Draft East African Standard: DEAS 186-2: 2020

Download as pdf or txt
Download as pdf or txt
You are on page 1of 22

DEAS 186-2: 2020

ICS 71.100.40

DRAFT EAST AFRICAN STANDARD

Bathing soap — Specification ― Part 2: Liquid

EAST AFRICAN COMMUNITY

© EAC 2020 Second Edition 2020


DEAS 186-2: 2020

Copyright notice
This EAC document is copyright-protected by EAC. While the reproduction of this document by
participants in the EAC standards development process is permitted without prior permission from EAC,
neither this document nor any extract from it may be reproduced, stored or transmitted in any form for
any other purpose without prior written permission from EAC.

Requests for permission to reproduce this document for the purpose of selling it should be addressed as
shown below or to EAC’s member body in the country of the requester:

© East African Community 2020 — All rights reserved


East African Community
P. O. Box 1096
Arusha
Tanzania
Tel: 255 27 2504253/8
Fax: 255 27 2504481/2504255
E-mail: [email protected]
Web: www.eac-quality.net

Reproduction for sales purposes may be subject to royalty payments or a licensing agreement. Violators
may be persecuted

ii © EAC 2020 – All rights reserved


DEAS-2: 2020

Contents Page

1 Scope ............................................................................................................................................. 1
2 Normative references ................................................................................................................... 1
3 Terms and definitions .................................................................................................................. 1
4 Requirements ................................................................................................................................ 2
4.1 General requirements .................................................................................................................. 2
4.2 Specific requirements .................................................................................................................. 2
6 Packaging and labelling............................................................................................................... 3
6.1 Packaging ...................................................................................................................................... 3
6.2 labelling ......................................................................................................................................... 3
7 Sampling ....................................................................................................................................... 3
8 Criteria for conformity.................................................................................................................. 3
Annex A (normative) Permitted antibacterial agents ............................................................................ 4
Annex B (normative) Determination of Trichlorocarbanilide (TCC) and TricIosan (TCN) in soaps
by HPLC ......................................................................................................................................... 5
B.1 Principle ........................................................................................................................................ 5
B.2 Normal phase HPLC ..................................................................................................................... 5
B.2.1 Reagents ....................................................................................................................................... 5
B.2.2 Apparatus ...................................................................................................................................... 5
B.2.3 Procedure ...................................................................................................................................... 6
B.2.4 Calculation .................................................................................................................................... 6
B.3 Reverse phase .............................................................................................................................. 7
B.3.1 Reagents ....................................................................................................................................... 7
B.3.2 Apparatus ...................................................................................................................................... 7
B.3.3 Procedure ...................................................................................................................................... 7
B.3.4 Calculations .................................................................................................................................. 8
Annex C (normative) Determination of chloroaniline ........................................................................... 9
C.1 Principle ........................................................................................................................................ 9
C.2 Safety precautions ....................................................................................................................... 9
C.3 Reagents ....................................................................................................................................... 9
C.4 Apparatus .................................................................................................................................... 10
C.5 Procedure .................................................................................................................................... 10
C.6 Determination of chloroanilines ............................................................................................... 11
C.7 Calculations ................................................................................................................................ 11
Annex D (normative) Determination of pH ........................................................................................... 12
D.1 General ........................................................................................................................................ 12
D.2 Apparatus .................................................................................................................................... 12
D.3 Reagents ..................................................................................................................................... 12
D.4 Procedure .................................................................................................................................... 12
Annex E (normative) Sampling ............................................................................................................. 13
E.1 Procedure .................................................................................................................................... 13
E.2 Preparation of test samples ...................................................................................................... 13
E.2.1 Composite sample ...................................................................................................................... 13
E.2.2 Samples for testing .................................................................................................................... 13

