Agilent Technologies 55B AA User manual

Agilent 55B AA
Spectrometer
User’s Guide

2 Agilent 55B AA Spectrometer User’s Guide
Notices
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2013, 2016, 2017
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Manual Part Number
8510154100
Edition
Twelth edition, December 2017
Printed in Malaysia
Agilent Technologies Australia [M] Pty
Ltd
679 Springvale Road
Mulgrave, Victoria 3170, Australia
www.agilent.com
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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.
WARNING
CAUTION

Contents
Agilent 55B AA Spectrometer User’s Guide 3
Contents
1. Safety Practices and Hazards 11
Verifying Safe State 12
Electrical Hazards 12
Heat, Vapors and Fumes 13
Compressed Gases and Cylinders 14
Gas Hoses and Connections 15
Ultraviolet Radiation 16
Other 16
Warning Symbols 16
CE Compliance 18
Electromagnetic Compatibility 19
EN55011/CISPR11 19
ICES/NMB-001 20
Flame Operation 20
Flammable Solvents 20
Compressed Gases and Cylinders 22
Acetylene 22
Nitrous Oxide 24
Burners 24
Nebulizer 25
Liquid Trap 26
Heat Hazards 26
Perchloric Acid 27

Contents
4 Agilent 55B AA Spectrometer User’s Guide
Flashbacks 28
2. Introduction 31
Site Preparation Requirements 32
Documentation 32
Conventions 32
Specifications 33
Environmental Specifications 33
Gas Supplies 34
3. Installation 35
Instrument Overview 36
Connections 37
Power 38
Moving Your Instrument 39
Lamp Compartment 39
Hollow Cathode Lamps 40
D2Lamp 41
Sample Compartment 42
Nebulizer 42
Spraychamber 45
Burner 54
Sample Compartment Front Panel 55
Flame Shield 56
4. Interface 57
Introduction 57
Display 58

Contents
Agilent 55B AA Spectrometer User’s Guide 5
Keypad 61
Agilent 55B AA Pages 63
Load Method Page 63
Instrument Parameters Page 63
Measurement Parameters Page 65
Options Page 66
Optimization Page 69
Calibration Parameters Page 69
Results Page 70
Navigating the Interface 71
Changing Pages 71
Selecting Menus 71
Moving Between Fields 72
5. Operation 75
Pre-Analysis Checklist 75
Starting the System 76
Method Development 77
Selecting the Language of the Interface 77
Loading a Method 77
Setting the Instrument Parameters 78
Setting the Measurement Parameters 79
Defining the Calibration Standards 79
Saving/Deleting Methods 80
Optimization 81
Aligning Lamps 81
Aligning the Burner 83
Lighting the Flame 83

Contents
6 Agilent 55B AA Spectrometer User’s Guide
Optimizing the Flame Signal 85
Nebulizer Setup 86
High Vacuum Setting 86
Low Vacuum Setting 87
Setting Zero Uptake Rate 87
Setting the Uptake Rate for Organic Solvents 88
Performance Checks 88
Calibrating the Method 89
Measuring Standards Manually 89
Measuring Standards Using SIPS 10 90
Displaying the Calibration Graph 90
Resloping the Calibration 91
Sample Measurement 92
Measuring Samples Manually 92
Measuring Samples with SIPS 92
Results 93
Printing the Results 93
Output to LIMS System 93
Shutting Down the System 94
6. Maintenance 95
Maintenance Schedule 95
Daily 95
Weekly 96
Yearly 96
Cleaning 96
General 96

Contents
Agilent 55B AA Spectrometer User’s Guide 7
Windows 96
Filters 97
Burners 97
Cleaning the Burner 97
Nebulizer 99
Routine maintenance 99
Removing the Nebulizer Block 100
Disassembling the Nebulizer 101
Cleaning a Blocked Nebulizer 102
Reassembling the Nebulizer 103
Impact Bead 104
Removing the Impact Bead 104
Installing and Adjusting the Impact Bead 107
Spraychamber 108
Disassembling the Spraychamber 108
Cleaning the Spraychamber 108
Gas Supplies 109
D2Lamp 109
Fuses 111
7. Spare Parts 115
Sample Introduction 115
Other 118
Covers/Doors 118
Fuses 118
Miscellaneous 118

