you shut down the instrument, for example at the end of the working
day, shut all the gas lines at the cylinder or regulator valves. Bleed the lines
between the regulator and instrument to atmosphere before switching off
the ventilation system.
Air Supply
An air compressor is recommended for the air supply to the burner system.
Cylinders of compressed air should only be used as an emergency or short-term
solution.
• If you use cylinder air, make sure that it is compressed air and not oxygen-
enriched air (e.g. breathing air); the use of oxygen-enriched air can cause
a flashback of the flame.
• Never use oxygen as the oxidant since this can cause an explosion.
Acetylene
• Always use “Atomic Absorption Grade” acetylene (ethyne) dissolved in
acetone (propane-2-one). This is satisfactory for all PerkinElmer AA
spectrometers.
• Do not store acetylene in close proximity to oxidizing gases, such as
nitrous oxide.
• Use approved tubing and fittings for acetylene. Never use copper fittings
since acetylene forms an explosive compound with copper.
• Prevent acetylene from coming into contact with copper, silver, mercury
or gaseous chlorine.
• Periodically check for the presence of acetylene in the laboratory
atmosphere, especially near the ceiling.
• For acetylene, set an outlet gauge pressure of between 90 kPa and 100 kPa
(0.9-1.0 bar, 13-14.5 psig). Never allow the outlet gauge pressure to
exceed 103 kPa (1.03 bar, 15 psig); acetylene can explode spontaneously
above this pressure.
• Solvent Carryover:
If the acetylene cylinder pressure falls to below 600 kPa / 6.0 bar / 87 psig
(at 20 °C), some of the solvent used to stabilize the acetylene (such as
acetone) may be carried over into the burner. This could influence the
characteristics of the burner with a resulting influence on the analytical
results.
Change to a new acetylene cylinder when the cylinder pressure falls to
below this value.
• Do not leave the flame unattended. Always make sure that there is a fire
extinguisher near the instrument.
• Never change the gas pressure or shut a gas valve while the flame is
burning.
• Do not allow the burner head slot to become blocked. This can cause a
flashback of the flame.
• Do not place open containers of flammable liquids and solvents near the
flame. Be especially careful with samples that contain highly volatile
solvents.
• When you have analyzed samples containing organic solvents, flush all
traces of solvent from the burner system.
Warning: Do not open the flame door during flame operation. When
the flame is ON, do not open or remove the burner door. The burner
! door is there to protect the operator from the hot flame and UV radiation
while running the flame atomization.
Warning
• Empty the drain vessel frequently; especially do not allow the drain vessel to
fill with organic solvent (Burner Drain Assembly for Organic Solutions Part
No. N3150232).
• Thoroughly flush the drain system, as described in the guide, when you shut
down the system.
• Check the condition of the drain tube regularly, especially if you use organic
solvents. Replace the drain tube when it first shows signs of cracking or
discoloration.
Flashbacks
A flashback is an explosion of the premixed gases in the spray chamber. The safety
interlocks normally prevent conditions that could cause a flashback, but if a
flashback should ever occur:
• Check that the burner head slot is clean.
• Make sure that you are using compressed air and not oxygen-enriched air.
• Check the flow spoiler or impact bead for damage, and replace any damaged
parts.
• Carefully check and tighten all connections to, and seals on, the burner unit,
and check the gas flow settings before you attempt to ignite the flame. Seepage
of fuel and oxidant from the spray chamber may cause a flashback.
• Check that the burner head is seated correctly.
High Temperatures
The flame can generate temperatures of up to 2800 °C.
Safety Practices for Electrothermal Atomization 29
• To avoid serious burns, never touch the burner head until it has cooled to room
temperature.
UV Radiation
The flame, especially the nitrous oxide/acetylene flame, emits ultraviolet radiation.
• Keep the atomizer compartment door closed when the flame is burning and
never directly view the flame unless you are wearing UV-absorbing glasses.
Acetylides
If you have aspirated high concentrations of copper, silver, or mercury solutions
into an acetylene flame, unstable acetylides may have formed in the spray chamber.
If permitted to dry, these compounds may explode.
• Aspirate solution continuously to prevent residues from drying.
• Thoroughly flush the spray chamber and drain system with water immediately
after such an analysis.
Cyanide Solutions
If you intend to aspirate cyanide solutions, make sure that the pH of the liquid in
the drain vessel is greater than pH 10; toxic hydrogen cyanide gas is formed when
cyanides contact acidic solutions.
Safety Interlocks
PerkinElmer provides a number of safety interlocks on the graphite furnace
(electrothermal atomization) system that monitor the gas pressure and the
temperature of certain system components.
• Do not attempt to defeat these interlocks; you may compromise your own, or
someone else's, safety.
30 Safety Practices
Inert Gas
The graphite furnace requires a supply of inert gas. PerkinElmer recommends
argon.
Although nitrogen can be used, it is not recommended for the inert gas supply. At
furnace temperatures above 2300 °C, nitrogen reacts with graphite to form toxic
cyanogen gas (CN)2.
Safety Checks
Before you start an analysis, make sure that:
• The laboratory fume ventilation system is operating;
• The inert gas supply is connected and set to the correct pressure;
• The cooling water supply is turned on;
• The autosampler waste bottle is empty.
Toxic Products
Toxic metal vapors, ozone, etc., can be generated by the system, depending on the
type of analyses being performed.
• You must provide an efficient laboratory ventilation system to remove toxic
products generated during instrument operation.
• If you use nitrogen as the inert gas, toxic cyanogen gas (CN)2 will be produced
when the furnace temperature is above 2300 °C.
High Temperatures
The THGA graphite furnace can generate temperatures of up to 2600 °C.
The HGA graphite furnace can generate temperatures of up to 2700 °C.
• To avoid serious burns, never touch the graphite components until the furnace
has cooled to room temperature.
Safety Practices for FIAS and Mercury Hydride Systems 31
• Do not attempt to inject a sample into the graphite tube when the furnace is hot.
You may be subjected to fumes from the sudden vaporization of the sample,
and may damage the pipette.
UV Radiation
The graphite furnace emits ultraviolet radiation when it is heated to incandescence.
• Never directly view the graphite furnace unless you are wearing UV-absorbing
glasses.
Safety Checks
Before you start an analysis, make sure that:
• The laboratory fume ventilation system is operating;
• The tubing in the fluid system is not constricted since this could lead to a
pressure build-up in the system;
• The drain tubing is inserted in the waste container and that this container
is empty.
• If you are using a flame to heat the QTA-cell or if you intend to perform
flame-FIAS analyses, refer to the information under Safety Practices for
Flame Atomization before you ignite the flame.
32 Safety Practices
Toxic Products
• Toxic metal vapors, etc., can be generated by the system, depending on the
type of analyses being performed.
• You must provide an efficient laboratory ventilation system to remove
toxic products generated during instrument operation.
High Temperatures
The QTA-cell used for the hydride-generation technique can reach temperatures of
up to 1000 C.
• Do not touch any part of the heating mantle (electrically heated systems),
or the cell holder (flame-heated systems), or the QTA-cell until they have
cooled to room temperature.
Hazardous Chemicals
Some of the chemicals required for analyses are corrosive and/or toxic.
Note The responsible body has the responsibility for usage of decontamination
or cleaning agents that could cause a hazard as a result of a reaction with
parts of the equipment or with materials contained in it.
Decontamination
Customers wishing to return instrumentation and/or associated materials to
PerkinElmer for repair, maintenance, warranty or trade-in purposes are
advised that all returned goods must be certified as clean and free from
contamination.
The customer's responsible body is required to follow the “Equipment
Decontamination Procedure” and complete the “Certificate of Decontamination”.
These documents are available on the PerkinElmer public website:
Procedure:
http://www.perkinelmer.com/Content/technicalinfo/dts_instrumentdeconprocedure.pdf
Certificate form:
http://www.perkinelmer.com/Content/technicalinfo/dts_perkinelmercertificationofdecontaminationform.pdf
If you do not have access to the internet and are located in the U.S., call toll free at
1-800-762-4000 or (+1) 203-925-4602, 8:30 a.m. - 7 p.m. EST and speak to
Customer Support.
In Canada, call toll free 800-561-4646 and speak to Customer Support.
If you are located outside of the United States or Canada, please call your local
PerkinElmer sales office for more information.
A label with a crossed-out wheeled bin symbol and a rectangular bar indicates that
the product is covered by the Waste Electrical and Electronic Equipment (WEEE)
Directive and is not to be disposed of as unsorted municipal waste. Any products
marked with this symbol must be collected separately, according to the regulatory
guidelines in your area.
The objectives of this program are to preserve, protect and improve the quality of
the environment, protect human health, and utilize natural resources prudently and
rationally. Specific treatment of WEEE is indispensable in order to avoid the
dispersion of pollutants into the recycled material or waste stream. Such treatment
is the most effective means of protecting the customer's environment.
Requirements for waste collection, reuse, recycling, and recovery programs vary
by regulatory authority at your location. Contact your local responsible body (e.g.,
your laboratory manager) or authorized representative for information regarding
applicable disposal regulations. Contact PerkinElmer at the web site listed below
for information specific to PerkinElmer products.
Web address:
http://www.perkinelmer.com/pages/010/onesource/environmental-health-and-
safety/environmental-directives-compliance.xhtml
For Customer Care telephone numbers select “Contact us” on the web page.
Products from other manufacturers may also form a part of your PerkinElmer
system. These other producers are directly responsible for the collection and
processing of their own waste products under the terms of the WEEE Directive.
Please contact these producers directly before discarding any of their products.
Consult the PerkinElmer web site (above) for producer names and web addresses.
References for Laboratory Safety Practice 35
• Hazards in the Chemical Laboratory, 5th edition, Luxon, S.G., ed., Royal
Society of Chemistry, London, UK, 1993.
• CRC Handbook of Laboratory Safety, 5th edition, Furr, K., ed., The Chemical
Rubber Co. Press, Florida, USA, 2000.
• Sax's Dangerous Properties of Industrial Materials, 11th edition, Sax, N.I. and
Lewis, R.J., eds., Wiley, New York, USA, 2004.
• Pohanish, R.P., HazMat Data, 2nd edition, Barnes & Noble, New York, USA,
2004.
Environmental Requirements
The location where the PinAAcle 900 Series is to be installed must fulfill the
criteria listed below:
• Indoors
• Free from vibrations
• Free from dust, smoke and corrosive fumes.
• Out of direct sunlight.
• Away from radiators and heaters.
• Have a suitable fume ventilation system.
• Room temperature between +15 °C to + 35 °C (59-95 °F), with a maximum
change rate of 3 °C (5.4 °F) per hour.
• Relative humidity between 20 and 80%, non-condensing.
38 Preparing Your Laboratory
At least 15 cm (6 in) free space must be available behind the instrument for
ventilation purposes and servicing. Do not block the fans operating on both sides
of the instrument.
Make sure that there is enough room on the work bench. The monitor can usually
be placed on top of the PC unit in order to save working space. Some clearance
between the instruments should be provided to ensure sufficient air circulation.
Weight
Instrument Width Depth Height
(Mass)
Fume Ventilation
For the high temperatures of the nitrous oxide-acetylene flame, the fume hood and
ducting should be made of stainless steel.
PerkinElmer offers an accessory, Blower and Vent Kit (Part No. 03030406), which
will fulfill the exhaust requirements for all AA instruments (see Figure 1). Included
in the kit are a rotary blower with capacitor and hardware, a vent to be located
above the instrument, and an adapter to permit connection of the blower
and vent with suitable metal tubing. The adapter and vent are made of stainless
steel sheets.
The metal tubing required to connect the vent to the blower and to provide suitable
exhaust from the blower is not included in the Blower and Vent Kit. Flexible
stainless steel tubing is recommended for this purpose and can be obtained from
the companies listed in the following table and from various other firms. In some
instances, this type of flexible metal tubing is sold only in minimum lengths of 3
meters (10 feet).
For the names of suppliers in other areas, contact your PerkinElmer representative.
The capacity of the blower depends on the duct length and the number of elbows
or bends used to install the system. If an excessively long duct system or a system
with many bends is used, a stronger blower may be necessary to provide sufficient
exhaust volume. Alternatively, smooth stainless steel tubing may be used instead
of flexible stainless steel tubing where flexibility is not required to reduce system
friction loss or "drag." A length of smooth stainless steel ducting has 20-30% less
friction loss than a comparable length of flexible ducting. When smooth stainless
steel tubing is used, elbows must be used to turn corners. These elbows should turn
at a center line radius of 45 degrees to reduce friction losses, and the number of
elbows should be minimized.
When installing a venting system, all connections should be made with metal
screws or rivets. Solder must not be used. The blower should be located at least 4
meters (12 feet) and not more than 6.5 meters (20 feet) from the flame or the
graphite furnace and should exhaust to the atmosphere or into a considerably wider
exhaust duct. Under these conditions, the following temperatures have been
measured during operation of a nitrous oxide-acetylene flame: 310 °C at the vent
intake; 160 °C at 2.4 meters (8 feet) from the vent intake; 105 °C at the blower
intake; and 50 °C at the blower motor housing near the front bearing. Instructions
Fume Ventilation 43
for installation (Part No. 09936775) are provided with the Blower and Vent
assembly. The blower provided in the
Item Description
G 10 cm (4 inches) in all cases
H 30 cm (12 inches) in all cases
J 15 cm (6 inches) in all cases
The magnetic field affects an area radius 0.6 m (24 in) around the graphite furnace.
The affected area extends all around the furnace, including above and below the
furnace. In addition to posting a health hazard for persons wearing heart
pacemakers, the magnetic field can also affect other instruments, watches and
magnetic storage devices (disks, credit cards, etc.).
Warning - No Pacemakers
There is a potential hazard due to a strong magnetic field and persons
wearing heart pacemakers or other metallic implants should remain at
Warning least 0.6 m away from the furnace.
Line Power Requirements 47
Power Consumption:
10100 VA for the PinAAcle 900T and the PinAAcle 900Z
The PinAAcle 900T and 900Z will ship standard an IEC 60309 32A power
connector.
The mains line house wiring must have a minimum wire cross section of 6 mm²
(8 gauge) or 10 mm² (6 gauge) for distances > 10 m.
The PinAAcle 900H will ship standard an IEC 60309 16/20 A power connector.
The mains line house wiring must have a minimum wire cross section of 4 mm²
(10 gauge) or 6 mm² (8 gauge) for distances > 10 m.
Line Power Requirements 49
Operating Range
90-253 VAC, 4A - 8A, 47 - 63 Hz
Operating voltage range must be maintained both at nominal and under load of
maximum power. For the PinAAcle 900H, PinAAcle 900T and the PinAAcle 900Z
it is recommended to install a Buck Boost transformer if the line drops below 208
volts at maximum power during atomization. If the line sags to 200 volts or lower,
excessive current draw will occur to provide the power needed, which will lead to
excessive heat dissipation. This excessive heat dissipation and current draw will
stress the furnace power supply, cause overheating failures, and shorten the life of
the supply.
Power that does not meet these minimum specifications will need the installation
of a Buck-Boost transformer, or a PowerVar Line Conditioner with built in boost
capabilities. Please refer to SDB # 4200041B.STS for more information on
whether the uses of a Buck-Boost transformer in necessary. If the voltage drops
below 195 VAC during atomization peak power, it is highly recommended that a
Buck-Boost or Line-Conditioner with boost be installed at Installation. Large
voltage drops (>16v) during atomization, or abnormally low nominal "no-load"
voltage (< 200 VAC) are an indication that the wiring requirements are not to our
required Preparing Your Laboratory or Site Readiness specifications.
Note The PinAAcle 900T and 900Z standard IEC 60309 should not be replaced
will an L6-30R twist lock plug, or any other Non-IEC 60309 type plug or
receptacle. The PinAAcle 900T and 900Z Series Instruments require the
IEC 60309 PLUG to prevent the inherent high leakage current from
shocking the user. Removing the IEC 60309 plug and replacing it with a
Non-IEC 60309 type plug violates all safety labels and approvals for the
PinAAcle.
Noise Specifications
The electrical noise levels of the incoming power to the customer's lab should be
checked to insure safe and reliable operation of our instrumentation and relative
electronics used for analysis. The electrical noise levels should be within the
following specifications:
Common Mode Noise: Neutral to ground noise should be 0.5 volts peak-to-
peak
Line Conditioners
PowerVar makes a series of line conditioner units that are suitable for all PinAAcle
900 Series model Instruments we sell. Line conditioner units are strongly
recommended where the customer's lab does not meet our minimum noise
specification requirements for both common and normal mode allowable line noise
levels. Please see the table below for the line conditioner models that are suitable
for each PinAAcle Instrument model we sell:
Line Power Requirements 51
Instrument
Instrument
Model Description Output Frequency Part No. Description Frequency Part No.
Voltage
PinAAcle 5.8 KVA Line 208/240 60 Hz N9307511 10 KVA 50/60 Hz N0777613
900T/Z Conditioner True On-Line
Power
Conditioned
UPS
PinAAcle 6.0 KVA Line 220 50 Hz N9307523 10 KVA 50/60 Hz N0777613
900T/Z Conditioner True On-Line
Power
Conditioned
UPS
PinAAcle 720 VA Line 120 60 Hz N9307515* 800 VA 60 Hz N0777681
900F Conditioner Power
Conditioned
UPS
PinAAcle 750 VA Line 220 50 Hz N9307521 800 VA 50 Hz N0777689
900F Conditioner Power
Conditioned
UPS
PinAAcle 3.8 KVA Line 120 60 Hz N9307512 5.2 KVA Line 50/60 Hz N0777511
900H Conditioner Conditioned
UPS
PinAAcle 3.8 KVA Line 220 50 Hz N9307522 5.2 KVA Line 50/60 Hz N0777511
900H Conditioner Conditioned
UPS
UPS Systems
The PowerVar 10.0 KVA On-Line Conditioned UPS 50/60Hz unit is currently
available for the THGA PinAAcle models (900T/Z). It meets the minimum surge
current handling rating of 90 A for about 3 seconds during Atomization stage peak
power. The PerkinElmer part number for the 10.0 KVA UPS is N0777613.