© EAC 2020 – All rights reserved iii


DEAS 186-2: 2020

Foreword

Development of the East African Standards has been necessitated by the need for harmonizing requirements
governing quality of products and services in the East African Community. It is envisaged that through harmonized
standardization, trade barriers that are encountered when goods and services are exchanged within the Community
will be removed.
The Community has established an East African Standards Committee (EASC) mandated to develop and issue
East African Standards (EAS) and other deliverables. The Committee is composed of representatives of the
National Standards Bodies in Partner States, together with the representatives from the public and private sector
organizations in the community.
East African Standards are developed through Technical Committees that are representative of key
stakeholders including government, academia, consumer groups, private sector and other interested parties.
Draft East African Standards are circulated to stakeholders through the National Standards Bodies in the Partner
States. The comments received are discussed and incorporated before finalization of standards, in accordance
with the Principles and procedures for development of East African Standards.
East African Standards and other deliverables are subject to review, to keep pace with technological advances.
Users of the East African Standards are therefore expected to ensure that they always have the latest versions
of the standards they are implementing.
The committee responsible for this document is Technical Committee EASC/TC 074, Surface active agents
Attention is drawn to the possibility that some of the elements of this document may be subject of patent rights.
EAC shall not be held responsible for identifying any or all such patent rights.
This second edition cancels and replaces the first edition (EAS 766-2:2013), which has been technically revised
and numbered as EAS 186-2.
EAS 186 consists of the following parts, under the general title Bathing soap — Specification:

- Part 1: Solid.

- Part 2: Liquid.

iv © EAC 2020 – All rights reserved


DEAS-2: 2020

Introduction
Human skin provides a favourable environment for the existence and multiplication of a variety of microbes. The
conventional toilet soap washes away the germs but does not kill them. The function of an antibacterial or
antiseptic toilet soap is not only to clean the skin, but also to reduce drastically the bacterial count on the skin.
This prevents skin infections and perspiration odour caused by the decomposition of perspiration by bacteria.

Antibacterial toilet soap is a toilet soap that has antibacterial agents incorporated into it. It not only cleans the
skin, but also reduces drastically the bacterial count on the skin. This prevents skin infections and perspiration
odour caused by the decomposition of sweat by bacteria. The antibacterial toilet soap is especially effective
against staphylococcus and similar bacteria which have the habit of residing in the under layers of the skin. The
antibacterial soaps have to be used regularly to be effective.

In this revision, hexachlorophene has not been permitted to be used as antibacterial agent. The
Trichlorocarbanilide (TCC) on heating decomposes to chloroanalines which are harmful to skin hence the limit
and method for determination of chloroanaline is included. Use of other antibacterial agents not included in
Annex A will be considered when need arises as long as their safety is assured.

© EAC 2020 – All rights reserved v


DRAFT EAST AFRICAN STANDARD DEAS 186-2: 2020

Bathing soap — Specification ― Part 2: Liquid

1 Scope

This Draft East African Standard specifies requirements, sampling and test methods for liquid bathing soap. It
does not apply to hand wash liquid detergents, shampoo and products for specific purposes such as those for
industrial and surgical uses.

2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced document
(including any amendments) applies.

EAS 127, Synthetic laundry detergents for household use — Specification

EAS 377-1, Cosmetics and cosmetics products — Part 1: List of substances prohibited in cosmetic products

EAS 377-2, Cosmetics and cosmetics products — Part 2: List of substances which cosmetic products must not
contain except subject to restrictions laid down

EAS 377-3, Cosmetics and cosmetics products — Part 3: List of colourants allowed in cosmetic products

EAS 377-4, Cosmetics and cosmetics products — Part 4: List of preservatives allowed in cosmetic products

EAS 377-5, Cosmetics and cosmetics products — Part 5: Use of UV filters in cosmetic products

EAS 794 Determination of the microbial inhibition of cosmetic soap bars and liquid hand and body washes —
Test method

ISO 456, Surface active agents — Analysis of soaps — Determination of free caustic alkali

ISO 685, Analysis of soap — Determination of alkali content and total fatty matter content

ISO 673, Analysis of soap — Determination of matter insoluble in ethanol

ISO 862, Surface active agents — Vocabulary

ISO 2271 Surface active agents — Detergents — Determination of anionic-active matter by manual or
mechanical direct two-phase titration procedure

3 Terms and definitions


For the purposes of this standard the terms and definitions given in ISO 862 apply.

© EAC 2020 – All rights reserved 1


4 Requirements

4.1 General requirements

4.1.1 The liquid bathing soap shall consist of essentially of an aqueous solution of potassium soaps, sodium
soaps or both, made from oils, fatty acids or their mixture. It shall be a homogeneous, clear, translucent or
opaque liquid with good lathering and cleaning properties. It may contain permissible synthetic detergents.

