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Agilent 280 Series AA Spectroscope User's Guide V2 PDF

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Summary of Content for Agilent 280 Series AA Spectroscope User's Guide V2 PDF

Agilent 240/280 Series AA (including Zeeman)

Users Guide

2 Agilent 240/280 Series AA (including Zeeman)

Manual part number 8510154700 Edition 18, June 2022

Copyright Agilent Technologies, Inc. 1997, 20002004, 20102013, 2015, 2016, 2018, 2021, 2022 No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws. Agilent Technologies Australia [M] Pty Ltd 679 Springvale Road Mulgrave, Victoria 3170, Australia www.agilent.com

Errata statement NOTICE: This document contains references to Varian. Please note that Varian, Inc. is now part of Agilent Technologies. For more information, go to www.agilent.com

Warranty The material contained in this document is provided as is, and is subject to being changed, without notice, in future editions. Further, to the maximum extent permitted by applicable law, Agilent disclaims all warranties, either express or implied, with regard to this manual and any information contained herein, including but not limited to the implied warranties of merchantability and fitness for a particular purpose. Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing, use, or performance of this document or of any information contained herein. Should Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms, the warranty terms in the separate agreement shall control.

Technology licenses The hardware and/or software described in this document are furnished under a license and may be used or copied only in accordance with the terms of such license.

Restricted rights legend U.S. Government Restricted Rights. Software and technical data rights granted to the federal government include only those rights customarily provided to end user customers. Agilent provides this customary commercial license in Software and technical data pursuant to FAR 12.211 (Technical Data) and 12.212 (Computer Software) and, for the Department of Defense, DFARS 252.227-7015 (Technical Data - Commercial Items) and DFARS 227.7202-3 (Rights in Commercial Computer Software or Computer Software Documentation).

Safety notices

A CAUTION notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in damage to the product or loss of important data. Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met.

A WARNING notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in personal injury or death. Do not proceed beyond a WARNING notice until the indicated conditions are fully understood and met.

Notices

WARNING

CAUTION

Contents

Agilent 240/280 Series AA (including Zeeman) 3

Contents 1 Safety Practices and Hazards 7

General 7

Agilent AA documentation 8

Conventions 8

Other messages 8

Verifying safe state 8

Electrical hazards 9

Heat, vapors and fumes 10

Compressed gascylinder storage and handling 11

Gas hoses and connections 12

Ultraviolet radiation 12

Warning symbols 13

Color coding 14

Flame operation 15

Flammable solvents 15

Compressed gases and cylinders for flame operation 16

Acetylene 17

Nitrous oxide 18

Burners 18

Nebulizer 19

Liquid trap 20

Heat hazards 21

Perchloric acid 21

Flashbacks 22

Contents

4 Agilent 240/280 Series AA (including Zeeman)

What to do in the Event of a Flashback 25

Resuming Operation after a Flashback 25

Furnace and Zeeman operation 26

Gases 26

Heat hazards 26

Vapors and fumes 26

UV radiation 26

Magnetic field (Zeeman only) 26

2 Introduction 27

Instrument Overview 28

Flame instruments front view 28

Flame instruments back view 29

Furnace (Zeeman) instruments front view 30

Furnace (Zeeman) instrument back view 31

Furnace (D2) instruments front view (240FS with GTA 120 accessory fitted) 32

Furnace (D2) instruments back view (240FS with GTA 120 accessory fitted) 33

Installation requirements 33

Electrical Connections 34

Gas supplies 36

3 Installation 37

PC requirements 37

Installation procedure overview 38

GPIB communications 38

Installing the USB-GPIB converter 38

Connecting and configuring an Agilent AA spectrometer Duo system 39

Contents

Agilent 240/280 Series AA (including Zeeman) 5

Setting up for Duo operation and connecting the IEEE cables 39

Configuring the IEEE addresses for Agilent AA-Duo operation 40

Configuring the SPS 4 autosampler 41

Determining the SPS 4 COM port 42

Configuring the software to use manual sampling 42

USB to RS-232 interfaces 43

Starting the SpectrAA software 44

SpectrAA Release Notes and Software Status Bulletin 44

Installing the drivers for the Tube-CAM Furnace Camera option 45

Printer setup 45

Troubleshooting 45

Service installation module 45

4 Software Overview 47

Starting the SpectrAA software 47

SpectrAA windows 47

Index page 47

Worksheet window 48

Reports window 49

Administration window 50

Working with the SpectrAA software 50

Menu bar 50

Toolbar 50

Dialog boxes 50

Help 51

Searching for help 51

Contents

6 Agilent 240/280 Series AA (including Zeeman)

5 Getting Started 53

Instrument setup 53

Connections 53

Power 54

Moving your instrument 55

Starting the system 55

Pre-analysis checklist 55

6 Maintenance and Troubleshooting 57

Schedule 58

Daily before operation 58

Daily after operation 58

Weekly 58

Yearly 59

Cleaning 59

Instrument surfaces 59

Windows 60

Filters 60

Gas cylinders 60

Preventing flashbacks 61

Spare parts 61

Safety Practices and Hazards

Agilent 240/280 Series AA (including Zeeman) 7

1Safety Practices and Hazards General 7 Agilent AA documentation 8 Verifying safe state 8 Electrical hazards 9 Heat, vapors and fumes 10 Compressed gascylinder storage and handling 11 Gas hoses and connections 12 Ultraviolet radiation 12 Warning symbols 13 Color coding 14 Flame operation 15 Flashbacks 22 Furnace and Zeeman operation 26

General

Your Agilent AA instrument and accessories have been carefully designed so that when used properly you have an accurate, fast, flexible and safe analytical system.

If the equipment is used in a manner not specified by the manufacturer, the protection provided by the equipment may be impaired.

Operation of an atomic absorption spectrometer can involve the use of compressed gases, flames, and hazardous materials including corrosive fluids and flammable liquids. Unskilled, improper, or careless use of this instrument can create explosion hazards, fire hazards, or other hazards that can cause death, serious injury to personnel, or severe damage to equipment and property.

Information on safety practices is provided with your instrument and operation manuals, and also referenced in your Agilent accessory manuals. Thoroughly read these safety practices before using your instrument or accessories.

Observe all relevant safety practices always.

The safety practices described below are provided to help you operate the instrument safely. Read each safety topic thoroughly before attempting to operate

Safety Practices and Hazards

8 Agilent 240/280 Series AA (including Zeeman)

the instrument and always operate the spectrometer in accordance with these safety practices. Only trained operators should use this instrument.

Agilent AA documentation

This manual covers the installation of the Agilent 240/280 series AA instruments. Instructions for installing, operating, and maintaining the instruments and components are included in the SpectrAA Help (see Page 51). Operating instructions for the Sample Introduction Pump System (SIPS) and other AA accessories are given in the manuals accompanying the accessories or in the SpectrAA Help

Conventions

The following conventions have been used throughout this manual: Single quotes ( ) indicate a selection that you can make from several choices,

such as radio buttons, checkboxes, and software items. ALL CAPITALS indicates text that you must type in from the keyboard (for

example, type SETUP at the prompt).

Other messages

Other messages appear in the manual and in the online Help where appropriate, and detail advice, information specific to the topic, or helpful tips.

NOTE A Note message is used to give advice or information.

Verifying safe state

The following general safety precautions must be observed during all phases of operation, maintenance and service of this instrument.

To ensure continued safety of the instrument after maintenance or service procedures, verify the instrument is returned to a safe state for the user. This includes running performance checks to verify the instruments safety systems are

Safety Practices and Hazards

Agilent 240/280 Series AA (including Zeeman) 9

functioning correctly. Check the general condition of the instrument during operation for wear or signs of corrosion that are likely to inhibit function or safety.

Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design, manufacture, and intended use of the instrument. Agilent Technologies assumes no liability for the customers failure to comply with these requirements.

Electrical hazards

The instrument and accessories contain electrical circuits, devices, and components operating at dangerous voltages. Contact with these circuits, devices and components can cause death, serious injury, or painful electric shock.

Panels and covers that are retained by fasteners which require the use of a tool for removal must only be opened by Agilent field service engineers. Consult the manuals or product labels supplied with your PC, monitor, printer/plotter, water- cooling system, and vacuum pump (where required) to determine which parts are operator-accessible.

Application of the wrong supply voltage, connection of the instrument to an incorrectly wired supply outlet, or lack of proper electrical grounding can create a fire hazard or a potentially serious shock hazard. This could seriously damage the instrument and any attached ancillary equipment.

Always use a 3-wire outlet with ground connection that is adequately rated for the load. The installation must comply with local and national safety regulations. Use only an Agilent supplied power cord. Replace the power cord only with a cord equivalent to the one specified in the AA Site Preparation Guide.

Do not connect the instrument to the mains power supply until you have made sure that the operating voltage is correctly set for the mains power supply in the specific outlet in your laboratory to which the equipment is connected.

WARNING

Electrical shock hazard To avoid electric shock this equipment must be disconnected from the mains supply before servicing.

Safety Practices and Hazards

10 Agilent 240/280 Series AA (including Zeeman)

Heat, vapors and fumes

Heat, vapors and fumes generated by flame, furnace and vapor generation methods can be hazardous to personnel.

