9 troubleshooting, 1 karl fischer titration, Karl fischer titration – Metrohm 899 Coulometer User Manual

Page 99

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9 Troubleshooting

899 Coulometer

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89

9 Troubleshooting

9.1

Karl Fischer titration

Problem

Cause

Remedy

The drift is very high
during conditioning.

The coulometer cell is not
leak-proof.

■

Check the septum and replace it if neces-
sary.

■

Replace the molecular sieve.

■

Check the ground-joint sleeves for frayed
edges. If necessary, trim the edges cleanly
or replace the ground-joint sleeves.

Aqueous deposits are to be
found in the coulometer
cell.

■

Shake the coulometer cell.

The reagent is exhausted
or contaminated.

■

Replace the reagent.

The catholyte is old or
moist.

■

The catholyte must be replaced at least
once per week.

■

Dry the catholyte with KF single-compo-
nent reagent.

The diaphragm of the gen-
erator electrode is conta-
minated.

■

Clean the diaphragm (in accordance with
directions in the leaflet for the generator
electrode).

A side reaction is taking
place.

■

Possibly use a KF oven.

■

See technical literature.

The molecular sieve on the
KF oven has reached its
capacity limit.

■

Replace the molecular sieve.

The gas flow from the KF
oven into the coulometer
cell is too high.

■

Reduce the gas flow (if you are working
with the oven method with sample vials,
set the gas flow between 40…60 mL/min).

The drift becomes
greater after each
titration.

The sample releases water
very slowly.

■

Possibly use a KF oven.

■

See technical literature.

The drift is fluctuat-
ing.

The sample solution is
poorly stirred.

■

Set the stirring rate in such a way that the
sample solution will become very well
mixed.

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