Академический Документы
Профессиональный Документы
Культура Документы
Release History
Part Number
Release
09936667
Publication Date
December 2003
Any comments about the documentation for this product should be addressed to:
PerkinElmer Inc.
710 Bridgeport Avenue
Shelton
Connecticut 06484-4794
U.S.A.
Or emailed to: info@perkinelmer.com
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 particular
purpose.
PerkinElmer shall not be liable for errors contained herein for incidental consequential
damages in connection with furnishing, performance or use of this material.
Copyright Information
This document contains proprietary information that is protected by copyright.
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 Instruments Inc.
Copyright 2003 PerkinElmer Instruments Inc.
Trademarks
Registered names, trademarks, etc. used in this document, even when not specifically
marked as such, are protected by law.
PerkinElmer is a registered trademark of PerkinElmer, Inc.
e-ssentials is a trademark of PerkinElmer, Inc.
Table of Contents
Chapter 1 Introduction
About This Manual.................................................................................. 1
Conventions Used in this Manual.............................................................. 2
Notes, cautions and warnings ............................................................. 2
Warning Signs on the Instrument .............................................................. 3
Chapter 2 Safety Practices
Chapter Overview.................................................................................... 5
Safety Conventions .................................................................................. 6
Correct use of the instrument ............................................................. 7
Precautions.............................................................................................. 8
Environmental Conditions ........................................................................ 9
Electrical Safety .....................................................................................10
Safe Handling of Gas Cylinders...............................................................12
Identification of Gas Cylinders..........................................................12
Storing Cylinders .............................................................................13
Handling Cylinders ..........................................................................14
Handling compressed gases ..............................................................15
Operating Conditions ..............................................................................16
Laboratory hygiene ..........................................................................17
Laboratory ventilation ......................................................................17
Waste disposal.................................................................................17
Safe handling of chemicals ......................................................................18
Safety practices for electrothermal atomization .........................................20
Safety interlocks ..............................................................................20
Hazards with electrothermal atomization ...........................................21
References for laboratory safety practice..................................................22
Regulatory information ...........................................................................23
Electrical protection .........................................................................23
Electromagnetic compatibility (EMC) ...............................................24
Symbols used on the instrument...............................................................25
Warning markings on the instrument........................................................26
Warning markings on the graphite furnace.........................................26
Warning markings on the power unit .................................................27
Table of Contents
ii
iii
Table of Contents
iv
Introduction
Introduction
All eight digit numbers are PerkinElmer part numbers unless stated otherwise.
CAUTION
We use the term CAUTION to inform you about situations that could result in
serious damage to the instrument or other equipment. Details about these
circumstances are in a box like this one.
We use the term WARNING to inform you about situations that could result in
personal injury to yourself or other persons. Details about these
circumstances are in a box like this one.
WARNING
Introduction
Safety Practices
Chapter Overview
This chapter describes the general safety practices and precautions that must be
observed when operating the HGA 900.
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 HGA 900 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.
Safety Practices
Safety Conventions
Possible hazards that could harm the user or result in damage to the instrument
are clearly stated at appropriate places throughout this manual.
Translations of the warning messages used in this guide are given in Chapter 8,
Warnings.
The following safety conventions are used:
This symbol alerts you to situations that could result in personal
injury to yourself or other persons.
WARNING
This symbol alerts you to the risk of electric shock that could result in
personal injury to yourself or other persons.
Details about these circumstances are in a box like this one.
This symbol alerts you to the risk of hot surfaces that could cause
personal injury to yourself or other persons.
Details about these circumstances are in a box like this one.
This symbol alerts you to the risk of ultraviolet radiation that could
cause eye damage to yourself or other persons.
Details about these circumstances are in a box like this one.
CAUTION
Safety Practices
Precautions
Be sure that all instrument operators read and understand the
precautions listed below. It is advisable to post a copy of the
precautions near or on the instrument shelf.
WARNING
The following precautions must be observed when using the HGA 900:
Be sure that the voltage of the HGA 900 corresponds to the voltage used in
your laboratory.
Never remove the side panels of the HGA 900 without shutting down the
instrument and disconnecting the instrument power cord from line power.
Do not immerse the purge gas exit line in a liquid, as the liquid may be
drawn back into the sample holder.
Only high quality purge gases should be used with the HGA 900. Minimum
purity of 99.9% is recommended. A high quality filter-dryer accessory is
recommended for the removal of any moisture from the purge gases.
Environmental Conditions
The instrument should be used indoors in a laboratory having the environmental
conditions as recommended in the Installation chapter (Chapter 5) in this guide.
Safety Practices
Electrical Safety
The instrument has been designed to protect the operator from potential electrical
hazards. This section describes some recommended electrical safety practices.
WARNING
WARNING
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.
10
Disconnect the instrument from all voltage sources before changing any
fuses.
NOTE: The HGA 900 power unit is provided with an operational on/off switch and with
a circuit breaker. The operational on/off switch turns the instrument on and off,
but it does not disconnect the instrument from the line power supply. The circuit
breaker functions as a disconnecting device and disconnects the instrument
entirely from the line power supply.
Further information on these two switches is provided in chapter 5,
Installation, the section called Electrical connectors and switches.
11
Safety Practices
WARNING
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.
NOTE: The permanent installation of gas supplies is the responsibility of the user and
should conform to local safety and building codes.
If liquid argon or nitrogen is used, the gas cylinder must be fitted with an overpressure regulator, which will vent the cylinder as necessary to prevent it from
becoming a safety hazard.
Listed below are some general safety practices for the proper identification,
storage, and handling of gas cylinders. Consult the following references for more
detailed information and additional guidelines.
12
Legibly mark cylinders to identify their contents. Use the chemical name or
commercially accepted name for the gas.
Storing Cylinders
Review the following precautions with the customer to ensure the safe use and
storage of gas cylinders.
When cylinders are stored indoors in storage rooms, the storage room
should be well ventilated and dry. Ensure that the ventilation is adequate to
prevent the formation of dangerous accumulations of gas. This is
particularly important in small or confined areas.
Use and store cylinders away from exits and exit routes.
Locate cylinders away from heat sources, including heat lamps. Compressed
gas cylinders should not be subjected to temperatures above 52 C (126 F).
Do not allow ignition sources in the storage area and keep cylinders away
from readily ignitable substances such as gasoline or waste, or combustibles
in bulk, including oil.
Mark gas cylinders clearly to identify the contents and status (full, empty,
etc.).
Arrange gas hoses where they will not be damaged or stepped and where
things will not be dropped on them.
Perform periodic gas leak tests by applying a soap solution to all joints and
seals.
13
Safety Practices
Handling Cylinders
Review the following precautions with the customer to ensure the safe use and
handling of gas cylinders.
Arrange gas hoses where they will not be damaged or stepped on and where
objects will not be dropped on them.
Check the condition of pipes, hoses and connectors regularly. Perform gas
leak tests at all joints and seals of the gas system regularly, using an
approved gas leak detection 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.
14
Gas
Suffocation
Explosion
Spontaneous Decomposition
or Combustion
Argon
Nitrogen
Contact the gas supplier for a Material Safety Data Sheet containing detailed
information on the potential hazards associated with the gas.
15
Safety Practices
Operating Conditions
Warning: Explosive Atmosphere
This instrument is not designed to operate in an explosive atmosphere.
WARNING
The instrument will operate correctly under the following conditions:
Indoors.
Indoor
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.
16
Laboratory hygiene
Keep the work area scrupulously clean to avoid contaminating your samples
and to maintain a safe working environment. Clean up spilled chemicals
immediately and dispose of them properly.
Laboratory ventilation
Toxic combustion products, metal vapor, ozone, etc., can be generated by the
system, depending on the type of analyses being performed.
Waste disposal
Contents of waste containers
The materials that you collect in waste containers may include small amounts of
the substances that were analyzed and other chemicals used in the analyses. If
these materials are toxic, corrosive, or contain organics you may have to treat the
collected effluent as hazardous waste. Refer to your local safety regulations for
proper disposal procedures.