Contents
8 Agilent 55B AA Spectrometer User’s Guide
8. Troubleshooting/Errors 119
Common Problems 119
Error Messages 122
0804 LIMS port error 122
2851 SIPS comms error 122
3800 EEPROM storage error 123
5004 Signals not increasing 123
5005 Slope test failure 123
5006 Calibration fit failure 123
5008 Reslope signal out of range 123
6000 Check HC lamp selection 124
9159 EEPROM checksum zero wl 124
9160 EEPROM checksum mono correction 124
9307 RBC/Mains frequency below 48Hz. 124
9308 RBC/Mains frequency 124
9309 RBC/Mains frequency above 62Hz 125
9310 Optical RBC frequency 125
9311 Instrument Fault +12V PSU 125
9312 Instrument Fault -12V PSU 125
9313 Instrument Fault 5V PSU 125
9316 Wavelength out of range 126
9317 No Peak: Low HC Lamp Energy 126
9318 No Peak: High HC Lamp Energy 126
9319 No Peak: Low BC Lamp Energy 127
9320 No Peak: High BC Lamp Energy 127
9321 No Peak: Low HC Lamp Energy 127
9322 No Peak: High HC Lamp Energy 128
9323 Low Emission: No Peak 128
9324 High Emission: No Peak 128
9329 No Peak detected 129
9330 No Peak detected 129

Contents
Agilent 55B AA Spectrometer User’s Guide 9
9337 Instrument Fault 310V PSU 130
9339 Mono resetting. Please wait 130
9415 Instrument Fault: Lamp code 130
9422 Instrument Fault: Lamp current 130
9514 Instrument Signal saturation 131
9517 Low HC Lamp Energy 131
9518 High HC Lamp Energy 131
9524 Low BC Lamp Energy 132
9525 High BC Lamp Energy 132
9527 Instrument Fault: EHT failed 132
9528 Background Lamp failed 132
9529 Background Lamp interlock 133
9530 Instrument Fault: Signal diagnostics 133
9531 No Lamp Current detected 133
9602 Instrument Fault: Mono Datum 133
9911 No Burner Fitted 133
9912 N2O Burner not fitted 134
9914 No Gas Control Unit 134
9915 Flame Shield Open 134
9916 Fault: Gas pressure sensor 134
9917 No Oxidant gas pressure 134
9920 Fault: Flame detected 135
9921 Flame Out Detected 135
9922 Flame Shutdown: Gas type 135
9923 Flame Ignition Timeout 135
9934 Flame Shutdown: host offline 136
9937 Flame Pressure Relief Bung 136
9938 Liquid Trap Not Ready 136
9xxx GPIB Fault 136
9xxx Instrument Error 136
9xxx SpectrAA Error 136

Contents
10 Agilent 55B AA Spectrometer User’s Guide
This page is intentionally left blank.

Safety Practices and Hazards
Agilent 55B AA Spectrometer User’s Guide 11
1. Safety Practices and Hazards
Verifying Safe State 12
Electrical Hazards 12
Heat, Vapors and Fumes 13
Compressed Gases and Cylinders 14
Gas Hoses and Connections 15
Ultraviolet Radiation 16
Other 16
Warning Symbols 16
CE Compliance 18
Electromagnetic Compatibility 19
Flame Operation 20
Flammable Solvents 20
Compressed Gases and Cylinders 22
Acetylene 22
Nitrous Oxide 24
Burners 24
Nebulizer 25
Liquid Trap 26
Heat Hazards 26
Perchloric Acid 27
Flashbacks 28
Your Agilent 55B AA instrument and accessories have been carefully
designed so that when used properly you have an accurate, fast,
flexible and safe analytical system.

Safety Practices and Hazards
12 Agilent 55B AA Spectrometer User’s Guide
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 which 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. Before using your instrument or accessories, you must
thoroughly read these safety practices.
Observe all relevant safety practices at all times.
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 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 customer’s 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.

Safety Practices and Hazards
Agilent 55B AA Spectrometer User’s Guide 13
Panels and covers that are retained by fasteners which require the
use of a tool for removal may be opened only 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, and could seriously damage the instrument and any
attached ancillary equipment.
Always use a 3-wire outlet with ground connection which is
adequately rated for the load. The installation must comply with
local, State, and Federal safety regulations.
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 will be connected.
Heat, Vapors and Fumes
The heat, vapors and fumes generated can be hazardous, toxic, or
otherwise injurious to personnel.
Heat, vapors and fumes must be extracted from the instrument by
means of 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.