5.2 KVA Line Conditioned UPS 50/60Hz unit is currently available for the HGA
PinAAcle model 900H. The PerkinElmer part number for the 5.2 KVA UPS is
N0777511.
Power Outlets
In addition to the above, the following are required:
• For connection of the Cooling System, a 230 VAC socket is provided at
the rear of the PinAAcle Series 900 T/H/Z models.
• For the PC, monitor, printer, and addition accessories, e.g., FIAS or Auto
Prep 50, suitable outlets must be provided. Protecting earth and ground
must be the same as for the PinAAcle Series 900 T/H/Z models (avoid
ground loops).
Gas Requirements
Note Standards for cylinder dimensions, regulator connections, gas fittings, etc.
vary from country to country. The information provided here is for the
U.S. Contact your PerkinElmer representative for information on the
specific requirements of your area.
Gas Requirements 53
Note The permanent installation of gas supplies is the responsibility of the user
and should conform to local safety and building codes.
While the installation and operation of all gas supplies is the responsibility of the
user, the following safety information concerning the handling of gas cylinders is
included for your reference:
• Flammable gas cylinders (such as acetylene) should not be stored with
oxygen, or nitrous oxide cylinders, or adjacent to oxygen charging
facilities.
• Fasten all gas cylinders securely to an immovable bulkhead or a permanent
wall.
• When gas cylinders are stored in confined areas, such as a room,
ventilation should be adequate to prevent toxic or explosive
accumulations. Move or store gas cylinders only in a vertical position with
the valve cap in place.
• Locate gas cylinders away from heat or ignition sources, including heat
lamps. Cylinders have a pressure-relief device that will release the
contents of the cylinder if the temperature exceeds 52 °C (125 °F).
• When storing cylinders external to a building, the cylinders should be
stored so that they are protected against temperature extremes (including
the direct rays of the sun) and should be stored above ground on a suitable
floor.
• Mark gas cylinders clearly to identify the contents and status (full, empty,
etc.).
• Do not attempt to refill gas cylinders.
54 Preparing Your Laboratory
Gas Specifications
Air: Please refer to the Flame Gas Requirements below.
Gas Specifications:
Normal Gas
Usually argon is used to prevent the tube and the atoms from being oxidized when
the tubeis heated. If you cannot obtain argon, you can use nitrogen, but nitrogen
does not provide such efficient protection as argon at temperatures above 2000 °C.
Nitrogen may react with samples and the tube at typical atomization temperatures.
Special Gas
For some applications a special gas, for example, a gas mixture containing oxygen,
could be useful for the pre-treatment of organic samples.
Gas Specification
Air: Compressed air is required as oxidant for flame operation.
For flame operation, the air supply should provide a minimum of 28 liters/min (1
cubic foot/min) at a minimum pressure of 350 kPa (50 psig). The pneumatics of the
Flame Gas Requirements 57
PinAAcle 900H and PinAAcle 900T systems require a minimum air pressure of
350 kPa (50-58 psig).
It is desirable to have a water and oil trap or filter between the compressor and the
instrument gas control system. The use of an Air Filter Accessory (Part No.
00470652) or an Air/Acetylene Filter Accessory (Part No. N9301398) is strongly
recommended to remove entrained water, oil, water aerosols and solid particles
from compressed air lines.
If there is any doubt regarding the usability of a central air supply (insufficient
volume or pressure or excessive oil or water contamination), the quality of the
supply should be checked prior to the arrival of the instrument. A small, oil-less air
compressor meeting the stated requirements is available from PerkinElmer (Part
No. 03030313 for 115 volts, 60 Hz or Part No. 03030314 for 230 volts, 50 Hz
service).
Cylinders of compressed air can also be used but are recommended only as an
emergency or short-term solution for the following reasons:
• A standard #1 size air cylinder contains about 6200 liters (220 cubic feet)
of air at standard temperature and pressure (STP). A premix burner-
nebulizer system uses about 20 liters/min (0.7 cubic feet/min), and,
therefore, a cylinder will last only about five hours. Unless an instrument
is used only a few hours per day, changing cylinders becomes a nuisance
as well as being expensive.
• Occasionally, cylinder air may be obtained from a liquefaction process
during which the oxygen-to-nitrogen ratio can change. Therefore, it is not
uncommon to find other than 20% oxygen in air cylinders. This can cause
erratic burner operation and non-reproducible analytical results and, in
extreme cases, may provide a potential safety hazard. In general, if
58 Preparing Your Laboratory
The use of air cylinders requires the use of a suitable dual-stage regulator. A
regulator for cylinders with a CGA 590 connection is available from PerkinElmer
(Part No. 03030264)
Acetylene:
For the overwhelming majority of analyses, acetylene is the preferred fuel gas with
AA spectrometers. Air/acetylene is the preferred flame for the determination of
about 35 elements by AA. The temperature of the air/acetylene flame is
approximately 2300 °C. For most air/acetylene flames, the acetylene flow used is
about 4 liters/min or 0.14 cubic feet/min. Using a heat-combustion value of 1,450
BTU per cubic foot, the heat given off would be approximately 12,300 BTU per
hour (3,600 W). An air/acetylene flame can be used with all PerkinElmer burner
heads but is most commonly used with the supplied 10-cm (4-inch) burner head.
Suitable acetylene typically has a minimum purity specification of 99.6% with the
actual assay being about 99.8%. In general, ordinary welding-grade acetylene is
adequate for most AA analyses, though sometimes a particular tank may be
contaminated. Special higher purity "atomic absorption" grade acetylene is also
available from some vendors, and its use is recommended when the available
welding-grade acetylene is not sufficiently pure.
A size 1A acetylene cylinder contains about 8,500 liters (300 cubic feet) of
acetylene and usually lasts about 30 hours of burning time with an air/acetylene
flame. The cylinder requires an acetylene pressure regulator, which can be
obtained from the supplier of the gas or from PerkinElmer (Part No. 03030106).
Flame Gas Requirements 59
It may be desirable to have an acetylene filter between the acetylene tank and the
instrument gas control system to remove particulates and acetone droplets from
acetylene, protecting the gas controls and AA burner system from contamination
and corrosion. An Acetylene Filter (Part No. N9301398) and an Air/Acetylene
Filter Accessory (Part No. N9301398) are available from PerkinElmer. Some
countries also require the use of a flashback arrestor, such as PerkinElmer Part No.
N9307506 in the acetylene fuel line.
Caution Failure to change the acetylene cylinder before the cylinder pressure drops
below 600 kPa (85 psig) may cause damage to valves or tubing within the
burner gas control system due to high acetone carryover. Such damage
from acetone is not covered by instrument warranties.
60 Preparing Your Laboratory
Usually acetylene is dissolved in acetone, thus the tanks must be operated in the
upright position in order to prevent acetone from entering the tubing and hoses. At
low acetylene tank pressure the amount of acetone in the gas increases and may
produce an unstable flame. Therefore exchange the acetylene tank when the
cylinder pressure falls below 600 kPa (6 bar, 85 psig).
New tanks should be positioned vertically for at least 8 hours prior to use. The
practice of "cracking the valve" of an acetylene tank (that is, opening the valve
slightly fora very short period prior to attaching the regulator) is not recommended.
While such an action will clear the valve opening of dust or dirt particles and may
remove acetone from the cylinder valve, it is a potentially hazardous practice and
one which should never be attempted in the presence of an open flame, sparks or
other possible sources of ignition.
! Acetylene line pressure from the tank to the instrument should never
exceed 103 kPa (1.03 bar, 15 psig). At the higher pressures, acetylene
Warning can spontaneously decompose or explode.
Both fuel and oxidant gas lines should be relieved of pressure at the end of the
working day or if the instrument is to remain unused for an extended period.
Cylinder valves should be closed to avoid the possibility of pressure regulators
failing and gas lines being subjected to the full cylinder pressure.
Nitrous Oxide:
Caution All lines carrying nitrous oxide should be free of grease, oil or other
organic material, as it is possible for spontaneous combustion to occur.
Cylinders of nitrous oxide should be considered high-pressure cylinders
and should be handled with care at all times.
A dual-stage heated nitrous oxide pressure regulator for use with gas cylinders with
a CGA 326 connection is available from PerkinElmer [Part No. 03030204 (115
volts) or 03030349 (230 volts)]. These regulators provide pressure control from
350-520 kPa (50-75 psig) and contain an integral thermostatted heater to prevent
freezing of the regulator diaphragm. A color-coded hose with suitable connectors
at each end is supplied with the regulators to provide connection to the instrument
gas controls.
62 Preparing Your Laboratory
Argon:
Argon is required for external and internal gas streams through the THGA or HGA
graphite furnace or as a carrier gas with mercury/hydride systems such as the FIAS
or FIMS flow injections systems or the MHS-15. The quality criteria listed in the
following table for argon are suitable for these applications. Normally, for graphite
furnace operation, gaseous argon is used, although either liquid or gaseous argon
can be used. The choice of liquid argon or gaseous argon tanks is determined
primarily by the availability of each and the usage rate. Liquid argon is usually less
expensive per unit volume to purchase, but cannot be stored for extended periods.
If liquid argon is used, the tank should be fitted with an over-pressure regulator
which will vent the tank as necessary in order to keep the liquid argon cool enough
to remain in the liquid state. Gaseous argon tanks do not require venting and
consequently can be stored for extended periods without loss.
A dual-stage cylinder regulator that can be used with either gaseous argon or
nitrogen is available from PerkinElmer (Part No. 03030284). The regulator has a
CGA 580 fitting, and includes a color-coded hose with 1/4-inch Swagelok®
fittings to permit direct connection to the regulator and to the instrument gas
controls.
Hollow cathode lamps (HCLs) are excellent for most elements; however, there are
a number of "difficult" elements for which an improved light source is desirable.
PerkinElmer electrodeless discharge lamps (EDLs) provide improved performance
in most instances. EDLs are more intense than their corresponding HCLs. Most
also provide better lamp life and stability as well as better sensitivity. EDLs do not
require a separate power supply as it is built-in the PinAAcle systems.
A lamp mount or turret is supplied with all PerkinElmer AA instruments and will
accommodate all PerkinElmer HCLs or EDLs. Users who may have lamps with
1.5-inch diameters rather than the standard PerkinElmer 2-inch diameter can adapt
those lamps for use in PerkinElmer lamp mounts with the Small Diameter Lamp
Adapter Kit, (Part No. 03030870).
Hollow Cathode Lamps (HCLs). The PerkinElmer Atomax 1.5 inch lamps do not
require an adapter. The use of other 1.5 inch HCLs you will need an adaptor kit to
connect in the lamp compartment area. PerkinElmer Coded Electrodeless
Discharge Lamps (EDL s) can also be used.
Drain Vessels
A specially-configured drain vessel is supplied with all PerkinElmer AA
instruments with burner systems. That vessel must be used to gather the effluent
from the AA burner drain.
The drain vessel should NOT be stored in an enclosed storage area. Rather, the
drain vessel should be stored in plain sight of the operator, usually on the floor in
front of the instrument or on an open shelf underneath the instrument table.
The drain system should be checked regularly and replaced when necessary.
Follow the directions in the instrument manuals regarding the proper placement of
the drain tube in the drain vessel and the proper liquid level in the drain vessel.
Cooling Requirements 65
Cooling Requirements
Furnace Cooling
The graphite furnace uses water cooling to allow the graphite tube to return to its
equilibrium temperature (approximately ambient) quickly between measurements.
Cooling System
A water recirculating system and a cooling water system are offered as options for
the PinAAcle 900H, PinAAcle 900T and PinAAcle 900Z systems. These water
systems provide coolant at a constant temperature and flow to allow the most
reproducible analytical conditions. They also makes the system independent of
external water supplies and saves water.
External Cooling
If you intend to run the spectrometer system without the PerkinElmer cooling
system, you must connect another suitable source of cooling. The main water
system supply to the lab can be used if it meets the specifications defined in the
charts below. Laboratory water cooling systems can also be used if they meet our
specifications of the recirculating system we offer.
66 Preparing Your Laboratory
If the water is too cold or flowing too fast, moisture may condense on the
Caution graphite contacts, on the furnace windows or inside the water cooled
furnace power supply resulting in malfunction and severe damage.
Moisture on the contacts causes rapid attrition of the graphite surface,
while moisture on the furnace windows leads to attenuation of the energy.
Installation Preparation
• The PC, printer and all other accessories should not be unpacked but be
available in their boxes at the installation location.
• If the PC is going to be networked, the customer should have an IT Specialist
available during the installation.
PC Skills
• The customer should have a basic working knowledge of Windows and how to
operate WinLab32 for AA.
The customer should have a fundamental knowledge of atomic absorption
spectroscopy.
68 Preparing Your Laboratory
System Description 3
The PinAAcle 900 Series Spectrometer System
Concept
The PinAAcle 900 series spectrometer from PerkinElmer is a compact, high
performance atomic absorption spectrometer incorporating a burner system for
flame atomization and a graphite furnace for electrothermal atomization. The
spectrometer is capable of fully automatic single-element analyses. The complete
system is operated from the associated computer using the Winlab32 for AA
software.
• The PinAAcle models H and T has a stacked design with the graphite furnace
located on the bottom of the stack.
• Intuitive, easy-to-use WinLab32 for AA software with which you control the
spectrometer system. WinLab32 for AA also incorporates a range of powerful
quality control functions.
System Components
The PinAAcle 900 is a compact bench top spectrometer. The major components of
the system are:
• The spectrometer, containing the optical system, the electronics, and the
atomizer compartment.
• The burner system can be driven into and out of the atomizer compartment by
software command.
System Control
To control the spectrometer and perform your analyses, you use the WinLab32 for
AA application program, which runs under the Microsoft Windows operating
system. The computer keyboard, the screen, and the mouse form the user interface.
72 System Description
You can obtain more information about the application program in the WinLab32
for AA online help.
Accessories
PerkinElmer offers autosamplers for operation with the burner system, flow
injection systems, autoprep, and much more. Please contact your local
PerkinElmer office to obtain detailed information.
Four different types of instruments are available, PinAAcle 900F, 900H, 900T and
900Z. But two parts of the optical layout are common to all versions, the lamp
compartment and the monochromator:
The lamp compartment has positions for up to eight spectral sources, HCL and/or
EDL lamps. The radiation from the requested source lamp is collected by a
movable mirror and coupled into the source fiber.
At the other end of the optical path the fiber bundle coming from the sample
compartment is coupled onto the Litttrow-configuration monochromator. This
contains of a parabolic mirror and a large area reflecting grating blazed at two
wavelengths; 236 nm for operation in the UV spectral range and 597 nm for
operation in the visible spectral range. Various slit widths are available to adjust
the signal throughput and resolution to the requirements of each measurement.
The PinAAcle 900 Series Spectrometer System 73
The PinAAcle 900T and PinAAcle 900H can both be used for flame and furnace
atomization. They use a double-beam configuration as depicted in the following
schematics beginning on page 74. In addition to the HCL and EDL source lamps
both models are equipped with a deuterium lamp for background correction. The
light from the source and the deuterium lamps are guided to a fiber coupler, which
splits the light into separate sample and reference beams. Thus each channel,
sample and reference, contains a certain percentage of the source and deuterium
lamp. Both beams pass through the sample compartment before they are coupled
into another pair of fibers by a set of ellipsoidal mirrors and guided to the
monochromator and detector.
The deuterium and source light is split into two beams---one that passes through
the upper part of the sample compartment, and one that passes through the lower
part of the sample compartment. In the flame mode, the upper beam is the the
"sample" beam and the lower beam (which passes through the graphite furnace) is
the "reference" beam. In the furnace mode, only the lower beam (that passes
through the graphite furnace) is used..
The main difference between the PinAAcle 900T and 900H lies in the type of
furnace atomizer. The PinAAcle 900H uses a HGA atomizer. The PinAAcle 900T
is equipped with a THGA atomizer using Zeeman background correction.
The PinAAcle 900F flame system is similar to the 900T model as it uses a double-
beam configuration and a deuterium lamp for background correction. However
instead of passing through the sample compartment, the reference beam is directly
guided from the fiber coupler to the monochromator.
The PinAAcle 900Z is a Zeeman-THGA furnace only system and uses a single
fiber to transmit the source light to graphite furnace and then to the monochromator
and detector.
74 System Description
Spectrometer
You normally switch the system on and off with the operational on/off switch on
the front panel of the spectrometer.
The Electrical Connectors and Switches 79
Cooling System
The cooling system requires a 230 V line power supply, which is supplied and
controlled from the spectrometer. A special line power cord is provided for this
purpose. Do not connect the cooling system to an external power source.
You can leave the on/off switch on the cooling system in the "on'" position since
the system is controlled from the spectrometer.
80 System Description
1
3 4
8
2 6
5
Figure 3-6. Gas, cooling and electrical connectors on the rear panel
Item Description
1 Power circuit breaker 5 230 v power receptacle
2 Main power cord 6 Water hose in
3 Argon (or Nitrogen) gas line 7 Water hose out
4 Special gas line 8 Purge gas connection
The Gas and Cooling Connectors 81
Furnace Cooling
Furnace Gases
3 Ar/N2 Connector for the connection of the normal gas supply to the
Normal furnace (argon or nitrogen).
4 Special Gas Connector for the connection of the special gas supply to the
furnace. If you are not using a special gas, you must also
connect the normal gas to this connector.
Burner Gases
6 N2O Fitting for connection of the nitrous oxide supply to the burner.
• Nebulizer
• Burner chamber
• End cap
• Burner head
• Drain system
2 1
3
5
4
A sample solution is aspirated through the nebulizer and sprayed as a fine aerosol
mist into the burner chamber. Here, the sample mist is thoroughly mixed with the
fuel and either air or nitrous oxide gases. Fuel gas enters the chamber through the
fuel inlet hose while the oxidant enters through the inlet built into the burner
chamber body.