17
Safety Practices
CAUTION
Depending on the types of chemicals you are handling, wear safety glasses
with side shields, or goggles, or a full-face shield.
Responsible body: individual or group responsible for the use and maintenance of equipment, and
for ensuring that operators are adequately trained.
Operator: person operating equipment for its intended purpose.
18
19
Safety Practices
Do not attempt to defeat these interlocks; you may compromise your own,
or someone elses, safety.
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 inert gas supply is connected and set to the correct pressure;
20
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 HGA graphite furnace can generate temperatures of up to 3000 C
To avoid serious burns, never touch the graphite components until the
furnace has cooled to room temperature.
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.
21
Safety Practices
22
Regulatory information
This instrument has been designed to comply with a wide variety of international
standards governing the safety of laboratory equipment. In routine use, the
instrument poses virtually no risk to you. If you take some simple, commonsense precautions, you can maintain the continued safe operation of the
instrument.
Electrical protection
Insulation
Class I as defined in IEC 1010-1.
Installation category
This instrument is able to withstand transient overvoltage according to
Installation Category II as defined in IEC 1010-1 and IEC 664.
Pollution degree
This equipment will operate safely in environments that contain nonconductive
foreign matter and condensation up to Pollution Degree 2 as defined in IEC
1010-1 and IEC 664.
23
Safety Practices
24
This symbol indicates the off position of the 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 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.
This symbol indicates the operational on/off switch. This switch
turns the instrument on and off, but it does not disconnect the
instrument from the line power supply.
This symbol indicates alternating current.
25
Safety Practices
A
Risk of hot surfaces
Risque de surfaces chaudes
Gefahr durch heisse Oberflchen
Safety/Regulatory Information
26
B
Power outlets
Power outlets for a printer, computer, or monitor.
Only connect a printer, a computer, or a monitor to the respective power outlet
when the equipment requires 230 V AC, 50/60 Hz.
C
Cooling system outlet
Connect the cooling system to this power outlet only.
Do not connect the cooling system to any other supply.
Do not connect other equipment to this power outlet.
27
Safety Practices
28
Preparing Your
Laboratory
Chapter Overview
The items shown in the following checklist need to be considered when preparing
the laboratory for the HGA 900.
Electrical requirements
Operating conditions
29
Electrical requirements
The HGA 900 graphite furnace requires a stable electrical supply of 230 V,
50 Hz or 60 Hz, capable of delivering 16 A, that has a correctly wired protective
earthling system (ground connection).
The line power cable has a 3-pole connector (line + neutral + protective earth),
conforming to IEC 309-2, rated for 16 A. The cable is 3 meters long.
The line power supply should be free of line transients in excess of 50 V peak. If
the electrical supply voltage produces large AC line voltage fluctuations, a
qualified electrician should install a voltage regulator between the electrical
outlet and the instrument.
The power demand of the graphite furnace is approximately 3600 VA, the
maximum graphite tube temperature is 3000 C. Monitoring of the energy
required for each user-defined furnace program reliably prevents the line power
supply from being overloaded.
The line power supply point must be within 3 meters of the rear of the
spectrometer.
We recommend that you connect the spectrometer, computer, printer, and any
accessories to the same phase of the line power supply and the same protective
earth.
The line power supply must conform with local safety regulations and be
checked by a qualified electrician before you connect the instrument to line
power.
See the guides for the computer and printer and any other instruments for
information about their power requirements.
30
Operating conditions
Warning: Explosive Atmosphere
This instrument is not designed for operation in an explosive atmosphere.
WARNING
Operating requirements
The instrument will operate correctly under the following conditions:
Indoors.
31
Position the bench or trolley out of direct sunlight and away from
radiators and heaters.
Position the system near to the electricity and gas supply points, and
close to a source of cooling water.
Make sure that there is space at the rear and sides of the system for air to
circulate freely.
Make sure that there is sufficient room for you to work comfortably with
the instruments, and that you can reach the connections at the rear of the
instruments and the electricity and gas supply points.
Fume ventilation
You must provide an efficient fume ventilation system to remove the fumes
generated by the atomizer.
The specification for a suitable system is described in brochure no. L-301
Preparing Your Laboratory for PerkinElmer Atomic Spectroscopy Instruments.
This brochure is available from PerkinElmer.
Warning: Toxic Gases Fume Ventilation System
WARNING
32
You laboratory must have a reliable fume ventilation system before you
use this instrument.
The user must provide the gas supplies, regulators, connectors, and
valves.
Either the gas supplier or PerkinElmer can supply the correct regulators
and valves.
You must be able to reach the on/off valves easily and see the pressure
indicators.
WARNING
Always handle gas cylinders with the caution and observe your local
regulations for the safe handling of gas cylinders.
Furnace gases
Inert gas
The graphite furnace requires a supply of inert gas to prevent the tube and the
analyte atoms from being oxidized when the tube is heated.
Argon is the recommended inert gas.
If you cannot obtain argon, you can use purified nitrogen, but nitrogen does not
provide such efficient protection as argon at temperatures above 2000 C.
Nitrogen can also react with the samples and the graphite tube at typical
atomization temperatures.
33
WARNING
Make sure that the main laboratory fume ventilation system removes
all gases and fumes emitted by the furnace.
Special gas
For some applications you may want to use a special gas. A typical example is
the use of air during one of the pyrolysis steps to better ash organic materials.
Table 3-1 Specifications and Requirements of the Furnace Gases
Gas
Purity
P min
P max
P min
P max
99.996%
350
400
3.5
4.0
50.0
58.0
1.2
Nitrogen 99.996%
350
400
3.5
4.0
50.0
58.0
1.2
400
3.5
4.0
50.0
58.0
1.2
Argon
Special
bar
Max.
flow rate
L/min
psig
Set the outlet gauge pressure for each gas to a value just below the maximum
value (Pmax).
Never set the outlet pressure for each gas to a value exceeding the maximum
(Pmax).
34
Cooling system
PerkinElmer offers a recirculating cooling system; it is provided with one version
of the HGA 900 system and can also be purchased as an option. It provides
coolant at a constant temperature and flow rate, to allow the most reproducible
analytical conditions. It also makes the system independent of external water
supplies and saves water (see chapter 4, System Description for more
information). This cooling system includes a pressure-sensitive safety device that
opens a bypass if the internal pressure in the circulatory system increases to
above a safe value.
Power requirements: 230 V; 50/60 Hz (electrical power is supplied by the HGA
900 power unit).
Part Number: B019-8072
External cooling
If you intend to run the graphite furnace without the PerkinElmer cooling system,
you must connect another suitable source of cooling, such as the main water
supply or a laboratory thermostat. If you connect the HGA 900 system to the
main water supply, make sure that the water meets the requirements given in
Table 3-2.
35
Temperature
20-40 C
Flow rate
Pressure
pH
Hardness
36
37
38
System Description
Major Components
Furnace design
The HGA 900 is a longitudinally-heated graphite furnace for electrothermal
atomization in atomic absorption spectrometry. The furnace is heated electrically.
The voltage is applied along the graphite tube, parallel to the radiation beam.
The HGA 900 system is comprised of a graphite furnace with a power unit, and
an AS-800 autosampler. The system mounts at the left-hand end of the
spectrometer. The graphite furnaceautosampler assembly is mounted on a swing
arm at the front of the power unit. The swing arm allows you to move the
graphite furnace autosampler assembly from the standby position in front of the
power unit into the spectrometers atomizer compartment. Alignment controls on
the furnace enable you to align the furnace accurately in the spectrometers
radiation beam.
The power unit houses the power supply, system electronics, and the inert gas
control pneumatics for the furnace. The power unit is connected to the furnace
via a flexible conduit which carries the electrical cables and the gas and water
tubes. The gas and electrical supplies for the furnace are controlled from the
power unit.
The HGA 900 system does not have any operating controls (except for the
electrical on/off switch). Control is via the same software that is used to control
the spectrometer system.
39
System Description
40
41
System Description
Temperature control
The temperature regulation system of the HGA 900 continuously monitors the
effective voltage across the tube and uses this together with the initial and final
temperatures to control the heating during program steps other than atomization.
