Agilent Technologies 55B AA Manual de usuario

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

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Ltd

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Mulgrave, Victoria 3170, Australia

www.agilent.com

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Restricted Rights Legend

If software is for use in the

performance of a U.S. Government

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Software is delivered and licensed as

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technical data.

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

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