Content of free Al kali in Colorati ons,

P er ms a nd S trai ght e ners,

Ti trim etri c
Test Method No.: 95000 (F05.0) Revision No.: 2

Principle of Test Measurement:

This procedure is an acid-base titration with 0.1N hydrochloric acid. The endpoint is detected
visually or by using a pH-electrode.

Purpose and Application:

This method is applicable for the determination of the free alkali content in colorations, perms,
and straighteners. The results are calculated as percent ammonia or monoethanolamine (MEA).

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. Automatic titrator (e.g. Metrohm Titrando 907) and pH-electrode (e.g. Schott N 61) or
appropriate burette for visual endpoint determination
2. Volumetric pipette, Class A
3. Analytical balance capable of weighing to a resolution of 0.0001g
4. Magnetic stirrer and magnetic stir bars
5. Beaker
6. Disposable syringes

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. Deionized water
2. 0.1N hydrochloric acid (HCl) – (e.g. VWR# BDH 7200-1)
3. Mixed indicator 5, for ammonia titrations (e.g. Sigma Aldrich 69793-250ML, Merck
Millipore# 1061300250)
4. Tris-(hydroxymethyl)-aminomethane p.a.,(C4H11NO3) (CAS-No 77-86-1) for titer
determination – (e.g. VWR# MK180657)

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. Add a small amount (just covering the bottom of the beaker) of deionized water to a
beaker.
2. The amount of sample specified in the Raw Material or Product Data Sheet is weighed
(W, in g) into the beaker to the nearest 0.0001g. It is recommended that the sample be
weighed into the beaker by difference using a disposable syringe.
3. Add a magnetic stir bar and turn the sample into a slurry.
4. Add another 80ml of deionized water to the beaker while stirring until the sample is
completely suspended.
5. a) A few drops of mixed indicator No. 5 are added and the solution is titrated with 0.1N
hydrochloric acid until the color changes from green to violet.
Or

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 Content of free Al kali in Colorati ons,
P er ms a nd S trai ght e ners,
Ti trim etri c
Test Method No.: 95000 (F05.0) Revision No.: 2

b) Titrate with 0.1N hydrochloric acid until the equivalence point is reached. An example
for the instrument setting of the titrator is given in Appendix A
6. Record the amount of titrant consumed (V, in ml) to the nearest of 0.01 ml

Titer/Calibration/Standardization:
The titer of the 0.1 HCl solution should be checked against standard reagent Tris-
(Hydroxymethyl)-aminomethane quarterly.

1. 50-70 mg (W) Tris-(Hydroxymethyl)-aminomethane p.a. are weighed (accuracy 0.1 mg)

into a beaker and dissolved in 60ml of deionized water. The sample should be stirred
and may require ultrasonication. Titrate the resulting solution with 0.1N hydrochloric acid
using mixed indicator 5 to the visual endpoint. Record the volume of titrant (V, in ml) to
the nearest 0.01ml.
2. Calculate the titer of the 0.1N hydrochloric acid using the equation 1, below.

W W
t (HCl) = = (1)
121.14g/mo l * 0.1mol/L * V 12.114 * V

W = sample weight in mg
V = consumption in ml
121.14 g/mol = molecular weight of Tris-(hydroxymethyl)-aminomethane

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. Calculate the amount of ammonia (%) in the sample using equation 2.

V * t * c * 17.03 * 100% V * t * 0.1703

NH3 (%) = = (2)
W * 1000 W

2. Calculate the amount of monoethanolamine (MEA, in %) in the sample using equation 3.

V * t * c * 61.1 * 100% V * t * 0.611

MEA (%) = = (3)
W * 1000 W

V = volume of titrant consumed in the assay (ml)

c = concentration of the HCl solution = 0.1 mol/L
t = titer
17.03 = molecular weight of ammonia g/mol
61.1 = molecular weight of MEA g/mol
W = sample weight (g)

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 Content of free Al kali in Colorati ons,
P er ms a nd S trai ght e ners,
Ti trim etri c
Test Method No.: 95000 (F05.0) Revision No.: 2

Information in Raw Material or Product Data Sheet:

1. Alkali to be calculated (ammonia or monoethanolamine)

2. Sample weight (g)
3. Alternative sample preparation

References:

1. Autenrieth-Keller, Quantitative Chemical Analysis, p. 156

Comments:

1. Samples are to be tested in duplicate.

2. Repeatability

Rec.-no Product Average (n=6) Standard Coefficient of Variation

Deviation COV ± %
FAR09CB0114\22 Sensual Colors 9-4 5.55 0.039 0.70

History/Changes:

1. Updated to Harmonized format. (2014)

Original Issue Date: 27.12.1971 Created by: Ms. Schaefer

Revision No / Issue Date: 02 / 08.05.2014 Revised by: Mathiesen / Lefev

Appendix A

Example for the instrument setting of the titrator (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
5. Potentiometric endpoint evaluation:
Endpoint criteria: 5

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