Once the sample aerosol is thoroughly mixed in the chamber, it then advances to
the burner head where atomization occurs.
The gas control system monitors and controls fuel and oxidant flows. Burner
operation, including flame ignition, flame shutoff and gas flow settings, is
controlled through the Winlab32 for AA software.
The next figure shows a "block diagram" of how the burner system flows, from the
gas supplies, to the gas box, to the burner hardware itself and out to the drain vessel.
Burner Assembly System 85
• N3161040: burner head adjustment tool. Insert the adjustment tool into the
burner head and adjust the angle to extend the linear range. This tool
allows you to do adjustments while the burner is hot.
Burner Assembly System 87
2 3
1 4
5
6
Figure 3-9. The four burner heads available and adjustment tool.
Item Description Part Number
1 5-cm, single-slot burner head (for N0400100
Nitrous oxide-acetylene flame)
2 5-cm, single-slot burner head (for N0400101
air-acetylene flame)
3 10-cm, single-slot burner head N0400102
4 10-cm, three-slot burner head N0400103
5 Burner head adjustment tool N3161040
6 Burner head adjustment hole for -
adjustment tool
activated (automatically), the glow plug is energized and heats up. The ignitor
solenoid, which is also energized, swings the ignitor arm into place. The ignitor
arm is a gas-capture tube through which the gases flow from the burner to the glow
plug. The gases in the tube are ignited by the heat of the glow plug, which, in turn,
ignite the flame at the burner head slot.
The burner will be shut down in a safe sequence in the event of a power failure.
The siphon interlock drain trap is integral with the burner end cap and includes an
internal trap to make certain that back pressure is applied to the burner chamber.
This ensures that a fuel/oxidant mixture cannot enter the drain vessel. There is a
magnetic float in the drain trap that shuts down the flame if the drain system is not
functioning properly. If the liquid level in the trap is too low, the switch is activated
and the flame is shut down.
Burner Assembly System 89
Burner Installation
The burner is shipped in place so it does not need to be installed in the instrument.
for information on burner installation after maintenance procedures refer to
Chapter 6, Maintenance, in this hardware guide. See Chapter 4, Installation, in this
hardware guide, for information on connecting the burner gases.
Specifications
System Design:
Instrument Description
PinAAcle 900T and PinAAcle 900T and PinAAcle 900H are fully-integrated bench
PinAAcle 900H: top design atomic absorption spectrometers, incorporating all
spectrometer, flame atomizer and graphite furnace atomizer
components in a single instrument.
PinAAcle 900Z: PinAAcle 900Z is fully-integrated bench top design atomic
absorption spectrometer that incorporates a single-beam
spectrometer system and graphite furnace atomizer in a single
instrument.
PinAAcle 900F: PinAAcle 900F is a fully-integrated bench top design atomic
absorption spectrometers, incorporating the spectrometer, and
flame components in a single instrument.
Optical System Photometer: Real-time double-beam optical system. Front-surfaced,
reflecting optics with protective coating. Optical system sealed
within protective cover.
Monochromator: Littrow design with motorized drive for automatic wavelength
selection and peaking.
Wavelength range: 184 - 900 nm. Diffraction grating: 1800 lines/mm blazed at
236 nm and 597 nm.
Spectral bandwidths: Slits available are 0.2, 0.7 and 2.0 nm.
Detector: Wide-range segmented solid-state detector, including a built-in
low-noise CMOS charge amplifier array.
Automatic Lamp Selection: 8-lamp holder with built-in power supplies for hollow cathode
and electrodeless discharge lamps. Computer-controlled lamp
selection and alignment via WinLab32 for AA™ software.
Lamp elements and recommended operating currents are
automatically recognized and set when using PerkinElmer
Lumina™ hollow cathode lamps.
92 System Description
Background Correction
Deuterium arc lamp: PinAAcle 900H and PinAAcle 900F Auto Built-in continuum
source double-beam background correction using a high-
intensity deuterium arc lamp.
PinAAcle 900Z and PinAAcle 900T use Longitudinal AC
Zeeman-effect background correction using a modulated 0.8
Tesla magnetic field oriented longitudinal to the optical path.
The magnet is automatically switched on during the
atomization step only. Also built-in is continuum source
double-beam background correction for uses with flame
operation.
Flame Atomizer
Burner System: This system has a stacked design, with flame unit on the top,
and graphite furnace at the bottom. The burner is equipped
with a high-strength inert mixing chamber, angled to ensure
proper drainage. Depending on the type of analysis you can
use either the high sensitivity corrosion-resistant plastic
nebulizer and stainless steel nebulizer. There are separate part
numbers for the plastic or stainless steel nebulizers.
Furnace Autosampler
Data System
Specifications Descriptions
Specifications Descriptions
Specifications Description
Specifications Description
Unpacking Instructions
Carefully read these instructions before unpacking the PinAAcle Series to avoid
damage to the instrument. The PinAAcle Series is packed in a cardboard box that
has been designed to safely move and unload the instrument. The bottom of the
crate is a shipping platform designed for use with a forklift.
The PinAAcle 900 Series in the box, can weigh as much as 160 kg (352
! lbs). When using a forklift to move the instrument between the unloading
area and the installation site, the instrument must remain on the shipping
Warning platform. Position the hand truck or forklift under the end of the box. The
instrument should not be lifted without the shipping platform.
The shipping platform used to pack the instrument is returnable for reuse within the
U.S.A. only.
Tools Needed
Wear safety glasses when cutting the steel banding to prevent injury.
!
Warning
1. Check the shock watch and the two tip-and-tell indicators. Record the status of
the indicators on the waybill if they have been tripped.
2. Record any visible damage on the waybill before accepting the shipment.
Notify your local PerkinElmer customer support engineer immediately.
3. Pull out all the foam pieces that secure the instrument in the box.
4. The two cardboard boxes containing the accessories are shipped separately.
7. Prepare to lift the instrument out of the carton. You will need four people to
do this. The bench should be nearby and if the bench has wheels make sure that
the wheels are locked.
The instrument can weigh at least 94 kg (207 lbs). Use proper lifting
! posture when lifting the instrument out of the carton. Be aware that most
of the weight is located at the right side of the instrument. It will want to
Warning tip forward when it is lifted out of the carton, so be prepared to support
that corner.
Before You Install the Spectrometer 103
8. Along the underside of the instrument are hidden handles. Locate these handles
and position two people on each where these handles are located.
9. Squat down and place both hands underneath the instrument handles. Spread
your hands as far apart as possible while grasping the underside of the
instrument.
10. With knees bent, simultaneously lift the instrument up as you end up in a
standing position. Carefully place the instrument on the bench.
• You must make sure that the fume ventilation system and the necessary gas
supply lines and regulators are installed.
104 Installation
These instructions are also provided in case you need to alter any of the
connections or move the instrument, autosampler or accessories in your
laboratory.
• The service engineer will remove the shipping locks, perform pre-installation
checks, install the spectrometer, and make sure that everything functions
correctly.
The instructions here are primarily intended for occasions where the customer may
want to move the spectrometer short distances to a new location within the
laboratory.
Have the customer read the instructions carefully and be sure they understand them
thoroughly before they attempt to move the spectrometer. Have the customer read
the detailed information given in the relevant sections of this chapter before they
reinstall the spectrometer.
If the customer intends to transport the spectrometer over a longer distance, have
them contact their local PerkinElmer office since internal shipping locks must be
set via the service software, inside the spectrometer.
If You Must Move and Reinstall the Spectrometer 105
2. Switch off the spectrometer power switch including the rear circuit breaker,
the computer, and all the accessories.
5. Disconnect the burner gas supplies. Bleed the flame gases if moving to another
location.
6. Flush with DI water for 1-2 minutes and then aspirate dry air for 1 minute if
moving to another location. This will prevent clogging and contamination of
the nebulizer.
9. Prepare the computer and other system components for transport as described
in their own guides.
Carefully lift the spectrometer onto a movable table to transport it to the new
location.
2. For PinAAcle 900T and 900Z, make sure that the furnace knob is securely
tightened all the way so that the furnace head will not move if the spectrometer
must be relocated.
If You Must Move and Reinstall the Spectrometer 107
Tools Needed
• Phillips screwdriver
• Adjustable wrench
Note The instrument ships with the nebulizer in place based on the part number
configuration ordered (a stainless steel or high sensitivity corrosion
resistant plastic nebulizer).
1. Prepare the new site for the spectrometer; see Chapter 2, Preparing Your
Laboratory on page 37.
6. Make sure that the main power switches of all the instruments are in the off
position, then connect the electrical cables.
• Suitable pressure regulators and on/off valves near to the spectrometer for the
gas supplies.
The gas supply systems must comply with your local safety regulations. Also refer
to the information given under Gas Requirements on page 52.
Connecting the Gases 109
Air
1. Make sure that the air supply is turned off.
2. Use the black hose assembly to connect a source of clean, dry, and filtered air
to the fitting labeled Air on the rear panel of the spectrometer. Use an
adjustable wrench to tighten the connections.
Nitrous oxide
1. Make sure that the nitrous oxide supply is turned off.
2. Use the blue N2O hose assembly to connect a source of clean, dry nitrous oxide
to the fitting labeled N2O on the rear panel of the spectrometer. Use an
adjustable wrench to tighten the connections.
110 Installation
Acetylene
1. Make sure that the acetylene supply is turned off.
2. Use the orange C2H2 hose assembly to connect a source of clean, dry acetylene
to the fitting labeled C2H2 on the rear panel of the spectrometer. Use an
adjustable wrench to tighten the connections.
3
2
Note The furnace will operate correctly only if there is gas pressure at both the
Normal Gas and Special Gas inlets. If you are using only an inert gas you
must connect the gas to both inlets using the Y-connector.
• Suitable pressure regulators and on/off valves near to the spectrometer for the
inert and special gas supplies.
• A tube cutter for the special gas tube. This is an optional accessory; Part No.
09923183.
The gas supply systems must comply with your local safety regulations. Refer also
to the information given under Gas Requirements on page 52.
• Two screw connectors, R ¼'' for the gas regulator. These are not supplied with
all instrument versions.
1. Make sure that the argon (or nitrogen) supply is turned off.
2. Use the special tube cutter to cut two, 10 cm lengths of tube from the special
gas tube. The ends of the tubes must be cut squarely.
3. Connect the long gas tube to the argon (or nitrogen) pressure regulator. Use the
R ¼'' screw connector provided or use a connector or adapter suitable for the
gas regulator. Make sure that all the connections are secure.
4. Pass the gas tube to the rear of the spectrometer. Make sure that it cannot be
damaged or strained.
5. Push the two short tubes and the long tube into the connectors on the Y-
connector as shown on the figure on page 114.
6. Push the free ends of the two short gas tubes into the Normal Gas and Special
Gas connectors on the manifold as shown on the figure on page 114.
Push the tubes into the connectors until the tubes butt up to the end of the
connector.
Note To disconnect the gas tube from a connector: Carefully push the black
locking ring of the connector into the connector and pull the tube out of the
connector.
114 Installation
1
2
2. Use the special tube cutter to cut the special gas tube into two pieces for the
two gas supplies. The ends of the tubes must be cut squarely.
3. Connect the gas tubes to the argon (or nitrogen) and special gas pressure
regulators. Use the R ¼'' screw connectors provided or use a connector or
adapter suitable for the gas regulator. Make sure that all the connections are
secure.
4. Pass the gas tubes to the rear of the spectrometer. Make sure that they cannot
be damaged or strained.
5. Push the free ends of the gas supply tubes into the Normal Gas and Special Gas
connectors on the manifold as shown. Push the tubes into the connectors until
the tubes butt up to the end of the connector.
Note To disconnect the gas tube from a connector: Carefully push the black
locking ring of the connector into the connector and pull the tube out of the
connector.
116 Installation
Figure 4-5. Connecting the Argon (or Nitrogen) and a Special Gas
Item Description
1 Argon (or Nitrogen) gas line
2 Special gas line
3 230 V power receptacle
Connecting the Computer and Printer 117
1. Place the computer on the bench and position the monitor on top of the
computer.
3. Connect the Ethernet and furnace camera USB connection from the instrument
to the back of the computer.
12
1
11
7 3
9
10
2
6
5 4
Item Description
5 Ethernet instrument connection (to computer)
6 Furnace camera USB connection (to computer), view partially obstructed
7 Keyboard and mouse (one connection hidden from view)
8 Monitor connection from monitor to computer
9 Monitor connection to computer
10 Computer main power cord
11 Monitor main power cord
12 Back of monitor
Electrical Connections
Warning: Electrical Hazard
To prevent potential injury to yourself and damage to the instrument,
! switch OFF all instruments in the system and disconnect them from the
line power supply before you perform the procedures described below.
Warning
Read the following instructions very carefully before connecting any cables.
See Chapter 2, Preparing Your Laboratory on page 37 for the specification of the
line power supply.
3. If there is a circuit breaker on the rear of your instrument , confirm that the
power circuit breaker is in the off position. See the following figure.
This indicates the off position of the main power switch or circuit breaker.
With the switch in this position, the instrument is disconnected entirely
from the line power supply.
Electrical Connections 121
This indicates the on position of the main power switch or circuit breaker.
With the switch in this position, the instrument is connected to the line
power supply but not necessarily switched on and operational.
4. Please make sure that the computer, and all other accessories that will connect
to the instrument or computer are off. Please refer to the guides of all attached
accessories for procedures on how to use them.
5. Connect the line power cords of the spectrometer and all other accessories to
the main power supply.
122 Installation
6. From the front of the instrument toggle on the on/off green switch.
Electrical Connections 123
• There is space at the rear and sides of the cooling system for air to circulate
freely.
2. Push the hose connectors onto the correct fittings on the spectrometer as shown
opposite. The connectors are spring loaded. Push them straight onto the fittings
until they click into place. Lightly tug on the water line connections on the back
of the instrument to ensure that they are secure, and will not pop off.
See the following procedure Filling the Cooling System on page 127 before you
plug in and start the cooling system.
The cooling system contains 0.5 L glycerol when it leaves the factory
Note (do not use antifreeze).
1. Remove the stopper from the top of the cooling system - twist and pull.
2. Fill the system to the Max mark with sediment-free drinking water - about 4.5
L. Do not use deionized water since this can cause corrosion.
4. Plug the power patch cord into the receptacle on the back of the Cooling
System. Refer to the figure on page 125.
5. Plug the other end of the power patch cord into 230 V receptacle on the back
of the instrument. Refer to the figure on page 116.
6. Turn the On/Off rocker power switch on the Cooling System down to the On
position.
1. Carefully take the drain tubing and attach it to the drain fitting.
2. Take the clamp and use a flat bladed screwdriver to secure around the drain
hose fitting.
130 Installation
3 4
3. Take the other end of the drain hose, where the drain float assembly is located,
and secure it to the drain waste bottle (Carboy 15L).
5. Before connecting the drain tube to the burner assembly, pour about 250 mL
of water into the free end of the drain tube to fill the drain loop and to activate
the drain float. Both the Air pressure and Drain interlocks will be activated
until the magnetic sensor is engaged. Both interlocks should clear once the
drain float is filled with water.
Note The safety interlock connection goes to the instrument. Until you
precondition the drain tube, a drain and air pressure interlock error
message will appear on the computer. See the following procedure to
satisfy the drain interlock.
Note You must perform this procedure directly after installation of a new burner
system and you should repeat it if you replace the drain tube or any of the
sample introduction component.
Nebulizer Installation
The instrument is shipped with the nebulizer already installed. Depending on the
instrument model ordered, it will be shipped with either a standard stainless steel
or a high sensitivity plastic nebulizer.
For information on removing and reinstalling the stainless steel or high sensitivity
plastic nebulizer see Nebulizer Removal and Reinstallation on page 230.
Note The figures shown in this section are of a PinAAcle 900T but the
installation of a AS 900 Furnace Autosampler is the same for the PinAAcle
900H and 900Z.
The AS 900 autosampler can be installed on the PinAAcle 900H, 900T and 900Z.
Tools Needed
• T10 Torx driver
Caution Do not lift the autosampler by the motor, the autosampler arm or any of
the plastic components. This can cause irreparable damage.
The autosampler is packed in a separate box. Carefully unpack the autosampler and
set it up near the instrument.
Note .When attaching the metal boom to the mounting arm make sure not to lose
the metal boom pin because it can easily get loose. The guide pin is a stop
which prevents the arm and boom from moving past the mechanical stop
point on the mounting arm assembly.
2. Attach the metal boom to the mounting arm and make sure that the metal boom
guide pin goes behind the mounting arm.
2 3
1. Connect the autosampler connection cable (Part No. B3002201) to the RS 232
connection port underneath the autosampler.
136 Installation
2. Feed the other end of the connector through the back of the boom mount
assembly.
3. Attach the autosampler to the metal boom, and from the underside of the metal
boom, fasten the Auto sampler to the boom with the four T10 Torx screws
located on the bottom of the Autosampler. Refer to the figure of page 136 for
details.
4. Connect the cable to the RS 232 connection port in the front of the instrument.
5. To lock the autosampler in place, tighten the right locking knob first and then
tighten the left locking knob.
4
2 3
You may have to change the drain tube more often if you use an aggressive rinsing
solution.
• the rinse feed assembly, consisting of a flexible PTFE tube with two screw
fittings and a rigid FEP tube complementary screw thread
1. Push one end of the drain tube into the drain nipple on the rinsing port.
2. Slip the rinsing port onto the guides on the left side of the trough for the sample
tray.
Installing AS 900 Furnace Autosampler 139
3. Slide the waste bottle into the left-hand bracket on the boom.
4. Place the end of the drain tube into the mouth of the waste bottle. If necessary,
shorten the drain tube so that it protrudes only about 30 mm into the waste
bottle. Do not put a cap on the bottle. The drain tube must hang straight down,
without any loops, and the end must never be immersed in the liquid in the
bottle.
