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IS 4956 (2002) :Synthetic Detergent for Industriel Purposes

[CHD 25: Soaps and other suriace Active Agents]

Satyanarayan Gangaram Pitroda

"Invent a New India Using Knowledge"

Made Available By
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 IS 4956: 2002

fafRrfe
(THRT TerT)
Indian Standard
SYNTHETIC DETERGENTS FOR INDUSTRIAL
PURPOSES-SPECIFICATION
(Second Revision )

ICS 71.100.40

BIS 2002
BUREAU OF INDIAN STANDAR DS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

April 2002
Price Group 7
 Soaps and other Surface Active Agents Sectionai Committee, CHD 25

FOREWORD

This Indian Standard (Second Revision) was adopted by the Bureau of Indian Standards, after the draft finalized
by the Soaps and other Surface Active Agents Sectional Committee had been approved by the Chemical Division
Council.
Synthetic detergents or non-soapy detergents (NSD), as they are usually termed, are products specially formulated
to promote the development of detergency, and comprise essential components (surface active agents), and
generally, complementary components like builders, etc. The NSD produced in this country at present are
mainly of the alkyl aryl type, such as sodium salt of dodecyl benzene sulphonic acid and thus they are different
from soaps, the other class of detergents, which are mainly sodium salts of higher fatty acids. The limitations of
soaps for use in hard water areas have led to the development of synthetic detergents.
This standard was first published in 1968 and subsequently revised in 1977, during which the requirement for
matter insoluble in alcohol and non detergent organic matter were dropped, the limit for moisture content was
reduced and the requirement for active ingredient for Type 2 of the material was increased from 30 to 40 percent
and that for Type I was reduced from 40 to 35 percent based on that periods industrial practice. The method for
determination of active matter by cationic titration was also incorporated.
This revision is taken up to incorporate the declaration of ingredients used in the manufacture of detergents in
the marking clause and also to incorporate the existing six amendments to this standard.
This standard contains 5.1 which calls for agreement between the purchaser and the supplier.
A scheme for labelling environment friendly products known as EcO Mark has been introduced at the instance
of the Ministry of Environment and Forests (MEF), Government of lndia. The ECO Mark would beadministered
by the Bureau of Indian Standards (BIs) under the BIS Act, 1986 as the Resolutions No. 71 dated 21 February
1991 and No. 425 dated 28 October 1992 published in the Gazette ofthe Government of India. For a product to
be eligible for marking with ECO logo, it shall also carry the ISI Mark of BIS besides meeting additional
environment friendly requirements. The requirement to be satisfied for a product to qualify for the BIS Standard
Mark for ECo friendliness, has been included in this revision. These requirements will be optional; manufacturing
units will be free to opt for the ISI mark alone also.
It is necessary that the raw materials used in the production are such that inthe concentrations in which they
will be present in the finished product, after interaction with the raw material usedin the formulation, are free
from any harmful effects. For determining the suitability ofa new formulation or of a new raw material used in
old formulations in the skin, reference may be made to IS 1 1601 (Part 1).

The Composition of the Committee responsible for formulation of this standard is given in Annex J.
For the purpose of deciding whether a particular requirement of this standard is complied with, the final value,
observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with
Is 2: 1960 Rules for rounding offnumerical values (revised)'. The number ofsignificant places retained in the
rounded off value should be the same as that of the specified value in this standard.
 IS 4956:2007

Indian Standard
SYNTHETIC DETERGENTS FOR INDUSTRIAL
PURPOSES-SPECIFICATIOON
(SecondRevision)
1 SCOPE b)Type2- Paste, and
This standard prescribes requirements and methods c)Type3- Liquid.
of sampling and test for synthetic anionic detergents 5 REQUIREMENTS
for industrial purposes.
5.1 Description
2 REFERENCES
The active ingredient shall be the sodium salt of alkyl
The Indian Standards listed below contain provisions benzene sulphonic acid conforming to IS 8401. The
which through reference in this text, constitute formulation may contain one or more of the builders
provisions of this standard. At the time of publication, r additives given in Annex A or any other builders
the editions indicated were valid. All standards are or additives keeping in view the end-use of the product.
subject to revision, and parties to agreements based
on this standard are encouraged to investigate the 5.2 The material shall be in the form of free flowing
possibility of applying the most recent editions of the powders, paste or clear liquid, free from visible dirt
standards indicated below: and impurities. It shall not give any unpleasant odour
It shall have good cleaning and lathering properties.
IS No. Title
5.3 The material shall pass the test for skin sensitiza-
286: 1978 Methods of sampling and test for tion potential when evaluated as per the method
soaps (second revision) prescribed in IS 11601(Part 1) and for skin sensitiza-
1070: 1992 Reagent grade water{third revision) tion potential when evaluated as per the method
4707 Classification for cosmetics raw
prescribed in IS 11601 (Part 2).
(Part 1): 1988 materials and adjuncts: Part 1 dyes,
colours and pigments (first revision) 5,4 The material shall also comply with the require
Methods for random sampling ments given in Table 1.
4905: 1968
7597: 1974 Glossary of terms relating to surface
5.5 Additional Requirements for ECO Mark
active agents
8401 1994 Alkyl benzene sulphonic acid (acid 5.5.1 General Requirements
slurry) (first revision) 5.5.1.1 The product shall conform to the requirements
l1601 Method of safety evaluation of
for quality, safety and performance prescribed
synthetic detergent: under 5.1 to 5.4.
(Part ): I986 Method of test for irritant potential
of synthetic detergents 5.5.1.2 The manufacturer shall produce to BIS
1992 Method of test for skin sensitization
environmental consent clearance from the concerned
(Part 2):
potential of synthetic detergents State Pollution Control Board as per the provisions of
(Guinea pig maximization test) Water (Prevention and Control ofPollution) Act, 1974
13933 1995 Method of test for ready biodegrada and Air (Prevention and Control of Pollution) Act.
bility of surface active agents (Modi 1981 along with the authorization, if required, under
fied Strum test) the Ervironment (Protection) Act, 1986 while applying
for ECO Mark.
3 TERMINOLOGY
5.5.2 Specific Requirements
For the purpose of this standard, the definitions given
in IS 7597 shall apply. 5.5.2.1 The material shal not contain any phosphate
when tested as per the method given in Annex D of
4 TYPES IS 4955.
The material shall be of follow ing three types based 5.5.2.2 The material shall pass the test when evaluated
on its physical form, namely: for irritant potential as per the method prescribed in
IS 1601 (Part 1) and for skin sensitization potential
a) Type 1-Powder or Flakes,
IS 4956: 2002

when evaluated as per the method prescribcd in 3) Soda ash,

IS 11601 (Part 2). 4) Fillers, and
5) Enzymes, if added.
5.5.2.3 The activeingrediet u_ed in the manufacture
of synthetic detergents for industrial purposes shall 6.2.2 Additional Marking Requirementsfor ECO Mark
be readily biodegradable when tested as per 1S 13933. :

The package shall also be marked with the criteria for

6 PACKING AND MARKING which the product has been labelled as ECO Mark.

6.1 Packing 6.2.3 BIS Certification Marking

6.1.1 The material shall be supplied in HDPE drums The packages may also be marked with the Standard
or in suitable, well-closed containers, as agreed to Mark.
between the purchaser and the supplier.
6.2.3.1 The use of the Standard Mark is governed by
6.1.2 For ECO Mark the product shall be packed in the provisions of the Bureau of Indian Standards Act,
such packages which are made from 1986 and the Rules and Regulations made thereunder.
recyclable The details of conditions under which the licence for
reusable or biodegradable material and declared by
the manufacturer and may be accompanied with the use of the Standard Mark may be granted to
detailed instructions for proper use. manufacturers or producers may be obtained from the
Bureau of Indian Standards.
6.2 Marking
7 SAMPLING
6.2.1 The containers shall be and legibly indelibly
marked with the following information: Representative samples of the material shall be drawn
as prescribed in Annex H.
a) Name of the manufacturer;
b) Name, type and recognized trade-mark ofthe 8 TESTS
product, if any;
8.1 Tests shall be carried out as prescribed in Annexes
c) Net mass when packed; B to G. Reference to the relevant annex is given in col
d) Batch No. or lot No. in code or otherwise; 6 of Table 1.
e) Month and year of manufacture; and
8.2 Quality of Reagents
The following
identified critical ingredients
in descending order of quantity, percent by Unless specified otherwise, pure chemicals and
mass distilled water (see IS 1070) shall be used in tests.
1) Active ingredients,
NOTE-Pure chemicals" shall mean chemicals that do not
2) Builders used, contain affect the results of
impurities which analysis.

