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6 voltammetric problems, Low background current or unstable baseline – Metrohm 797 VA Computrace User Manual

Page 274

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9 Troubleshooting

797 VA Computrace – Software

262

11. CPVS (

Cyclic Pulse Voltammetric Stripping) is mainly used for

the determination of organic additives in electroplating elec-
trolytes. CPVS is a chronoamperometric mode, current is meas-
ured against time.

9.6 Voltammetric

problems

Low background current or unstable baseline

With all types of electrodes:
1. Check electrolyte concentration and pH of the solution.
2. Check

Start potential

and

End potential

of the sweep.

3. If the ion concentration in the solution is too high: dilute the

electrolyte.

4. Has the sample been degassed? Degassing with nitrogen for at

least 5 min is recommended, for alkaline solutions approx. 10
min is recommended.

5. Is the reference electrode sufficiently full (inside and outside,

see Hardware Manual)?

6. Electrolyte solution too old: make up a new one. Its working

life with organic additives may be as short as 1 day or less.

With DME/SMDE:
1. If the electrode drops irregularly: check the MME.

Adjust sealing needle. If necessary, change capillary and replace
sealing needle (see Hardware Manual).

2.

Check tapping mechanism on VA Stand. If tapping strength is
too weak, turn corresponding slotted screw on the valve block
during operation in an anticlockwise direction until a drop falls
each time the tapper is triggered (see Hardware Manual).

3. Is the gas pressure correctly set (1 bar)?
4.

If the concentration to be determined is considerably lower
than expected: increase sample volume or change the elec-
trode mode (e.g. HMDE).

With HMDE:
1. I

f the electrode drops or the drops do not remain hanging:

check the MME.

Change capillary and replace sealing needle

(see Hardware Manual).

2.

If the concentration to be determined is considerably higher
than expected: reduce sample volume or change the electrode
mode (e.g. from HMDE to SMDE or DME).

With RDE/SSE:
1. The electrode surface must be repolished.
2. Has the correct RDE type been used?