Note You may use a 1.2 mL sample cup inserted into the rinse position of the
rinse port. This minimizes the volume of the overflow rinse container.
140 Installation
5. Slide the rinse bottle into the right hand bracket on the boom.
Installing AS 900 Furnace Autosampler 141
6. Connect the other end of the flexible tube to the inlet fitting of the rinse pump.
You may have to shorten the flexible tube,
1. Grip the hub of the sample tray and lower it onto the drive spindle.
2. Rotate the tray gently until the key on the hub engages into the keyway on the
drive spindle. There is a notch in the outer ring of the sample locations to mark
the position of the key.
142 Installation
3. Place the sample tray cover over the hub and line it up so that the lugs on the
sample tray trough engage in the notches in the cover. the ports in the cover are
to the left.
Note Always place the cover on the sample tray to protect the samples from
contamination and to reduce the rate of evaporation of the solvent. You can
reduce the rate of evaporation further by pouring a small volume of water
into the trough.
1 2
1. Carefully remove any tape used for holding the capillary during transportation.
2. Push the metal mount of the sample capillary into the clip at the end of the
pipette arm. Make sure that the sharp side of the metal mount goes first.
3. Pass the sample tube through the hooks on the pipette arm such that it forms a
smooth loop from the metal mount.
4. Pass the sample tube around the hooks on the sample table, leaving a
sufficiently large loop so that the pipette arm can move freely.
capillary flushing the system will remove air from the system. Flush the system
when you complete an analysis in order to prevent future contamination..
1. Make sure that the rinsing system components are correctly installed, are in
good condition, and suitable for the rinsing fluid you will use.
3. Fill the rinse bottle with clean, filtered and degassed rinsing fluid. To reduce
surface tension you may add 0.1% of Triton X-100. If there are particles in the
rinsing fluid they can clog the valves, causing leaks and non-reproducible
results.
Note Make certain there are no air bubbles in the rinsing system. Air bubbles
lead to non-reproducible results.
Installing the Sample Capillary 145
Note If you want to use a different rinsing fluid to that already in the rinsing
system, rinse all traces of the previous fluid out of the rinsing system. Use
a rinsing fluid that is miscible with both the new and the old rinsing fluids.
You may have to use intermediate rinsing fluids. For example, if you are
changing from an acidic fluid to an organic solvent, you could use:
1. Deionized water.
2. Ethanol or another water-miscible solvent.
3. An organic solvent.
• From the Align Autosampler Tip Wizard select Align the autosampler tip
in the graphite tube. The autosampler arm is unlocked and the pipette tip
moves to a position directly above the graphite tube.
Installing the Sample Capillary 147
2. Using the depth control wheel, very carefully lower the pipette tip to just
above the graphite contact.
Do not allow the pipette tip to touch any part of the furnace.
3. Continue lowering the tip and adjusting the left/right and forward/backward
controls on the autosampler until the pipette tip is positioned just inside the
dosing hole of the graphite tube.
148 Installation
4. Use the TubeView window that is currently open on the WinLab32 for AA
workspace to see the tip in the tube.
5. Use the Depth Knob to set the depth of the autosampler tip in the tube so that
it is 1-2 mm above the platform; view the alignment within the TubeView
window. Only adjust in the down direction. If you adjust too low, click on the
< Back button and try again. Do not lower the pipette tip so far that it could
strike the platform.
Refer to the following figure for an example of a well aligned tip.
The steps described in this section describe how to make sure the tip is properly
aligned in the tube. If it is not properly aligned, click < Back and select Align the
autosampler tip in the graphite tube.
Caution
Risk of damage to the pipette tip
The pipette tip enters the graphite tube when you issue the In Tube command.
The pipette tip can strike the edge of the injection hole if the autosampler arm
has not been aligned.
Make sure that the autosampler arm has been aligned before you issue the In Tube
command.
Installing the Sample Capillary 151
Before you perform the steps outlined in this procedure, make sure you have
aligned the autosampler arm as described in To align the autosampler tip in the
graphite tube.
1. From the Furnace Control window select Align Tip > Check autosampler tip
alignment in the graphite tube.
The autosampler arm is unlocked and the pipette tip enters the graphite tube.
Make sure that the tip is centered in the hole in the tube. Do not allow the tip
to touch any part of the furnace.
2. Using the TubeView window that is currently open make sure that the tip is 1-
2 mm above the platform. If not, click on< Back and try again to adjust its
position.
152 Installation
Figure 4-25. Penetration depth of pipette tip in the graphite tube, as viewed from
the Furnace Camera Window on the screen.
3. If you make any additional adjustments in the depth (down only), click on
Finish to save the revised position for use in performing analyses.
4. If the position is not correct, click < Back and perform the Align Tip procedure
again.
5. Adjust the depth control wheel so that the pipette tip is at the depth where you
want it to withdraw samples.
6. If you make any additional adjustments to the depth, click on Finish to save
the revised depth for use when performing analyses.
Installing the Sample Capillary 153
3. In the Automated Analysis Control window, on the Setup page, in the Locations
column, enter the autosampler location of the blank solution.
5. Look in the TubeView camera window and watch the delivery of the solution
droplet onto the platform.
6. If the solution droplet delivery was unsatisfactory, make the appropriate small
adjustments to the penetration depth of the pipette tip. See To check and make
fine-adjustments to the penetration depth of the pipette tip in the graphite tube
on page 150.
7. Repeat step 4 through step 8 to dispense further aliquots of blank solution until
you are satisfied with the delivery.
154 Installation
Note If the pipette tip is too far above the platform and the droplet does not
contact the graphite surface, the liquid may remain in the tip, leading to
pipetting errors.
If the pipette tip is too close to the platform, the liquid may hang up on the
tip, leading to pipetting errors.
8. The pipette tip is at the correct height when the solution droplet contacts the
graphite surface just before leaving the tip.
Installing the Sample Capillary 155
Figure 4-26. Checking the solution droplet delivery, as viewed from the Furnace
Camera Window on the screen
Item Description
1 Wrong: Tip too far above the platform
2 Wrong: Tip too near the platform
3 Correct
156 Installation
Lamps
The spectrometer has an eight position motor controlled lamp selector, and is
designed to hold eight PerkinElmer Lumina hollow cathode lamps (HCLs) or two
electrodeless discharge lamps (EDLs) and six PerkinElmer Lumina hollow cathode
lamps (HCLs). This spectrometer also comes with a background corrector
deuterium lamp (D2).
For information on adding or replacing see Replacing the Lamps on page 250.
Replacement Parts
Every day you count on PerkinElmer to provide you with solutions that deliver
reliable performance, control operating costs and maximize operational time. Our
complete portfolio of consumables, parts, supplies, training and service helps you
meet both routine and demanding measurement challenges. We invest heavily in
testing and validating our products to ensure you receive guaranteed compatibility
and performance-on-time, every time, for every instrument in your laboratory.
Supplies, replacement parts, and accessories can be ordered directly from
PerkinElmer, using the part numbers quoted in the guides provided with the
instrument.
See our website:
http://perkinelmer.com
PerkinElmer's catalog service offers a full selection of high-quality supplies.
To place an order for supplies and many replacement parts, request a free catalog,
or ask for information:
If you are located within the U.S., call toll free 1-800-762-4002, 8 a.m. to
8 p.m. EST. Your order will be shipped promptly, usually within 24 hours.
If you are located outside of the U.S., call your local PerkinElmer sales or service
office.
Shipping List for the PinAAcle 900F 157
2. Make sure that the spectrometer system and other ancillary instruments are
correctly installed and connected to their power supplies. Make sure that the
coolant hoses are connected correctly to the spectrometer. Where applicable,
make sure that the cooling system is filled to the Max mark (see Filling the
Cooling System on page 127).
4. Turn on the burner gases and adjust the outlet gauge pressures to the
recommended values. See Table 5-1 Required Pressures for the Burner Gases
on page 167.
5. Turn on the inert (and special) gas for the furnace and adjust the outlet gauge
pressures to the recommended values. See Table 5-2 Required Pressures for
the Furnace Gases on page 168 .
Note You must always turn on the air supply since air pressure is required for
the internal pneumatic system. If you intend to work with only one
atomizer, you only need to additionally turn on the gas supplies for that
atomizer.
166 Preparing the System
6. Turn on the cooling water to the system: Switch on the circulatory cooling
system by pressing the power switch located on the rear panel.
7. You can leave this switch permanently in the on position since power is
supplied by the spectrometer. Switch the circuit breaker on the rear panel of the
spectrometer to the on position (marked I).
You can leave this switch permanently in the on position during routine
operation; you switch the spectrometer system on and off via the operational
on/off switch located on the front panel.
9. Switch on the spectrometer system with the operational on/off switch located
on the front panel.
10. If you need the diluter, autosampler, or flow injection system, switch on the
respective systems.
11. If you have changed the configuration of the system, such as installed a
different autosampler or added or removed any accessories, use the
Reconfigure utility to reconfigure the software (see the Online Help in
WinLab32 for AA).
12. Start WinLab32 for AA: In the WinLab32 for AA group, double click on the
WinLab32 for AA icon.
• Install any further lamps that you require for the analyses. See Installing
the Lamps on page 168.
• Set up the burner system. See Setting up the System for Analyses Using the
Flame Technique on page 176.
• Set up the graphite furnace system. See Setting up the System for Analyses
Using the Furnace Technique For the PinAAcle 900 T/Z on page 181.
Procedures for shutting down the system are described see Shutting Down the
System on page 191.
Switching on the System 167
• Set the outlet gauge pressure for each gas to a value just below the
maximum value (see Pmax column).
• Always set the same outlet gauge pressure for air and nitrous oxide.
• Never set the outlet gauge pressure to a value exceeding the maximum
pressure (see Pmax column).
• Always turn on the air supply since air pressure is required for the
spectrometer's pneumatic system.
• Set the outlet gauge pressure for each gas to a value just below the
maximum value (see Pmax column).
• Never set the outlet gauge pressure to a value exceeding the maximum
pressure (see Pmax column).
For information on lamp maintenance and cleaning see Nebulizer Removal and
Reinstallation on page 230.
Installing the Lamps 169
Lamp Compartment
The lamp compartment is located behind the door on the right-hand side at the front
of the spectrometer.
An EDL consists of a quartz bulb under an inert gas atmosphere, containing the
element or a salt of the element for which the lamp is to be used. When an RF field
is applied to the bulb, the inert gas is ionized and the coupled energy excites the
vaporized analyte atoms inside the bulb, causing them to emit their characteristic
spectrum. The emission spectra produced is typically much more intense than that
from hollow cathode lamps, frequently tenfold larger or more.
EDL
1. Open the lamp door.
Installing the Lamps 171
2. Insert the coding plug over the receptacle on the lamp holder.
3. Slide the lamp carefully into the lamp holder. Do not push in until the
mechanical stop since this will push in the lamp too far to function properly.
Do not cover the venting slots of the lamp driver or overheating, drift and/or
event shutoff will occur. See the following figure for the proper lamp postion.
4. Connect the lamp cable to an EDL cable connection (see the previous figure)
to the EDL driver power supply connection. Use the Lamp Setup window in
WinLab32 for AA software to automatically align the lamp.
Note EDLs may only be installed in positions 1 and 2 of the lamp housing.
Refer to the figure on page 169 for the assigned lamp numbers on the turret
(mount). For example, if the EDL lamp is installed in position 1 of the
turret, connect the EDL cable to the EDL 1 cable connection on the EDL
driver power supply connection.
Removing lamps
Do not unplug and remove lamps while they are switched on.
2. Make sure that the lamps you want to remove are switched off: The On buttons
must not be green. If necessary, click on the respective On buttons.
4. Unplug and remove the lamps. For EDLs, remove the coding plugs as well.
• We recommend the use of PerkinElmer lamps. You can use both hollow
cathode and electrodeless discharge lamps.
• If you install more than one lamp containing a particular element, for example,
a single-element copper lamp and a multi-element lamp containing copper, the
system will use the lamp in the holder with the lower number when you
perform determinations of that element. Make sure that you place the preferred
lamp in the holder with the lower number.
• With EDLs, connect each lamp plug to the socket that has the same number as
the holder of the lamp.
• With EDLs, make sure that you use the correct coding plug and connect it to
the receptacle on the lamp holder containing the EDL.
• If you use the wrong coding plug or connect the coding plug to the wrong
receptacle, you will cause the spectrometer to malfunction and may cause
irreparable damage to the lamp.
1. Take the sample tray, place the drain hose in the notched area of the tray.
3. Secure the sample tray in place. Make sure that the instrument is not pushed so
far back on the bench that the drain tube bends when the tray is installed.
3. Create or open a method (see the Online Help in WinLab32 for AA).
5. If you intent to make absorption measurements, install the lamps that you
require (see Installing the Lamps on page 168).
6. Set up the burner system (see Setting Up the Burner System on page 176)
7. Perform the safety checks (see Safety Checks for the Flame Technique on page
177).
You should now set up the nebulizer, then optimize the burner and nebulizer before
checking the sensitivity. Refer to the Online Help in WinLab32 for AA.
1. Make sure that the correct nebulizer is installed – the stainless steel nebulizer
or a high sensitivity plastic nebulizer (see Nebulizer Installation on page 132).
Setting up the System for Analyses Using the Flame Technique 177
2. Perform the safety checks (see Safety Checks for the Flame Technique on page
177).
For the correct procedure to extinguish the flame see Extinguishing the Flame on
page 179.
• The burner head is correctly installed and the end cap is secured.
• The fuel and oxidant hoses are correctly fitted to the (back of the) instrument.
If WinLab32 indicates an interlock error, one or more of the following may be the
cause:
• The burner head, the nebulizer, or the drain system is not correctly
installed.
• The liquid level in the drain trap is too low or there is no liquid in the drain
trap.
Note In an emergency, switch off the spectrometer using the operational on/off
switch on the front panel.
The flame is automatically extinguished and the gases shut down in a safe
sequence. See Emergency Shutdown on page 192 for the procedure to
follow after an emergency shutdown.
1. Switch on and set up the spectrometer system (see Setting up the System for
Analyses Using the Flame Technique on page 176).
2. Perform the safety checks (see Safety Checks for the Flame Technique on page
177).
3. Adjust the outlet gauge pressures of the burner gases to the recommended
values (see Table 5-1 on Required Pressures for the Burner Gases on page
167).
5. Select the oxidant: In the Flame Control window, click on Air or N2O.
6. Ignite the flame: In the Flame Control window, click on Flame On/Off.
Setting up the System for Analyses Using the Flame Technique 179
For the correct procedure to extinguish the flame see Extinguishing the Flame on
page 179.
The procedure for rinsing the burner system depends on the type of samples that
you have analyzed.
Recommendations:
• If the sample solutions contained toxic substances, you must rinse all traces of
these substances out of the system.
Procedure:
2. Aspirate for five minutes an organic solvent that is miscible with the samples
that have just been aspirated.
3. Aspirate for five minutes methanol or another solvent that is miscible both with
water and the solvent used previously.
3. Select the Off side of the Flame On/Off switch. The indicator in the switch
goes off.
Figure 5-1. Furnace covers in place (for the PinAAcle 900T and 900Z)
Item Description
1 Furnace cover down in flame position
2 Furnace stage cover (remains in place and is not removed)
1. For the PinAAcle 900T, with one hand on each side of the furnace cover, tilt
the cover up and back.
2. Gently snap the cover into place. It is now secured for furnace analysis.
Note The furnace cover must be locked in the up position when running furnace
analysis. The cover should remain in place down while running the flame
analysis to protect the furnace from corrosion and contamination from
accidental acid and sample spills.
Setting up the System for Analyses Using the Furnace Technique For the 183
3. Carefully swivel the AS 900 autosampler in front of the graphite furnace and
secure it with the large securing knobs.
4. Create or open a method (see the Online Help in WinLab32 for AA).
5. Install the lamps that you require (see the procedure, Installing the Lamps on
page 168).
6. If required, install or change and condition a graphite tube (see Changing the
Contact Cylinders on page 270 and Conditioning the Graphite Tube on page
291).
7. Set up the furnace autosampler. Refer to the Online Help in WinLab32 for AA).
You should now optimize the analytical conditions. Refer to the Online Help in
WinLab32 for AA.
2. Remove the burner assembly from the spectrometer (see Removing the Burner
Head on page 219).
4. Move In/Place the auto-sample. Lock the auto-sampler in position with the
knobs.
2
3
1. Check that a lamp for the element you intend to determine is installed in the
spectrometer and properly aligned.
3. Check that the graphite tube you intend to use for your analyses is installed in
the furnace.
4. Remove both window assemblies from the furnace (see Checking and
Cleaning the Furnace Windows on page 293).
8. Refit both window assemblies (see To refit the windows: on page 320).The
absorbance reading after replacing the windows should be about 0.06-0.09
when measured at the Cu line at 324.8 nm using the AA mode. The absorbance
increases toward shorter wavelengths.
190 Preparing the System
1. Fill and flush the rinsing system (see Filling and Flushing the Rinsing System
on page 143).
2. Align the autosampler arm (see To Align the Autosampler Tip in the Graphite
Tube on page 145).
3. Adjust the penetration depth of the pipet tip in the graphite tube (see the
procedure, To check and make fine-adjustments to the penetration depth of the
pipette tip in the graphite tube on page 150).
4. Adjust the immersion depth of the pipet tip in the sample cup (see the
procedure, To check the depth of the autosampler tip in the sampling cup on
page 152).
5. Check delivery of the solution droplet (see the procedure, Checking the
solution droplet delivery on page 153).
Shutting Down the System 191
Note In an emergency, switch off the spectrometer using the operational on/off
switch on the front panel.
The flame is automatically extinguished and the gases shut down in a safe
sequence. See Emergency Shutdown on page 192 for the procedure to
follow after an emergency shutdown.
• In the Flame Control window, click on the Flame icon. The system uses a
predetermined shutdown sequence to extinguish the flame safely.
2. Switch off the spectrometer at the operational on/off switch on the front panel.
192 Preparing the System
4. If you do not want to use the computer for other tasks, shut down the computer
and printer as described in their user's guides.