During maximum power heating, the emission temperature of the tube, measured
by an optical sensor, is also used to control the heating.
42
The inert gas that prevents the graphite tube and sample from oxidizing
at high furnace temperatures.
The pneumatic pressure that holds the furnace closed and ensures that the
graphite tube makes good electrical contact with the graphite contacts.
Even when the spectrometer is switched off, the furnace is held closed if
there is pressure in the gas supply line. If you release the pressure in the
lines you can open the furnace.
The Special Gas inlet supplies the furnace with a special purge gas during some
steps of a furnace program. This is optional but is useful for particular
applications; for example, air may produce more effective ashing of organic
materials.
The gas connections are located at the front of the power unit, behind the cover
panel.
NOTE: The furnace will operate correctly only if there is gas pressure at both gas inlets.
If you are not using a special gas, you must connect the inert gas to both inlets
using the Y-connector provided.
43
System Description
44
also use a special gas for the internal gas flow. This is optional but is useful for
particular applications. For example, air may produce more effective ashing of
organic materials.
For each step of the furnace program you must select either the inert gas or the
special gas and the required flow rate.
The flow values are valid for argon. If you use nitrogen, the actual flow rate will
differ slightly from the values indicated.
During each step of the furnace program the gas flows at the rate specified for
that step. For any step where you specify a lower flow rate than that for the
previous step, the system reduces the flow five seconds before the step starts.
This ensures that the flow is stable when the step starts.
Selecting zero flow for the atomization step ensures that the graphite tube and
sample are in thermal equilibrium; an important requirement of the STPF
concept.
Inert gas
Argon is the recommended inert gas. It does not react with either the graphite
tube or the sample at the temperatures used in the furnace.
Although nitrogen can be used, it is not recommended as an inert gas for the
furnace. It can react both with the graphite tube and samples at normal
atomization temperatures. Nitrogen does not provide such efficient protection for
the graphite tube as argon at temperatures above 2000 C and can react with the
graphite tube to form toxic cyanogen gas, (CN)2, at temperatures above 2300 C.
45
System Description
Cooling system
PerkinElmer offers a recirculating cooling system. It provides coolant at a
constant temperature and flow, to allow the most reproducible analytical
conditions. It also makes the system independent of external water supplies and
saves water. Electrical power to the cooling system is provided by the power
unit. The system shuts down automatically if the furnace has been idle for more
than 10 minutes.
The cooling system uses a 1:10 solution of glycerol in sediment-free drinking
water.
The cooling system also includes a pressure-sensitive safety device. If the
pressure in the circulatory system increases to above a factory-preset value an
internal bypass opens. This feature eliminates the risk of damage to the furnace
system through excess pressure. A pressure increase could be caused, for
example, if one of the hoses is kinked.
46
Technical data
Graphite furnace
Principle
Longitudinally-heated graphite furnace for electrothermal
atomization.
Temperature range Ambient temperature (20 C) to 3000 C, programmable in steps of
10 C.
Heating rate
Programmable up to approx. 2000 C/s (maximum power heating).
Gas requirements
Inert gas supply required for operation (not provided); argon
recommended. A second, special gas can also be used.
Automatic gas shutdown when the furnace has been idle for 10
minutes.
Pressure: 350400 kPa (3.54 bar, 5158 psig) Gas flow: max. 1200
mL/min
Gas flows
Internal flow, selectable flow rates: 2x 0, 10, 160 mL/min
External flow, fixed: 2 x 450 mL/min
Cooling
Sediment-free drinking water.
Water consumption: max. 2.5 L/min
Water pressure: max. 3.5 bar (350 kPa, 50 psig)
The use of the (optional) Recirculating Cooling System is
recommended (see earlier in this chapter and chapter 7,
Maintenance, for more information).
Furnace program
Up to twelve independent steps.
Parameters: Isothermal temperature holding time: 099 s, in steps of
1s
Isothermal temperature: 203000 C in steps of 10 C. Heating rate:
programmable, time-dependent or maximum power.
Internal gas flow
Read delay
Read time
Power
230 V; 50/60 Hz; power consumption 3600 VA
requirements
47
System Description
Safety features
Electrical
protection
Technical
standards
48
Environmental
requirements
Dimensions
Mass (weight)
Cooling System
Principle
Self-priming recirculating system with fan-assisted heat exchanger.
Coolant
1:10 mixture of glycerol in sediment-free drinking water.
Volume
Approx. 5 L
Water
Output: 36 C 5 C
temperature
Inlet max: 90 C
Fan cut-in temp: 40 C
Flow
2.5 L/min
3
Air flow
Approx. 400 m /hour
Water pressure 300 kPa, (3 bar, 43 psig). Pressure-sensitive safety device opens if the
internal pressure increases to above a factory-preset value.
Connections
Reinforced hose, i.d. 8 mm; automatic connectors with integral shut-off
valves.
Power
230 V, 50/60 Hz, Power consumption: approx. 140 VA
requirements
Technical
Classified as a laboratory instrument accessory. Complies with the
standards
applicable European Union directives and standards for safety and
electromagnetic compatibility for CE marking. Complies with the
applicable Canadian standards for safety for CSA/NRTL marking. The
instrument has been developed and is produced in compliance with ISO
9001.
Dimensions
Width: 200 mm
Height: 375 mm
Depth: 500 mm
Mass (weight)
Approx. 18 kg with coolant.
49
System Description
50
The sample tray sits in the sample tray trough, which has a plastic cover. The
cover protects the samples from contamination and reduces the rate of
evaporation of the solvent. You can reduce the rate of evaporation further by
pouring a small volume of water into the sample tray trough.
The sample tray is removable. It is useful to have several trays so that you can
load trays while one tray of samples is being analyzed.
There are two types of sample tray available, with either 88 or 148 locations for
samples and reagents.
51
System Description
52
53
System Description
To pipet some or all of the solutions one after another and inject them
into the graphite tube together.
54
6. The autosampler arm swings over to the graphite furnace and injects
the solutions into the graphite tube.
7. The autosampler arm swings back to the sample table and
simultaneously the movable plate positions the rinsing port at the
pipetting location. The rinse pump rinses the pipet tip with rinsing
liquid.
8. Steps 3 through 7 are repeated for each step of the analysis program
that requires solutions to be pipetted.
9. When all the solutions have been injected into the graphite tube, the
pipet tip returns to the rinsing port and the rinse pump rinses the
pipet tip with rinsing liquid.
10. The furnace program continues to the end and the analyte signal is
measured.
11. The preceding steps are carried out for each replicate of every
sample and calibration solution.
55
System Description
Technical data
AS-800 furnace Autosampler
Principle
Random access furnace autosampler with programmable
sample volume.
Can combine and dilute solutions automatically in the
graphite tube and produce calibration solutions from a stock
solution.
Control
From the spectrometers application program.
Sample trays
Removable trays with 88 and 148 locations.
Rinsing
A rinsing port is integrated with the sample table. This
rinses the inside and outside of the pipet tip.
Minimum required 0.1 mL
sample volume
Pipetted volume
Minimum: 1.0 L; maximum: 99 L.
For the best precision a minimum of 5 L is recommended.
Maximum = volume of one solution or the sum of individual
solution volumes pipetted together; for example: [sample +
matrix modifier + diluent
+ air bubble volumes].
Power
The autosampler draws its power from the furnace power
requirements
unit.
Safety and
As defined in EN 61010-1-1993 (IEC 1010-1: 1990 + A1 +
EMC standards
A2) and EN 61010-2-061:1996.
Electromagnetic compatibility: EN 61326-1:1997.
Environmental
Ambient temperature +15 C to +35 C (+59 F to +95 F),
requirements
with a maximum change not exceeding 2.8 C (5 F) per
hour.
2080% relative humidity; non-condensing.
Dimensions
Width: 270 mm
Height: 200 mm
Depth: 340 mm
Mass
approx. 6 kg
(weight)
56
57
System Description
58
Installation
WARNING
Visually check the HGA 900 and any other equipment for obvious signs
of damage. If you find that something is damaged, file a claim with the
authorized carrier immediately and inform your local PerkinElmer office.