4.1.2 The liquid bathing soap shall remain as homogeneous stable product and shall show no sign of
separation or sedimentation when kept at 5 °C for 24 h.

4.1.3 The liquid antibacterial bathing soap shall contain permitted antibacterial agent in accordance with
Annex A.

4.1.4 All the substances used in the liquid bathing soap shall comply with the requirements of all parts of EAS
377.

4.1.5 Liquid bathing soap shall pass the test for dermatological safety.

4.2 Specific requirements

Liquid bathing soap shall also comply with the specific quality requirements specified in Table 1.

Table 1 — Specific requirements for liquid bathing soap

Requirement Test method

Antibacteria
SI No. Characteristic l liquid
liquid bathing soap
bathing
soap

i. Total fatty matter, % by mass, min 15.0 15.0 ISO 685


ii. Free caustic alkali, (K2O), % by mass, max. 0.03 0.03 ISO 456
iii. Synthetic detergents, % by mass, max. 2.0 2.0
ISO 2271
iv. Matter insoluble in ethanol, % by mass, max 5.0 5.0 ISO 673

v. Antibacterial agent TricIosan (TCN) and n/a 1.0 Annex B


Trichlorocarbanilide (TCC), % by mass, max either singly
or in
combination
vi. Chloroaniline content, ppm, max n/a 10.0 Annex C
vii. Phosphate absent absent EAS 127

viii. Antibacterial activity n/a To pass test EAS 794

ix. pH at 27 ± 2°C 7.5 – 9.5 7.5 – 9.5 Annex D

NOTE Trichlorocarbanilide (TCC) is not heat stable and decomposes into chloroanilines on prolonged heating above 60 °C. If TCC is used
in soap, the manufacturer should take care that such soap is not subjected to temperature above 60°C during the entire manufacturing process
or during storage.

2 © EAC 2020 – All rights reserved


6 Packaging and labelling

6.1 Packaging

The bathing soap shall be packed in protective containers that will not allow for damage of the product or its
contamination.

6.2 labelling

a) Each container shall be legibly and indelibly labelled either in English, Kiswahili or French or
combination or any other language as agreed between the manufacturer and supplier with the following
information name of the product as “liquid bathing soap or antibacterial liquid bathing soap”;

b) manufacturer’s name and physical address;

NOTE The name, physical address of the distributor/supplier and trade mark may be added as required.

c) net content;

d) batch number or lot number;

e) date of manufacture and best before date;

f) country of origin;

g) the antibacterial agent used (for antibacterial bathing soap); and

h) list of ingredients in descending order of quantity

7 Sampling
Sampling shall be done in accordance to Annex E

8 Criteria for conformity

The lot shall be deemed to comply with the requirements of this standard if, after inspection and testing, the
requirements of Clause 4 and 5 are satisfied.

© EAC 2020 – All rights reserved 3


Annex A
(normative)

Permitted antibacterial agents

The following is the list of antibacterial agents used generally in antibacterial soap:

a) Triclosan (TCN);

b) Trichlorocarbanilide (TCC);

c) Zinc oxide;

d) Chloro xylenols;

e) Plant extracts;

f) Any other internationally accepted antibacterial agent.

4 © EAC 2020 – All rights reserved


Annex B
(normative)

Determination of Trichlorocarbanilide (TCC) and TricIosan (TCN) in


soaps by HPLC

B.1 Principle
TCC and TCN are antibacterial agents, which are separated from other components in soap by normal phase
or reverse phase liquid chromatography, detected spectrophotometrically and quantified by comparison with
standard TCC and TCN. The method can estimate as low as 1 ppm of the above compounds:

Procedures for both normal and reverse HPLC has been described and provide the option to use either method
whichever is available to the users. Both methods are comparable.