Heat, vapors and fumes must be extracted from the instrument by an exhaust system. The instrument must be vented into a self-contained arrangement of collector hood, ducting, and exhaust fan. The system must be vented to the outside air, never within the building. Locate the system outlet such that the exhaust cannot re-enter the building through any door, window, air conditioning inlet, or other ventilator. Construct the system in accordance with local codes and regulations for ventilation.

The exhaust system must provide an exhaust ventilation rate of at least 6 cubic meters per minute (200 cfm). Locate the exhaust fan at least 3 meters (10 feet) away from the flame and as close to the outlet as possible. The motor must be mounted away from the hot gases, and plastic parts must not be used as they will melt. Fit a back-draft damper to the outlet end of the system. Equip the exhaust fan power supply with an indicator close to the instrument to indicate whether the exhaust fan is on or off. Always switch on the exhaust fan before lighting the flame.

Use fireproof ducting that is in accordance with your local fire prevention regulations. Locate the ducting away from fire alarms, sprinkler heads, and other heat-sensitive devices. Do not make solder joints in the ductingthe hot exhaust in the duct may melt the joint.

Regularly check the system by smoke test to ensure that the exhaust system is working.

When operating the atomic absorption spectrometer, always have the chimney in place to ensure correct ventilation.

Safety Practices and Hazards

Agilent 240/280 Series AA (including Zeeman) 11

Compressed gas cylinder storage and handling

All compressed gases (other than air) can create a hazard if they leak into the atmosphere.

WARNING

Explosion Hazard, Fire Hazard, Noxious Gas

Even small leaks in gas supply systems can be dangerous.

A leak can create an explosion hazard, a fire hazard, or can result in an oxygen- deficient atmosphere.

Such hazards can cause death, serious injury, asphyxiation, anesthetic effects, and serious damage to equipment and property.

Cylinder requirements: Stored and handled strictly in accordance with local safety codes and

regulations. Used and stored only in a vertical position. Secured to an immovable structure or a properly constructed cylinder stand. Stored in an adequately ventilated area to prevent toxic or explosive

accumulations. Moved only on a properly constructed trolley. Never locate gas cylinders near a source of ignition or in a position that is

subject to direct heat. Keep cylinders cool. This rule applies to every cylinder of compressed gas.

Cylinders have pressure relief devices that will release the contents of the cylinder if the temperature exceeds 52 C (125 F).

Ensure that all cylinders are clearly labeled so that there can be no doubt about the contents. If the cylinder label is not legible, do not use the cylinder return it to your supplier.

Always ensure that you have the right cylinder before connecting the cylinder to the instrument.

Use only approved regulators and hose connectors. Never attempt to refill a cylinder.

Safety Practices and Hazards

12 Agilent 240/280 Series AA (including Zeeman)

For cylinder connections, left-hand thread fittings are used for fuel; right-hand thread fittings are used for support gases.

When your analytical program is complete, or at the end of the working day, always ensure that all gas supplies are turned off at the cylinder.

If air is supplied from a compressor, all moisture must be extracted from the air before it is supplied to the gas control module. Moisture can affect the internal tubing and components of the gas control system and create a potentially hazardous situation.

Gas hoses and connections

Use only approved regulators, connectors, and fittings. If in any doubt, consult your local gas supplier or your Agilent representative. Ensure that all gas connectors and hoses are correctly assembled. Arrange gas hoses so that they will not be damaged, stepped on, or have things dropped on them. Never use frayed or damaged hoses. Frayed or damaged hoses must be replaced immediately. This should be done by a trained Agilent representative. Perform leak tests at all joints and seals every day before the instrument is used. Test for leaks with a brush and soapy water or a proprietary leak-detecting solution. Never use a naked flame when testing for leaks.

Ultraviolet radiation

Flames, hollow cathode lamps, and deuterium lamps emit hazardous ultraviolet radiation. This radiation can cause serious damage to human eyes and skin. Always wear safety glasses conforming to an approved standard, and certified

or otherwise warranted to protect the eyes from ultraviolet radiation. Never look directly at the light emitted by a hollow cathode lamp. When using a flame, always operate your spectrometer with the flame shield

closed, and the sample compartment front panel and chimney in place.

Safety Practices and Hazards

Agilent 240/280 Series AA (including Zeeman) 13

Warning symbols

The following is a list of symbols that appear in conjunction with warnings in this manual and on the spectrometer. The hazard they describe is also shown. A warning icon indicates the beginning of the warning text:

WARNING

A triangular symbol indicates a warning. The meanings of the symbols that appear alongside warnings in the documentation or on the instrument itself are as follows:

Corrosive liquids

Electrical shock

Explosion hazard

Eye hazard

Fire hazard

Heavy weight

(danger to feet)

Heavy weight

(danger to hands)

Hot surface

Magnetic field

Moving part

Noxious gases

Sharp object

Toxic material

Read all warnings and cautions carefully and observe them always.

The following symbol may be used on warning labels attached to the instrument. When you see this symbol, refer to the relevant operation or service manual for the correct procedure referred to by that warning label.

The following symbols may appear on the instrument for your information.

Safety Practices and Hazards

14 Agilent 240/280 Series AA (including Zeeman)

I Mains power on

0 Mains power off

Fuse

Single phase alternating current

Flame off

Flame on

Indicates lamp present

Disconnect all power plugs.

Caution, disconnect all supplies, risk of electric shock

Color coding

The various indicator lights appearing on Agilent instruments and associated accessories are color coded to represent the status of the instrument or accessory. A green light indicates that the instrument is in normal/standby mode. An orange light indicates that a potential hazard is present. A blue light indicates that operator intervention is required. A red light warns of danger or an emergency.

Safety Practices and Hazards

Agilent 240/280 Series AA (including Zeeman) 15

Flame operation

Flammable solvents

Unskilled, improper, or careless use of flammable solvents in or near an atomic absorption spectrometer can create explosion hazards and fire hazards. This can result in death, or severe personal injury or burns.

Remember always that the combination of a flame and flammable solvents can present a serious hazard. All relevant safety practices governing the use of flammable solvents must be strictly followed.

To reduce the possibility of fire or explosion: When initially selecting an organic solvent, choose a solvent having the

highest flash point consistent with your analytical requirements. Never use a solvent having a specific gravity lower than 0.75. Never leave uncovered containers of flammable solvent standing near the

burner. When aspirating such solvents, always use a covered container and feed the capillary tubing through a 2-mm diameter hole in the cover. Always use the smallest volume of solvent consistent with your analytical requirements.

Always use solvent-resistant tubing such as nitrile rubber for the drainage system and the vapor vent. Lead the drainage tube to a suitable wide-necked waste vessel (as described in the next paragraph).

The standard plastic laboratory tubing supplied with your instrument is not suitable for draining organic solvents or venting organic vapors.

If organic or toxic solutions are being used in the spray chamber, vent tubing must be connected to the vapor vent on the liquid trap, run parallel to the drain tubing, and led to an active exhaust system. Do NOT lead the vapor tubing to the waste vessel.

If you are not using toxic or hazardous liquids in the spray chamber, leave the vapor vent uncovered.

Use small, wide-necked waste vessels and empty them frequentlydo not accumulate large volumes of flammable solvent.

Do not use glass waste vesselsuse vessels made of a material that will not shatter in the event of a flashback. See Flashbacks on Page 22 for more information. Metal vessels will corrode and it is difficult to determine the level of liquid in them.

Safety Practices and Hazards

16 Agilent 240/280 Series AA (including Zeeman)

Ensure that your waste vessel is below the instrument and located in an open, well-ventilated position where you can see it. Never locate the vessel in a confined space. When your analytical program has been completed, or at the end of the working day, always empty and rinse the waste vessel.

When your analytical program has been completed, or at the end of the working day, always empty, clean, and refill the liquid trap.

Do not mix nitric or perchloric acid residues with organic solvent residues. Keep the burner slot, spray chamber, and liquid trap clean. Always use the internal igniter to light the flame as the flame will not operate

unless all the safety interlocks are satisfied. Do not attempt to bypass these safety interlocks.

Figure 1. System setup diagram

Compressed gases and cylinders for flame operation

CAUTION This spectrometer is to be used only with air, nitrous oxide, and acetylene for flame operation.

Exhaust system operating

Chimney

Burner adjuster

Vapor vent

Drain tubing must slope downwards for full length with no kinks

Keep the end of the tube above the highest liquid level

Large stable base

Wide waste vessel opening Small, non-glass waste vessel in full view of the operator

Safety Practices and Hazards

Agilent 240/280 Series AA (including Zeeman) 17

WARNING

Explosion Hazard

Never use oxygen or oxygen-enriched air as the oxidant because this will result in an explosion.

NEVER use any gas except acetylene as the fuel gas.

Acetylene

Unskilled, improper, or careless use of acetylene can create explosion hazards and fire hazards that can result in death, severe personal injury, or burns.

Adhere to your local regulations governing the use of acetylene.

Use acetylene at pressures lower than 105 kPa (15 psig). At pressures above this level, acetylene can explode spontaneously. Your Agilent AA is designed to operate at fuel supply pressures between 65 and 100 kPa (9.514.5 psig). Refer to the Specifications section or the rear of the instrument for the exact range and recommended pressure.

