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Page 1 of 4 UMA-5182

March 2015

UMA-HPC Method of Analysis

UMA Number: 5182

Old UMA Code: N/A Date of issue: Mar. 2015

Status Current

Method owner: Toilet Soap Bars GDC Brazil

Source: UMA B.X.a.1

Author (year): Lidiane de Oliveira (2011) (Updated AMS-Trumbull 2015)

Approved by (year): Adriana Aoki (2011) (Updated AMS-Trumbull 2015)

QUALITY CONTROL TEST METHOD - ACTIVE & TOTAL


ALKALINITY
Printed Copy = Uncontrolled Copy

The information contained in this document is proprietary to Unilever. No further distribution is


permitted without prior consent of Unilever.

1. WARNING AND SAFETY PRECAUTIONS:

THE MAIN HAZARDS OF THE MATERIALS INVOLVED ARE INDICATED BELOW. USERS SHOULD REFER TO SUPPLIER SAFETY
INFORMATION FOR FURTHER DETAILS. AN ASSESSMENT OF THE RISK TO EMPLOYEES, AND SAFETY PRECAUTIONS
REQUIRED SHOULD BE CARRIED OUT LOCALLY BEFORE COMMENCEMENT OF WORK. IN SOME COUNTRIES THERE IS A
REQUIREMENT TO DOCUMENT THIS ASSESSMENT.

2. SCOPE:

This procedure can be used for aqueous solutions of Raw Materials and finished products capable of being
neutralised w ith a titration grade hydrochloric acid solution.

3. NORMATIVE REFERENCES:

Not available.

4. DEFINITIONS:

Not available.
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March 2015

5. PRINCIPLE:

The active and total alkalinity of alkaline Raw Materials and finished products is determined at pH 8.2 (active) and pH 3.6
(total) respectively w ith the use of an automatic titrator.

6. REACTIONS:

Not available.

7. REAGENTS AND MATERIALS:

7.1 Hydrochloric acid 0.5 N (titration grade)


7.2 pH buffer solutions (pH 4 and pH 10)

8. APPARATUS AND EQUIPMENT:

8.1 Normal laboratory glassw are


8.2 Automatic titrator capable to determine the ml's of titrant used at 2 fixed pH's.
8.3 Combination pH-electrode w ith low alkali error.
8.4 Precision balance (to w eight to ± 1 mg)

9. SAMPLING TECHNIQUE:

Not available.

10. PROCEDURE:

10.1 Titration of a preferably 1 %-solution using a standard volumetric solution of hydrochloric acid and measuring the millilitres
necessary to reach pH 8.2 and pH 3.6 respectively of the solution using an automatic titrator.

10.2 Method
10.2.1 Standardize the electrodes w ith the pH-buffer solutions according to the manufacturer's instructions.
10.2.2 Accurately w eigh 20 g ± 0.001 g of the sample, let the sample dissolve completely w ith distilled or demineralised w ater
and make up in a volumetric flask. Pipette 50 ml of this solution into a 250 ml beaker, add a magnetic stirrer and stir the solution.
Wash the electrodes w ith demineralised w ater and place them into the sample solution.
10.2.3 Titrate w ith 0.5 N HCI using the appropriate method indicated by the titrator till pH 2.5. Setpoints are reached at pH 8.2 and
pH 3.6.

11. CALCULATION & EXPRESSION OF RESULTS:

The results are expressed as % Na20 or NaOH.

V1  N  V3  100  31
Active alkalinity expressed as % Na20 at pH 8.2:
W  V4  1000
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March 2015

V2  N  V3 100  31
Total alkalinity expressed as % Na20 at pH 3.6:
W  V4 1000
Where:

V1 = Volume of 0.5 N HCI needed to reach pH 8.2


V2 = Volume of 0.5 N HCI needed to reach pH 3.6
V3 = Volume of volumetric flask
V4 = Aliquot used for the titration
W = Mass of Raw Material/product w eighed (g)
N = Normality of hydrochloric acid solution

Total alkalinity expressed as %NaOH:

V1  N  40  100
% NaOH 
W  1000

Where:
V1 =endpoint volume of titration
N =normality of hydrochloric acid titrant
40 =molecular w eight of NaOH
W =w eight of sample tested

12. RAW AND PROCESSED DATA:

Not available.

13. QUALITY ASSURANCE AND CONTROL:

Not available.

14. SPECIAL CASES AND NOTES:

14.1 Titrating to fixed setpoints offers the possibility to calculate the theoretical value of active and total Na20 of products if the
values of the appropriate Raw Materials are know n. This also holds if acids are present.
14.2 The method to determine acidity is similar using NAOH as titrant and is expressed as neg. Na 20.
14.3 pH 8.2 and pH 3.6 are chosen because they are used in the Recommended Formulations from ex -Li. Also method G10
from Diversey (Villefranche) is based on the same pH's.
14.4 The pH-determination is part of the method. So the use of a 1 %-solution is preferred.
14.5 Alkali reserve is expressed as % NaOH after titration to pH 10. This alkali reserve can be calculated if a third setpoint at
pH 10 can be settled.
14.6 It is possible to back titrate the same solution to pH 8.2 after boiling the solution for a few minutes and cooling dow n to
room temperature. The difference in mls is determined by the amount of carbonate present in the product.
14.7 Zeolite interferes because it dissolves in acid. Therefore the measurement should be restricted to the active alkalinity
only w hen the zeolite-content is higher than 5%.
14.8 It is possible to express the result as % NaOH. In this case, the calculation described above must be used and the result
must be multiplied by 1.29, i.e., the conversion factor from Na2O to NaOH is 1.29.
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March 2015

15. REFERENCES:

15.1 Unilever Reference: UMA B.X.a.1

16. ANNEXES:

Not available.

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