B.2 Normal phase HPLC

B.2.1 Reagents

B.2.1.1 Iso-octane, HPLC grade

B.2.1.2 Iso-propanol (2-propanol), HPLC grade

B.2.1.3 Hexane, HPLC grade

B.2.1.4 Standard TCC, 99 % pure

B.2.1.5 Standard TCN, 99 % pure

B.2.2 Apparatus

B.2.2.1 High Performance Liquid Chromatograph consisting of a pump, a sample injector of fixed
volume with UV detector having variable wavelengths and a recorder

B.2.2.2 Standard volumetric flasks

B.2.2.3 Pipettes

B.2.2.4 Magnetic stirrer

B.2.2.5 Millipore filter apparatus with 0.5 micron filter

B.2.2.6 Column, comprising:

a) Silica column, stainless steel 25 cm x 0.46 cm packed with Normal phase-silica 5 micron
(Lichrosorb Si -60); or

b) Cyano column, stainless steel 25 cm x 0.40 cm packed with (Lichrospher 100) cyano 5 micron

NOTE Either, of the above columns can be used depending on the availability.

B.2.2.7 Mobile phase:

© EAC 2020 – All rights reserved 5


a) for silica column, transfer 20 mL of iso-propanol into a 500-mL volumetric flask and make up to mark
with iso-octane and mix well. Assemble millipore filter apparatus and filter the solvent system prior to
use; and

b) for cyano column, transfer 50 mL of HPLC grade iso-propanol (2-propanol) into a 500-mL volumetric
flask, fill up to the mark with hexane and mix well. Assemble millipore filter apparatus and filter the
solvent system prior to use.

B.2.2.8 HPLC conditions which include the following:

a) Detector wavelength flow rate: 280 nm;

b) Flow rate: 0.5 ml/min;

c) Injection volume: 20 µl;

d) Retention time;

e) Silica column:

 TCN - 7.5 min; and

 TCC - 19.2 min;

f) Cyano column:

 TCN - 4.0 min; and

 TCC - 7.5 min.

B.2.3 Procedure

B.2.3.1 Standard preparation (see note under B.3.4)

Weigh accurately 25 mg of triclosan (TCN) and 25 mg of TCC into a 100-mL volumetric flask and make up to
volume with the mobile phase and mix well. Pipette 1.0 mL of this solution in a 50 mL volumetric flask and dilute
with mobile phase. Final concentration of TCC and TCN is 250 µg/50 mL (5.0 ppm).

B.2.3.2 Sample preparation

Weigh accurately 1 g of homogenized sample into a 100-mL standard flask, and dilute to the mark with mobile
phase. Pipette 10 mL of the supernatant liquid to a 50-mL volumetric flask, dilute with mobile phase, to the mark,
and filter through 0.45 m filter.

B.2.3.3 Chromatography

Equilibrate the column, maintained at a temperature of 30 °C, with the mobile phase with a flow rate of 0.5 mL
/min for iso-octane - iso-propanol mobile phase and 1.0 mL/min for Hexane - iso-propanol mobile phase for 30
min. Set the wavelength at 280 nm. Inject 20 µL of standard solution and then sample solutions.

Measure area of the peaks of respective retention time for standard and sample.

B.2.4 Calculation

TCN shall be expressed as follows:

6 © EAC 2020 – All rights reserved


Area of sample for TCN x Concentration of standard TCN
TCN, percent by mass  x 100
Area of standard TCN x Concentration of sample

Area of sample for TCC x Concentration of standard TCC


TCC, percent by mass  x 100
Area of standard TCC x Concentration of sample

B.3 Reverse phase

B.3.1 Reagents

B.3.1.1 Methanol, HPLC grade

B.3.1.2 Sodium Dihydrogen Phosphate Monohydrate, chemical grade

B.3.1.3 Standard TCC

B.3.1.4 Standard TCN (TCS)

B.3.2 Apparatus

B.3.2.1 Column

B.3.2.1.1 Octyldimethylsilyl (C-DB)

B.3.2.1.2 Supercosil LC-8-DB, 15 cm x 4.6 mm. 5 micron

B.3.2.2 Mobile phase

MeOH/0.01 M Phosphate buffer 62:38 v/v

0.01 M Phosphate buffer: Dissolve 1.38 g sodium dihydrogen phosphate monohydrate in 1 000 mL of distilled
water. Prepare to pH 3.0 by 10 % phosphate solutions.

B.3.3 Procedure

B.3.3.1 Standard preparation (see Note under B.3.4)

B.3.3.1.1 Weigh accurately about 90 mg of TCN. Dissolve in methanol and make up to 1 000 mL volumetric
flask with methanol.

B.3.3.1.2 Weigh about 110 mg of TCC, dissolve well with methanol, and make up the volume to 1 000 mL.