5. Empty the burner drain vessel (see Emptying the Drain System on page 227).
Emergency Shutdown
Note Only use the on/off switch in an emergency. Do not use the on/off switch
as a routine shutdown procedure.
If a situation arises where you have to shut down the system quickly and you can
use the on/off switch on the front panel of the instrument.
Shutting Down the System 193
Note The responsible body has the responsibility for carrying out appropriate
decontamination if hazardous material is spilled on or inside the
equipment.
196 Maintenance
Decontamination
Note If the instrument or an accessory requires decontamination before
repair, maintenance, warranty or trade-in purposes at PerkinElmer, the
responsible body should read the procedure and complete the certificate which is
available on the PerkinElmer public website:
http://las.perkinelmer.com/OneSource/decontamination.htm
• For safety reasons, and to avoid contaminating new samples, you should
ensure that the work area is kept absolutely clean. This is especially
important when working with toxic substances and when measuring trace
amounts of any elements.
Checks
Periodic Checks
The frequency of maintenance required will be determined by the amount of use
the system receives, the cleanliness of the environment, and the number and nature
of the samples being analyzed.
• Nebulizer: Check the wear and tear of the o-rings on the end caps and on the
burner head. To replace the o-rings, see Disassembling the Burner Chamber
later in this chapter.
• Drain System Maintenance: Check for wear and/or chemical attack. The drain
tubing should be clear with as few bends as possible. The drain system should
be replaced if it has deteriorated. See Drain System Maintenance later in this
chapter.
• Burner System: Check for uneven flame and deposits build up along the burner
slot.
If you analyze samples that have 'dirty' matrices, such as blood, sugar or oil, you
will probably have to clean the components more often than if you were analyzing
'clean' samples, such as drinking water.
Part Maintenance
Burner system Always rinse the burner system correctly before extinguishing the flame.
If you are analyzing samples with high solids content: Clean the burner
chamber at least once daily.
If you are using organic solvents: Clean the burner chamber before you switch
to aqueous solutions. Empty the drain vessel and dispose of hazardous
solutions properly.
Part Maintenance
Drain vessel This is not a waste storage, but it is a waste collection device for the daily
operation, so empty the drain vessel regularly. Do not allow it to fill with
corrosive, toxic, or organic solutions. Dispose of hazardous solutions properly.
Drain trap Periodically remove the drain trap and clean.
Drain tube Inspect the drain tube regularly for wear and/or chemical attack. Replace it if it
has deteriorated.
O-rings Check the condition of the o-rings regularly: burner end cap o-ring; o-ring in
neck of burner chamber; there are four o-rings on the stainless steel nebulizer,
and five o-rings on the high sensitivity plastic nebulizer. Either of these
nebulizers can be used on the (different) end-cap of the burner assembly.
Gas hoses Check the gas hoses regularly for leaks, particularly at the fittings, using a
proprietary leak testing fluid. Call a PerkinElmer service engineer if a leak is
detected.
Acetylene cylinder If the cylinder pressure falls to below 600 kPa (6 bar; 85 psig) some of the
solvent used to stabilize the acetylene (e.g. acetone) may be carried over into
the burner. This could influence the characteristics of the burner and could
eventually cause irreversible damage to the gas box. Always change to a new
acetylene cylinder when the cylinder pressure falls to below this value.
• You should only perform the maintenance procedures described in this guide.
Burner Maintenance Checklist 201
For any other maintenance or service contact your local PerkinElmer office to
arrange for a service engineer to visit. In particular you should only allow a
PerkinElmer service engineer or similarly trained and authorized person to perform
any work on:
• Make sure that the instrument and work area are clean.
Part Maintenance
Instrument and work For safety reasons, and to avoid contaminating new samples, you should make
area sure that the instrument and the work area are always absolutely clean. This is
especially important when you are working with toxic substances and when
you are measuring trace amounts of any elements. Wipe up spills immediately
before they can cause further contamination or damage. Before you leave the
instrument standing idle for any period of time, make sure that all the
components are clean.
Fume ventilation Make sure that the main exhaust ventilation system functions correctly. Always
switch it on when you are using the instrument.
Environmental Make sure that the environmental conditions are as described in Chapter 2
conditions
Part Maintenance
External Surfaces Wipe over the surfaces with a lint-free cloth moistened with a dilute solution of
laboratory detergent. The surfaces are resistant to dilute acids and alkalis, and
to a lesser extent to strong acids and alkalis and organic solvents.
Air filters Replace filter yearly or more often in a dusty environment.
Changing the Air Filter 203
You should not need to change the filters more than once every year if the
environmental conditions are as described in the Spectrometer Maintenance
Checklist located in this chapter.
Replacement filters (Part No. B0501696) are available; see Replacement Parts
on page 327, for the part number.
4
3
Figure 6-7. Location of air filters on the right side of the instrument
Item Description Item Description
1 Air filter cover tab 3 Air filter cover
2 Air filter location 4 Air filter
3. Depress the tab and lift out the air filter cover that holds the air filter in place.
4. Replace the air filter (Part No. B0501696) and then put the air filter cover back
into place.
Changing the Vent Filter 205
5. The vents located on the left side of the instrument are for the furnace power
supply. Hot air is blown out of these vents and no air filters are needed. Do
not restrict the air flow exhaust from these vents.
2. Take the filter out from the frame and replace with a new filter.
3. Snap the frame with the new filter back into place.
Caution Use only fuses with the required current rating and of the specified type for
replacement.
Changing the Fuses 207
1. Switch off the spectrometer and all other instruments in the system
2. Switch the circuit breaker on the rear panel of the spectrometer to the off
position.
1 2
3. Disconnect the spectrometer's line power cord from the line power supply.
4. Disconnect all the line power cords from the sockets at the rear of the
spectrometer.
a). Insert the tip of a suitable screwdriver in the slit of the fuse holder and
unscrew the fuse holder.
b). Remove the blown fuse, and then insert a new one of the correct type and
rating. The correct rating is shown on the label of the fuse on the rear panel
of the spectrometer.
Note Do not scrape the plastic components with metal tools. Do not soak the
burner chamber in acid or use an abrasive cleaner.
2. The end cap must be removed to access the inside of the burner chamber.
3. The end cap is secured to the burner chamber by the latches located on each
side. Pull both latches back to remove the end cap from the burner chamber.
210 Maintenance
1 2
3 4
4. Clean the burner chamber and flow spoiler with a soft brush and a mild
laboratory detergent solution.
5. Clean the inside of the burner end cap with a soft wireless brush and a mild
laboratory detergent solution.
Note If the solid deposits cannot be removed with a soft brush and a mild
laboratory detergent solution, the internal cavity of the chamber may be
soaked overnight with the 0.5% Triton X-100 + 5% HNO3 acid when the
opening for the burner head is closed. Thoroughly rinse the internal cavity
with de-ionized water before use. If solid deposits still remain, you will
need to replace the spray chamber.
1. Aspirate for 5 minutes an organic solvent that is miscible with the samples that
have just been aspirated.
2. Aspirate methanol or another solvent miscible with both the organic solvent
and water, for 5 minutes.
4. Flush the drain tube thoroughly with water. Empty the collection vessel and
refill with water. Dispose of hazardous or corrosive solutions properly and
observe local codes concerning the effect of the waste on the environment.
212 Maintenance
1. Aspirate dilute acid (1% (v/v) HCl solution) for 5 minutes before turning off
the flame.
4. Flush the drain system see Cleaning (or Flushing) the Drain System on page
226.
• The burner should provide an even flame over the length of the burner slot. An
uneven flame may indicate that the slot needs cleaning. A badly clogged slot
may cause a flashback of the flame.
Cleaning the Burner System 213
• Aspirating samples with high solids content may cause deposits to build up
along the burner slot
Flashbacks
A flashback is an explosion of the premixed gases in the burner chamber. The
safety interlocks normally prevent conditions that could cause a flashback, but if a
flashback should ever occur:
• Check the flow spoiler or impact bead for damage, and replace any damaged
parts
• Make sure that you are using compressed air and not oxygen enriched air
• Carefully check and tighten all connections to, and seals on, the burner unit,
and check the gas flow settings before you attempt to ignite the flame. Any
seepage of fuel and oxidant from the burner chamber may cause a flashback.
3. Remove the burner head up and out by pushing the latch located on the left side
of the burner head to the rear. Refer to the figure on page 217.
4. Carefully work along and through the burner head slot with the cleaning tool
provided. Do not nick the edges of the slot.
Note The cleaning tool resembles a strip of thin metal sheet. Do not use other
tools to clean inside the burner slot since they may have burrs that could
nick the slot.
5. Rinse the burner head well with deionized water and make sure that all
scrapings are removed from inside and outside the burner head.
Wear safety glasses when blowing the burner head with clean
! compressed air.
Warning
Feeler Gauge
Burner Head Slot Width Tolerance
for check
This procedure should be done directly after installation of a new burner and
repeated if the drain tube or any of the sample introduction system components are
replaced.
In order for a new sample introduction system to aspirate sample and drain
smoothly, all the internal surfaces need to be prepared. This is easily accomplished
by aspirating a 0.1% Triton X-100 solution for approximately five minutes.
3. Locate and press the locking pin down, and push the locking lever backward
to disengage the whole burner assembly. The burner assembly will be pushed
forward, and can now be removed. See the following figure.
Removing the Burner Assembly From the Instrument 217
1
2
3
4
Figure 6-13. Remove the burner head from the burner chamber
Item Description Item Description
1 Safety latch 3 Pressing the safety latch
2 Burner lever 4 Pushing the burner lever
218 Maintenance
4. The burner assembly is now accessible for maintenance. Remove the burner
assembly.
5. Place the burner assembly on a bench for routine maintenance and cleaning.
Removing the Burner Head 219
Depending on the type of analysis you need to do, you may need to change the
burner head, see Burner Head Options on page 86.
1. The burner head should also be removed by following the procedure Removing
the Burner Assembly From the Instrument on page 216
220 Maintenance
2. Unscrew the retaining ring (see figure below) and pull out the burner o-ring.
3 1
5
4
3. Remove the nebulizer from the end cap assembly. Refer to Removing the
Stainless Steel Nebulizer on page 231. Refer to Removing the High Sensitivity
Plastic Nebulizer on page 236
4. Clean the chamber. Place the parts in a detergent solution until they are
completely clean. See Cleaning the Burner Chamber on page 208 for details.
5. Remove and rinse with deionized water. Allow time for complete drying.
1. Before you reassemble the burner system, verify that the o-rings are in good
condition. If an o-ring appears damaged, replace it.
3. Carefully slide the nebulizer into the end cap and lock into place with the
nebulizer clamp.
4. Place the burner o-ring into the burner chamber and screw on the retaining ring.
5. Press the safety latch on the ignitor box while gently pushing and twisting the
burner head onto the chamber.
2. Push the burner assembly in so that the rear gas fittings line up with the gas
connectors at the back of the Burner Assembly mount. Push the burner
assembly fully in until it clicks into place. Pull the locking level forward until
it locks the burner assembly in place. The locking pin automatically locks.
222 Maintenance
3. Locate the drain vessel. The drain tube and interlock cable will be attached to
the drain vessel retainer cap.
4. Place the drain vessel in full view on the floor in front of the instrument. Never
place the drain vessel inside a cabinet.
5. Before connecting the drain tube to the burner assembly, if necessary pour
about 250 mL of water into the free end of the drain tube to fill the drain loop
and to activate the drain float.
6. Place the hose clamp over the free end of the drain tubing.
Caution When installing the free end of the drain tubing over the drain outlet, take
care not to damage the inner Teflon lining of the drain tube.
7. Carefully install the free end of the drain tubing over the drain outlet, making
sure that the inner Teflon lining of the drain tube does not get damaged.
9. Plug the white drain interlock connector into the drain interlock plug on the
burner assembly as shown in the figure below.
To Install the Burner in the Spectrometer 223
2
3
1. Put the burner head back onto the burner chamber while pressing the safety
latch tab.
2. Position the magnetic strip on the burner head ring around the back of the
assembly - it should face the ignitor box. Release the safety latch. Be sure the
burner head is fully seated on the chamber. A gentle twisting and pushing may
be necessary. You will know that the burner head is fully seated because the
ignitor will swing over the burner.
4. Check the burner alignment. You should readjust the burner any time the
burner is aligned.
2
1
The drain hose and vessel must be checked periodically for wear and/or chemical
attack. The drain tubing should be clear with as few bends as possible. The drain
system should be replaced if it has deteriorated.
3. Pour about 250 mL deionized water slowly through the drain tube to
completely flush the chamber and the drain system.
1. Extinguish the flame, allow the burner head to cool, shut down the gases at
source, and bleed the gas supply lines.
3. Flush the drain system. See Cleaning (or Flushing) the Drain System on page
226.
228 Maintenance
5. Carefully lift out the drain trap assembly. Do not disconnect the electrical lead.
6. Place the drain trap assembly into a suitably large bucket or container so that
it is vertical. If the drain trap assembly is laid on its side, liquid can run out onto
the floor.
9. Place the drain trap assembly back into the drain bottle and screw on the
retainer cap.
3. Unplug the drain interlock connector from the burner (see the previous figure).
4. Remove the spiral wrap from the drain tubing by unwrapping it. This will
release the drain interlock cable.
Drain System Maintenance 229
5. Disconnect the drain tubing from both the drain vessel and the drain outlet on
the burner end cap by loosening the clamps on each end of the tubing. Once the
clamps are loosened, the tubing should easily pull out.
6. Place the new piece of drain tubing (Part No. 02507987) next to the drain
interlock cable and carefully rewrap the spiral wrap around them both.
7. Place the drain clamp on the upper end of the new drain tubing. Then attach the
tubing to the drain outlet on the burner end cap. Tighten the clamp securely.
8. Place the other drain clamp on the lower end of the drain tubing. Then attach
the tubing to the drain trap switch assembly. Tighten the clamp securely.
9. Plug the drain interlock connector into the receptacle under the burner. Make
sure the interlock connector is plugged in all the way.
10. Go to Preparing the New Drain Tubing for Use on page 229.
Note This important procedure MUST be performed at this point of the drain
tube replacement process.
In order for the sample introduction system to drain smoothly, the internal surface
of the new drain tube needs to be prepared. This is easily accomplished when you:
1. Loosen the drain clamp and remove the drain tubing from the drain outlet on
the burner end cap.
3. Carefully reconnect the drain tubing to the burner end cap. Replace the drain
clamp and tighten securely.
3
4
3. Pull the nebulizer out from the nebulizer assembly end cap.
2 7 10
3 8
5
1 4 6 9 11
Note Do not use Apiezon grease of unknown source and quality as it may
contain trace metals. Make sure that no grease gets onto the tip of the
capillary.
4. Inspect all the o-rings in the nebulizer assembly end cap. Replace any cracked
or damaged o-rings.
Nebulizer Removal and Reinstallation 233
5. Apply a small amount of Apiezon grease (Part No. 03030405) onto the o-rings
(Part No. 09902015). The nebulizer will then slide easily into the end cap.
7. For information on cleaning the nebulizer, see Cleaning the Stainless Steel
Nebulizer on page 235.
1
2
4 3
Note Do not use Apiezon grease of unknown source and quality as it may
contain trace metals. Make sure that no grease gets onto the tip of the
capillary.
2. Apply a small amount of Apiezon grease (Part No. 03030405) onto the o-rings
(Part No. 09902015) on the nebulizer body. The nebulizer will then slide easily
into the end cap.
3. Insert the re-assembled nebulizer into the end cap in the unlocked position.
5. Push the locking clamp all the way in to lock the nebulizer in place.
Note When the nebulizer is securely in place, the nebulizer interlock will be
depressed and you will be able to run the instrument. If the nebulizer
interlock is not depressed, the WinLab32 for AA software will indicate
that the safety lock is not satisfied.
A checked green box in the WinLab32 for AA software will indicate that
the safety locks are engaged and the instrument can be run.
1. Aspirate pure solvent with the flame on until a stable baseline signal is
achieved. Then aspirate a known standard solution, within the linear range for
this element. Please refer to the Analytical Methods for AA Spectroscopy (Part
No. 03030152) for this concentration. The achieved absorbance should be +/-
236 Maintenance
20% the expected absorbance for this known concentration as shown in the
Analytical Methods for AA Spectroscopy (Part No. 03030152).
2. If you cannot obtain a satisfactory absorbance for this standard, try to clear the
obstruction by pushing the copper cleaning wire through the capillary and into
the nebulizer. Move the wire in and out to dislodge any solid particles
Caution Use only the copper cleaning wire provided with the nebulizer to clean
the capillary. Other wire may be burred and can damage the nebulizer.
3. Clean the nebulizer body and any other parts that appear dirty in a mild
laboratory detergent solution, or a solvent such as isopropanol, preferably in an
ultrasonic bath.
5. Inspect the all o-rings on the nebulizer body and clean them if necessary in
mild laboratory detergent solution, followed by a thorough rinsing with
deionized water. If they look damaged, replace them.
2. Pull back the locking clamp and rotate the plastic arm to the unlock position.
Nebulizer Removal and Reinstallation 237
3. Grasp the plastic arm from the locked position and firmly rotate it up (the arm
will be tightly in place).
2 1
6
7
5
8
9
4. Wiggle the nebulizer out from the nebulizer assembly end cap.
5. The nebulizer assembly end cap is secured to the burner chamber by the latches
located on each side. Push both latches back to remove the nebulizer assembly
end cap from the burner chamber.
6. Inspect the o-rings in the nebulizer assembly end cap. Replace any cracked or
damaged o-rings.
2 1
4
5
3
4 5 7
9
1 2 3
6 8
11
10
Note Located on the spring are two o-rings, one larger and one very small one.
The small o-ring can be lost very easily if the Apiezon grease (Part No.
03030405) is not applied on the needle valve.