59
Installation
Although you should not attempt to install the HGA 900 on the spectrometer
yourself, we recommend that you read the installation instructions to learn about
the HGA 900 and its requirements before you start using it.
Warning: Risk of injury
WARNING
Never move the graphite furnace away from the standby position
when the HGA 900 System is not bolted to the spectrometer.
60
61
Installation
62
4. Pass the long-head bolt through the hole in the casting and tighten with a
7 mm socket wrench. You may have to maneuver the HGA 900 system
slightly until the holes line up before you can tighten the long-head bolt.
Make sure that there is enough space at the rear and sides of the
spectrometer/ HGA 900 system for air to circulate freely.
63
Installation
64
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.
0992-3183.
The gas supply systems must comply with your local safety regulations.
Refer also to the information given in chapter 2, Safety Practices.
What is provided with the HGA 900 system:
65
Installation
3. 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.
4. Connect the long gas tube to the argon (or nitrogen) pressure regulator. Use a
connector or adapter suitable for the gas regulator. Make sure that all the
connections are secure.
5. Pass the gas tube to the front of the power unit. Make sure that it cannot be
damaged or strained.
6. Push the two short tubes and the long tube into the connectors on the Yconnector as shown on the following page.
7. Push the free ends of the two short gas 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: Turn the gas off at the tank.
Carefully push the black locking ring of the connector into the connector and
pull the tube out of the connector.
8. Replace the front panel (see the procedure earlier in this chapter).
66
67
Installation
68
69
Installation
There is space at the rear and sides of the cooling system for air
to circulate freely.
3. Pass the two hoses from the cooling system to the front of the power unit.
Make sure they are not strained.
4. Push the hose connectors onto the correct fittings on the spectrometer as
shown on the following page.
The connectors are spring loaded. Push them straight onto the fittings until
they click into place.
70
Figure 5-6 Connecting the cooling system to the power unit (front of
instrument)
71
Installation
72
If the water inlet pressure is too high, hose fittings may leak or hoses
may even burst.
For reliable and safe operation, you must install the pressure
relief valve kit B313-0124 in the water supply line.
The hoses provided in the kit are fitted with automatic connectors that
incorporate stop valves; these valves prevent water from running out when the
hoses are disconnected. The hoses are marked with the direction of the water
flow.
73
Installation
Pmin
Pmax
250
350
kPa
2.5
3.5
bar
36
50
psig
Check the water pressure to your laboratory and make sure that the water
inlet pressure is set to a value between the minimum value (Pmin) and the
maximum value (Pmax).
Make sure that the outlet pressure is never set to a value exceeding the
maximum pressure (Pmax).
1. The PerkinElmer service engineer will connect the pressure relief valve to
the water tap (faucet).
2. Make sure that the drain hose from the pressure relief valve hangs down into
a suitable laboratory sink or drain.
3. Remove the front panel of the power unit (see the procedure earlier in this
chapter).
4. Connect the inlet hose (marked WATER IN) to the fitting at the bottom of
the pressure relief valve.
5. Connect the other end of the inlet hose to the fitting marked H2O In on the
HGA 900 power unit.
The connectors are spring loaded. Push them straight onto the fittings until
they click into place.
74
6. Connect the outlet hose (marked WATER OUT) to the fitting marked H2O
Out on the HGA 900 power unit.
NOTE: To disconnect the water hoses:
Carefully pull the knurled locking ring down slightly, to release the lock, and pull
the connector off the fitting on the power unit.
7. We recommend that you fit a proprietary flow indicator in the outlet hose so
that you can easily monitor that cooling water is flowing.
8. Place the free end of the outlet hose in a suitable laboratory sink or drain.
Make sure that the hose cannot slip out.
9. Replace the front panel (see the procedure earlier in this chapter).
Figure 5-8 Connecting the main water supply to the power unit (front of
instrument)
75
Installation
76
5. Position the waste bottle so that when you move the graphite furnace
assembly into and out of the atomizer compartment the drain tube does not
pull out of the bottle or catch on any objects.
Figure 5-9 Connecting the main drain tube and waste bottle (front of
instrument)
77
Installation
the rinse feed assembly, consisting of a flexible PTFE tube with two
screw fittings and a rigid FEP tube with a complementary screw thread.
2. Push the notched end of the rigid tube through the bottle cap until the tube
touches the base of the bottle.
3. Connect one end of the flexible tube to the rigid tube.
4. Place the rinse bottle in a convenient location underneath the autosampler,
such as on a shelf underneath the laboratory bench.
The top of the rinse bottle must be lower than the rinse pump to prevent
siphoning.
5. Connect the other end of the flexible tube to the inlet fitting of the rinse
pump.
6. Position the rinse bottle so that when you move the graphite furnace
assembly into and out of the atomizer compartment the rinse feed tube does
not pull the bottle over or catch on any objects.
78
Figure 5-10 Connecting the rinse feed tubes and rinse bottle
79
Installation
80
Figure 5-11 Location of the notch and hub on the sample tray.
81
Installation
88-location tray
locations
148-location tray
locations
Not suitable
1-80
7 mL; polypropylene
81-88
141-148
Quick Reference
A slot is provided underneath the autosampler into which you can insert the
Quick Reference. We recommend that you keep the Quick Reference with the
autosampler at all times since it contains important maintenance information,
particularly maintenance of the valves.
82
Electrical connections
Warning: Electrical Hazard
WARNING
Read the following instructions very carefully before connecting any cables.
See chapter 3, Preparing Your Laboratory, for the specification of the line
power supply.
Summary
83
Installation
84
Figure 5-12 Electrical connections for the HGA 900 to the AAnalyst 400
85
Installation
Figure 5-13 Operational on/off switch on the HGA 900 power unit
86
87
Installation
Item
1
Designation
Communication
Instrument
Cooling System
~230 V 50/60 Hz
5
6
7
~230 V 50/60 Hz
~230 V 50/60 Hz
~230 V 50/60 Hz
88
Function
Designation
Function
9
10
F1
11
F2
12
F3
13
F4
89
Installation
Installation Kit
Items Included in the Installation Kit with a circulating cooling
system (Part No. N315-0005)
Part No.
Description
Quantity
B315-0050
B300-1500
AS 800 Autosampler
B019-8072
B000-8286
Washer #DIN125
B000-8943
Washer # DIN9021
B003-9777
Lock Washer
B005-4945
Nut
B005-5474
B005-5883
Screw Clamp
B005-5934
B011-2552
B016-0561
10
90
Description
Quantity
B315-0050
B300-1500
AS 800 Autosampler
B000-8286
Washer #DIN125
B000-8943
Washer # DIN9021
B003-9777
Lock Washer
B005-4945
Nut
B005-5474
B005-5883
Screw Clamp
B005-5934
B011-2552
B016-0561
10
B313-0124
NOTE: This installation kit does not contain a circulating cooling system.
91
Installation
Description
Quantity
0992-0179
Y-connector
0992-0583
Union Nut
0992-3472
0992-3473
B001-8079
Union Nut
B002-3662
Disk
B004-8138
Clamping Utter
B007-2601
B008-0112
B008-0259
Instrument Mirror
B012-8495
1 pair
B014-7498
B015-5574
Safety Insert
B016-0561
B016-6485
Gas Connection
B016-6859
92
Description
Quantity
B050-2706
Air Filter
B050-5368
Cleaning Tips
B050-8264
10 m
B050-9449
Suitcase AAnalyst
B051-0293
Communication Cable
B300-1262
B312-1301
B312-1302
Read Cable
B313-0064
B313-0085
B313-0127
Insertion Sheet
B315-0163
B315-1264
Left-hand bracket
B315-1265
Right-hand bracket
B011-2552
Plug
N315-0331
Cable
0993-6667
93
Installation
Pkg
20
5
50
20
5
50
20
5
50
20
5
50
20
1 pair
5
Part No.
