9 troubleshooting, 1 karl fischer titration, Karl fischer titration – Metrohm 899 Coulometer User Manual
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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.
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Check the septum and replace it if neces-
sary.
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Replace the molecular sieve.
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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.
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Replace the reagent.
The catholyte is old or
moist.
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The catholyte must be replaced at least
once per week.
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Dry the catholyte with KF single-compo-
nent reagent.
The diaphragm of the gen-
erator electrode is conta-
minated.
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Clean the diaphragm (in accordance with
directions in the leaflet for the generator
electrode).
A side reaction is taking
place.
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Possibly use a KF oven.
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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.
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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.
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Possibly use a KF oven.
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See technical literature.
The drift is fluctuat-
ing.
The sample solution is
poorly stirred.
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Set the stirring rate in such a way that the
sample solution will become very well
mixed.