D4377_10
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Add the fresh sample solvent
to the titration vessel
and bring the solvent
to endpoint conditions
as described in 9.2 of
the written standard.
Add the crude to
the titration vessel
immediately after the
mixing step described
in 8.1.2.1 of the
written standard using
one of the following methods.
Starting with a
clean, dry syringe--
10 or 5 milliliters, rinse
the syringe two times
with the sample and
discharge to waste.
Withdraw the required
amount of sample.
And discharge any air bubbles.
Weigh the syringe to the
nearest 0.1 milligrams.
Inject the sample into
the titration vessel.
Clean the needle
with a paper tissue,
and reweigh the syringe.
Titrate the sample until a
steady endpoint for at least
30 seconds is reached.
And record the volume of Karl
Fischer reagent to the nearest
0.01 milliliters.
See note 2 and note 4
of the written standard.
The solvent should be changed
when the sample content exceeds
2 grams of crude per 15
milliliters of solvent,
or when 4 milliliters of titrant
per 15 milliliters of solvent
has been added to
the titration vessel.
For viscous crudes,
add the sample
to a clean, dry dropper bottle
and weigh the bottle and crude.
Quickly transfer the
required amount of sample
to the titration vessel
with the dropper.
Reweigh the bottle.
Titrate the sample as in
10.2.1 of the written standard.
After adding the sample,
do not shake the cell.