B300-1264
B300-1262
B010-9322
B300-1254
B013-7111
B010-9324
B300-1256
B013-7112
B009-1504
B300-0342
B010-5197
B007-0699
B300-1253
B012-8495
B010-5113
Matrix modifiers
Description
Magnesium nitrate modifier (10 g/L Mg, 100 mL)
Palladium nitrate modifier (10 g/L Pd, 50 mL)
Part No.
B019-0634
B019-0635
Window components
Description
Window
Mount
Collar
94
Part No.
B008-0850
B312-0683
B312-0294
Tools
Description
Set of tools, for changing the contacts
Tube alignment tool
Insertion tool for Lvov platforms
Part No.
B312-1301
B008-0112
B011-2657
Part No.
B019-3243
B050-8264
0992-3183
0992-0179
B019-8072
B313-0124
B050-5133
95
Installation
you are located within the U.S., call toll free 1-800-762-4000, 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.
96
Preparing for
Analysis
II. If you are using the main water supply, set a flow rate of
approximately 2.5 L/min.
NOTE: If the water is too cold or flowing too fast, moisture may condense on the
graphite contacts or on the furnace windows. Moisture on the graphite contacts
leads to shorter lifetimes of the graphite tube and contacts, while moisture on the
windows leads to a reduction in the radiant energy.
7. Switch the circuit breaker on the rear panel of the HGA 900 power unit to the
on position (marked). You can leave this switch permanently in the on
position during routine operation; you switch the power unit on and off via
the operational on/off switch located on the lower left-hand side of the unit.
8. Switch on the power unit with the operational on/off switch.
9. Switch on the computer.
If your computer has a power management system, switch this off.
10. Switch on the spectrometer and other accessories (see Switching on the
System in the Online Help in AA WinLab32).
11. Start AA WinLab32: In the AA WinLab32 group, double click on the AA
WinLab32 icon.
12. Select the atomization technique:
I. In the File menu, click on Change Technique.
or
II. On the Toolbar, click on Technique. In the Select Technique dialog,
click on Furnace and then on OK.
13. Create or open a method (see the Online Help in AA WinLab32).
14. Install and align the lamp(s) that you require (see Installing the Lamp(s) and
Aligning Lamps sections in the AAnalyst 400 Hardware Guide or AAnalyst
200 Users Guide).
15. If required, install and condition a graphite tube (for more information see
the procedures for installing and conditioning a graphite tube in Chapter 7
Maintenance).
16. Optimize the position of the furnace (see the procedure, Aligning the
graphite furnace later in this chapter).
17. Set up the furnace autosampler (see the procedure later in this chapter).
98
You should now optimize the analytical conditions. Refer to the Online Help in
AA WinLab32.
Procedures for shutting down the system are described on the last page of this
chapter.
Table 6-1 Required Pressure for the Furnace Gases
Gas
bar
psig
P min
P max
P min
P max
P min
P max
Argon
350
400
3.5
4.0
50.0
58.0
Nitrogen
350
400
3.5
4.0
50.0
58.0
Special
350
400
3.5
4.0
50.0
58.0
Set the outlet gauge pressure for each gas to a value just below the
maximum value (Pmax).
Never set the outlet gauge pressure to a value exceeding the maximum
pressure (Pmax).
Warning: Toxic Gases
If you use nitrogen as the inert gas, toxic cyanogens gas (CN)2 will be
produced when the furnace temperature is above 2300 C.
WARNING
Make sure the main laboratory fume ventilation system removes all
gases and fumes emitted by the furnace.
99
100
Figure 6-1 moving the furnace assembly into and out of the atomizer
compartment
101
WARNING
The graphite furnace can generate very high temperatures, and can emit
UV radiation which can damage your eyes when it is heated to
incandescence. The furnace is exposed when it is in the standby position,
thus increasing these risks.
when you move it into the atomizer compartment in case someone has
altered the alignment controls while the furnace was in the standby position.
if you change from a graphite tube without a platform to one with a platform.
102
103
5. Check that the graphite tube you intend to use for your analyses is installed
in the furnace.
6. Remove both window assemblies from the furnace (see the procedure in
chapter 7, Maintenance).
7. Autozero the spectrometer.
I. In the Tools menu, click on Continuous Graphics.
II. Click on Autozero.
8. Move the furnace back into the atomizer compartment (see the procedure
earlier in this chapter). The absorbance reading should be less than 0.002.
If it is not, align the furnace as described in step 9.
9. Align the furnace:
I. Move the locking lever to the left to release lateral (left-right)
movement of the furnace.
II. Rotate the vertical (up-down) and horizontal (forward-backward)
alignment controls alternately and in small increments to find the
position that gives minimum absorbance reading on the display.
III. Grasp the furnace assembly at the base and carefully move the
furnace laterally to the left and to the right to find the position that
gives minimum absorbance reading on the display.
IV. Repeat the horizontal, vertical, and lateral adjustments until you
have obtained the min imum absorbance reading.
V. Move the locking lever to the right to lock the furnace.
10. When you have completed furnace alignment, autozero the spectrometer:
I. In the Tools menu, click on Continuous Graphics.
II. Click on Autozero.
11. Refit both window assemblies (see the procedure in chapter 7, Maintenance).
12. The absorbance reading after replacing the windows should be about 0.06
0.09 when measured at the Cu line at 324.75 nm. The absorbance increases
toward shorter wavelengths.
104
You must fill the rinsing system before the start of every analysis run to
make sure that the tubes are completely filled with fresh rinsing liquid, to
remove entrained air bubbles, and as part of routine valve maintenance.
You must flush the rinsing system at the end of every analysis run as part of
routine valve maintenance.
Follow the steps below to fill and flush the rinsing system:
1. Make sure that the rinsing system components are correctly installed, in good
condition, and suitable for the rinsing liquid you will use.
2. Prepare the rinsing solutions that you require, see following page.
3. Fill the rinse bottle with the first, clean, particle-free, rinsing liquid. If there
are particles in the rinsing liquid they can lodge in the valves, causing leaks
and non-reproducible results.
105
Rinsing solutions
Use the following rinsing solutions in the given sequence:
Before the start of every analysis series:
If the rinsing solution you intend to use is miscible with the solution currently in
the system, use your intended rinsing solution. If the rinsing solution you intend
to use is not miscible with the solution in the system, you must use intermediate
rinsing liquids.
For example, to change from an acidic liquid to an organic solvent, you could
use:
1. Deionized water.
2. Isopropanol or other water-miscible solvent.
3. Final organic solvent.
After an analysis series:
1. If you have been using an organic rinsing liquid, use isopropanol or other
water-miscible solvent.
106
2. Dilute nitric acid. This is especially important for elements with a tendency
to carryover.
3. Isopropanol.
4. Deionized water.
107
You can cause irreparable damage to the gears if you attempt to move
the autosampler arm by hand.
1. Never attempt to move the autosampler arm by hand. Move it only
with the depth control wheel.
108
WARNING
109
WARNING
110
The pipet tip enters the graphite tube when you issue the In Tube command.
The pipet 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.
1. Before you use this procedure, align the autosampler arm as described in the
procedure above.
2. In the Furnace Control window, click on Align Tip.
The Align Autosampler wizard appears.
3. In the wizard select Check the autosampler tip alignment in the graphite
tube. The autosampler arm is unlocked and the pipet tip enters the graphite
tube.
4. View the inside of the furnace:
I. Place a piece of white card behind the right-hand furnace window
to provide a white background when you view the inside of the
graphite tube.
II. Hold the instrument mirror provided with the autosampler next to
the left-hand furnace window and position it so that you can see
into the graphite tube. Wear UV-absorbing glasses when viewing
the graphite tube. Select Next in the Wizard.
5. View the depth of the capillary in the graphite tube.
6. If no adjustments are made, select Cancel in the Wizard. If adjustments are
made to the depth of the capillary, select Finish on the Wizard to save the
new position.
111
NOTE: Once you have saved this depth position, do not inadvertently change it by
clicking on Yes to the query Do you want to save this position? Only click on Yes
when you have readjusted the depth.
