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Samples, Blank values, contamination, Selection of va measurement mode – Metrohm 797 VA Computrace User Manual

Page 272

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9 Troubleshooting

797 VA Computrace – Software

260

Samples

1. The amount of sample depends on the concentration of the

element to be determined.

2. If the sample matrix is known, a better assessment of the

analysis can be made (organic components?).

3. A digestion must be carried out on contaminated samples and

on samples where contamination is suspected (see Metrohm
Monograph «Sample preparation for techniques in voltam-
metric trace analysis»).

4. A lot of errors are made during sampling and when storing the

sample. Caution and a critical approach are required.

5. The sample should have a good solubility in the electrolyte and

be mixable with it.

Blank values, contamination

The following points should be checked if the results are too
high
:
1. Have the dilutions been made correctly?
2. Have contamination risks been excluded?
3. Contamination risks are very high at low concentrations:

measuring vessels should be conditioned with dilute HNO

3

so-

lution.

4. Are the chemicals pure enough?

"Suprapure" grade reagents should be used at low concentra-
tions.

5. Very high concentrations were measured in the previous analy-

sis:
electrodes and measuring vessels must be carefully cleaned and
conditioned (memory effects).

6. Has the standard addition been carried out properly?

Was the volume set correctly on the pipetting unit?

The following points should be checked if the results are too
low
:
1. Concentration too high?

HMDE overloaded, use DME/SMDE instead?

2. Buffer not correct?

Make up new one if necessary.

3. Addition ratio too low?
4. Addition ratio too high?

Selection of VA Measurement mode

The following points should be considered by selecting the VA
measurement mode: