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Metrohm 746 VA Trace Analyzer User Manual

Page 535

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7 Safety, Errors, Troubleshooting, Diagnosis, GLP

746 VA Trace Analyzer / 747 VA Stand

7-36

Peak displacement

Check and adjust the pH of the solution.

Check electrolyte composition and correct if necessary. Use a buffer solution

instead of an acid.

Carry out a standard addition to check whether the correct peak has been

evaluated.

Organic components interfere with the analysis: carry out a UV digestion or

other suitable sample preparation.

Enter a new half-wave potential in the instrument and recalculate the results.

Check reference electrode (see section 3.6).

No peak found

The peak is only displaced: adjust the half-wave potential and recalculate the

results.

The sample concentration is too low: increase the sample volume or the

amount of sample.

The concentration of the ion to be determined is too low: use HMDE (inverse

voltammetry) instead of DME or SMDE.

Are the initial and final potentials correct?

Peak is in the highest

µ

A range

The concentration of the ion to be determined is too high: reduce the sample

volume and carry out the analysis again.

The preconcentration time under

MEAS

is too high, reduce it and try the

analysis again.

Double peak

Check MME. If necessary, change capillary (see section 3.4.8) or replace

sealing needle (see section 3.4.9).

Organic components interfere with the analysis: carry out a UV digestion or

other suitable sample preparation.

If a second element is present at the same potential: add this element to the

sample and carry out the analysis again. If the second peak has become

higher then the second element is present.

Has any substance been precipitated out in the measuring vessel (e.g. lead

perchlorate standard with KCl as electrolyte)?

Try out eluents with different compositions (addition of complex formers).

Check analysis parameters.

Try another measurement mode like AC1. If one substance is reversible and

the second one irreversible, only the reversible substance is detected by

AC1.

Standard addition peaks displaced

Standard solutions have been made too acidic.

Buffering capacity of the electrolyte is not sufficient: increase electrolyte vol-

ume.