112
6. In the Align Autosampler wizard click on Finish to save the new position.
Finely adjusting the depth in the sample cup
1. Make a preliminary adjustment as described above.
2. Put a sample cup in location 1 of the sample tray.
3. In the Align Autosampler Wizard, select Use a Sample Cup. The pipet tip
moves into the sample cup. Select Next.
4. Adjust the depth control wheel so that the pipet tip is at the correct depth
inside the cup.
5. In the Align Autosampler Wizard, select Finish to save the new position.
NOTE: Once you have saved this depth position, do not inadvertently change it by
clicking on Yes to the query Do you want to save this position
WARNING
113
114
not contact the graphite surface, liquid may remain in the tip, leading to
pipetting errors.
If the pipet tip is too near to the platform or tube wall, liquid may hang up on
the tip, leading to pipetting errors
115
116
Maintenance
Introduction
This chapter describes the routine maintenance procedures required to keep your
instrument in proper working condition and to ensure the highest possible level
of performance. It includes maintenance checks that should be done on a daily
basis and maintenance procedures that should be done periodically depending on
instrument use. This chapter is divided into several sections, each section
covering maintenance procedures for a particular component of the system.
You should perform only the maintenance procedures described in this chapter. If
additional maintenance is required, contact a PerkinElmer Service Engineer.
Before using any cleaning or decontamination methods except those
specified by the manufacturer, users should check with the
manufacturer that the proposed method will not damage the
equipment.
CAUTION
Switch off the HGA 900 system and make sure it cannot be operated.
WARNING
117
Maintenance
You should only perform the maintenance procedures described in this guide.
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:
118
Graphite contacts
Furnace windows
119
Maintenance
Make sure that the water level is always at the MAX. mark. Fill
up the system when necessary (see the procedure later in this
chapter).
Complete rinsing
system
Valves
120
Waste bottle
Rinse bottle
All tubing
Make sure that all the tubes are clean and free from
kinks.
Change any tubes that may be damaged or
contaminated.
Pipet tip
Make sure that the pipet tip is not damaged. If the tip is
damaged you may get pipetting errors during the
analyses. Repair the tip or install a new pipet assembly
if necessary (see the procedure later in this chapter).
Pump heads
Make sure that the pump heads are not loose. Tighten
the pump head retaining ring if necessary. Make sure
that pump heads remain vertical, with the arrow
aligned vertically (see the procedure later in this
chapter).
121
Maintenance
WARNING
122
123
Maintenance
124
125
Maintenance
NOTE: 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 the procedure in chapter 6,
Preparing for Analysis).
8. Check alignment of the furnace autosampler (see the procedure in
chapter 6, Preparing for Analysis).
126
WARNING
The graphite furnace can generate very high temperatures and can emit UV
radiation which can damage your eyes, when it is heated to incandescence.
The furnace is exposed when it is in the standby position, thus increasing
these risks.
Never heat the furnace when it is in the standby position. Always move it
into the atomizer compartment before you heat it.
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 the procedure later in this chapter). If there are stubborn deposits in the tube
that you cannot remove, discard the tube and use a new one.
Cleaning the contact surfaces of the graphite tube and contacts
Warning: High Temperatures-Risk of Burns
The graphite furnace can generate very high temperatures.
WARNING
Maintenance
5. 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 the procedure later in this chapter).
6. Insert the graphite tube and close the furnace (see the procedure later in this
chapter).
7. Refit the windows (see the procedure later in this chapter).
8. If using a new tube, condition the graphite tube (see the procedure later in
this chapter).
128
The standard graphite tubes have integrated platforms. If you are going to use a
tube without an integrated platform, insert a Lvov platform into the graphite
tube by following the instructions in the next section. Once the platform is
installed, proceed as given below to install the graphite tube.
NOTE: Do not handle graphite tubes with bare fingers. Perspiration from your fingers
can attack the pyrolytic coating.
Warning: High Temperatures-Risk of Burns
The graphite furnace can generate very high temperatures.
WARNING
129
Maintenance
130
6. If you have installed a new graphite tube, perform the procedure outlined
in Conditioning the graphite tube (later in this chapter).
If you are reusing a previously conditioned graphite tube, heat manually
at 2500 C for 5 seconds to remove surface contamination (see the
procedure later in this chapter).
NOTE: Every time you open the furnace, subsequently always heat it out manually at
2500 C for approximately 5 seconds.
Inserting a Lvov platform
This procedure is only required when you are using graphite tubes without
integrated platforms.
NOTE: Do not handle graphite tubes and Lvov platforms with bare fingers. Perspiration
from your fingers can attack the pyrolytic coating.
1. Place the Lvov platform with the sample cavity downward onto the flat
surface of the insertion tool.
Take care not to touch the platform, and especially the sample cavity, with
bare fingers. Wear gloves or handle the platform carefully by its ends.
Lvov
platform
Graphite tube
Insertion tool
131
Maintenance
3. Guide the edges of the platform into the grooves in the graphite tube and then
push the platform into the tube with the insertion tool. While inserting the
platform, squeeze the handle of the insertion tool so that the edges of the
platform are pressed into the grooves in the tube.
The platform is seated correctly when you feel resistance to further insertion.
Figure 7-7 Inserting the Lvov platform into the graphite tube
4. Carefully remove the insertion tool.
5. Lightly shake the graphite tube to make sure that the Lvov platform is
securely seated. It the platform falls out, repeat the above steps.
6. If required, you can push the platform out of the tube by inserting the
insertion tool into the other end of the tube.
7. Insert the graphite tube and close the furnace (see the procedure earlier in this
chapter).
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.
Lvov 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.
Conditioning the graphite tube
We recommend that you run the graphite tube conditioning program every time
that you change the graphite tube or platform. The conditioning procedure
132
removes adsorbed gases and surface contamination from the graphite, and
ensures reproducible performance.
After conditioning, it is good practice to verify that the tube and/or platform are
sufficiently clean for the element you wish to determine.
In order to do this, run your method for this element, but do not inject a sample.
Perform a dry fire instead. Evaluate the results obtained. If the absorbance
value is too high for this element, heat the tube manually at 2500 C for 10
seconds and then repeat the dry fire.
Warning: High Temperatures-Risk of Burns
The graphite furnace can generate very high temperatures.
WARNING
Toxic Gases
WARNING
If you use nitrogen as the inert gas, toxic cyanogen gas (CN)2 will
be produced when the furnace temperature is above 2300 C.
Make sure that the main laboratory fume ventilation system
removes all gases and fumes emitted by the furnace.
133
Maintenance
WARNING
134
135
Maintenance
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.
Risk of damage to the optical sensor.
CAUTION
Take care not to damage the optical sensor when you remove
or install the graphite contacts.
136
137
Maintenance
138
139
Maintenance
140
141
Maintenance
142
143
Maintenance
144
6. Slide the graphite shield ring with its large flat face toward the furnace
block over the left-hand contact.
Maintenance
146
147
Maintenance
148
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.
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.
5. Reassemble the windows:
a. Carefully drop the window into the mount, making sure that it sits
correctly.
b. Push in the collar.
6. Refit the windows in the furnace (see the previous procedure).
149
Maintenance
150
151
Maintenance
WARNING
Electrical Hazard
Use only fuses with the correct current rating and of the specified
type for replacement.
Do not use makeshift fuses and do not short-circuit the fuse
holders.
Disconnect power cord from the AC power outlet before replacing
any fuses.
1. Switch off the power unit and all other instruments connected to it as
described in the relevant guides.
2. Switch the circuit breaker on the rear panel of the power unit to the off
position (marked O).
3. Disconnect the power units line power cord from the line power supply.
4. Disconnect all the line power cords from the sockets at the rear of the power
unit.
5. To change the fuses numbered F1, F2, F3, F4:
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.
c. Screw the fuse holder into the correct socket.
6. Reconnect the line power cords correctly.
152
153
Maintenance
154
Procedures described
155
Maintenance
7. If there is sediment in the water when you empty the cooling system, fill the
system with water and pump it out again several times to completely flush
the system.