B.3.3.1.3 Accurately pipette 10 mL of the solution prepared in B.3.3.1.1 into the volumetric flask containing
TCC (B.3.3.1.2). And make up to the volume with methanol. Then accurately pipette 5 ml of the solution into a
50-mL volumetric flask. Make up to the volume with methanol. Filter this standard solution through 0.45 µm
filter.

B.3.3.2 Sample preparation

Weigh accurately about 1.0 g of product, dissolve in methanol and make up to 100 mL in a volumetric flask with
methanol. Filter this sample solution through 0.45 m filter.
B.3.3.3 HPLC conditions

The HPLC conditions include the following:

a) Detector wavelength: 280 nm;

© EAC 2020 – All rights reserved 7


b) Column temperature: 35 ºC;

c) Flow rate: 1.0 mL/min; and

d) Injection volume: 10 µL.

Prepare the standard solution and the sample solution at the same time. Inject the standard solution three times
and calculate the average of each ingredients peak count. Inject 10 µg the sample solution and determine each
ingredients percentage by the calculation shown.

B.3.4 Calculations

The TCN and TCC shall be expressed as follows:

TCN, percent by mass =


M s Ar  F 
As  Mt  100

TCC, percent by mass =


M  Ar  F 
s

As  Mt  100
where

Ar is the peak area of the test sample;

As is the averaged peak area of the standard;

F is the purity, expressed as percent, of the standard;

Ms is the mass, in grams, of the standard; and

Mt is the mass, in grams, of the test sample.

NOTE Both TCC and TCN are photosensitive, hence standards should be freshly prepared.

8 © EAC 2020 – All rights reserved


Annex C
(normative)

Determination of chloroaniline

C.1 Principle

The chloroanilines are extracted from soap with dimethyl sulfoxide and diazotized with nitrous acid. The reaction
products are then coupled with N-1-(naphthyl) ethylenediamine hydrochloride to produce coloured compounds
which are estimated spectrophotometrically.

C.2 Safety precautions


Dimethyl sulfoxide (DMSO) is readily absorbed into the skin. Inhalation or skin penetration must be avoided.
DMSO should never be pi petted using mouth. Always use pipette bulb. The standard chloroanilines and N-1-
(naphthyl)-ethylenediamine hydrochloride shall not be allowed to come into contact with the skin. If they should,
then wash the contaminated parts thoroughly with soap and water.

A supply of diluted sodium hypochlorite should be at hand at all times to deal with accidental spillages of
chloroaniline solution. Spillage on laboratory surface should be treated immediately with the sodium hypochlorite
solution, followed by water.

C.3 Reagents
C.3.1 Dimethyl Sulphoxide (DMSO), AR grade

C.3.2 Hydrochloric acid, concentrated (specific gravity, 1.18)

C.3.3 Sodium nitrite, 0.4 % w/v analytical grade, freshly prepared (aqueous)

C.3.4 Ammonium sulphamate, 2 % w/v solution freshly prepared (aqueous)

C.3.5 N-1-(naphthyl) ethylene, 0.1 % w/v solution diamine hydrochloride freshly prepared (aqueous)

C.3.6 n-Butanol, AR grade

C.3.7 Sand, acid purified 40 - 100 micron mesh

C.3.8 Solvent mixture comprising:

 DMSO 5 volumes

 n-Butanol 2 volumes

 Distilled water 2 volumes

 Hydrochloric acid 1 volume

Mix n-butanol, water and HCI. Cool the mixture and add DMSO.

C.3.9 4-Chloroaniline and 3, 4-Dichloroaniline, AR grade

© EAC 2020 – All rights reserved 9


C.4 Apparatus
C.4.1 Spectrophotometer, suitable for use at 554 nm

C.4.2 Cuvettes, glass (matched pair) 10 mm

C.4.3 Water bath, thermostatically controlled at 25 °C

C.4.4 Stopwatch

C.4.5 Standard laboratory glassware

C.4.6 Filter Paper, Whatman No. 541

C.5 Procedure
C.5.1 Dissolve 0.349 8 g of 3,4-dichloroaniline and 0.2753 g of 4-chloroaniline in solvent mixture (see C.3.8)
in a 250 mL amber volumetric flask.

Dilute to mark with solvent mixture. [1 mL is 2.5 mg mixed chloroanilines (stock solution)].