240 Maintenance
8. Inspect the all the o-rings. Replace any cracked or damaged o-rings. Apply a
small amount of Apiezon grease (Part No. 03030405) onto the o-rings (Part
No. 09902015). The nebulizer will then slide easily into the end cap.
10. For information on cleaning the nebulizer, see Cleaning the High Sensitivity
Plastic Nebulizer on page 241.
Note If not already done, inspect the tiny o-ring on the capillary assembly for
damage and replace them if necessary. Lightly lubricate the surface of the
o-rings with a minimum of Apiezon grease. Make sure that no grease gets
onto the tip of the capillary.
1. Slide the spring back onto the capillary assembly (if it was removed).
3. Line up the alignment key with the keyway in the nebulizer body.
4. Push the capillary assembly in until it bottoms out in the nebulizer body.
5. If you inserted the capillary assembly correctly, it should move freely in and
out of the nebulizer body. If it does not, remove and reinstall, paying particular
attention to the alignment key.
7. Where applicable, refit the fragile impact bead and spacer onto the plastic
nebulizer.
9. Take the plastic arm on the nebulizer and lower it into the lock position and
lock it in place with the locking clamp.
Nebulizer Removal and Reinstallation 241
Note When the nebulizer is securely in place, the nebulizer interlock will be
depressed and you will be able to run the instrument. If the nebulizer
interlock is not depressed, the WinLab32 for AA software will indicate
that the safety lock is not satisfied.
A checked off green box in the WinLab32 for AA software will indicate
that the safety locks are engaged and the instrument can be run.
If you suspect that the nebulizer is causing poor sensitivity (e.g. cannot obtain
expected characteristic concentration) or poor precision (fluctuating absorbances),
before cleaning the nebulizer check that:
• The sample tube is in good condition (i.e. no kinks), is not too long, and is
clean. With a longer sample tube, the rate of sample uptake, and thus the
sensitivity, will decrease. Recommended length: 20 cm.
• The first (simplified) way should be used if the nebulizer is not difficult to
clear. This method involves simply passing one of the cleaning wires,
supplied, through the capillary holder.
Caution In the simplified method of cleaning the nebulizer the impact bead is not
removed. Use the cleaning wire carefully so as not to damage the impact
bead.
2. Take one of the cleaning wires (Part No. 03030135) supplied, and push it
through the capillary holder from its wider (open) end.
Note It may take several attempts to pass the wire through the nebulizer.
3. Repeat step 2 several times. Then replace the capillary (sample) tubing.
4. Run one or more standards to determine if the capillary holder has been
cleared. If it has been cleared, proceed with normal spectrometer operation;
otherwise, proceed with the next procedure.
Nebulizer Removal and Reinstallation 243
Wear protective gloves when you remove the nebulizer from the end cap
! if you were analyzing toxic samples.
Warning
2. Pull back the locking clamp that secures the nebulizer in place.
3. Rotate counter clockwise to the unlock position and gently pull the nebulizer
out of the burner end cap.
4. Remove the impact bead from the plastic nebulizer and, if using the impact
bead spacer, remove the spacer as well. Handle with care. (See the next page
for instructions.)
6. See the figure on page 239 and loosen and then remove the knurled needle
valve adjustment knob and locking washer.
Cleaning
1. While holding the capillary assembly in one hand, take one of the cleaning
wires (Part No.03030135) supplied.
2. Push it through the capillary assembly from its wider (open) end.
Note It may take several attempts to pass the wire through the nebulizer.
244 Maintenance
3. Clean the nebulizer body and any other parts that appear dirty in a mild
laboratory detergent solution, or a solvent such as isopropanol, preferably in an
ultrasonic bath.
5. Inspect the all o-rings and clean them if necessary in mild laboratory detergent
solution, followed by a thorough rinsing with deionized water. If they look
damaged, replace them.
The bead structure mounts directly on the plastic nebulizer's body assembly, see
the figure on page 239.
2. Then rotate it, holding only the base, approximately 1/8 turn clockwise, i.e.,
until it reaches a stop and "locks" itself.
The addition of the spacer reduces the amount of sample delivered to the flame. It
is recommended to use the spacer for all elements analyzed with the nitrous oxide-
acetylene flame and for elements which are air-acetylene flame sensitive such as
calcium, chromium and gold. When analyzing some complex sample matrices, it
may be desirable to add the spacer to reduce chemical interferences.
3. Place the spacer onto the back of the nebulizer and replace the impact bead.
4. Rotate the bead 1/8 turn clockwise to "lock" the bead in place.
4. If you see bubbles at the end of the capillary tube (in the sample solution),
loosen the nebulizer locking nut and slowly turn the adjustment nut clockwise
until the bubbling stops.
5. Aspirate a standard and adjust the burner position. Optimize the burner head
position through the WinLab32 for AA software.
6. While still aspirating the standard, turn the nebulizer locking nut clockwise
until it is free of the nebulizer adjustment nut.
7. Slowly turn the nebulizer adjustment nut counter clockwise until bubbles begin
to appear at the end of the capillary tube in the sample solution.
8. Slowly turn the nebulizer adjustment nut clockwise until the absorbance goes
to a maximum and then begins to decrease.
9. Lock the nebulizer adjustment nut in its current (optimum) position by turning
the nebulizer locking nut counter-clockwise while carefully holding the
nebulizer adjustment nut, until this locking nut locks the adjustment nut.
By reducing the uptake rate to 2-4 mL/min, it is usually possible to operate with a
leaner (blue) flame than is possible with higher nebulizer uptake rates. This leaner
flame typically provides improved precision, particularly when aspirating xylene.
To adjust the nebulizer uptake rate, unlock the nebulizer locking nut and rotate the
nebulizer adjustment nut until you locate a position which provides reduced sample
uptake. Then lock the nebulizer locking nut.
Replacing Parts of Wear 247
Also, the nebulizer is only a part of the overall burner system. For optimum burner-
system performance, it is important to periodically clean the nebulizer, burner
chamber, burner heads, and the end cap.
The surfactant solution will encourage constant drainage, which is required for
obtaining optimum burner system performance.
When using the nebulizer, the impact bead may have to be replaced. Also, to avoid
damage to the impact bead, the bead should be removed when cleaning the
capillary holder assembly. Steps for removing and replacing the bead are included
in this instruction document.
2. Inspect the large o-ring located in the neck of the burner chamber. Carefully
lever the o-ring out of the neck of the burner chamber using a plastic pipette tip
or the like.
Note Never use sharp or pointed tools to remove the o-ring. Examine the o-ring.
If it is damaged, replace it.
3. Place the large o-ring back into the neck of the burner chamber and press it
down with your finger.
4. Inspect the four smaller o-rings and the large o-ring located in the burner end
cap. Very carefully pry them out and inspect the o-rings for nicks, cuts and
deterioration . Replace the o-rings as needed.
6. Gently place the o-rings back into the end cap and then press them into place
with your finger.
Nebulizer O-Rings
There are o-rings on the nebulizer. Always carefully check the condition of these
o-rings whenever you take the nebulizer apart.
Maintaining the Acetylene Supply 249
• Depressurize both the fuel and oxidant gas hoses at the end of the working day
or if you are not going to use the instrument for an extended period. Close the
cylinder valves to avoid the possibility of gas hoses being subjected to the full
cylinder pressure in the event that a pressure regulator should fail.
• Always store and use acetylene cylinders vertically, rather than horizontally,
to prevent liquid acetone from reaching the cylinder valve.
• The practice of "cracking the valve" of an acetylene tank (that is, opening the
valve slightly for a very short period previous to attaching the regulator) is not
recommended. While such an action will clear the valve opening of dust or dirt
particles and may remove acetone from the cylinder valve, it is a potentially
hazardous practice and one which should never be attempted in the presence of
an open flame, sparks or other possible sources of ignition.
250 Maintenance
Lamp Life
Both hollow cathode and electrodeless discharge lamps have a finite lifetime.
Electrodeless discharge lamps typically last longer than hollow cathode lamps for
the same element. If, while aligning a lamp, you are not able to obtain a satisfactory
energy value, this may indicate that the lamp is starting to deteriorate. As a hollow
cathode lamp reaches the end of its useful life, the current on the lamp may be
increased up to the maximum current recommended on the label. Once the
intensity of a lamp begins to deteriorate, it should be replaced. The Lumina lamps
comes with an electronic means of monitoring its usage, also in mA-Hours, with
an in-built EEPROM, that can be addressed and read from the PinAAcle AA.
PerkinElmer lamps are warrantied for 5000 mA-hour or six months whichever
comes earlier.
Lamp Troubleshooting
Refer to Chapter 8, Troubleshooting, in this manual for lamp troubleshooting
information.
Caution To avoid damages to the instrument optics, do not insert uncoded non-
Lumina lamps, such as Intensitron lamps, too far into the lamp holder.
Removing lamps
Danger HOT SURFACE
The lamp is hot when it is in operation..
! Make sure that the lamp is completely cooled down when you remove
Na, Li and K lamps, since the cathode will be in the molten form when it
Warning is in use and will be hot and could cause a burn.
1. Do not unplug and remove lamps while they are switched on.
2. Using the WinLab32 for AA software click on the Lamp icon to display the
Lamp Setup page.
3. In the LampSetup window, go to the On/Off column and click on each green
button to turn the lamp off. The button will change color from green to dark
gray.
4. Make sure that the lamp is switched off before you remove it.
6. Unplug and remove the lamp. For EDLs, remove the coding plug as well.
2. The access to the D2 lamp compartment cover is located on the right side of the
instrument. Use a Phillips screwdriver to remove the screw that holds the cover
in place. Remove the cover.
2
1
Item Description
1 D2 lamp compartment cover
2 Phillips screw
Caution As you slide out the D2 lamp assembly take care not to damage the cable.
254 Maintenance
3
2
3 Bracket
Removing and Replacing the Deuterium Arc Background Corrector Lamp 255
Caution Wear contaminant-free gloves when handling the new lamp to prevent
getting fingerprints on the viewing area of the lamp, as this will decrease
the UV performance and damage the lamp.
5. Replace the assembly with a new bracket/ bulb set by sliding the cutout on the
metal bracket over the alignment pin on the instrument.
256 Maintenance
1 2
Item Description
1 D2 lamp
2 Cutout
3 Alignment pin
2. Carefully slide the deuterium lamp assembly down on to the alignment pin on
the D2 lamp housing.
4. Return the screw to the D2 lamp compartment cover and tighten down the
cover.
Reassembly is complete. Next you may have to align the deuterium lamp.
5. While watching the computer screen, use a 2 mm Allen key to adjust the
vertical and horizontal alignment screws located on the rear of the deuterium
lamp compartment, until you achieve the maximum energy counts. See the
following figure.
Removing and Replacing the Deuterium Arc Background Corrector Lamp 259
After aligning the deuterium lamp you need to reset the hours.
4. Swing the support lever to the side. Tilt the front contact housing downward.
See the following figure.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 261
2
1
5. The graphite tube is now visible in the rear contact. Use the insertion/removal
tool provided to remove the graphite tube. Do not touch the tube with bare
fingers.
262 Maintenance
Note Do not touch the graphite tube or contacts with your fingers. Wear
contaminant-free gloves when changing the contact cylinders and graphite
tube.
2
1
• The side of the tube to which the platform is attached faces the left of the
furnace. The platform is then higher toward the rear.
264 Maintenance
2. Use the insertion/removal tool provided to insert the graphite tube into the rear
contact.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 265
3. Carefully tilt the front contact housing up into the closed position (1).
4. Swing the support lever underneath the front contact housing (2).
266 Maintenance
2 1
6. Carefully swivel the furnace autosampler back into place and secure it with the
large securing knobs.
Note Do not touch the graphite tube or contacts with your fingers. Wear
contaminant-free gloves when changing the contact cylinders and graphite
tube.
268 Maintenance
1
4
4
3
You can sometimes remove contamination from the graphite tube by heating the
tube. Heat the graphite tube manually at 2500 °C for approximately 5 seconds
(see Manually Heating the Graphite Tube on page 292).
You may need several cycles to remove this element. Discard the tube for this
element, as this element is the contaminant. This tube may still be clean for other
elements and could still be used for other elements. But if there are stubborn
deposits in the tube that you cannot remove, discard the tube and use a new one.
1. Open the furnace and remove the graphite tube (see Removing the Graphite
Tube on page 260).
2. Use a dry, clean swab to clean the inside of the contacts, especially around the
apertures where the radiation beam enters and exits.
Remove any particles from inside the contacts using clean, dry compressed
air.
Be careful not to scratch the inner surfaces of the contacts.
If the surfaces of the contacts are pitted or cracked, remove the contacts and
install new ones (see Changing the Contact Cylinders on page 270).
270 Maintenance
3. Heat out the graphite tube to remove contamination (see Manually Heating the
Graphite Tube on page 292).
Note It is recommended that you visually inspect the contact cylinders for wear
and tear and also for corrosion on the surfaces of the cylinders. If there is
visible wear and corrosion on the surfaces, then the contacts should be
replaced, since this can impact the quality of the analytical results.
Unexplainable spikes on the peak profile of the analysis are also an
indication that the contact cylinder is wearing off and may need to be
replaced. The precision of the analysis degrades once these components
start to show signs of wear and tear.
Note If the graphite tube breaks inside the contact cylinder, you must clean the
contact cylinder/furnace housing thoroughly and may have to replace the
contact cylinder.
2. In the Furnace Control window click Open/Close and remove the graphite
tube using the tube insertion/removal tool, and then tilt the furnace forward .
3. Switch off the spectrometer at the operational on/off switch at the front of the
instrument.
You must open the furnace to install or change the graphite tube, and also to clean
inside the graphite contacts.
1. Extinguish the flame, turn off the gases, and switch off the instrument. Let the
burner head cool. Open the Sample Introduction compartment door.
2. Loosen the furnace locking screw all the way. See the figure Tilting the
Graphite Furnace Back Into Position on page 296.
3. Grasp the graphite furnace with both hands and carefully tilt it forward.
Support its weight until it reaches the end stop. Never allow the graphite
furnace to swing down with force. This will damage the furnace assembly and
the base of the instrument.
272 Maintenance
Note This procedure is easier to do if the furnace is in the forward position. See
Tilting the Graphite Furnace Forward on page 271.
1. From the tools provided, you require the contact removal tool, the hex-driver,
and the Torx driver (star-shaped cross-section).
2. Loosen the two socket-head screws that secure the pressure cylinder to the
front contact housing.
3. Carefully pull the pressure cylinder out of the front contact housing. Make sure
that you do not damage the O-ring. Put the pressure cylinder and screws in a
safe place.
274 Maintenance
4. Attach the removal tool to the front contact housing with the two captive
screws on the tool.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 275
5. Use the hex-driver to screw the bolt on the removal tool into the tool to push
out the contact.
276 Maintenance
6. Unscrew the two screws that secure the tool to the contact housing and remove
the tool.
2. From the tools provided, you require the contact removal tool, the short
posidriver (P2 size), and the Torx driver (star-shaped cross-section T20 size).
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 277
Note Make sure that you do not bend or twist the temperature sensor connector.
Also, do not damage the insulating washers.
278 Maintenance
1
4
3 5
3. Using the Torx driver unscrew the two captive, socket-head screws that secure
the optical sensor to the rear contact housing.
4. Carefully pull the optical sensor out of the rear contact housing. Make sure that
you do not damage the O-ring. Move the optical sensor to the side.
5. Use the posidrive to remove the screw that hold the temperature sensor in
place.
6. Attach the removal tool to the rear contact housing with the two captive screws
on the tool.
7. Use the hex-driver to screw the bolt on the removal tool into the tool to push
out the contact.
8. Unscrew the two screws that secure the tool to the contact housing and remove
the tool.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 281
Note Do not scratch the new contact and do not touch it directly. Wear
contaminant-free gloves when changing the contact cylinders and graphite
tube. Perspiration can contaminate the contact and cause poor analytical
results
Tilt the furnace forward. See Tilting the Graphite Furnace Forward on page 271.
1. Make sure that the contact housing is completely clean and free from particles.
If necessary, blow out any graphite particles from the contact housing with
clean, dry compressed air. Wear safety glasses when doing this.
• the long bolt, front contact guide, and threaded cylinder as shown below.
3. Move the swing arm, located below the furnace, out of the way. Carefully tilt
the graphite furnace forward and support it with one hand.
4. Slide the guide and the front contact onto the long bolt as shown.
282 Maintenance
4
1
2
3
5. Slid the bolt into the front contact housing such that the new contact sits in the
opening of the housing. Screw the threaded cylinder on to the bolt
6. Put the threaded cylinder into the opposite end of the contact housing and
screw the bolt into the cylinder until the contact is pressed up against the
housing.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 283
7. Tilt the graphite furnace back into its original position. Use the hex-driver to
screw the bolt into the threaded cylinder and push the contact into the contact
housing. Screw in the bolt until the rim of the contact is flush with the contact
housing.
Note There must be no gap between the rim of the contact and the housing.
Do not use excessive force to push the contact into the housing, otherwise
the contact may shatter.
If there is substantial resistance, check that the parts are aligned correctly.
284 Maintenance
8. Screw the bolt out of the threaded cylinder and carefully remove the tools. Do
not scratch the contact when you remove the tools.
9. Blow out any graphite particles from the contact housing with clean, dry
compressed air. Wear safety glasses when doing this.
10. Check the O-ring on the pressure cylinder; if it is damaged, fit a new one. See
Replacement Parts on page 327.
11. Push the pressure cylinder carefully into the front contact housing. Make sure
that you do not damage the O-ring.
12. Tighten the two screws to secure the pressure cylinder to the front contact
housing.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 285
Note Do not scratch the new contact and do not touch it directly. Wear
contaminant-free gloves when changing the contact cylinders and graphite
tube. Perspiration can contaminate the contact and cause poor analytical
results
1. Make sure that the contact housing is completely clean and free from particles.
If necessary, blow out any graphite particles from the contact housing with
clean, dry compressed air.
Wear safety glasses when doing this.
• the long bolt, rear contact guide, and threaded cylinder as shown below.
