Agilent Technologies 55B AA User manual

Agilent 55B AA Spectrometer
User’s Guide

2 Agilent 55B AA Spectrometer User’s Guide
Notices
Manual Part Number
8510154100
Edition 13, February 2019
Copyright
© Agilent Technologies, Inc. 1997,
2000, 2002, 2009, 2010, 2012 and
2013, 2016, 2017, 2019.
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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

Safety Practices and Hazards
Agilent 55B AA Spectrometer User’s Guide 3
Contents
Contents 3
1Safety Practices and Hazards 11
Verify safe state 12
Electrical hazards 12
Heat, vapors and fumes 13
Compressed gases and cylinders 14
Gas hoses and connections 17
Ultraviolet radiation 18
Other 18
Warning symbols 18
CE compliance 20
Electromagnetic compatibility 21
EN55011/CISPR11 21
ICES/NMB-001 22
Flame operation 22
Flammable solvents 22
Burners 24
Nebulizer 25
Liquid trap 26
Heat hazards 27
Perchloric acid 27
Flashbacks 29
What to do in the event of a flashback 31

Safety Practices and Hazards
4 Agilent 55B AA Spectrometer User’s Guide
2Introduction 33
Site preparation requirements 33
Documentation 34
Conventions 34
Specifications 34
Environmental specifications 34
3Overview 37
Installation checklist 37
Instrument overview 37
Power 39
Gas hoses 39
Printer 39
Accessories 39
Moving your instrument 40
Lamp compartment 40
Hollow cathode lamps 40
Deuterium (D2) lamp 41
Sample compartment 41
Nebulizer block assembly 42
Burner 46
Sample compartment front panel 46
Flame shield 47
Chimney 48
4Interface 49
Front panel overview 49

Safety Practices and Hazards
Agilent 55B AA Spectrometer User’s Guide 5
Display screen 50
Keypad 53
Navigating the interface 56
Changing pages 56
Selecting menus 56
Moving between fields 58
Display pages 58
Load Method page 58
Instrument Parameters page 58
Measurement parameters page 60
Options page 61
Optimization page 63
Calibration Parameters page 64
Results page 64
5Operation 67
Pre-analysis checklist 67
Start the system 69
Method development 69
Select the language of the interface 69
Load a method 70
Save/Delete methods 71
Set the instrument parameters 72
Set the measurement parameters 72
Define the calibration standards 73
Optimization 74

Safety Practices and Hazards
6 Agilent 55B AA Spectrometer User’s Guide
Align lamps 74
Align the burner 76
Light the flame 78
Optimize the flame signal 80
Nebulizer setup 81
High vacuum setting 82
Low vacuum setting 83
Set zero uptake rate – organic solvents 83
Set the uptake rate for organic solvents 84
Flame types 84
Performance checks 85
Calibrate the method 86
Measure standards manually 86
Measure standards using SIPS 10 86
Display the calibration graph 87
Reslope the calibration 87
Sample measurement 88
Measure samples manually 88
Measure samples with SIPS 88
Results 89
Print the results 89
Output to LIMS system 90
Shut down the system 90
6Maintenance 91
Maintenance schedule - general 91

Safety Practices and Hazards
Agilent 55B AA Spectrometer User’s Guide 7
Maintenance schedule – nebulizer/spray chamber 92
Cleaning 93
General 93
Windows 93
Filters 93
Nebulizer 93
Remove the nebulizer block 94
Disassemble the nebulizer 95
Clean a blocked nebulizer 96
Reassemble the nebulizer block 97
Impact bead 101
Spray chamber 108
Disassemble the spray chamber 108
To clean the spray chamber 109
To assemble the spray chamber 109
Assemble the spray chamber and nebulizer block: 111
Attach the drain tube/float/liquid trap to the nebulizer block 111
Installing the spray chamber/nebulizer assembly 113
Burners 116
To install a burner: 116
Clean the burner 118
Gas supplies 122
Lamps 122
To install a hollow cathode lamp: 122
Removing hollow cathode lamps 123

Safety Practices and Hazards
8 Agilent 55B AA Spectrometer User’s Guide
D2lamp 124
Fuses 126
7Spare Parts 129
Sample lists 129
Other 132
Covers/doors 132
Fuses 132
Miscellaneous 133
8Troubleshooting/Errors 135
Common problems 137
Error messages 140
0804 LIMS port error 140
2851 SIPS comms error 140
3800 EEPROM storage error 140
5004 Signals not increasing 141
5005 Slope test failure 141
5006 Calibration fit failure 141
5008 Reslope signal out of range 141
6000 Check HC lamp selection 141
9159 EEPROM checksum zero wl 141
9160 EEPROM checksum mono correction 142
9307 RBC/Mains frequency below 48Hz. 142
9308 RBC/Mains frequency 142
9309 RBC/Mains frequency above 62Hz 142
9310 Optical RBC frequency 143