8. For each hose, carefully pull the locking ring on the drain fitting down
slightly to release the lock, and then pull the drain fitting out of the
connector.
9. Reconnect the cooling system hoses to the power unit.
10. Reconnect the line cord to the special outlet at the rear of the power unit.
156
157
Maintenance
158
WARNING
Electrical Hazard
Use only fuses with the correct current rating and of the specified type
for replacement.
Do not use makeshift fuses and do not short-circuit the fuse holders.
Disconnect power cord from the AC power outlet before replacing any
fuses.
159
Maintenance
NOTE: In addition to the fuse in the cooling system, shown here, there is a fuse in the
power outlet on the HGA 900 power unit.
1. Switch off the cooling system with the switch on the rear panel.
2. Disconnect the line power cord from the socket.
3. Behind this socket is the cover of the fuse holder.
Use the tip of a small screwdriver to carefully lever open the fuse holder.
4. Remove the blown fuse.
5. Insert a new fuse of the correct type and rating. Correct fuse: 230 V, 1.6 A,
slow-blow.
6. Close the fuse holder and reconnect the line power cord.
7. Switch on the cooling system with the switch on the rear panel.
160
Valve maintenance
CAUTION
You can cause irreparable damage to the gears if you attempt to move
the autosampler arm by hand.
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 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.
161
Maintenance
The only routine maintenance that the valves require is to flush them thoroughly
before and after every analysis.
Flushing the valves and rinsing system
1. Make sure that the rinsing system components are correctly installed, in
good condition, and suitable for the rinsing liquid you will use.
2. Prepare the rinsing solutions that you require, see following page.
3. Fill the rinse bottle with the first, clean, particle-free, rinsing liquid.
If there are particles in the rinsing liquid they can lodge in the valves,
causing leaks and non-reproducible results.
4. Flush the system:
a. In the Furnace Control window, click on Flush Sampler.
This activates a rinse cycle.
b. Repeat sub step 1 as often as required to completely flush the rinsing
system with rinsing liquid and flush all the air out.
5. Empty the waste bottle. Dispose of any hazardous waste correctly.
6. Repeat steps 2 through 4 for each rinsing solution.
NOTE: Make certain there are no air bubbles in the rinsing system. Air bubbles can lead
to non-reproducible results.
Rinsing solutions
Use the following rinsing solutions in the given sequence:
Before the start of every analysis series:
If the rinsing solution you intend to use is miscible with the solution in the
system, use your intended rinsing solution. If the rinsing solution you intend to
use is not miscible with the solution in the system, you must use intermediate
rinsing liquids.
162
For example, to change from an acidic liquid to an organic solvent, you could
use:
1. Deionized water.
2. Isopropanol or other water-miscible solvent.
3. Final organic solvent.
After an analysis series:
1. If you have been using an organic rinsing liquid, use isopropanol or other
water-miscible solvent.
2. Dilute nitric acid. This is especially important for elements with a tendency
to carryover.
3. Isopropanol.
4. Deionized water.
Before performing maintenance on the system:
1. Isopropanol.
2. Deionized water.
After performing maintenance on the system:
1. Isopropanol.
2. The rinsing solution you intend to use next or deionized water.
163
Maintenance
You can cause irreparable damage to the gears if you attempt to move
the autosampler arm by hand.
If you experience problems such as poor precision or recovery, check to see if the
rinse pump valves are leaking.
To check the outlet valve
1. Raise the pipet tip out of the rinsing port:
a. In the Furnace Control window, click on Align Tip.
The Align Autosampler Wizard appears.
b. In the Wizard, select Set the depth of the autosampler tip in the
sampling cup and Use the rinse location. The pipet tip rises to a
position directly above the rinsing port.
c. Select Next and then Finish.
2. Start a rinse cycle (see the previous procedure).
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.
164
165
Maintenance
You can cause irreparable damage to the gears if you attempt to move
the autosampler arm by hand.
166
167
Maintenance
168
169
Maintenance
170
171
Maintenance
172
The rinse feed tube has a larger diameter than the other tubes and uses larger
ferrules and a larger nut.
173
Maintenance
Repairing a pipet
The complete pipet is an assembly that consists of the sample tube fitted through
a mount and a flexible sleeve. The mount is provided with a groove that locates
the mount in the correct position in the clip at the end of the autosampler arm.
The pipet tip is that portion of the sample tube protruding from the mount.
If the pipet tip becomes damaged you can repair it as given below:
Risk of damage to the autosampler
CAUTION
You can cause irreparable damage to the gears if you attempt to move
the autosampler arm by hand.
174
175
Maintenance
5. Using a sharp blade, cut off the PTFE tube at a slight angle to leave
approximately 7 mm of tube extending out of the sleeve.
176
You can cause irreparable damage to the gears if you attempt to move
the autosampler arm by hand.
177
Maintenance
178
3. Pass the sample tube around the back of the motor assembly and thread it
through hook H1 on the sample table. Leave a sufficiently large loop so that
the autosampler arm can move freely.
4. Thread the sample tube through hooks H2 and H3 on the sample table and
pass it to the top of the sample pump.
5. Take two new ferrules from the ferrule kit provided with the autosampler.
Slide the knurled nut, the back ferrule, and then the front ferrule onto the
tube.
NOTE: Make sure the ferrules are the correct way round.
6. Screw the knurled nut finger-tight onto the sample pump.
Do not use force.
7. When you have finished select Next in the Wizard.
8. Adjust the depth control wheel so that the pipet tip is at the correct depth
inside the rinsing port (see chapter 6, Preparing for Analysis).
9. Select Finish.
10. Fill and flush the rinsing system (see the procedure earlier in this chapter):
a. Flush the rinsing system with isopropanol.
b. Flush the rinsing system well with the usual rinsing liquid.
NOTE: Always fill and flush the rinsing system after you have performed any work on the
components.
179
Maintenance
180
181
Maintenance
182
Warnings
Warnings
This section contains translations of the safety conventions and warnings used in
this guide.
Deutsch
espaol
franais
italiano
183
This symbol alerts you to situations that could result in personal injury to
yourself or otherpersons.
Details about these circumstances are in a box like this one.
WARNING
Deutsch
Dieses Symbol warnt vor Situationen, in denen Sie oder andere Personen
verletzt warden knnen.
Einzelheiten darber sind in einem Rahmen wie diesem angegeben.
espaol
franais
italiano
184
Warnings
185
Caution, risk of electric shock. This symbol alerts you to the risk of
electric shock that could result in personal injury toyourself or other
persons.
Details about these circumstances are in a box like this one.
Deutsch
espaol
franais
italiano
186
Warnings
187
Caution, hot surface. This symbol alerts you to the risk of hot surfaces
that could cause personal injury toyourself or other persons.
Details about these circumstances are in a box like this one.
Deutsch
Dieses Symbol warnt vor Gefahr durch heie Oberflchen, durch die
Sie oder anderePersonen verletzt werden knnen.
Einzelheiten darber sind in einem Rahmen wie diesem angegeben.
espaol
franais
italiano
188
Warnings
189
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.
Deutsch
Dieses Symbol warnt vor Gefahr durch UV-Strahlung, die bei Ihnen
oder anderen Personen zu Augenverletzungen fhren knnen.
Einzelheiten darber sind in einem Rahmen wie diesem angegeben.
espaol
Este smbolo le advierte del peligro de que usted u otras personas sufran
lesiones en los ojos a consecuencia de la radiacin ultravioleta.
En los recuadros como ste se proporciona informacin sobre este tipo
de circunstancias.
franais
italiano
190
Warnings
191
CAUTION
The term CAUTION alerts you to situations that could result in serious damage
to theinstrument or other equipment.
Details about these circumstances are described in a message similar to this
one.
Deutsch
Achtung:
Der Ausdruck CAUTION (ACHTUNG) warnt vor Situationen, die eine ernste
Beschdigung des Gerts oder anderer Systemteile zur Folge haben knnen.
