6 voltammetric problems, Low background current or unstable baseline – Metrohm 757 VA Computrace User Manual

Page 177

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8.6 Voltammetric problems

757 VA Computrace – Software

167

8.6 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 or re-
place 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. If the electrode drops or the drops do not remain hanging:

check the MME. Change capillary if necessary or replace
sealing needle (see Hardware Manual).

2. If the concentration to be determined is considerably higher

than expected: reduce sample volume or change the elec-
trode 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?
3. Exchange the RDE.

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