Do not use any tubing or connector that reacts chemically with acetylene. Never pass acetylene through copper tubing, or brass tubing or fittings containing more than 65% copper, since this may provoke an explosion. Never bring acetylene into direct contact with copper, silver, liquid mercury, gaseous chlorine, or grease, as an explosion could result.

Use only acetylene that is packed in acetone. Some gas suppliers offer acetylene packed in material other than acetone. While these alternatives may overcome some of the disadvantages of acetone, they may also introduce the more serious problem of corrosion in the gas control module and must not be used with Agilent atomic absorption spectrometers.

WARNING

Explosion Hazard, Fire Hazard

Unskilled, improper, or careless use of acetylene can create explosion hazards and fire hazards which can result in death, severe personal injury or burns.

Safety Practices and Hazards

18 Agilent 240/280 Series AA (including Zeeman)

Acetone in the spectrometer can damage seals, O-rings and hoses, degrade analytical performance and precipitate flashbacks. Acetone maybe carried over from the cylinder and into the spectrometer if either of the following conditions occur: Pressure in the acetylene cylinder falls below 700 kPa (100 psig). Consumption is greater than 1/7 of the cylinder contents per hour.

Minimize the amount of acetone that is carried over with the acetylene by: Replacing cylinders when their contents pressure drops below 700 kPa (100

psi) Ensuring that the rate of acetylene drawn off from each cylinder is not

excessive. If high rates of consumption are observed, then connect two or more cylinders

in parallel to a manifold. This reduces the rate at which acetylene is drawn from each cylinder.

To reduce the possibility of fire or explosion: Test the supply plumbing regularly for leaks with a brush and soapy water or

a proprietary leak-detecting solution (never use a naked flame when testing for leaks)

Keep the valve outlet free from dust and debris. Before assembling regulators and fittings ensure there are no particles of dirt in the cylinder valve outlet. As regulations covering preparation and handling of gas cylinders vary from country to country, refer to local regulations to ensure compliance before connecting to your instrument.

Use Instrument Grade acetylene that is at least 99.5% pure.

Turn off fuel gas at the cylinder when you have completed your flame analysis.

Nitrous oxide

The decompression of high-pressure N2O gas at the regulator can cause excessive cooling and eventual freezing of the regulator. To prevent regulator malfunction and possible flashback, the gas should be heated with an in-line or wrap-around heater.

Burners

Improper or careless use of burners can create explosion hazards and fire hazards that can cause death, serious injury to personnel and damage to equipment and property.

Safety Practices and Hazards

Agilent 240/280 Series AA (including Zeeman) 19

WARNING

Hot Surface

The burner will remain hot for some time after the flame has been turned off. Always use protective gloves to handle hot burners.

Burners are clearly identified by the fuel/oxidant combination for which they are intended. Always fit the correct burner. Never attempt to use an air-acetylene burner for nitrous oxide-acetylene, as this causes a flashback.

If the width of the burner slot exceeds 0.47 mm (0.0185 in) for a nitrous- oxide/acetylene burner or 0.54 mm (0.021 in) for an air/acetylene burner, the burner cannot be refurbished and must be replaced with a new one.

To ensure safe operation of burners: Use only acetylene as the fuel gas. Use only air or nitrous oxide as oxidant. Never attempt to use oxygen or

oxygen-enriched air, as this causes a flashback. Burner interlocks are incorporated to minimize the possibility of using the

wrong burner. Never interfere with or attempt to bypass any interlock fitted to this instrument.

To minimize the rate of burner blockage, the burner slot must be cleaned and polished as described in the Maintenance section.

Never allow burners to become blocked. Progressive burner blockage can increase the static pressure in the liquid trap to the point at which the liquid seal is breached. This can cause a flashback and create an explosion hazard or a fire hazard.

Never allow carbon to build up on the slot, as glowing particles can dislodge and fall through the slot, causing a flashback.

Always turn off the flame before attempting to clean the burner slot. Never clean the slot of a burner while a flame is running.

Never leave a flame unattended. Never disassemble or modify a burner. Never use a damaged burner.

Nebulizer

Incorrect assembly and fitting of nebulizers to an atomic absorption spectrometer can create explosion hazards and fire hazards that can cause serious injury to personnel and damage to equipment and property.

Safety Practices and Hazards

20 Agilent 240/280 Series AA (including Zeeman)

Ensure that the nebulizer is correctly assembled and correctly fitted to the spray chamber before lighting the flame. Nebulizers should be correctly adjusted before lighting the flame.

Never remove a nebulizer from the spray chamber while the flame is on, and do not use a mechanical device (for example, a wire) to clean the capillary of a nebulizer while a flame is operating. Always extinguish the flame before removing the nebulizer from the spray chamber.

Regularly test all connections for leaks. Rectify all leaks before lighting the flame.

Liquid trap

WARNING

Explosion Hazard, Fire Hazard, Noxious Gas

Improper use of the liquid trap can create explosion hazards, fire hazards, and toxic vapor hazards which can result in death or serious personal injury.

Never use a solution or solvent having a specific gravity lower than 0.75, otherwise the liquid seal can be breached. This can create a flashback and create an explosion hazard or a fire hazard.

The liquid trap interlock is incorporated to minimize the possibility of attempting to operate the instrument with an empty trap or with the drain tube missing. Never interfere with this interlock. Never attempt to bypass this interlock.

Always fill the liquid trap with the same solvent that is being used for your samples.

The trap is designed to provide a liquid seal under all normal conditions with solutions having a specific gravity greater than 0.75.

A length of tubing must be connected to the drain outlet on the trap and led to a suitable waste vessel. The free end of the tubing must remain above the liquid in the waste vessel. Do not use glass waste vesselsuse vessels made of a material that will not shatter in the event of a flashback.

A length of tubing should be connected to the vapor vent (the upper nipple) on the liquid trap when you are analyzing organic or toxic liquids. This tubing should be led out from the sample compartment, parallel to the drain tubing, and must slope downwards to enable any liquid overflow to drain out and prevent the tubing from

Safety Practices and Hazards

Agilent 240/280 Series AA (including Zeeman) 21

becoming blocked. Do not lead the vapor tubing to the waste vessel. If necessary, an active exhaust system should be used to draw away toxic vapors. If you are not analyzing solutions of a toxic nature, leave the vapor outlet uncovered.

Heat hazards

An open flame, burners, and other hot surfaces can present heat hazards that can result in severe burns.

When operating a flame system, always operate your spectrometer with the flame shield closed, and the sample compartment front panel in place. Keep your hands out of the sample compartment while a flame is burning.

When operating a flame system make sure that the chimney is in place. Before you touch the instrument chimney, turn off the flame and allow the chimney to cool.

WARNING

Hot Surface

The burner and flame compartment become extremely hot during instrument operation and remain hot for some time after the instrument has been switched off.

Allow the system time to cool before attempting to access the burner or sample compartment components.

Always use protective gloves when removing a burner from the instrument.

Perchloric acid

WARNING

Explosion Hazard, Fire Hazard

Aspiration of perchloric acid and perchlorates into a nitrous oxide-acetylene flame can create an explosion hazard which can result in death or serious injury, including temporary or permanent impairment of hearing.

Safety Practices and Hazards

22 Agilent 240/280 Series AA (including Zeeman)

Do not use perchloric acid unless it is absolutely essential for sample preparation. If perchloric acid must be used, it may be possible to reduce the risk of explosion by taking the following measures: Use an air-acetylene flame instead of a nitrous oxide-acetylene flame. Reduce the concentration of perchloric acid and metal in all analytical

solutions to the lowest practicable level. The concentration of perchloric acid should be reduced in the digestion stage and further reduced by extending the fuming stage.

Aspirate all solutions for the shortest practicable period. Aspirate distilled water between samples. Minimize the aspiration of air. Use separate spray chamber/liquid trap and drain assemblies for perchloric

acid analyses and organic solvent analyses to prevent perchloric acid from mixing with organic solvent residues.

NOTE When solvent extractions of perchloric solutions are performed, some of the acid may dissolve in the organic solvent that is subsequently aspirated. Also, if the organic solution is aspirated while floating on the surface of the acid, do not allow the capillary tube to drop below the organic layer and suck up aqueous perchloric acid.

When using perchloric acid, wear approved ear protectors and approved safety glasses and ensure that all instrument safety covers are in position.

Flashbacks

A flashback is an explosion of the gas mixture in the spray chamber, which can occur for several reasons. For more details, refer to the SpectrAA software Help.

Agilent AA spectrometers have several safety features in place to prevent flashbacks, and flashbacks are very rare in circumstances where instruments are properly maintained.

In the rare event that a flashback does occur, the Agilent AA instrument safety features are designed to safely relieve the pressure and minimize damage. In addition to reading the list below, refer to the Maintenance section of this Users Guide and the SpectrAA software Help for recommended maintenance procedures to prevent flashbacks.

Safety Practices and Hazards

Agilent 240/280 Series AA (including Zeeman) 23

Analysis over many years has shown that in most cases, flashbacks are associated with one or more of the following points. If you experience a flashback, check this list to see if any of the points are relevant, and take steps to remedy the situation. 1 Keep the burner clean. Deposits must not be allowed to build up in or on the

burner slot because they can partially block it. Blockages can cause the pressure to build up in the spray chamber and breach the seal provided by the liquid trap. Alternatively, glowing particles can fall down through the slot into the spray chamber and ignite the combustible gas mixture inside.