C.5.2 Dilute this stock solution with solvent mixture as given below:

a) take 5 mL of stock solution and dilute it to 250 mL with solvent mixture (1 mL = 50 µg mixed
chloroanilines); and

b) take 5 mL of the above solution [see (a)] and further dilute to 250 mL with solvent mixture. [1 mL = 1 µg
mixed chloroanilines].

Use this solution for preparation of calibration curve.

Transfer using a burette 0, 1 mL, 2 mL, 5 mL, 10 mL, 20 mL, 40 mL into 50 mL amber volumetric flasks.

C.5.3 From a burette, add sufficient solvent mixture to make total volume to 40-mL in each flask. The flasks
are incubated in a water bath at 25 °C for 20 min: After exactly 20 min, add 2-mL of reagent (see C.3.3) into
each flask and return them to the water bath for exactly 10 min (measure with a stop watch).

Then add 2 mL of reagent (see C.3.4) into each flask and return them to the water bath for exactly 10 min. Swirl
the flask occasionally.

Then add 2 mL of reagent (see C.3.5) into each flask and remove them from the water bath. Dilute to volume
with distilled water, mix and allow to stand for 30 min. Measure absorbance at 554 nm against the blank solution
as prepared in C.5.4.

C.5.4 In preparing the blank solution, take 40 mL of solvent mixture in a 50 mL amber volumetric flask.
Incubate the flask in a water bath at 25 °C for 20 min. After exactly 20 min, add 2 mL of reagent (see C.3.3) into
the flask and return it to the water bath for exactly 10 min. Then add 2 mL of reagent (see C.3.4) into the flask
and return it to the water bath for exactly 10 min (swirl the flask occasionally). Then add 2 mL of reagent (see
C.3.5) into the flask and remove it from the water bath. Dilute to volume with distilled water, mix and allow to
stand for 30 min. Use this blank solution for preparation of calibration curve only.

C.5.5 Prepare a graph by plotting weight (g) of chloroanilines contained in each 50 mL-flask against
absorbance. The linear calibration will pass through the origin/or determine the average absorbance (AA) of 1
g of mixed chloroanilines by dividing sum of absorbances of all different aliquots of the standard by sum of g
of chloroanilines in all different aliquots of standard.

10 © EAC 2020 – All rights reserved


C.6 Determination of chloroanilines
C.6.1 Weigh to the nearest mg 3.0 g - 15 g of finely grated soap and add 10.0 g - 15.0 g of acid purified sand.
Transfer quantitatively the sample and the sand into a mortar and grind the mixture thoroughly with a pestle to
give a homogenous mass. Transfer the mass to a previously weighed 250-mL flat bottom flask quantitatively
and reweigh. Add DMSO (100 mL), stopper firmly and attach the flask to an automatic shaker. Shake for 1 h.
Filter the DMSO extract through Whatman No. 541 into a 250 mL amber volumetric flask. Wash the flask and
filter paper with small aliquots of DMSO. Allow the filtrate to drain completely, dilute to volume with DMSO and
mix. Transfer 20 mL DMSO extract into a 50-mL amber volumetric flask. Add 20 mL of solvent mixture. The
flask is incubated in a water bath at 25 °C for 20 min. After exactly 20 min, add 2 mL of reagent (see C.3.3) into
the flask and return it to the water bath for exactly 10 min (measure with a stop watch). Then add 2 mL of
reagent (see C.3.4) into the flask and return it to the water bath for exactly 10 min (swirl the flask occasionally).
Then add 2 mL of reagent (see C.3.5) into the flask and remove it from the water bath. Dilute to volume with
distilled water, mix and allow to stand for 30 min. Read the absorbance at 554 nm against blank (prepared as
below).

C.6.2 Prepare the blank solution by mixing 20 mL of DMSO extract of sample and 20 mL of solvent mixture
in a 50 mL amber volumetric flask. Incubate the flask in a water bath at 25 °C for 20 min.

After exactly 20 min, add 2 mL of distilled water into the flask and return it to the water bath for exactly 10 min.
Then add 2 mL of reagent (see C.3.4) into the flask and return it to the water bath for exactly 10 min (swirl the
flask occasionally). Then add 2 mL of reagent (see C.3.5) into the flask and remove it from the water bath. Dilute
to volume with distilled water, mix and allow to stand for 30 min. Use this solution as a blank for reading sample
only.