3. Move the swing arm, located below the furnace, out of the way. Carefully tilt
the graphite furnace forward and support it with one hand.
4. Slid the bolt into the rear contact housing such that the new contact sits in the
opening of the housing. Screw the threaded cylinder on to the bolt
2
3 4
5. Make sure that the graphite contact is correctly orientated, with the sample
injection hole at the top.
6. Put the threaded cylinder into the opposite end of the contact housing and
screw the bolt into the cylinder until the contact is pressed up against the
housing.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 287
1
2
4
7. Tilt the graphite furnace back into its original position. Use the hex-driver to
screw the bolt into the threaded cylinder and push the contact into the contact
housing.
Screw in the bolt until the contact is flush with the contact housing.
Note There must be no gap between the contact and the housing.
Do not use excessive force to push the contact into the housing, otherwise
the contact may shatter.
If there is substantial resistance, check that the parts are screwed in straight
and not at an angle.
288 Maintenance
8. Screw the long bolt out of the threaded cylinder and carefully remove the tools.
Note Do not scratch the new contact when you remove the tools.
9. Blow out any graphite particles from the contact housing with clean, dry
compressed air. Wear safety glasses when doing this.
10. Check the O-ring on the optical sensor; if it is damaged, fit a new one. See
Replacement Parts on page 327.
11. Push the optical sensor into the rear contact housing. Make sure that you do not
damage the O-ring.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 289
12. Tighten the two screws to secure the optical sensor to the rear contact housing.
2. Insert a graphite tube into the furnace, close the front contact housing, and
swing the support lever under the contact housing (see Inserting the Graphite
Tube on page 263).
290 Maintenance
3. Switch on the spectrometer at the operational on/off switch located at the front
of the instrument.
4. If you have installed a new graphite tube, see Conditioning the Graphite Tube
on page 291).
Note Every time you open the furnace, subsequently always heat it out manually
at 2500 °C for approximately 5 seconds.
Note It is recommended that you visually inspect the graphite tube and the
contact cylinders for wear and tear and also for corrosion on the surfaces
of the tube and cylinders. If there is visible wear and corrosion on the
surfaces, then the contacts and/or tube should be replaced, since this can
impact the quality of the analytical results. Unexplainable spikes on the
peak profile of the analysis is also an indication that the graphite tube or
the contact cylinder is wearing off and may need to be replaced. The
precision of the analysis degrades once these components start to show
signs of wear and tear.
Note If the graphite tube breaks inside the contact cylinder, you must clean the
contact cylinder/furnace housing thoroughly in addition to replacing the
contact cylinder.
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 291
Contact Cycles
Use this value to show the number of times that the furnace has been used since the
contacts were changed.
Click on Reset to reset the value to zero when you install new graphite contacts.
Check the Display warning message when cycles exceed check box to have a
warning message displayed when an analysis is started and the contact cycles have
exceeded a user specified number. The warning message will not prohibit a user
from performing an analysis, but rather serves as a reminder to the user that the
contacts should be inspected and, if necessary, replaced.
Note Do not heat the graphite furnace for longer than about 10 s when the
temperature exceeds 2000 °C. Heating for longer periods will markedly
reduce the lifetime of the graphite tube.
2. In the Furnace Control window, click on the Cleanout Temp. entry field and
type the required temperature (e.g. 2500 °C).
Graphite Furnace Maintenance for the PinAAcle 900T/900Z 293
3. Tilt the furnace forward (see Tilting the Graphite Furnace Back Into Position
on page 296).
4. Use the key provided to unscrew the left-hand and the right-hand windows
from the furnace.
294 Maintenance
2. Dismantle the window assemblies and carefully remove the quartz windows
carefully from the mounts.
1 2 3
3. Blow any dust or particles off the surface of the window with clean dry air
before you start.
4. Clean the windows carefully with a tuft of cotton moistened with a dilute
solution of mild laboratory detergent.
Rinse the windows several times with deionized water.
If the windows are not clean after this procedure, clean them with a soft lint
free cloth moistened with spectroscopic grade alcohol.
Note To avoid scratching the windows, rub the surfaces of the windows as little
as possible. Discard scratched windows.
296 Maintenance
2. Tilt the furnace back into its original position and tighten the furnace locking
screw to lock the furnace into place (see Tilting the Graphite Furnace Back
Into Position on page 296).
2. Tighten the furnace locking screw to lock the furnace into place.
4. Switch on the instrument, turn on the gases and restore the flame.
1. Take a graphite tube with integrated platform and insert it into the right-hand
graphite contact, so that the sample introduction hole lines up roughly with the
sample port in the graphite contact.
Note Make sure that the side of the tube to which the integrated platform is
attached is rear of the furnace.
298 Maintenance
2. Insert the alignment tool (provided) into the sample port while carefully
moving and turning the tube so that the tip of the alignment tool goes into the
sample introduction hole in the tube.
3. With the alignment tool still in position, activate the pressure that holds the
furnace closed:
In the Furnace Control window, click on Open/Close.
The furnace closes.
4. Remove the alignment tool.
(If the furnace closes abruptly, you can adjust the speed with the speed reducer
located behind the HGA Furnace)
1
2
3 4 6
5
5. If you have installed a new graphite tube, perform the procedure outlined in
Conditioning the graphite tube on page 305.
If you are reusing a previously conditioned graphite tube, heat manually at
2500 °C for 5 seconds to remove surface contamination.
6. Every time you open the furnace, subsequently always heat it out manually at
2500 °C for approximately 5 seconds.
7. Check alignment of the furnace (see Aligning the Graphite Furnace on page
186).
8. Check alignment of the furnace autosampler (see To Align the Autosampler
Tip in the Graphite Tube on page 145).
Note Do not touch the graphite tube or contacts with your fingers. Perspiration
can affect the tube lifetime and the analytical results by contaminating and
damaging the surface of the graphite.
If a graphite tube breaks inside the furnace you must remove all the
remnants and thoroughly clean the contacts.
Graphite Furnace Maintenance for the PinAAcle 900H 301
You can sometimes remove contamination from the graphite tube by heating the
tube. Heat the graphite tube manually at 2500 °C for approximately 5 seconds.
If there are stubborn deposits in the tube that you cannot remove, discard the
tube and use a new one.
1. Remove the furnace windows (see To remove the windows: on page 318).
2. Open the furnace and remove the graphite tube (see Open the Furnace and
Remove the Graphite Tube on page 296).
3. Use a dry, clean swab to clean the contact surfaces of the graphite tube. If the
surfaces of the graphite tube are pitted or cracked, discard the graphite tube and
use a new one.
4. Use a dry, clean swab to clean the inside of the contacts, especially around the
apertures where the radiation beam enters and exits.
Remove any particles from inside the contacts using a small vacuum cleaner.
Be careful not to scratch the inner surfaces of the contacts.
If the surfaces of the contacts are pitted or cracked, remove the contacts and
install new ones (see Changing the graphite contacts on page 306).
302 Maintenance
5. Insert the graphite tube and close the furnace (see Open the Furnace and
Remove the Graphite Tube on page 296).
6. Refit the windows (see To refit the windows: on page 320).
7. Condition the graphite tube (see Conditioning the graphite tube on page 305).
Changing the graphite tube
2 3
1
Note Do not handle graphite tubes with bare fingers. Perspiration from your
fingers can attack the pyrolytic coating.
Graphite Furnace Maintenance for the PinAAcle 900H 303
1. If required, open the furnace and remove the graphite tube (see Open the
Furnace and Remove the Graphite Tube on page 296).
304 Maintenance
3. Insert the graphite tube and close the furnace (see Open the Furnace and
Remove the Graphite Tube on page 296).
4. If you have installed a new graphite tube, perform the procedure outlined in
Conditioning the graphite tube on page 305.
If you are reusing a previously conditioned graphite tube, heat manually at
2500 °C for 5 seconds to remove surface contamination.
Note Every time you open the furnace, subsequently always heat it out manually
at 2500 °C for approximately 5 seconds.
Note When inserting the graphite tube into the furnace, make certain that the
tube end with the horizontal grooves is at the left. Otherwise sample will
be dispensed onto the wall of the tube and not into the cavity in the
platform.
L'vov platforms can only be inserted into the special graphite tubes with
horizontal grooves. These grooves have limited mechanical stability.
Repeated insertion and removal of integrated platforms causes abrasion, so
that ultimately the platforms will not seat correctly. You must then replace
the tube.
value is too high for this element, heat the tube manually at 2500 °C for 10
seconds and then repeat the ‘dry fire’.
Note Do not heat the graphite furnace for longer than about 10 seconds when the
temperature exceeds 2000 °C. Heating for longer periods will markedly
reduce the lifetime of the graphite tube.
2. In the Furnace Control window, click on the Cleanout Temp. entry field and
type the required temperature (e.g. 2400 °C).
2. Remove the right-hand contact (see To remove the right-hand contact: on page
308).
3. Remove the left-hand contact (see To remove the left-hand contact: on page
311).
4. Install a new left-hand contact (see To install the left-hand contact: on page
313).
5. Install a new right-hand contact (see To install the right-hand contact: on page
315).
6. Insert the graphite tube and close the furnace (see To close the furnace after
contact change: on page 317).
7. Condition the graphite tube (see Conditioning the graphite tube on page 305).
8. Align the furnace (see Aligning the Graphite Furnace on page 186).
9. Align the autosampler (see To Align the Autosampler Tip in the Graphite Tube
on page 145).
Special tools to change the contacts are provided with the furnace. These are
used in different configurations for different procedures as depicted in the
following illustrations.
2. Disconnect the normal gas tube from the inlet manifold on the power
unit:
Carefully push the black locking ring of the connector into the connector
and pull the tube out of the connector. This releases the gas pressure.
3. Pull the right-hand furnace block by hand to the side.
The graphite tube is now accessible.
4. Remove the graphite tube.
Do not touch the graphite tube with bare fingers.
6. Very carefully, using a small screwdriver, lever the graphite shield ring from
the left-hand contact.
right-hand contact and out through the window cavity. The lugs on the
extractor fit over the furnace block.
2. Screw the traction nut with its long side toward the furnace block onto the free
end of the bolt. Position the traction nut so that the flat side on the rim passes
under the optical sensor.
3. Carefully turn the bolt clockwise with the ratchet wrench provided to draw in
the traction nut and thus push the graphite contact out of the furnace block.
2
3
4
1
2. Screw the traction nut with its long side toward the furnace block onto the free
end of the bolt.
Position the traction nut so that the flat side on the rim is facing up.
3. Carefully turn the bolt clockwise with the ratchet wrench provided to draw in
the traction nut and thus push the graphite contact out of the furnace block.
2
1
4
3
2. Pass the bolt from the internal side through the left-hand furnace block and out
through the window cavity.
3. Screw the traction nut with its short side toward the furnace block onto the free
end of the bolt.
Position the traction nut so that the flat side on the rim is facing up.
4. Carefully turn the bolt clockwise with the ratchet wrench provided to draw the
contact into the furnace block. Make certain that the contact is not tilted.
Note Draw the contact firmly into place, but do not apply excessive force
otherwise the contact may shatter.
2 3
4
1
2. Pass the bolt from the internal side through the right-hand furnace block and
out through the window cavity so that the long arm of the alignment gauge rests
against the furnace block.
3. Screw the traction nut with its short side toward the furnace block onto the free
end of the bolt. Position the traction nut so that the flat side on the rim passes
under the optical sensor.
4. Carefully turn the bolt clockwise with the ratchet wrench to draw the contact
into the furnace block.
Make certain that the contact is not tilted.
Note Draw the contact firmly into place, but do not apply excessive force
otherwise the contact may shatter..
5. Disassemble and remove the installation tool. Take care not to scratch or
damage the contact.
316 Maintenance
1 2
3
6. Slide the graphite shield ring with its large flat face toward the furnace block
over the left-hand contact.
2. Reconnect the normal gas tube to the inlet manifold and turn on the gas
supplies for the furnace. The furnace closes.
8. Check alignment of the furnace (see Aligning the Graphite Furnace on page
186).
9. Check alignment of the furnace autosampler (see To Align the Autosampler Tip
in the Graphite Tube on page 145).
2. Dismantle the window assemblies and remove the quartz windows carefully
from the mounts as follows:
1. Carefully pull the collar out of the mount.
2. Carefully push the window out of the mount with a plastic pipet tip.
1 2
3
3. Blow any dust or particles off the surface with clean dry air before you start to
clean a window.
4. Clean the windows carefully with a tuft of cotton moistened with a dilute
solution of mild laboratory detergent.
322 Maintenance
Note To avoid scratching the window, rub the surfaces of the windows as little
as possible. Discard scratched windows..
6. Refit the windows in the furnace (see To refit the windows: on page 320).
Autosampler external Wipe over the surfaces with a lint-free cloth moistened with a dilute solution of
surfaces laboratory detergent.
The autosampler surfaces are resistant to dilute acids and alkalis, and to a lesser
extent to strong acids and alkalis and organic solvents.
AS 900 Furnace Autosampler Maintenance 323
Complete rinsing Fill and flush the rinsing system before the start of every analysis run.
system Flush the rinsing system when you have finished an analysis run.
Valves The valves must function correctly to maintain the precision of the dispensed
volumes. If the precision of the analytical results deteriorates, this can be an
indication that a valve is not functioning correctly.
If a valve seizes or leaks, for example because the pump has been idle for a long
time, or because of particles lodged in the valve, or because of worn seals, you
can remove the valves to clean or change them.
Waste bottle Empty the autosampler waste bottle regularly. Never allow it to overflow or allow
the liquid to reach the end of the drain tube.
If the bottle contains hazardous, toxic, or flammable substances, dispose of the
waste properly, according to the local safety regulations.
Rinse bottle Make sure that the rinse bottle is always filled with clean, particle-free rinsing
liquid.
All tubes Make sure that all the tubes are clean and free from kinks.
Change any tubes that may be damaged or contaminated.
Pipette tip Make sure that the pipette tip is not damaged. If the tip is damaged you may get
pipetting errors during the analyses. Repair the tip or install a new pipette
assembly if necessary.
Pump heads Make sure that the pump heads are not loose. Tighten the pump head retaining
ring if necessary. Make sure that the pump head remains vertical, with the arrow
aligned vertically.
Do not remove the pump heads from the pumps.
3. If there are particles in the rinsing liquid they can lodge in the valves, causing
leaks and non-reproducible results.
Note Make certain there are no air bubbles in the rinsing system. Air bubbles can
lead to non-reproducible results.
6. If you want to use a different rinsing liquid to that already in the rinsing system,
rinse all traces of the previous liquid out of the rinsing system. Use a rinsing
liquid that is miscible with both the new and the old rinsing liquids.
You may have to use intermediate rinsing liquids.
For example, if you are changing from an acidic liquid to an organic solvent,
you could use:
• Deionized water,
• Isopropanol or other water-miscible solvent,
• Final organic solvent.
Valve Maintenance
The autosampler pumps dispense microliter volumes of liquid with high precision.
To maintain this high precision it is essential that the valves function correctly. If
there is a deterioration in the precision of the analytical results, and other sources
of error can be excluded, this is an indication that a valve may not be functioning
correctly.
Only the rinse pump contains valves. The sample pump contains inserts that are a
similar shape to the rinse pump outlet valve.
AS 900 Furnace Autosampler Maintenance 325
Routine Maintenance
The valves require little routine maintenance except to flush them thoroughly
before and after every analysis series.
2. Flush the system well with dilute nitric acid (this step is especially important
for elements with a tendency to carryover).
2. In this dialog, click on Set the depth of the autosampler tip in the sampling
cup. Then select Use the rinse location. The pipet tip rises to a position
directly above the rinsing port.
4. In the Furnace Control window, click on Flush Sampler to start a rinse cycle.
5. The rinsing pump performs three cycles. During the suction phase of each
cycle (pump plunger moves backward) a droplet of rinsing liquid hangs on the
end of the pipet tip; this droplet must remain stationary.
At the end of a rinse cycle the sample pump draws the rinsing liquid droplet
back into the pipet tip.
2. Remove the rinse feed tube briefly from the rinsing liquid so that an air bubble
is drawn in and then replace the tube in the rinsing liquid.
3. Watch the meniscus of the air bubble: It must remain stationary during the
expulsion phase of each cycle (pump plunger moves forward).
4. When you have finished checking the outlet valve, in the In the Furnace
Control window, click on Align Tip.
5. In this dialog (see the previous screen shot), click on Set the depth of the
autosampler tip in the sampling cup. Select Use the rinse location and then
select Next.
6. Adjust the depth control wheel so that the pipet tip is at the correct depth inside
the rinsing port. Then click on Finish.
Note Do not attempt to take the valves apart or repair the valves or to
change individual components inside a valve. If repeated flushing does
not remedy a leaking valve, discard the valve and install a complete, new
valve.
Replacement Parts
Every day you count on PerkinElmer to provide you with solutions that deliver
reliable performance, control operating costs and maximize operational time. Our
complete portfolio of consumables, parts, supplies, training and service helps you
meet both routine and demanding measurement challenges. We invest heavily in
testing and validating our products to ensure you receive guaranteed compatibility
and performance-on-time, every time, for every instrument in your laboratory.
Supplies, replacement parts, and accessories can be ordered directly from
PerkinElmer, using the part numbers quoted in the guides provided with the
instrument.
See our website:
http://perkinelmer.com
328 Maintenance
N3050103 Aluminum
N3050170 N3050670 Antimony
N3050105 N3050605 Arsenic
N3050115 N3050615 Cadmium
N3050114 Calcium
N3050119 Chromium
N3050121 Copper
N3050107 Gold
N3050126 Iron
N3050157 N3050657 Lead
N3050144 Magnesium
N3050145 Manganese
N3050134 N3050634 Mercury
N3050152 Nickel
332 Maintenance
N3050139 Potassium
N3050172 N3050672 Selenium
N3050148 Sodium
N3050191 N3050691 Zinc
Standard Description
Part No.