Safety Practices and Hazards
Agilent 55B AA Spectrometer User’s Guide 9
9311 Instrument fault +12V PSU 143
9312 Instrument fault -12V PSU 143
9313 Instrument fault 5V PSU 143
9316 Wavelength out of range 143
9317 No peak: low HC lamp energy 143
9318 No peak: high HC lamp energy 144
9319 No peak: low BC lamp energy 144
9320 No peak: high BC lamp energy 144
9321 No peak: low HC lamp energy 145
9322 No peak: high HC lamp energy 145
9323 Low emission: no peak 145
9324 High emission: no peak 146
9329 No peak detected 146
9330 No peak detected 146
9337 Instrument fault 310V PSU 147
9339 Mono resetting. Please wait 147
9415 Instrument fault: lamp code 147
9422 Instrument fault: lamp current 147
9514 Instrument signal saturation 148
9517 Low HC lamp energy 148
9518 High HC lamp energy 148
9524 Low BC lamp energy 148
9525 High BC lamp energy 149
9527 Instrument fault: EHT failed 149
9528 Background lamp failed 149
9529 Background lamp interlock 149

Safety Practices and Hazards
10 Agilent 55B AA Spectrometer User’s Guide
9530 Instrument fault: signal diagnostics 149
9531 No lamp current detected 150
9602 Instrument fault: mono datum 150
9911 No burner fitted 150
9912 N2O burner not fitted 150
9914 No gas control unit 150
9915 Flame shield open 150
9916 Fault: gas pressure sensor 151
9917 No oxidant gas pressure 151
9920 Fault: flame detected 151
9921 Flame out detected 151
9922 Flame shutdown: gas type 151
9923 Flame ignition timeout 152
9934 Flame shutdown: host offline 152
9937 Flame pressure relief bung 152
9938 Liquid trap not ready 152
9xxx GPIB fault 152
9xxx Instrument error 152
9xxx SpectrAA error 152

Safety Practices and Hazards
Agilent 55B AA Spectrometer User’s Guide 11
1Safety Practices and Hazards
Verify safe state 12
Electrical hazards 12
Heat, vapors and fumes 13
Compressed gases and cylinders 14
Gas hoses and connections 17
Ultraviolet radiation 18
Other 18
Warning symbols 18
CE compliance 20
Electromagnetic compatibility 21
Flame operation 22
Your Agilent 55B AA instrument and accessories have been carefully designed so
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 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 referenced in your Agilent accessory manuals. Before using your
instrument or accessories, thoroughly read these safety practices.
Observe relevant safety practices at all times.

Safety Practices and Hazards
12 Agilent 55B AA Spectrometer User’s Guide
Verify safe state
The following general safety precautions must be observed during all phases of
operation, maintenance and service of this 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
instrument 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 items 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 may be opened only by Agilent trained and certified personnel. Consult
the manuals or product labels supplied with your PC, monitor, printer/plotter,
water-cooling system and/or vacuum pump 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. Any attached ancillary equipment could also be seriously damaged.
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.

Safety Practices and Hazards
Agilent 55B AA Spectrometer User’s Guide 13
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.
Position the system outlet so that the exhaust cannot re-enter the building
through any door, window, air conditioning inlet, or other ventilator.
Construct the system in accordance with the appropriate codes and
regulations for ventilation.
The exhaust system must be capable of 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.

Safety Practices and Hazards
14 Agilent 55B AA Spectrometer User’s Guide
Compressed gases and cylinders
All compressed gases can create a hazard. The volatile nature of the gases used
with this equipment increases this hazard.
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.
Cylinders must be:
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.
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
Agilent 55B AA Spectrometer User’s Guide 15
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.
CAUTION This spectrometer is to be used only with air, nitrous oxide, and acetylene for
flame operation.
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
Use acetylene at pressures lower than 105 kPa (15 psig). At pressures above this
level, acetylene can explode spontaneously. In some instances, local regulations
may prohibit the use of acetylene at pressures above 62 kPa (9 psig).
Your Agilent AA is designed to operate at fuel supply pressures between 49 and
105 kPa (7-15 psig). Refer to the Specifications section (Page 34) or the rear of the
instrument for the exact range and recommended pressure.
Do not use any tubing or connector that will react chemically with acetylene.
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
16 Agilent 55B AA Spectrometer User’s Guide
Never pass acetylene through copper 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 with the Agilent 55B AA system.
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.
If the pressure in the acetylene cylinder falls below 700 kPa (100 psig), or the
consumption is greater than 1/7 of the cylinder contents per hour, acetone may be
carried over from the cylinder and into the spectrometer. Acetone in the
spectrometer can damage seals, O-rings and hoses, degrade analytical
performance and precipitate flashbacks.
Minimize the amount of acetone which 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 will reduce 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).
‘Crack’ the cylinder before use by gently opening the valve to check for any
drops or spray of acetone. Any cylinder showing acetone should be returned
to the supplier for replacement.
Use ‘Instrument Grade’ acetylene that is at least 99.5% pure.
Turn off fuel gas at the cylinder when you have finished your flame analysis.
Refer also to your local regulations governing the use of acetylene.

Safety Practices and Hazards
Agilent 55B AA Spectrometer User’s Guide 17
Nitrous oxide - N2O
The conversion of high pressure N2O liquid to 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.
Prevent freezing by using a heater on the N2O regulator on the supply cylinder.
Contact the supplier of the regulator for a suitable heater.
Gas hoses and connections
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.
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.
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.

Safety Practices and Hazards
18 Agilent 55B AA Spectrometer User’s Guide
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 19
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.

Safety Practices and Hazards
20 Agilent 55B AA Spectrometer User’s Guide
The following symbols appear on the instrument
Table 1. Instrument symbols
I
Mains power on
0
Mains power off
Fuse
Single phase alternating current
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 European Norm (EN) standards.
Proof that a product complies with these directives is indicated by:
the CE Marking appearing on the rear of the product, and