Einzelheiten darber sind auf die gleiche Weise wie dieser Text hervorgehoben.
espaol
Advertencia:
El trmino CAUTION (ADVERTENCIA) le previene de situaciones que pueden
provocar averas graves en ste u otros equipos.
En los recuadros como ste se proporciona informacin sobre este tipo de
circunstancias.
franais
Attention:
Le terme CAUTION (ATTENTION) vous signale des situations susceptibles de
provoquer de graves dtriorations de l'instrument ou d'autre matriel.
Les dtails sur ces circonstances figurent dans un message semblable celui-ci.
italiano
Attenzione:
Con il termine CAUTION (ATTENZIONE) vi si mette in guardia da situazioni
che possono comportare il serio danneggiamento della strumentazione o di altre
apparecchiature.
Troverete informazioni su tali circostanze in un riquadro come questo.
192
Warnings
193
WARNING
Deutsch
espaol
Franais
194
Warnings
Italiano
195
Explosive Atmosphere
This instrument is not designed for operation in an explosive atmosphere.
WARNING
Deutsch
espaol
franais
italiano
196
Warnings
WARNING
Deutsch
espaol
franais
197
Italiano
198
Warnings
WARNING
Deutsch
Electrical Hazard
Any interruption of the protective conductor inside or outside the
instrument or disconnection of the protective conductor (earth/ground)
terminal is likely to make theinstrument dangerous.
Intentional interruption is prohibited.
Lethal voltages are present in the instrument
Even with the power switch off, line power voltages can still be
present within the instrument.
When the instrument is connected to line power, terminals may be live,
and opening covers or removing parts (except those to which access
can be gained without use of a tool) is likely to expose live parts.
Capacitors inside the instrument may still be charged even if the
instrument has been disconnected from all voltage sources.
Warnung: Gefhrdung durch Elektrizitt
Das Gert muss zum Betrieb immer geerdet sein.
Trennen oder entfernen Sie unter keinen Umstnden die Schutzleiter im
Gert oder in der Netzzuleitung.
Gefhrliche Spannung im Gert
Auch in ausgeschaltetem Zustand kann an einigen Stellen im
Gert Netzspannung anliegen, wenn das Gert am Stromnetz
angeschlossen ist.
Wenn das Gert am Stromnetz angeschlossen ist, stehen
Anschlsse mglicherweise unter Spannung. Durch das ffnen
von Abdeckungen und Entfernen von Teilen (mit Ausnahme derer,
auf die ohne Werkzeuge zugegriffen werden kann) werden u.U.
stromfhrende Teile freigelegt.
Auch bei ausgeschaltetem Gert und getrennter Netzverbindung
knnen Kondensatoren im Gert noch mit gefhrlicher Spannung
geladen sein.
199
espaol
franais
200
Warnings
Italiano
201
202
Warnings
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
Deutsch
espaol
franais
italiano
203
204
Warnings
WARNING
Electrical Hazard
Use only fuses with the correct current rating and of the specified type
for replacement.
Do not use makeshift fuses and do not short-circuit the fuse holders.
Disconnect power cord from the AC power outlet before replacing any
fuses.
Deutsch
espaol
franais
205
Italiano
206
Warnings
espaol
franais
Danger: Rayonnement UV
Les lampes peuvent mettre des UV susceptibles de provoquer des lsions
oculaires.
207
Italiano
208
Warnings
espaol
Warnung: Verbrennungsgefahr
Der Graphitofen erzeugt sehr hohe Temperaturen.
Vergewissern Sie sich, da der Ofen auf Raumtemperatur
abgekhlt ist, bevor Sie Ihn anfassen oder ffnen.
Advertencia: Altas temperaturas Riesgo de quemaduras
El horno de grafito puede alcanzar temperaturas muy altas.
Asegrese, antes de tocar cualquier parte del horno, sobre todo
sus componentes de grafito, de que ste se haya enfriado hasta
alcanzar la temperatura ambiente.
franais
209
Italiano
210
Warnings
Toxic Gases
WARNING
Deutsch
If you use nitrogen as the inert gas, toxic cyanogen gas (CN)2 will be
produced when the furnace temperature is above 2300 C.
Make sure that the main laboratory fume ventilation system
removes all gases and fumes emitted by the furnace.
Warnung: Giftiges Abgas
Bei Verwendung von Stickstoff als Inertgas bildet sich bei
Ofentemperaturen ber 2300 C giftiges Dicyan (CN)2.
espaol
franais
211
Italiano
212
Warnings
franais
italiano
Symbole am Gert
Eines der folgenden Symbole kann sich am Gert befinden:
Smbolos usados en el equipo
Usted puede aplicar al equipo cualquiera de los siguientes
smbolos:
Symboles utiliss sur l'instrument
Tous les symboles suivants peuvent tre utiliss sur l'instrument :
Contrassegni utilizzati sullo strumento
Qualsiasi dei seguenti contrassegni pu essere utilizzato sullo
strumento:
213
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.
Deutsch
espaol
franais
italiano
214
Warnings
Deutsch
espaol
franais
italiano
Deutsch
espaol
franais
italiano
215
Deutsch
espaol
franais
italiano
216
Warnings
This symbol indicates the on position of the 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.
Deutsch
espaol
franais
italiano
Dieses Symbol zeigt die Stellung Ein des Netzschalters oder Leistungsschalters. Wenn
der Schalter auf dieser Position steht, wird das Gert mit Netzstrom versorgt, mu
jedoch nicht notwendigerweise eingeschaltet und betriebsbereit sein.
Este smbolo indica que el interruptor principal de la red o del cortacircuitos est
conectado. Cuando el interruptor se encuentra en esta posicin, el equipo est
conectado a la red elctrica, pero no est necesariamente encendido o en estado
operacional.
Ce symbole indique que l'interrupteur ou le coupe-circuit principal est en position
marche. Quand l'interrupteur est dans cette position, l'instrument est connect
l'alimentation secteur, mais n'est pas ncessairement en circuit et oprationnel.
Questo simbolo indica la posizione di acceso dell'interruttore principale di
alimentazione o il separatore di circuito. Se l'interruttore si trova in questa posizione
lo strumento collegato all'alimentazione elettrica ma non necessariamente attivo e
operativo.
217
218
Index
A
AAnalyst, 84
About this manual, 1
Changing Air Filter;Replacing Air Filter
changing, 153
Automatic Circuit Breaker
resetting
Resetting, 150
Autosampler
alignment procedures, 107
connecting drain tube and waste
bottle, 76
connecting rinse feed tubes and rinse
bottle, 78
Index
220
E
External Cooling
connecting
external cooling sources, 73
F
Fitting ferrules
fitting, 172
furnace
viewing inside graphite tube;viewing
inside graphite tube
viewing inside graphite tube during
alignment, 110
setup procedures, 104
Furnace
Aligning, 102
closing;Closing the Furnace
aligning;Aligning Graphite Tube
inserting, 124
opening for contact change
for contact change, 136
opening;Opening the Furnace
graphite tube, 123
setup procedures, 100
Setting up for Furnace Analyses
setting up, 97
Fuses
Changing, 152
G
Graphite Components, 94
Graphite Contacts
changing
graphite contacts, 135
graphite tube
integrated platform, 129
Graphite Tube
cleaning
graphite tube
cleaning
graphite contacts, 126
conditioning, 132
Heating the Graphite Tube
heating
removing contamination by
heating, 127
I
Installation, 61
graphite components, 94
installation kit, 90
spares parts, 92
Installation Kit, 90
L
L vov Platform
inserting;Inserting a L vov platform
L vov platform, 131
Labels
warning signs, 3
M
Checklists for Maintenance Tasks
checklists, 119
O
P
Pipet
repairing;Repairing a Pipet
repairing a pipet, 174
Power Unit
electrical connectors and switches, 86
maintenance procedures
power unit, 150
Removing Front Panel of Power Unit
removing front panel, 64
S
Shutting Down the System, 116
Spares Parts, 92
V
Valves
assembling and installing, 170
autosampler
valves checking, 164
cleaning
valves
cleaning
pump heads, 169
W
connecting water hoses
connecting, 70, 74
221
Index
222