B0070699 Uncoated graphite tubes (not for use
with L’vov platforms) 50-Pack
B3001253 Uncoated graphite tubes (not for use
with L’vov platforms) 20-Pack
B3001264 Pyrocoated graphite tubes with
integrated platforms 20-Pack
B3001262 Pyrocoated graphite tubes with
integrated platforms 5-Pack
B0109322 Pyrocoated graphite tubes with grooves
for L’vov platforms 50-Pack
B3001254 Pyrocoated graphite tubes with grooves
for L’vov platforms 20-Pack
B0137111 Pyrocoated graphite tubes with grooves
for L’vov platforms 5-Pack
Introduction
PerkinElmer spectrometers are designed for routine, trouble-free operation. Many
errors are diagnosed immediately as they occur and a message containing details
of the problem appears on the screen. Often this information enables you to solve
the problem quickly.
Some difficulties may not be so easily diagnosed and solved. For this purpose, the
following troubleshooting suggestions are included to help you determine whether
the difficulties are due to unsuitable analytical techniques, incorrect instrument
parameters, or a malfunctioning of the instrument. If, after checking the instrument
against the symptoms described below, the instrument appears to be
malfunctioning, we strongly recommend that you contact your local PerkinElmer
service representative.
Performance Problems
Spectrometer
Initialization process fails. Communication cables Make sure that you use the
between the computer, spec- correct cables, and connect
trometer, and accessories are them to the correct communi-
not connected correctly. cation ports. See Connecting
the Computer and Printer on
page 117.
Lamp connector does not fit Lamp is not a PerkinElmer Use the lamps recommended
in the socket. lamp. Lamp is the older series for your spectrometer.
For some older lamps you
may need an adapter cable.
Lamp will not light. Lamp connector not plugged Connect the lamp to the cor-
in. rect socket in the lamp com-
partment.
Lamp old or damaged. Install a new lamp. See
Lamps on page 156.
Lamp energy low or no Lamp starting to deteriorate. Allow the lamp to warm up.
energy. EDL lamps may need 45 min-
utes to warm up. May also
use the maximum current,
within the recommended
range.
Wrong EDL coding plug con- Connect the correct EDL cod-
nected. ing plug to the correct socket.
The lamp is old. Install a new lamp. See
Lamps on page 156.
Performance Problems 341
The current setting is too low Use the Lamp Setup window
or high. to set the correct current. If
the current is too high, start
by reducing the current in
10% steps. With EDLs
reduce the current in 10-20
mA increments.
The system cannot find the EDL coding plug not con- Connect the correct EDL cod-
lamp nected, or the wrong EDL ing plug to the correct socket
coding plug is connected. as described in the user's
guide for your spectrometer.
The lamp is not coded, is an Use the lamps recommended
older lamp, or the lamp is not for your spectrometer.
from PerkinElmer.
Computer System
Computer not communicating Communication cable is not Make sure that you use the
with spectrometer. connected correctly. correct cable, and connect it
to the correct communication
ports.
WinLab32 for AA software is Reconfigure WinLab32 for
in Simulator mode. AA to communicate with the
spectrometer. See the online
help; keyword: Reconfigure.
WinLab32 for AA application Communication cable. Make sure that you use the
stops or hangs correct cable, and connect it
to the correct communication
ports.
Performance Problems 343
Burner System
Flame will not ignite. No fuel or oxidant. Make sure that the fuel and
oxidant gas supplies are
turned on and set at the cor-
rect pressures.
Air has diffused into the fuel You may have to perform the
line while the instrument was ignite cycle a number of times
idle. before all the air is expelled
from the fuel line.
Performance Problems 345
The igniter is not aligned cor- Make sure that the end of the
rectly. igniter moves exactly over the
burner slot and that the burner
head is installed correctly.
See the users guide for the
burner.
Interlocks on the burner sys- Install the burner and drain
tem or drain are open. systems correctly. See the
users guide for the burner.
Flame extinguishes automati- Low gas pressures. Make sure that the fuel and
cally. oxidant gas supplies are
turned on and set at the cor-
rect pressures.
Safety interlocks are open Make sure that the burner sys-
because the burner system has tem is correctly installed and
been changed. all the interlocks are closed.
See Reassembling the Burner
System on page 221.
Flame unstable. Drain system is not operating If there is not a constant,
correctly. smooth flow down the drain
tube, extinguish the flame and
re-install the burner and drain
system correctly. See Drain
System Maintenance on page
224.
Burner head dirty. Clean the burner head. See
Cleaning the Burner Head on
page 214.
346 Troubleshooting
Flashback of flame. Leaks in fuel or oxidant lines, Check for leaks using an
or drain system. approved leak detection kit.
Install the gas lines correctly
using approved components.
Blocked burner slot. Clean the burner head slot.
See Cleaning the Burner
Head on page 214.
Cylinder air contains excess Use compressed air not
oxygen. breathing air, which may be
enriched with oxygen.
Wrong regulators. Use the correct regulator for
each type of gas.
Wrong gases connected. Make sure that the correct
gases are connected to the
correct inlets on the spec-
trometer. See Connecting the
Gases on page 109.
348 Troubleshooting
The furnace does not operate Normal or special gas pres- Make sure the connections
sures too low. and pressures are correct. See
Connecting the Gases on
page 109.
No graphite tube installed, or Insert a new graphite tube.
the tube is defective. See Inserting the Graphite
Tube on page 263.
The contact breaker switch on This switch is activated when
the rear of the spectrometer is the system draws too much
in the OFF position. current. Wait a few moments
before putting this switch to
the on position. If this switch
is activated frequently, call
your local PerkinElmer
office.
Furnace overheats The cooling system is not Wait at least 30 minutes to
switched on or not operating allow the furnace to cool,
correctly. then switch on the cooling
system. If the furnace contin-
ues to overheat, contact your
local PerkinElmer office.
Rapid corrosion of tube Argon flow rate is too low. Set suitable flow rates in each
Make sure that the argon gas step of the furnace program.
(or Nitrogen gas, or any insert Set the correct inlet pressure
gas) is clean and DRY. The for the argon.
supply - piping and tubing, of
this clean and DRY gas to the
furnace must also be clean
and dry.
The drying step is not ade- With WinLab32 for AA, use
quate. Solvent fumes remain the Method Editor to enter a
in and around the tube after suitable furnace program. See
drying, when raising to higher the Recommended Condi-
temperatures of pyrolysis and tions.
atomization.
The samples/solutions ana- Dilute the solutions, to reduce
lyzed may be very corrosive, its corrosiveness, the acid
and/or also contain high con- concentration, and to use
centration of acids, so the appropriate temperature pro-
tube life is shorter. gram that may contain slower
ramp, lower pyrolysis and
atomization temperatures.
Develop equitable tempera-
ture program. Please seek
advice from the PerkinElmer
Product Specialists.
Autosampler does not go to The wrong configuration of Select the correct sample tray
the correct locations. the tray for the autosampler. in WinLab32 > Options >
Furnace Autosampler. See
the online help.
Autosampler does not oper- The communication cable is Make sure that you use the
ate. not connected correctly. correct cable, and connect it
to the correct communication
port.
350 Troubleshooting
Autosampler will not func- The autosampler is not Reconfigure WinLab32 for
tion. entered in the system configu- AA to communicate with the
ration or supported by this spectrometer. See the online
version of software/system. help; keyword: Reconfigure.
Use the system-supported
autosampler.
The autosampler is not If you are using the autosam-
switched on. pler with a controller, switch
this on.
The communication cable is Make sure that you use the
not connected correctly. correct cable, and connect the
cable to the correct communi-
cation port.
Computer cannot communi- FIAS not entered in the sys- Reconfigure WinLab32 for
cate with FIAS. tem configuration AA to communicate with the
spectrometer. See the online
help; keyword: Reconfigure
or the software installation
instructions.
Not switched on. Switch on.
Performance Problems 351
No gas flow. Gas pressure is too low. The Switch off FIAS. If necessary,
gas supply is turned off or connect a new cylinder, then
empty. set the outlet pressure recom-
mended in the user's guide for
the flow-injection system.
Switch on FIAS.
The automatic gas stop is In the FIAS Control window,
active. click on Valve Fill/Inject.
Pump heads stop rotating. The pressure on the pump Use the pressure adjustment
magazines is too high screws to reduce the pressure.
Solution is leaking from the The carrier flow rate exceeds Set the carrier flow rate to be
connections between the the aspiration rate of the neb- about 1-2 mL/min less than
flow-injection system and the ulizer. the aspiration rate of the neb-
nebulizer. ulizer.
352 Troubleshooting
The source lamp or the deute- With WinLab32 for AA, use
rium lamp is failing, or the the Lamp Setup window to
current is too high or too low set the correct current. Install
new lamps. See Lamp Life on
page 250.
Characteristic concentration Wrongly prepared reference Prepare new fresh, correct
is too high. solution or blank. concentration solutions.
Poor sensitivity.
Poor detection limit.
See the sections above on
noisy, erratic signals.
Unsuitable measurement With WinLab32 for AA, use
parameters in the method. the Method Editor to select
suitable measurement param-
eters.
Unsuitable flame conditions. With WinLab32 for AA, use
the Method Editor to select
suitable measurement param-
eters. See the Recom-
mended Conditions.
Burner position is not opti- To optimize the burner; see
mized. the online help.
Nebulizer sample tubing is Install new tubing of the cor-
too long. rect length. With WinLab32
for AA, use the Method Edi-
tor to select suitable values
for the read time and read
delay. See Nebulizer Removal
and Reinstallation on page
230.
354 Troubleshooting
The lamp current is too high With WinLab32 for AA, use
(line broadening) or too low. the Lamp Setup window to
set the correct current.
A low-sensitivity wavelength With WinLab32 for AA, use
is selected. the Method Editor to select
the correct wavelength. See
the Recommended Condi-
tions.
Poor sensitivity. Characteris- Wrongly prepared reference Prepare new standard solu-
tic mass is too high. solution or blank. tions correctly.
The standard solutions are too Prepare new standard solu-
"old" - solutions not prepared tions correctly.
fresh daily.
The standard and reference Prepare fresh acidified solu-
solutions are not acidified. tion daily.
The elements may drop out of
the solution.
See the sections on bad preci-
sion and erratic signals.
Performance Problems 355
Poor sensitivity. Characteris- Unsuitable time/temperature With WinLab32 for AA, use
tic mass is too high (contin- program in the method. the Method Editor to enter a
ued). suitable furnace program. See
the Recommended Condi-
tions. If this does not work,
seek advice from the Perki-
nElmer Product specialists.
Poor contact between the Clean the contact faces of the
graphite tube and the con- graphite tube and the con-
tacts. tacts. If the contacts show
signs of pitting or cracks,
replace them. Install a new
graphite tube and/or contact
cylinders if the change in the
tube does not resolve the
issue. See Inserting the
Graphite Tube on page 263.
Analyte has been lost during Use a lower pyrolysis temper-
the pyrolysis step. ature, especially if you are not
using a matrix modifier.
Unsuitable measurement With WinLab32 for AA, use
parameters in the method. the Method Editor to select
suitable measurement param-
eters. See the Recom-
mended Conditions.
Gas flow during atomization Use zero flow during the
too high. atomization step. Select this
on the Furnace page in the
Method Editor.
Low sensitivity wavelength Select the correct wavelength
selected. on the Instrument page in the
Method Editor. See the Rec-
ommended Conditions.
356 Troubleshooting
Poor sensitivity. Characteris- Graphite tube is old or faulty. Install a new tube.
tic mass is too high (contin-
ued).
The lamp current is too high With WinLab32 for AA, use
or too low. the Lamp Setup window to
set the correct current.
Old or faulty lamp. Use a new lamp.
Unsuitable sample volume. For example, a volume of 5
uL will spread out less than
50 uL, which can affect the
sensitivity.
Accurate volume dispensed. Ensure that the autosampler
Dirty autosampler probe probe (pipette tip) is clean,
(Pipette tip), such that the and also the volume dis-
volume dispensed is lower pensed is accurate.
than intended, so resulting in
lower signal, so higher char-
acteristic mass.
Characteristic mass is too The reference solution or sol- Prepare new fresh standard
low. vent is contaminated. solutions accurately.
Signal is too high.
Performance Problems 357
Very high blank signal for a Graphite tube or contacts are Install a new tube, and if nec-
dry firing contaminated. essary, new contacts. See
Inserting the Graphite Tube
on page 263.
Increased background signal Build up of matrix due to Increase the clean-out tem-
after several replicates inadequate clean-out. perature or time. Make a dry
firing to measure the signal.
Temperature above 2500 °C
for periods longer then 10
seconds will decrease the life-
time of the tube.
Poor precision The autosampler pipet tip is Make sure that the pipet tip
not aligned correctly. injects the solution at the cor-
rect place within the graphite
tube. Make sure that the pipet
tip enters the solution in the
sample cup. See AS 900 Fur-
nace Autosampler Mainte-
nance on page 322 or the
online help.
The autosampler probe is not Flush the inside and outside
clean. of the autosampler probe with
isopropyl alcohol for five
minutes before re-use. Should
consider to add 1% methanol
in the rinsing solution for rou-
tine operation.
Large symmetrical double A chemical modifier or lower
peak could also mean roll- atomization temperature may
over, indication of exceed- eliminate this problem.
ingly high concentration, for
Zeeman background correc-
tion system.
Performance Problems 359
Poor precision Lamp current is too low. Old See Troubleshooting: Spec-
or faulty lamp. trometer on page 340.
Build up of matrix due to Increase the clean-out tem-
inadequate clean-out. perature or time. Make a dry
firing to measure the signal.
Temperature above 2500 °C
for periods longer then 10
seconds will decrease the life-
time of the tube.
Spattering during the drying With WinLab32 for AA, use
or pyrolysis step. the Method Editor to
increase the ramp time for the
step.
Optimize the temperatures.
Spattering when the sample is The tube is too hot. With
injected. WinLab32 for AA, use the
Method Editor to set the
injection temperature for the
tube. Make sure that the cool-
ing system cools the tube to
the correct temperature before
the autosampler injects the
next sample.
Samples are highly acidic Acidic samples cause more
rapid degredation of the tube.
High acid concentrations
have an influence on the opti-
mal drying temperature.
Samples are in an organic sol- Organic solvents require indi-
vent. vidually optimized drying
temperatures.
360 Troubleshooting
Leaks in the fluid system. Make sure that all the connec-
tions are tight. Tighten them
by hand or with the tube con-
nector key. Do not over-
tighten or distort the
connectors. If necessary,
install new connectors.
Performance Problems 363
The first replicate of a series The Fill step in the FIAS pro- With WinLab32 for AA, use
gives a high reading. grams is too short. the Method Editor to increase
the time for the Fill step in the
FIAS program.
The first replicate of a series The Prefill step in the FIAS Use the Method Editor to
gives a low reading. programs is too short. increase the time for the Pre-
fill step in the FIAS program.
If possible, use a shorter tube
between the sample container
and the FIAS-valve.
Baseline shift. Air is trapped in the system. Make sure that all the connec-
tions are tight. Tighten them
by hand or with the tube con-
nector key. Do not over-
tighten or distort the
connectors. If necessary,
install new connectors. Flush
the fluid system thoroughly to
remove trapped air.
Double peaks - FIAS MHS. The concentration of the ana- Dilute the samples.
lyte is too high.
The temperature of the quartz See the Recommended Con-
tube is too low for atomiza- ditions. Use the Method Edi-
tion to occur. tor to set the correct
temperature on the FIAS
page. If necessary, increase
the temperature setting
slightly.
366 Troubleshooting
Air is trapped in, or entering Make sure that all the connec-
the fluid system. tions are tight. Tighten them
by hand or with the tube con-
nector key. Do not over-
tighten or distort the
connectors. If necessary,
install new connectors. Flush
the fluid system thoroughly to
remove trapped air.
The carrier or reductant flow Make sure that the feed tubes
rates are wrong. for the carrier and reductant
are in the correct containers.
Set the correct flow rates as
described in the users guide
for the flow-injection system
or the online help.
No acid in the sample solu- See the Recommended Con-
tions, or the acid concentra- ditions. Use more concen-
tion is too low. trated or more acid in the
sample solutions.
Index: A I-1
Flashbacks 28 G
Flow Injection Autosampler Gas Connectors 81
troubleshooting 350 Gas Controls 88
Flow Injection System Gas Cylinders
troubleshooting 350 handling 24
Flow Injection Technique identiying 22
troubleshooting 362 safe handling 22
Fume Ventilation 41 safety 53
Furnace storing 23
closing after contact change 289, 317 Gas Delivery Lines
opening for contact change 307 safety 53
troubleshooting 348 Gas Hazards
Furnace Analysis Technique summary 21
troubleshooting 354 Gas Requirements 52
Furnace Autosampler 94 Graphite Contact Surfaces
troubleshooting 348 cleaning 269, 301
Furnace Gas Requirements 55 Graphite Contacts
Furnace Gases changing 306
connecting 112 cleaning 300
Furnace System Graphite Furnace
shut down 191 high temperatures 19
Zeeman Graphite 18 maintenance for the PinAAcle 900H
Furnace Technique 296
setting up for the PinAAcle H 184 Graphite Furnace Atomizer 93
setting up for the PinAAcle T/Z 181 Graphite Furnace Maintenance 260
troubleshooting 354 Graphite Shield Ring
Furnace Windows installing 305
cleaning 293, 321 Graphite Tube
refitting 320 changing for the PinAAcle 900H 302
removing 318 cleaning 267, 300
Fuses conditioning 291
changing 206 conditioning for the PinAAcle 900H
safety 6 305
heating manually 292
inserting 263
removing contamination by heating 301
I-4 Index: H
WEEE Instructions 34
Weights 39
Windows
cleaning 321
refitting 320
removing 318
PerkinElmer, Inc.
710 Bridgeport Avenue
Shelton, CT 06484-4794, U.S.A.
Internet: http://www.perkinelmer.com
email: info@perkinelmer.com