C.6.3 Deduce the amount of chloroanilines (µg) from the calibration graph curve.

NOTE The determination should be completed in one day.

C.7 Calculations
Determine the amount of mixed chloroanilines in the aliquot of test solution from the calibration graph.

250M  M 1  M 3
Chloroaniline content (in ppm) =
20M 2M

where

M is the mass, in grams, of soap;

M1 is the mass, in grams, of sand;

M2 is the mass, in grams, of soap and sand transferred to the flask; and

M3 is the mass, in micrograms, of mixed chloroanilines found from calibration graph/or it can be calculated
as given below:

Mass of the sample


M3 =
Average absorbance of 1 μg mixed chloroanilines (AA)
where

Sum of the OD of the standards


AA =
Sum of concentration of standard chloroanilines in μg

M 2M
Weight of soap actually used, in g =
M  M1 

© EAC 2020 – All rights reserved 11


Annex D
(normative)

Determination of pH

D.1 General

pH determination should be made in an acid free atmosphere.

D.2 Apparatus
D.2.1 Any standard pH meter, equipped with a low sodium error glass electrode. The instrument shall be
calibrated and standardized with standard buffer solutions (see D.3.2) before use.

D.2.2 Volumetric flask, 1000-mL capacity

D.2.3 Beakers, 1000-mL

D.3 Reagents
D.3.1 Distilled water shall be boiled thoroughly or purged with carbon dioxide-free air to remove carbon dioxide
and shall be protected with soda lime or soda asbestos while cooling and in storage. The pH of this water shall
be protected with soda lime or soda asbestos while cooling and in storage. The pH of this water shall be between
6.2 and 7.2 at 27 °C. The residue on evaporation when heated at 105 °C for one hour shall not exceed 0.5 mL
per litre.

D.3.2 Standard buffer solutions with the pH range of 9 to 11 at 27 °C for calibrating the pH meter.

D.4 Procedure
Weigh to the nearest milligram approximately 10 g of the material and transfer to a 1-L volumetric flask. Partially
fill the flask with distilled water and agitate until the sample is completely dissolved. Adjust the temperature of
the solution and the distilled water to 27 °C ± 2 °C and fill to the calibration mark with distilled water, stopper the
flask mix thoroughly and allow the solution to stand at a temperature of 27 °C ± 2 °C for two hours prior to
measuring the pH. Measure the pH of the solution at 27 °C ± 2 °C using a glass electrode.

12 © EAC 2020 – All rights reserved


Annex E
(normative)

Sampling

E.1 Procedure
D.1.1 In a single consignment, all packages (cartons) containing toilet soap cakes drawn from the same batch
of production shall constitute a lot. For ascertaining the conformity of the lot to the requirements of this standard,
tests shall be carried out on each lot separately. The number of packages to be selected for drawing the sample
shall be in accordance with Table E.1.

Table E.1 — Scale of sampling

Number of packages (cartons) Number of packages (cartons) to be Number of samples


in the lot selected
N n

4 to 15 3 3
16 to 40 4 4
41 to 65 5 2
66 to 110 7 2
111 and above 10 1

E.1.2 The packages shall be selected at random, using tables of random numbers. If these are not available,
the following procedure shall be applied:

Starting from any package, count all the packages in one order as 1, 2, 3.... N, selecting every k th package,
where k is the integral part of N  n.

E.1.3 From each package thus selected, draw at random an equal number of cakes so as to obtain a total
mass of at least 2 kg.

E.2 Preparation of test samples

E.2.1 Composite sample

Weigh each cake separately (including any material that may have adhered to the wrapper), and calculate the
average mass. Cut each of the remaining cakes into eight parts by means of three cuts at right angles to each
other through the middle. Grate finely the whole of two diagonally opposite eighths of each specimen. Mix the
gratings and place in a clean, dry, airtight glass container.

E.2.2 Samples for testing

Immediately after preparation of composite sample (E.2.1), take at one time all test samples required for the
tests in 4.2. Weigh out the test sample required for determination of free alkali or acid content, and use it
immediately.

© EAC 2020 – All rights reserved 13


EAS 766-2: 2013

© EAC 2013 – All rights reserved

You might also like