Safety Practices and Hazards
14 Agilent 55B AA Spectrometer User’s Guide
The exhaust system must be capable of providing an exhaust
ventilation rate of at least 6 cubic meters per minute (200 scfm).
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 a pilot light
situated immediately adjacent to the instrument to indicate whether
the exhaust fan is on or off. ALWAYS switch the exhaust fan on
BEFORE lighting the flame.
Use fireproof ducting which 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 ducting—the hot exhaust in the duct may melt the joint.
Regularly check the system by smoke test to ensure that the exhaust
system is functioning correctly.
When operating the atomic absorption spectrometer, ALWAYS have
the chimney in place to ensure correct ventilation.
Compressed Gases and Cylinders
All compressed gases (other than air) can create a hazard if they leak
into the atmosphere. Even small leaks in gas supply systems can be
dangerous. Any 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.
Cylinders must be stored and handled strictly in accordance with
local safety codes and regulations. Cylinders must be used and stored
only in a vertical position. Secure all cylinders to an immovable
structure or a properly constructed cylinder stand. The area in which
cylinders are stored must be adequately ventilated to prevent toxic or
explosive accumulations. Move cylinders only on a properly
constructed trolley.

Safety Practices and Hazards
Agilent 55B AA Spectrometer User’s Guide 15
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.
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.
Use only approved regulators and hose connectors.
Never attempt to refill cylinders.
Remember that 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
cylinders.
Gas Hoses and Connections
Even small leaks in gas supply systems can be dangerous. Any 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.
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.

Safety Practices and Hazards
16 Agilent 55B AA Spectrometer User’s Guide
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
Hazardous ultraviolet radiation is emitted by flames, hollow cathode
lamps and deuterium lamps. 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.
Other
Other messages appear in the manual where appropriate, and detail
advice, information specific to the topic, or helpful tips.
NOTE A ‘Note’ message is used to give advice or information.
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. The beginning of the warning text is noted by
a warning icon:
WARNING
A triangular symbol indicates a warning. The meanings of the
symbols that may appear alongside warnings in the documentation
or on the instrument itself are as follows:

Safety Practices and Hazards
Agilent 55B AA Spectrometer User’s Guide 17
Corrosive liquid
Electrical shock
Eye hazard
Explosion hazard Fire hazard
Heavy weight
(danger to feet)
Heavy weight
(danger to hands)
Hot surface
Moving parts
Noxious gas
Toxic hazard
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 appear on the instrument for your
information.
I
Mains power on
0
Mains power off
Fuse
Single phase alternating current

Safety Practices and Hazards
18 Agilent 55B AA Spectrometer User’s Guide
Flame off
Flame on
Indicates lamp present.
Caution, disconnect all supplies, risk of electric shock
High leakage current – ensure proper grounding
CE Compliance
Your Agilent AA instrument has been designed to comply with the
requirements of the Electromagnetic Compatibility (EMC) Directive
and the Low Voltage (electrical safety) Directive (commonly referred
to as the LVD) of the European Union. Agilent has confirmed that
each product complies with the relevant Directives by testing a
prototype against the prescribed EN (European Norm) standards.
Proof that a product complies with these directives is indicated by:
the CE Marking appearing on the rear of the product, and
the documentation package that accompanies the product
containing a copy of the Declaration of Conformity. The
Declaration of Conformity is the legal declaration by Agilent that
the product complies with the directives listed above, and shows
the EN standards to which the product was tested to
demonstrate compliance.

Safety Practices and Hazards
Agilent 55B AA Spectrometer User’s Guide 19
Electromagnetic Compatibility
EN55011/CISPR11
Group 1 ISM equipment: group 1 contains all ISM equipment in
which there is intentionally generated and/or used conductively
coupled radio- frequency energy which is necessary for the internal
functioning of the equipment itself.
Class A equipment is equipment suitable for use in all
establishments other than domestic and those directly connected to a
low voltage power supply network which supplies buildings used for
domestic purposes.
This device complies with the requirements of CISPR11, Group 1,
Class A as radiation professional equipment. Therefore, there may be
potential difficulties in ensuring electromagnetic compatibility in
other environments, due to conducted as well as radiated
disturbances.
Operation is subject to the following two conditions:
1This device may not cause harmful interference.
2This device must accept any interference received, including
interference that may cause undesired operation.
If this equipment does cause harmful interference to radio or
television reception, which can be determined by turning the
equipment off and on, the user is encouraged to try one or more of
the following measures:
1Relocate the radio or antenna.
2Move the device away from the radio or television.
3Plug the device into a different electrical outlet, so that the device
and the radio or television are on separate electrical circuits.
4Make sure that all peripheral devices are also certified.
5Make sure that appropriate cables are used to connect the device
to peripheral equipment.
6Consult your equipment dealer, Agilent Technologies, or an
experienced technician for assistance.

Safety Practices and Hazards
20 Agilent 55B AA Spectrometer User’s Guide
Changes or modifications not expressly approved by Agilent
Technologies could void the user’s authority to operate the
equipment.
ICES/NMB-001
This ISM device complies with Canadian ICES- 001.
Cet appareil ISM est conforme à la norme NMB-001 du Canada.
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. These can result in death, or severe personal injury or
burns.
Remember at all times 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.