Be especially careful of very small deposits in the ends of the burner slot because they disrupt the laminar gas flow and allow the flame to burn back into the spraychamber at Flame Off when the gas flow is reduced.

The use of a hard object to brush off glowing carbon particles during flame operation is not recommended because of the increased risk of knocking one of the particles down the slot.

When using an organic solvent, a reduced uptake rate should be used to restrict the amount of liquid fuel that is fed to the flame.

2 The width of the burner slot must not exceed the maximum design specifications: Mark 7 0.46 mm (0.0181 in) for N2O/Acetylene burner Mark 7 0.54 mm (0.021 in) for Air/Acetylene burner

Even a small increase in width can greatly increase the possibility of a flashback occurring. The burner slot must be regularly cleaned according to the instructions included in the Maintenance chapter of this manual.

3 Ensure that the spray chamber and liquid trap are kept clean. If dirty solutions are being analyzed (for example, engine oils), ensure that the spray chamber, liquid trap, float, and drain tube are regularly cleaned and flushed with a suitable solvent so that sludge does not build up in the parts.

4 Ensure that the correct O-rings are used on the burner, nebulizer block and nebulizer, and that they remain undamaged. Damage to O-rings in the spray chamber can result in the leakage of gas that can be ignited by the flame and in turn set fire to the spray chamber. Damage to O-rings in the nebulizer can allow leakage of the oxidant that can reduce the total flow of gas through the burner slot and so increase the possibility of a flashback occurring. Any cracked or deformed O-rings must be replaced immediately. Ensure O-rings are correctly seated in the spray chamber, burner and flame

Safety Practices and Hazards

24 Agilent 240/280 Series AA (including Zeeman)

adjuster barbs prior to reassembly. (See the Maintenance and Troubleshooting section on Page 57.)

5 The liquid trap must be filled with the same solution as the matrix used for the standards and samples.

6 The drain tube must be attached to the lower nipple of the liquid trap. The tubing must slope downwards all the way to the drain vessel so that the waste liquid drains smoothly. The end of the drain tube must not be allowed to drop below the level of the liquid in the vessel. (Conversely, the level of liquid must not be allowed to rise sufficiently to cover the end of the tube.)

When using organic or toxic liquids in the spray chamber, a vent tube must be attached to the upper vent nipple of the liquid trap. It must slope downwards (running parallel to the drain tube) to prevent it becoming blocked should any liquid drain out, and be vented to an active exhaust system. All the above points must be observed because a sudden surge of waste liquid can affect the pressure in the spray chamber and result in a flashback.

7 Since N2O is stored in the cylinder under pressure as a liquid, when it expands through the regulator it can cool the regulator sufficiently to form ice on the outside and prevent it from operating correctly. Prevent freezing by using a heater on the N2O regulator on the supply cylinder. Contact the supplier of the regulator for a suitable heater.

8 As free acetylene is unstable at elevated pressure, it has to be stored in the cylinder by dissolving it in acetone. If the gas is withdrawn too quickly, or the cylinder pressure is allowed to drop below 700 kPa, acetone may be drawn off in sufficient quantities to affect analytical performance, damage seals, O-rings and hoses, or even cause a flashback. Observe the recommendations concerning the use of acetylene.

9 Where possible, do not perform digests with perchloric acid. As this acid is known for forming unstable salts, operators using this acid should ensure that the minimum amount is allowed to reach the spectrometer, and that the burner, spray chamber and liquid trap are thoroughly cleaned after each analysis to ensure that unstable salts are not allowed to build up. Failure to do this can result in unpredictable flashbacks.

10 Aspirating solutions (especially alkaline/ammoniacal ones) that contain high concentrations of Ag and Cu can lead to the formation of acetylides that can spontaneously decompose and cause a flashback.

Safety Practices and Hazards

Agilent 240/280 Series AA (including Zeeman) 25

What to do in the Event of a Flashback

Turn off the gas supply at the regulator. Turn off power to the instrument. Ensure the general area around the instrument safe by cleaning up and spills

in the sample introduction area or on the instrument Burners involved in a flashback event should not be re-used. Contact and report the incident to your local Agilent service representative

before commencing operation of the instrument.

Resuming Operation after a Flashback

A burner that has experienced a flashback should be considered damaged and destroyed. Once a flashback has occurred there is no guarantee that the slot of the burner has not become distorted and/or enlarged to the point that it is out of production specifications. Inspect the sample introduction components including the spray chamber and

nebulizer. Clean or replace as necessary. Check the new burner condition and O-ring for damage. Check the glass impact bead. Check the O-rings within the spraychamber, especially the pressure relief

bung for damage. Check the nebulizer for damage. Check the optical windows on either side of the flame area for damage. Ensure the waste tubing is out of the liquid. Check waste container.

Review the relevant Safety section in this manual or the section above for detailed information on how to prevent flashbacks.

For applications that create high particulate deposits on the burner, it is recommended that additional burner cleaning/maintenance be performed. Contact Agilent for assistance if your application requires additional cleaning procedures.

Safety Practices and Hazards

26 Agilent 240/280 Series AA (including Zeeman)

Furnace and Zeeman operation

Gases

The graphite tube atomizer gas supply system is designed for use with inert gases and air.

Never use pure hydrogen with the graphite tube atomizer since this could result in leakage and potentially explosive accumulation of hydrogen. You may, however, use a proprietary, prepackaged mixture of 95% argon (or nitrogen) and 5% hydrogen. Never attempt to create your own mixture of hydrogen and an inert gas for use with the GTA system.

Heat hazards

A hot furnace atomizer can present heat hazards that can result in severe burns to personnel. Never put your hands in the sample compartment while you are operating your furnace.

Allow the furnace atomizer to cool before removing it from the sample compartment.

Vapors and fumes

Never place your head over the graphite tube atomizer while it is operating. This could cause inhalation of hazardous or toxic fumes, or your skin and eyes could be injured by corrosive vapors or fumes.

The chimney or the optional exhaust accessory must be in place for furnace operation to ensure that toxic vapors and heat are exhausted.

UV radiation

When viewing the sample during the drying stage, use only a rear coated mirror (as supplied) or the Tube-CAM option. Never look directly at the furnace during either the ash or atomize stages.

Magnetic field (Zeeman only)

The magnet produces a variable magnetic field of up to 0.8 Tesla peak at mains frequency in the workhead during the read stage.

To avoid interference with heart pacemakers or magnetic storage media, keep them at least 300 mm from the magnet.

Introduction

Agilent 240/280 Series AA (including Zeeman) 27

2Introduction Instrument Overview 28 Installation requirements 33 Electrical Connections 34 Gas supplies 36

The Agilent 200 series AA spectrometers are controlled by Agilents innovative AA worksheet software. The Agilent series AA includes the following instruments:

This documentation is appropriate for the 240FS AA, 240Z AA, 280FS AA, and 280Z AA instruments.

The software is based on a spreadsheet that mimics an analysts workbook and combines flame, furnace, Zeeman, and vapor operation in one integrated package.

The SpectrAA Base, PRO and CFR software versions run under Windows 10 64-bit operating systems, and provides the following: Innovative, easy to use interface Dedicated function keys for critical functions Extensive Help including audio and video demonstrations of how to set up

your instrument Tool Tips state the allowed range for each field Comprehensive error system The capacity to simultaneously operate one flame and one furnace (deuterium

or Zeeman) spectrometer simultaneously from one computer (requires SpectrAA PRO version software)

Features to assist users to achieve compliance with US FDA 21 CFR Part 11 requirements (optional CFR version only)

Introduction

28 Agilent 240/280 Series AA (including Zeeman)

Instrument Overview

Flame instruments front view

Where: 1. Flame shield 7. Flame-on button 2. Burner adjustment handles 8. Instrument status LED 3. Burner height adjustment 9. Power switch 4. Nebulizer and flow adjustment 10. Spray chamber and liquid trap assembly

(behind the grey cover) 5. Impact bead adjustment 11. Lamp compartment (Four lamps are shown

here. An eight lamp compartment is also available.) 6. Flame-off button

6 7

8 9

11 1

2

3

4 5

10

Introduction

Agilent 240/280 Series AA (including Zeeman) 29

Flame instruments back view

Where: 1. Accessories serial port, such as the GTA Viewing/Fume Extraction accessory

7. Acetylene (C2H2) gas line

2. USB camera cable port 8. Air gas line 3. IEEE 488 cable port 9. Nitrous oxide (N2O) gas line 4. Power cable 10. Air purge port 5. Fuse and power setting housing 11. SIPS pump option port 6. UltrAA lamp option ports

5 4

11

1 2 3

6 8 7 9

10

Introduction

30 Agilent 240/280 Series AA (including Zeeman)

Furnace (Zeeman) instruments front view

Where: 1. GTA 120 Graphite Tube Atomizer 7. Zeeman AA instrument status LED and

power switch 2. Zeeman workhead 8. PSD 120 waste port 3. PSD 120 sample tray 9. PSD 120 rinse tube 4. PSD 120 Programmable Sample Dispenser

10. PSD 120 probe

5. Rinse solution 11. Lamp compartment (Eight lamps are shown here. A four lamp compartment is also available.)

6. GTA 120 instrument status LED and power switch

See the Users Guides supplied with the GTA 120 and PSD 120 for more information about those accessories.

