Agilent Technologies 55B AA Manual de usuario

Agilent 55B AA Spectrometer

User’s Guide

2 Agilent 55B AA Spectrometer User’s Guide

Notices

Manual Part Number

8510154100

Edition 13, February 2019

2000, 2002, 2009, 2010, 2012 and

2013, 2016, 2017, 2019.

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

Agilent Technologies Australia [M] Pty

Ltd

679 Springvale Road

Mulgrave, Victoria 3170, Australia

www.agilent.com

Instrument Manufacturing

Manufactured by Agilent Technologies

Bayan Lepas Free Industrial Zone,

Penang, PG, 11900, MY

Printed in Malaysia

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.

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

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