LUBRIZOL TEST PROCEDURE

TP-AATM-106B-a
Edition: July 22, 2015
Previous Editions: November 1, 1996 / October 16, 2006

Moisture - Karl Fischer Method

DEFINITION 4. This method is not intended for use with

certain chemicals such as aldehydes,
This method determines the amount of water
ketones, oxidizers or alkaline amines which
present in the test sample. It is reported as
require special precautions not within the
milligrams of water per 100 milligrams of sample, or
scope of this method.
percent water.
5. Only use volumetric Karl Fischer Titrator,
DESCRIPTION OF METHOD Coulometric Karl Fischer Titrator will give
different results.
This method is based on the stoichiometric reaction
of Karl Fischer reagent with water present in the EQUIPMENT REQUIRED
test sample. The amount of water equivalent to
1. Volumetric Karl Fischer Titrator, DL – series,
each milliliter of Karl Fischer reagent is determined
using a methanol water solution as the standard. V series or equivalent.
2. Analytical balance capable of weighing to the
The determination is carried out in a closed titration nearest 0.1mg.
cell containing a platinum electrode connected to a 3. Dropper bottle or glass shell vial with stopper.
galvanometer in a dead stop endpoint circuit. The
difference in the conductivity of the solution when REAGENTS
any unreacted Karl Fischer reagent is present is 1. Karl Fischer reagent with pyridine (available
used to determine the endpoint of the reaction. from EMD chemical Inc.), or Hydranal®
An accurately weighed amount of test sample is Composite 5, one component reagent
titrated against Karl Fischer reagent. 2. Methanol, anhydrous A.C.S. reagent
3. Chloroform, A.C.S. reagent
NOTES:
PROCEDURE
1. For fats, waxes, and similar non-water soluble
1. Periodically determine the titer strength
solids add approximately 25 mL of chloroform
(concentration) using water standard per
to the methanol cell for approximately 50%
instrument manual.
chloroform to 50% methanol mixture.
2. Run a drift periodically or when an abnormal
2. Solid products should be heated to melt and result occurs. Refer to instrument/manual for
mixed before testing.
instructions.
3. Sensitivity to pH: The Karl Fischer titration is 3. Sample Preparation: Sample size depends
pH sensitive. Suitable pH range is 4.0 to 8.5. on expected results. Refer to instrument/
For samples with pH greater than 8.5, manual for instructions.
neutralize with glacial acetic acid. 4. Follow the instructions for the specific
instrument to run percent water.

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 Lubrizol Test Procedure TP-AATM-106B-a
Moisture – Karl Fischer Method
Page 2 of 2

5. All solvents must be zeroed before adding the

sample. Do not run more than 3 samples in the
same cell, 2 if the % moisture is higher than
1%. The Drierite should be changed according
to the instruction manual.
6. Start titration and determine percent water in
the sample.
7. Run all samples in duplicate, compute the
average value.
8. If out of specification results occur twice on the
same sample, check the instrument manual for
possible trouble shooting of instrument.