1

2

3

4

5

6

7 8 9 10

11

Introduction

Agilent 240/280 Series AA (including Zeeman) 31

Furnace (Zeeman) instrument back view

Where: 1. Accessories serial port, such as the GTA Viewing/Fume Extraction accessory

8. GTA 120 power cable

2. USB camera cable port 9. GTA 120 fuses 3. AA instrument IEEE 488 cable port 10. Water in 4. Power cable 11. Water out 5. UltrAA lamp option port 12. Alternate gas inlet, typically nitrogen or air 6. UltrAA accessory and fuses 13. Normal gas inlet, typically argon 7. Air purge port 14. GTA 120 IEEE 488 cable port

1 2 3

7 5 6 8 9

10

11

12 13

14

4

Introduction

32 Agilent 240/280 Series AA (including Zeeman)

Furnace (D2) instruments front view (240FS with GTA 120 accessory fitted)

Where: 1. GTA 120 Graphite Tube Atomizer 8. AA instrument power switch 2. Flame shield 9. Burner height adjustment 3. Burner adjustment handles 10. Impact bead adjustment 4. GTA 120 instrument status LED and power switch

11. Nebulizer and flow adjustment

5. Flame-off button 12. Spray chamber and liquid trap assembly (behind the grey cover)

6. Flame-on button 13. Lamp compartment (Four lamps are shown here. An eight lamp compartment is also available.)

7. Instrument status LED

See the Users Guide supplied with the GTA 120 for more information about this accessory.

1

2

3

4

7

13

6 5 8 10 11 12 9

Introduction

Agilent 240/280 Series AA (including Zeeman) 33

Furnace (D2) instruments back view (240FS with GTA 120 accessory fitted)

Where: 1. Accessories serial port, such as the GTA Viewing/Fume Extraction Accessory

10. SIPS pump option port

2. USB camera cable port 11. Air purge port 3. AA instrument IEEE 488 cable port 12. GTA 120 power cable 4. AA instrument power cable 13. GTA 120 fuses 5. AA instrument fuse and power setting housing 14. Water in 6. UltrAA lamp option ports 15. Water out 7. Acetylene (C2H2) gas line 16. Alternate gas inlet, typically nitrogen or air 8. Air gas line 17. Normal gas inlet, typically argon 9. Nitrous oxide (N2O) gas line 18. GTA 120 IEEE 488 cable port

Installation requirements

Before you receive your instrument, you are given an Agilent AA Site Preparation Guide; which describes the environmental and operating requirements of the Agilent AA system. Prepare your laboratory according to those instructions before the Agilent AA can be installed. Keep the Site Preparation Guide for future reference. If you have misplaced your copy, you can obtain a replacement from your local Agilent office or the website at www.agilent.com.

1 2 3

5 4 11 6 8 7 9 10 12 13

14

15

16 17

18

Introduction

34 Agilent 240/280 Series AA (including Zeeman)

Electrical Connections

Rear of instrument: IEEE 488 Accessory, 9-way female D-range type Accessory, MCA, 6-way DIN type (AA280FS and AA280Z only) USB port, optional UltrAA lamp connections: Burndy circular 6-way, optional (actual number

depends on the model and option selected)

WARNING

Shock Hazard High voltage To maintain safety, only the UltrAA lamp power supplies should be used at these connections.

Some pins will become energized (300 VDC) when an UltrAA lamp is in a matching socket. To avoid death or electric shock, NEVER touch any exposed pins.

Certaines broches du culot des lampes sont sous tension (300 VCC) la mise en place dune UltrAA lampe. Pour viter llectrocution ou la mort, ne jamais toucher les broches sous tension.

Front of instrument: Zeeman workhead CPC 14 way connection behind the left cover (Zeeman

only).

WARNING

Shock Hazard To prevent connector damage, switch OFF the instrument before inserting the plug and always turn the locknut fully clockwise to the detent position. To maintain safety, only the Zeeman workhead connector should be used at this connection.

Lamp bay: Deuterium lamp:

Molex 3-way connection, in lamp compartment (behind lamp panel in lamp compartment on 240/280 series AA instruments).

Introduction

Agilent 240/280 Series AA (including Zeeman) 35

WARNING

Shock Hazard To maintain safety, only the deuterium lamp should be used at these connections.

Hollow cathode lamps: Four lamp capacity on the 240 series AA Eight lamp capacity on the 280 series AA

WARNING

Shock Hazard High voltage To maintain safety, only hollow cathode lamps should be used at these connections.

Fuses

CAUTION For continued protection against fire hazard replace fuse only with same type and rating.

Non-Zeeman 240 series AA T4 A H250 V, 5 x 20 mm (100120 & 220240 VAC) 280FS AA T4 A H250 V, 5 x 20 mm (100120 & 220240 VAC) Zeeman 240Z/280Z AA 15 A long delayed-action circuit breaker with a thermal cutout. T3.15 A H 250 V, 5 x 20 mm (208240 VAC) F315 mA L 250 V, 5 x 20 mm (208240 VAC) F1A L 250 V, 5 x 20 mm (208240 VAC) T6.3 A L 250 V, 5 x 20 F800 mA L 250 V, 5 x 20 mm (208240 VAC)

NOTE For safety reasons, any other internal fuse or circuit breaker is not operator accessible and should be replaced only by Agilent field service engineers.

Fuse information on the rear of the instrument is the most up to date.

Introduction

36 Agilent 240/280 Series AA (including Zeeman)

Gas supplies

Acetylene (C2H2) Air Nitrous oxide (N2O) Air purge Instrument grade

>99.5% pure Must be clean and dry. (Air filter to be used if required)

Instrument grade >99.5% pure

Allowed range 65100 kPa (9.514.5psi)

245455 kPa (3565 psi)

245455 kPa (3565 psi)

245455 kPa (3565 psi)

Recommended 75 kPa (11 psi) 350 kPa (50 psi) 350 kPa (50 psi) Typical flow rate 010 (L/min) 13.5-20 (L/min) 1116 (L/min) 10 (L/min) Connection 1.8 m (6 ft) length of

6.3 mm (1/4 in) ID red hose with 9/16 in- 18UNF L/H thread fitting#

1.8 m (6 ft) length of 6.3 mm (1/4 in) ID black hose with 9/16 in-18UNF fitting#

1.8 m (6 ft) length of 6.3 mm (1/4 in) ID blue hose with 3/4 in- 16UNF fitting#

Barb to take 6.3 mm (1/4 in) hose

#Adaptors are available

Other gas connections

Sample compartment: Push-on Air/N2O connector for burner Push-on C2H2 connector for burner

Installation

Agilent 240/280 Series AA (including Zeeman) 37

3Installation PC requirements 37 Installation procedure overview 38 GPIB communications 38 Connecting and configuring an Agilent AA spectrometer Duo system 39 Configuring the SPS 4 autosampler 41 Configuring the software to use manual sampling 42 USB to RS-232 interfaces 43 Starting the SpectrAA software 44 SpectrAA Release Notes and Software Status Bulletin 44 Installing the drivers for the Tube-CAM Furnace Camera option 45 Printer setup 45 Troubleshooting 45 Service installation module 45

This chapter describes how to prepare your personal computer (PC) and printer for use with the Agilent AA system and install the SpectrAA software on your PC.

Do not position the equipment or accessories so that it is difficult to operate the disconnecting device. This section covers the installation of the Agilent SpectrAA software for 240/280 series AA instruments. Instructions for installing, operating, and maintaining the instruments and components are included in the SpectrAA Help (see Page 51). Operating instructions for the Sample Introduction Pump System (SIPS) and other AA accessories are given in the manuals accompanying the accessories or in the SpectrAA Help

PC requirements

If you are supplying your own PC for use with an Agilent AA instrument, the recommended configurations of that PC are listed in the AA Site Preparation Guide.

Installation

38 Agilent 240/280 Series AA (including Zeeman)

Installation procedure overview

There are four software installation scenarios: SpectrAA Base SpectrAA PRO SpectrAA Base to PRO upgrade SpectrAA CFR

For installation instructions, refer to the appropriate instructions supplied with your software: SpectrAA Software installation instructions SpectrAA Software Installation Instructions for 21 CFR Part 11 Environments

GPIB communications

A USB-GPIB converter must be installed in your computer to interface the computer and the Agilent AA. See below for information on installing the USB-GPIB converter.

NOTE Although the Agilent field service engineer will install the GPIB communications device for you during the installation process, you may need to configure the driver yourself at some later stage, for example if you change the PC.

Installing the USB-GPIB converter

To install a USB-GPIB converter:

NOTE Ensure that the SpectrAA software has been installed ensuring the relevant driver (either National Instruments OR AD-Link) is selected during the installation.

1 Turn off the computer. 2 Connect one end of the converter to the instrument and the other end to the

USB connection on the back of the computer. 3 Turn on the computer.

