Content of Amines, used as Alkalizing Media, by

Potentiometric Titration
Test Method No.: 91600 (A31.0) Revision No.: 01

Principle of Test Measurement:

This test procedure is based on the direct potentiometric titration with 0.1N hydrochloric acid.

Purpose and Application:

This test method provides the procedure for determining the content of amines, used as
alkalizing media, at the incoming goods control.

Equipment:
The equipment listed in this section should be in proper working order, suitable for the analysis, and properly
documented as required by local operating procedures and/or regulations. The Raw Material or Product Data Sheet
should be reviewed to determine if specific test equipment is required to assay the sample material.

1. Titrator, capable of performing potentiometric titration (e.g. Metrohm 907 Titrando),

equipped with a combination electrode (e.g. N 61 combination electrode, Schott-Geräte).
2. Balance, capable of weighing to the nearest 0.0001g (capacity of at least 120g is
recommended).
3. Disposable plastic syringes or disposable pipettes.
4. 100ml Beakers.

Reagents and Solutions:

The materials listed in this section should be suitable for the analysis and properly documented as required by local
operating procedures and/or regulations. The Raw Material or Product Data Sheet should be reviewed to determine
if specific reagents or test solutions are required to assay the sample material.

1. 0.1N hydrochloric acid titrant

2. Distilled or deionized water
3. Tris-(hydroxymethyl)-aminomethane p.a., CAS-Nr. 77-86-1 (for titer determination)

Procedure:
The Raw Material or Product Data Sheet should be reviewed to determine if specific sample preparation is required
or if specific test parameters are stated.

1. Weigh the appropriate amount (given in the Raw Material Data Sheet) of sample into a
100ml beaker. Record the weight to the nearest 0.0001g. Note: Liquid sample can be
weighed directly into the beaker using a pipette, or can be determined by differential
weighing using a syringe. Solid sample can be weighed directly into the beaker.
2. Add approximately 80 ml of water and dissolve the sample
3. Titrate with 0.1N hydrochloric acid. Record the consumption of titrant used to the
nearest 0.01ml. Note: Example for titration conditions and titration curve in Appendix A.

Titer/Calibration/Standardization:
1. Check titer of the hydrochloric acid, 0.1N, at least quarterly.
2. Dissolve appr. 70 mg of tris-(hydroxymethyl)-aminomethane in appr. 80 ml of water.
Record the weight to the nearest 0.1mg.
3. Titrate with 0.1N hydrochloric acid. Record the consumption of titrant used to the nearest
0.01 ml.

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 Content of Amines, used as Alkalizing Media, by
Potentiometric Titration
Test Method No.: 91600 (A31.0) Revision No.: 01

Evaluation/Calculations:
Any deviations from the procedure described in this document or in the associated Raw Material or Product Data
Sheet shall be reported together with the analytical result.

1. Content of Raw Material:

V * t * c * M * 100 V * t * M * 0.01
% content of raw material = =
W * 1000 W

V = consumption HCl 0.1N (ml)

c = concentration HCl (=0.1 mol/l)
W = weighed amount of sample (g)
M = molecular weight (g/mol) of amine
t = titer of HCl 0.1N

2. Titer of 0.1 N HCl:

W W
t (HCl) = =
121.14g/mo l * 0.1mol/L * V 12.114 * V

W = sample weight in mg
V = consumption in ml

3. Report the results to the nearest 0.1%.

Information in Raw Material or Product Data Sheet:

1. Target sample weight (g)
2. Molecular weight of raw material (g/mol)

References:
1. Henkel Test Method 91600 (Revision 00)

Comments:
Not applicable

History/Changes:
1. Updated Henkel Test Method 91600 A31.0 to harmonized format and generalization.

Original Issue Date: 02.09.1992 Created by: I. Schaefer

Revision No / Issue Date: 01 / 03.2014 Revised by: Matthiesen /
Frauendorf

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 Content of Amines, used as Alkalizing Media, by
Potentiometric Titration
Test Method No.: 91600 (A31.0) Revision No.: 01

Appendix A

Example for the conditions of potentiometric titration (Titrando 907, Metrohm):

1. dynamic titration
2. drift of measuring points: 50 mV/min
3. frequency of measuring points: 4
4. minimal increment: 10 µL

Example for a titration curve

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