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

Page 99

Advertising
background image

■■■■■■■■■■■■■■■■■■■■■■

9 Troubleshooting

899 Coulometer

■■■■■■■■

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.

Advertising