Installation

Agilent 240/280 Series AA (including Zeeman) 39

Connecting and configuring an Agilent AA spectrometer Duo system

Setting up for Duo operation and connecting the IEEE cables

NOTE This function is not available in the SpectrAA Base version.

NOTE Install SpectrAA Base and PRO or CFR software and the USB-GPIB converter first before performing this procedure.

To set up and connect an AA Duo system: 1 Open SpectrAA. 2 On the Index page, click the instrument link on the left side of the page. The

SpectrAA Instrument Configuration dialog box opens. 3 Ensure Duo system is not ticked and that an instrument is selected in the

Instrument #1 tab. 4 Restart SpectrAA to save the configuration changes. 5 Connect both instruments to the PC using IEEE cables as shown in the

following diagram. Do not turn on the instruments.

Figure 2. Example of a Flame and Zeeman instrument connected with a GTA

6 Return to the Index page of SpectrAA and reopen the SpectrAA Instrument Configuration dialog box.

7 Select the Duo System checkbox. 8 Select the appropriate models in the drop-down box for Instruments #1 and #2.

NOTE If you are running a Duo system that includes an Agilent 55B AA instrument, the 55B AA MUST be entered as Instrument #1 in the SpectrAA Instrument Configuration dialog box.

9 Click OK to close the dialog box. 10 Restart SpectrAA to save the configuration settings. 11 Go to the next section Configuring the IEEE addresses for Agilent AA Duo

operation.

Instrument #1 Flame

Instrument

Instrument #2 Zeeman

Instrument PC GTA

Or other optional accessory

Installation

40 Agilent 240/280 Series AA (including Zeeman)

Configuring the IEEE addresses for Agilent AA Duo operation

If you are running an Agilent AA Duo system, you must reconfigure one of the instruments so they have different IEEE addresses. Agilent 55B AA instruments should have a default IEEE address of 1. Agilent 240FS AA, 240Z AA, 280FS AA and 280Z AA instruments should have a default IEEE address of 9. Because 55B AAs must be Instrument #1 in the configuration dialog, Instrument #2 will always have a default IEEE of 9. It is important not to change the IEEE address of a 55B AA as it may cause conflicts with the inbuilt computer. 1 Close SpectrAA if it is open. 2 Navigate to C:\Program Files (x86)\Agilent\sp100\Run and then double-click

DUAL.EXE. Click OK to start the program. 3 A window appears asking you to turn on the instrument you wish to

reconfigure. You must select Instrument #2 in the configuration. Switch on Instrument #2 and then click OK. Do not turn on the Instrument #1. A command window is displayed. The process may take about a minute. During this time, you will hear the instrument resetting. Once the process is complete, a message appears in the command window saying Addr changed from 9 to 8. Press any key to continue If this message does not appear, continue the procedure below. If it does appear, you have completed the setup.

4 In the search field type cmd.exe. Select cmd.exe from the list that appears.

5 Turn on Instrument #1 and Instrument #2, if not on. 6 Choose one of the following options:

For a Duo system with a 55B AA: Type: CD C:\Program Files (x86)\Agilent\SP100\Run\ and then press Enter. Type: setaddr.exe q1:8 and then press Enter.

For a Duo system without a 55B AA: Type: CD C:\Program Files (x86)\Agilent\SP100\Run\ and then press Enter. Type: setaddr.exe q9:8 and then press Enter.

The process may take about a minute after which a dialog will appear saying that both addresses (1 and 8 or 8 and 9) are found.

7 Restart the computer, turn on both AA instruments, and then start the Agilent SpectrAA software.

Installation

Agilent 240/280 Series AA (including Zeeman) 41

The instruments are now ready to be used as a Duo system. Refer to the Help for further information on dual instrument operation.

NOTE Duo mode will only work if the instrument selected as Instrument #1 in the SpectrAA Instrument Configuration dialog box retains its default IEEE address (that is, 1 for 55B or 9 for 240FS, 240Z, 280FS or 280Z.

NOTE During dual instrument operation, do not turn any connected instrument ON or OFF while readings are being taken.

NOTE You can only operate in Duo mode with one of each accessory type connected. That is, one GTA and one PSD and one SPS 3/SPS 4.

For the Base version of SpectrAA software, the check box will show one instrument.

NOTE For more information about changing the Duo system configuration or to revert back to single instrument use, see the Setup Agilent AA Duo operation instructions in the How to section in the SpectrAA Help.

Configuring the SPS 4 autosampler

To configure the SPS 4 autosampler: 1 Shut down the SpectrAA software if it is open. 2 Follow the instructions provided in the SPS 4 Autosampler Users Guide to set

up the hardware. 3 Plug one end of the USB cable into the USB port on the autosampler and the

other end into a USB port on the computer. 4 Navigate to C:\Program Files (x86)\Agilent\SP100\Run. 5 Double-click the IHelper.EXE application. 6 Click the Accessories tab. 7 Select Agilent SPS 4 Autosampler in the Flame Auto Sampler section if

needed. 8 Click OK to save the changes. 9 Continue to Installing the SpectrAA PRO software if applicable or skip to GPIB

Communications on Page 38.

Installation

42 Agilent 240/280 Series AA (including Zeeman)

Determining the SPS 4 COM port

When running the Calibration Wizard, you must select the SPS 4 COM port to start communication between the SPS 4 and the PC. The following procedure explains how to determine the COM port.

For information on how to use the Calibration Wizard, see the SPS 4 Autosampler Users Guide or the SpectrAA Help > Accessories >SPS 4 section.

To determine the COM port: 1 Right-click on Start and then select Device Manager. 2 Expand Ports. 3 Find the SPS4 USB Interface and note the assigned COM port (COM5 in the

example shown below).

Figure 3. Example of SPS 4 USB interface COM port

Configuring the software to use manual sampling

If you are NOT using any flame autosamplers, set the Sampler Type in the Accessories tab of SpectrAA Instrument Configuration dialog box to the SPS 5 Autosampler. The SPS 5 Autosampler uses IEEE communications instead of RS- 232 communications. By specifying the flame autosampler type as the SPS 5 Autosampler (even though no autosampler is used), the software will not capture the RS-232 port during start-up or shut down of the SpectrAA software. This will minimize delays during start-up, operation, and shut down of the software.

To define the SPS 5 flame autosampler: 1 Activate the IHelper.EXE application (from the installation drive: \Program Files

(x86)\Agilent\SP100\Run directory); OR click the model number displayed at the Main Index page of the SpectrAA software. This displays the SpectrAA Instrument Configuration dialog box.

Installation

Agilent 240/280 Series AA (including Zeeman) 43

2 From the SpectrAA Instrument Configuration dialog box, click the Accessories tab.

3 Select Varian SPS5 Autosampler in the Flame Auto Sampler section. 4 To complete the installation and configuration, shut down and restart the

SpectrAA software, as prompted.

USB to RS-232 interfaces

There are several USB to RS-232 adapters available for use on computers that are not fitted with or not equipped with sufficient RS-232 interfaces. Depending on the instrument configuration, operation of all accessories may require the use of two RS-232 interfaces: An RS-232 interface is required for operation with the SPS 3 autosampler Another RS-232 interface is required for software control of the ETC 60

Electrothermal Temperature Controller.

NOTE Other modem and LIMS system may be also connected to the available RS-232 COM ports.

Where there are not enough RS-232 interfaces to support all the devices that use these COM ports, an acceptable alternative is to use a USB to RS-232 adapter.

To use a USB to RS-232 adapter: 1 Install the USB-RS-232 device according to the manufacturers specification. 2 Right-click on Start and then select Device Manager. Locate the COM USB

Com port and open Properties. 3 Select the Port Settings tab and open the Advanced settings. 4 Set the COM PORT number to 1 to 4 using an available number from the drop-

down list. If the numbers are already used, you have to set one of the other Com ports to a higher number and then set the one you are going to use to the vacancy created. SpectrAA software only accepts values from 1 to 4.

5 Close all dialog boxes. 6 Shut down and restart the computer. You may need to repeat this process if

the port was not enabled the first time due to it being used by another device.

Installation

44 Agilent 240/280 Series AA (including Zeeman)

Starting the SpectrAA software

To start the SpectrAA software: 1 Double-click the SpectrAA icon on the desktop. 2 The first time the SpectrAA software is opened a Software Registration dialog

appears. Click Next.

NOTE Ensure that the user of the SpectrAA software completes the software registration. For further information, refer to the Software Registration Help.

3 Complete all the fields on the Customer Details page. Click Next.

NOTE The Product Key is found on the cover of the Agilent SpectrAA software CD case that was delivered with the instrument.

4 Complete all the fields on the Product Details page. Click Next. 5 Complete all the fields on the Work Environment Details page. 6 Click Register. 7 A dialog appears stating Your Agilent Software Registration has been

successful.

NOTE If your computer is not connected to the Internet, refer to the Software Registration Help for further information.

8 The application will now open, and you can collect your data.

SpectrAA Release Notes and Software Status Bulletin

Refer to the SpectrAAReleaseNotes.pdf file in the installation directory and the Software Status Bulletin document for further details. The file includes latest release information and important notes including the detail of any known problems and suggested work-arounds.

