7 safety, errors, troubleshooting, diagnosis, glp – Metrohm 746 VA Trace Analyzer User Manual

Page 7

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Table of contents

746 VA Trace Analyzer / 747 VA Stand

VI

7 Safety, Errors, Troubleshooting,

Diagnosis, GLP

.............................................................................

7-1

7.1 Electrical safety

...............................................................................

7-1

7.2 Safety considerations concerning mercury

.....................

7-2

7.2.1

Properties of mercury .................................................................. 7-2

7.2.2

Toxicity of mercury and its compounds ...................................... 7-3

7.2.3

Handling of mercury .................................................................... 7-3

7.2.4

References dealing with mercury ................................................ 7-5

7.3 Error messages

...............................................................................

7-6

7.3.1

General information on error messages...................................... 7-6

7.3.2

List of error messages ................................................................. 7-7

7.3.3

Instrument initialization .............................................................. 7-29

7.4 Troubleshooting

...........................................................................

7-33

7.4.1

General rules for VA trace analysis............................................ 7-33

7.4.2

Problems with DME/SMDE........................................................ 7-35

7.4.3

Problems with HMDE................................................................. 7-37

7.4.4

Problems with RDE.................................................................... 7-40

7.5 Hardware/software faults in the instruments

or simply the vagaries of the chemistry

..........................

7-42

7.5.1

General ...................................................................................... 7-42

7.5.2

Oxygen in the analysis solution ................................................. 7-42

7.5.3

Unsuitable bridging electrolyte solution
in the reference electrode.......................................................... 7-43

7.5.4

Overcharging of the working electrode ..................................... 7-43

7.5.5

Disturbances at the HMDE through gas formation ................... 7-45

7.5.6

Complex formation .................................................................... 7-46

7.5.7

Peak on highly curved baseline................................................. 7-47

7.5.8

Peak overlapping....................................................................... 7-47

7.5.9

Calibration with chemically non-isoformal standards................ 7-48

7.6 Diagnosis

.........................................................................................

7-49

7.6.1

General ...................................................................................... 7-49

7.6.2

Prepare instrument for diagnostic test ...................................... 7-50

7.6.3

Checking thermal printer ........................................................... 7-50

7.6.4

Checking RS232 interfaces ....................................................... 7-52

7.6.5

Checking control lines ............................................................... 7-52

7.6.6

Checking the keypad................................................................. 7-53

7.6.7

Checking the VA Stand.............................................................. 7-54

7.7 Standard operating procedure in the context of

GLP/ISO 9001 guidelines

.........................................................

7-58

7.7.1

Checking 747 VA Stand with polarogram simulator.................. 7-58

7.7.2

Loading the

TESTPb.mth method........................................... 7-60

7.7.3

Preparing the sample solution................................................... 7-60

7.7.4

Performing the determination .................................................... 7-61

7.7.5

Assessment of the determination.............................................. 7-62

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