Installation

Agilent 240/280 Series AA (including Zeeman) 45

Installing the drivers for the Tube-CAM Furnace Camera option

For instructions on how to install the Tube-CAM drivers, see the Tube-CAM Furnace Video Option Software Installation Instructions that came with your accessory.

Printer setup

The printer must be a make and model supported by Microsoft Windows. To install your printer, follow the instructions provided with the printer. For more information, refer to your printer documentation or Microsoft Windows Help.

Troubleshooting

This section contains solutions to some common problems you may encounter during the installation of the SpectrAA software.

The SpectrAA software is not communicating with the instrument. Ensure that the computer has been restarted after installing the software and

USB-GPIB converter. Check the cables and connections. Check that the instrument and any associated accessories are turned on. Check that you are not running the Simulator software. (Select Help about

system information.)

Service installation module

The installation test software is accessed directly from the Administration window. As shown below, this control is only activated when the software has

Installation

46 Agilent 240/280 Series AA (including Zeeman)

been installed. This software must be installed from the Service folder of the BASE UFD.

To do this: 1 Insert the SpectrAA Base UFD into a USB port on the computer. 2 Use Windows Explorer to open the Service folder D:\service, where D is the

USB drive letter. 3 Locate and run the setup.exe file to install the necessary components and

enable the VALIDATE button in the Administration window.

Installation and commissioning tests can be selected and run from the Installation test window that is displayed. This allows easy testing and provides a report of the tests conducted covering power-on self-tests, safety interlocks, and wavelength performance checks.

Software Overview

Agilent 240/280 Series AA (including Zeeman) 47

4Software Overview Starting the SpectrAA software 47 SpectrAA windows 47 Working with the SpectrAA software 50 Help 51

The Agilent AA system software (SpectrAA) is a powerful interface that provides high levels of spectrometer control and is easy to use. This chapter provides a brief overview of the SpectrAA software to help you familiarize yourself with its various windows. A more detailed description and instructions for use are included in the extensive Help. The optional SpectrAA CFR version software offers you the tools to help you achieve compliance with the US FDA 21 CFR Part 11 requirements. More information on the CFR compliance features of the software is detailed in the Help.

Starting the SpectrAA software

To start the SpectrAA software double-click on the desktop SpectrAA icon (created during the installation of the software).

SpectrAA windows

Index page

When you start the SpectrAA software, the first screen to appear is the introductory screen.

The Index page contains four buttons: Worksheet, Reports, Administration, and Exit.

Software Overview

48 Agilent 240/280 Series AA (including Zeeman)

The function of each button is as follows: Worksheet Opens the Worksheet window (see Page 48) Reports Opens the Reports window (see Page 49) Administration Opens the Administration window (see Page 50) Exit Shuts down the SpectrAA software.

Worksheet window

The Worksheet window allows you to develop and edit methods, sequences and labels, and initiate sample analysis.

The worksheet is the fundamental file type for SpectrAA, containing one or more methods, sample labels, sequence information, and analytical results. You can load an existing worksheet or develop a new one.

The Worksheet window consists of four tabbed pages: Filing, Develop, Labels, and Analysis. To access a particular page, click on the appropriate page tab appearing under the menu bar.

The Filing page

Use the Filing page to perform basic worksheet operations such as opening, saving, and closing worksheets, creating a template from a worksheet, and loading worksheets. You can also view information about the worksheet currently open. If you have the CFR version of the software, the Filing page enables you to apply electronic signatures (approval) to the worksheet.

The Develop page

Use the Develop page to add, delete, review and modify methods, modify sequence parameters, change the order of methods and copy methods to the Method Library.

The Labels page

Use the Labels page to set up solution labels, weights, volumes, and dilution factors and to configure SPS or PSD samplers.

The Analysis page

Use the Analysis page to control the AA and initiate analysis. Data is presented in the form of a spreadsheet, with one row per sample. The sample labels are displayed in the left-hand column with concentration results for each element across the remaining columns.

Software Overview

Agilent 240/280 Series AA (including Zeeman) 49

The SpectrAA software enables you to have up to a maximum of 10 worksheets open at the same time. The Worksheet tab at the bottom of the Analysis page enables you to switch between worksheets.

Worksheet menus

When you are viewing the worksheet, the following menu items are available: File This menu allows you to perform filing tasks such as opening, saving and renaming

files. Edit The Edit menu allows you to copy and paste information, Edit Replicates and Go To

certain parts of a worksheet. View The View menu enables you to nominate what is displayed on the Analysis page. Instrument This menu enables you to perform many Instrument functions such as Optimization,

Reslope, and Zero. Options The Options menu enables you to alter the displays on the Analysis page. Window This menu enables you to quickly move around the software. Help This menu enables you to access the Help.

NOTE Not all menu items are available on all pages of the Worksheet window. If an item or menu is grayed, it is unavailable on that page.

Menu items can be accessed by clicking the desired item with the mouse, or pressing Alt and the active (underlined) letter in the menu name (for example, Alt+E to access the Edit menu). This displays a menu list. The options in the menu list can be accessed in the same manner.

Reports window

The Reports window allows you to generate a report for the current worksheet or any of the worksheets saved in the system.

The Reports window consists of four tabbed pages: Worksheet, Select, Settings, and Report. To select a particular page, click on the appropriate page tab appearing under the menu bar.

Worksheet page

Use the Worksheet page to select the worksheet results to include in the report. You can use the Filter and Search buttons to refine your search.

Select page

Use the Select page to choose methods and solutions to include in the report.

Settings page

Use the Settings page to specify the report style and content.

Software Overview

50 Agilent 240/280 Series AA (including Zeeman)

Report page

Use the Report page to view and print the report, write it to a text file, or export it to a PRN file.

Administration window

The Administration window allows you to: migrate worksheets into the system (such as old worksheets on CD-ROM, etc.); delete worksheets and library methods; and activate and modify password protection of the system. The Administration window also allows you to configure your system.

Working with the SpectrAA software

Menu bar

The Worksheet window contains a menu bar directly beneath the window title bar. This bar displays several menu items. For more information on these menus, see Page 49.

NOTE When menu items or options appear grayed, they are unavailable for selection.

Toolbar

The Toolbar appears on the Index page and the Worksheet window and provides easy shortcuts to many common functions and other windows.

Dialog boxes

In some cases, selecting a menu option or pressing a button activates a dialog box. This is a box that contains several different input fields relevant to that operation.

You can move the focus from field to field in a dialog box either by clicking each entry item with the mouse or by pressing the Tab and arrow keys to move the cursor from field to field. After entering/changing any values in a dialog box, press OK to accept the changes and close the dialog.

Software Overview

Agilent 240/280 Series AA (including Zeeman) 51

Help

The SpectrAA software contains extensive Help, which serves as your primary source of information on how to use the software and the instrument. The Help consists of contextual help and multimedia help. The Help also contains an extensive How To section. This section provides many set by set instructions on how to perform common procedures.

The contextual help is accessed from any window, page, or dialog box in the SpectrAA software by pressing F1 (the Help function key), the Help button (where available), or by selecting On-line Help from the Help menu at the top of any page in the Worksheet window and provides help specific to that screen.

The multimedia help contains hardware-related information and other details to help you set up, operate and maintain your Agilent AA instrument.

For example, the Help includes: Installation procedures for the components of the instrument that are

customer-installable Maintenance procedures for the parts of the spectrometer that are customer-

serviceable Checklists to help you ensure that you have correctly prepared your system for

analysis.

Searching for help

You can quickly get help on a specific topic using keywords and the Search facility.

To search for information on a particular subject: 1 Open the Help (if it is not already open). 2 Select the Search tab at the top of the SpectrAA Help window. 3 Enter the word(s) you want to search for in the field provided and select List

Topics. 4 A list of all the Help topics associated with the keyword(s) displays in the

second list. 5 Select the desired topic and click Display.

Software Overview

52 Agilent 240/280 Series AA (including Zeeman)

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Getting Started

Agilent 240/280 Series AA (including Zeeman) 53

5Getting Started Instrument setup 53 Starting the system 55 Pre-analysis checklist 55

This chapter describes how to set up the Agilent AA system for analysis and get you started using the instrument.

You should have already: Prepared your PC and installed the SpectrAA software described in Chapter 3. Become familiar with the SpectrAA user interface as described in Chapter 4.

Instrument setup

Use the following checklist to ensure that you set up your system correctly. You must: Connect the components of the system to one another (see Connections on

Page 53). Connect the equipment to the power supply and check the setting of the two

voltage taps where fitted (see Power on Page 54). Install the hardware components as per your analytical requirements. Refer to

the Help for details.

Connections

Your Agilent AA instrument is supplied with a set of gas hose fittings and a mains cable that suits the common utility standard in the local region. A Country Kit must be ordered with the Agilent AA instrument.

Power

The mains power connection is located at the rear of the instrument. Refer to the next section for instructions on connecting the instrument to the mains power supply.

Getting Started

54 Agilent 240/280 Series AA (including Zeeman)

Gas hoses

Three rubber hoses are permanently attached to the instrument. Each hose is 1.8 meters long and is color-coded for air (black), nitrous oxide (blue), and acetylene (red). Each is fitted with female fittings suitable for USA standard regulators. Adaptors are supplied for other areas.

NOTE Gas hose connections are not detailed in this section as they are described in your Agilent AA Site Preparation Guide.

Accessories

For details on connecting accessories such as SIPS or UltrAA lamps, refer to the manuals accompanying the accessories.

Power

Requirements

Power requirements are detailed in your Agilent AA Site Preparation Guide. Check the power requirements and read through the section Electrical power supplies in the Site Preparation Guide before connecting the Agilent AA system to the power supply.

Consult the manuals supplied with your printer and PC (if required) for their power requirements.

Connection

Before connecting the instrument to the power supply, ensure that both the spectrometer and the mains power supply are turned off. Check that the two voltage selector switches on the instrument rear panel (if present) are set to the correct mains power supply voltagerefer to the table on the rear panel. The Agilent field service engineer sets the voltage selectors when the instrument is first installed.

To connect the instrument to the power supply, plug the mains power cord into the back of the instrument and the free end of the power cord into the mains power supply, and then switch on the mains power supply.

Getting Started

Agilent 240/280 Series AA (including Zeeman) 55

Moving your instrument

WARNING

Heavy Weight The instrument weighs over 50 kg (110 lb). Do not attempt to lift the instrument alone. Always use two or more people when lifting or carrying the instrument into position.

Starting the system

The instrument power switch is a rocker type, located on the front of the instrument on the left-hand side. Switch the power switch to I to start the system. The green indicator light will come on.

For instructions on how to start any accessories, refer to the manuals supplied with the accessories.

If you have not already done so, start the SpectrAA software as described on Page 47.

Pre-analysis checklist

The general preparation procedure is as follows: 1 Install all the required hardware, including any associated accessories such as

SIPS, according to the instructions in the Help (see Page 51) and any accessory manuals.

2 Turn on the instrument and any peripheral accessories as described in the previous section.

3 Hold a thin single-ply tissue up to the mouth of the extraction hood to ensure that the exhaust system is working. The tissue should be drawn towards the hood.

4 Check the gas supplies to make sure that you have enough gas to complete your analysis. Also, check that the acetylene cylinder pressure is above 700 kPa (about 100 psi) to ensure that acetone is not drawn into the instrument.

Getting Started

56 Agilent 240/280 Series AA (including Zeeman)

5 Set the delivery pressure of the gases to the following: Recommended Permissible kPa psi kPa psi

Acetylene 75 11 65100 9.514.5 Air 350 50 245455 3565 Nitrous oxide 350 50 245455 3565

6 Inspect the gas hoses for damage. Hoses showing any signs of damage or deterioration must be replaced immediately. This should be done by a trained Agilent representative. Turn on the gas supplies to your instrument and test all hoses and connections for leaks. If a leak is found, repair it immediately.

7 Load a worksheet and develop the method(s) as per your analytical requirements.

8 Optimize the system. 9 Start an Autorun.

NOTE Detailed procedural help for Steps 7 to 9 are provided in the Help. See Page 51 for details of how to find information in the Help.

Maintenance and Troubleshooting

Agilent 240/280 Series AA (including Zeeman) 57

6Maintenance and Troubleshooting Schedule 58 Cleaning 59 Gas cylinders 60 Preventing flashbacks 61 Spare parts 61

The following is a list of maintenance procedures that must be performed to keep your instrument running safely and with optimum performance. See the Maintenance section in the SpectrAA Help for replacing and cleaning procedures.

To access the Help click Start > All Apps > SpectrAA > SpectrAA Help or, with the SpectrAA software open, press F1 on your keyboard.

Do not perform any procedures not listed in this manual or in the SpectrAA Help. Contact your Agilent representative if further information is needed.

The procedures listed below may involve hazardous chemicals and fumes, hot surfaces, and handling fragile lamps and glass. Always follow the correct procedure listed in the SpectrAA Help, adhere to all safety and chemical disposal regulations, and wear the appropriate safety equipment.

WARNING

Corrosive liquid The contents of the liquid trap may be toxic or corrosive. Dispose of the contents in accordance with approved procedures and always wear the appropriate safety equipment.

WARNING

Hot surfaces Some components within the spectrometer may remain hot after turning off the instrument. Before performing any maintenance procedures always allow the components to cool.

Maintenance and Troubleshooting

58 Agilent 240/280 Series AA (including Zeeman)

WARNING

Sharp objects Great care should be taken when working with glass or quartz parts to prevent breakage and cuts.

Schedule

Daily before operation

Check that the exhaust system has positive extraction Check the gas supplies Check all hoses and connections for damage, leaks and wear Ensure end of the drain tube in not immersed below the liquid level in the drain

vessel

Daily after operation

Clean the instrument Clean the burner (Flame systems only) Rinse out the spray chamber and liquid trap (Flame systems only) Check graphite components including the shroud, electrode, and tube

(Furnace/Zeeman systems only) Clean the electrodes (Furnace/Zeeman systems only) Replace the tube if necessary (Furnace/Zeeman systems only) Empty the drain vessel Turn off the gas supplies at the regulator

Weekly

Check for o-ring deterioration: Three o-rings inside the burner, spray chamber, and the bung (see Figure 4) Two o-rings that seal the gas inlets to the spray chamber (see Figure 5)

Maintenance and Troubleshooting

Agilent 240/280 Series AA (including Zeeman) 59

NOTE Always ensure the sealing surfaces are clean and free of debris before re-inserting the component.

Figure 4. Disassembled spray chamber and burner where:

1. O-ring on burner assembly 2. O-ring inside the spray chamber 3. O-ring inside the bung

Figure 5. Spray chamber removed from gas inlet where:

1. O-rings (x2) that seal the gas inlets to the spray chamber

Clean the lamp and sample compartment windows Check the air compressor filter Check the water levels in recirculating supplies (Furnace/Zeeman systems

only)

Yearly

Arrange for an Agilent service engineer to perform preventative maintenance.

Cleaning

Instrument surfaces

Clean contamination immediately using the approved laboratory procedures.

If there is contamination inside the instrument immediately turn off the instrument and call your Agilent representative. 1 Switch off the instrument and allow it to cool.

1

2 3

1

Maintenance and Troubleshooting

60 Agilent 240/280 Series AA (including Zeeman)

2 Remove any hardware present in the sample compartment (refer to the appropriate instructions in this Users Guide and the SpectrAA Help if necessary).

3 Using a cloth dampened with water, clean the sample compartment, instrument cover, and chimney. On Flame systems, also clean the front panel and flame shield. If necessary, use a mild detergent to clean the cover. Do NOT use an abrasive cleaner. When analyzing biological samples, wipe the instrument with chlorhexidine in 95% ethanol.

Windows

Clean the sample compartment windows and the lamp compartment window with a gentle stream of filtered air, or a puffer brush, like those used to clean camera lenses.

If the windows are dirty, wipe them using an optical tissue held between tweezers and dampened with a 50% ethanol/water solution.

Filters

Check the filter in the air compressor supply line and clean if necessary (instructions are included with the filter).

Gas cylinders

Change gas cylinders according to the instructions supplied by the manufacturer.

When changing gas cylinders: Inspect all gas supply pipes and hoses. Hoses showing any signs of damage

or deterioration must be replaced immediately. This should be done by a trained Agilent representative.

Test all connections for leaks using a commercial leak testing solution, a mild dish washing soap solution, or an electronic leak detector.

Test the operation of all regulators. Ensure that shut off valves are correctly functioning.

Maintenance and Troubleshooting

Agilent 240/280 Series AA (including Zeeman) 61

Preventing flashbacks

Instrument and consumable maintenance is important to prevent flashbacks or unexpected flame events. See the Safety section on Page 22 for detailed information on how to prevent flashbacks and Page 25 for what to do in the event of a flashback.

Spare parts

See the Agilent website for ordering information.

Use only Agilent-supplied or approved spare parts with your instrument.

Maintenance and Troubleshooting

62 Agilent 240/280 Series AA (including Zeeman)

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Manualsnet FAQs

If you want to find out how the 280 Series AA Agilent works, you can view and download the Agilent 280 Series AA Spectroscope User's Guide V2 on the Manualsnet website.

Yes, we have the User's Guide for Agilent 280 Series AA as well as other Agilent manuals. All you need to do is to use our search bar and find the user manual that you are looking for.

The User's Guide should include all the details that are needed to use a Agilent 280 Series AA. Full manuals and user guide PDFs can be downloaded from Manualsnet.com.

The best way to navigate the Agilent 280 Series AA Spectroscope User's Guide V2 is by checking the Table of Contents at the top of the page where available. This allows you to navigate a manual by jumping to the section you are looking for.

This Agilent 280 Series AA Spectroscope User's Guide V2 consists of sections like Table of Contents, to name a few. For easier navigation, use the Table of Contents in the upper left corner.

You can download Agilent 280 Series AA Spectroscope User's Guide V2 free of charge simply by clicking the “download” button in the upper right corner of any manuals page. This feature allows you to download any manual in a couple of seconds and is generally in PDF format. You can also save a manual for later by adding it to your saved documents in the user profile.

To be able to print Agilent 280 Series AA Spectroscope User's Guide V2, simply download the document to your computer. Once downloaded, open the PDF file and print the Agilent 280 Series AA Spectroscope User's Guide V2 as you would any other document. This can usually be achieved by clicking on “File” and then “Print” from the menu bar.