Tabie 1 Requirements For Synthetie Detergents for Industrial Purposes

(Clauses 5.4 and 8.1)
SI Characteristic Requirements Method of test, Ref
No. to Annex

Type Type 2 Type 3

(1) (2) (3) (4) (5) (6)

i) Moisture and volatile matter content, percent by 5 B
mass, Max

Active ingredient, percent by mas, Min 35 20 C&D

ii) Clear point, °C, Max 10 E
iv) pH of I percent (m/v) at 30°C 7 to 9 7 to 9 6 to8 F
Matter insoluble in water, percent by mass, Max 0.5 0.5 Nil G
 IS 4956: 200

ANNEX A

(Clause 5.1)
LIST OF cONVENTIONAL BUILDERS AND ADDITIVESs

1. Trisodium phosphate 8. Sodium silicate

2. Sodium carbonate 9. Optical brightener
3. Sodium sulphate 10. Lather boosters
4. Tetrasodium pyrophosphate 11. Hydrotropes
5. Sodium tripolyphosphate 12 Perfumne
6. Sodium hexametaphosphate 13. Preservatives
7. Sodium carboxymethyl cellulose 14. Chelating agents (sequestering agents)
15. Colours

ANNEX B

[Table 1, S No. ()]

DETERMINATION OF MOISTURE AND VOLATILE MATTER

B-1 APPARATUS weigh. Constant mass shall be considered to have been

attained when successive heating for one-hour period
B-1.1 Porcelain or Silica Dish-6 to 8 cm in
shows a difference of not more than 5 mg in the net
diameter and 2 to 4 cm in depth.
loss in mass.
B-1.2 Desiccator-containing an efficient desiccant,
such as phosphorus pentoxide. B-3 CALCULATION

B-1.3 Air-Oven-preferably electrically heated, with Moisture and volatile matter, (M-m)x 100
temperature control device for maintaining Content, percent by mass
M
temperature at 105 + 1°C.
where
B-2 PROCEDURE M = mass in g of the material taken for the test,

and
Weigh accurately about 5g of the material into a dry
mass in g of the material after drying.
tared dish, and dry to constant mass in an air-oven at
a temperature of 105 1°C. Cool in a desiccator and
 IS 4956: 2002

ANNEX C
[Table 1, SI No. (i)]
DETERMINATION OF ACTIVE MATTER BY CATIONIC TITRATION

C-1 GENERAL C-4.3 Standard Sulphuric Acid- 1.0N.

in the method prescribed, the molecular mass of active C-4.4 Standard Sodium Hydroxide Solution
matter has been taken as 342. In
practice, the molecular 1.0 N.
mass of sodium alkyl benzene
sulphonate varies from C4.5 Standard Sodium Lauryl Sulphate Solution
337 to 347 depending on the molecular mass of
alkyl
benzene used for sulphonation. This method as 0.001 M. Check the purity of the sodium lauryl
prescribed should, therefore, be used for routine sulphate as given in C-4.5.1 and simultaneously
analysis. In case of any dispute or doubt, the molecular prepare the standard solution.
mass of sodium
alkyl benzene sulphonate shall be
determined as prescribed in Annex D and then used C-4.5.1 Determination of Purity of Sodium Lauryl
in calculating the active matter content
by the method. Sulphate
Weigh to the nearest I mg, 5 + 0.2 g of the material
C-2 OUTLINE OF THE METHOD
into a 250 ml round bottom flask with ground-glass
A solution of the anionic neck. Add exactly 25 ml of standard sulphuric acid
detergent containing added
methylene blue is shaken with chloroform, which solution (1.0 N) and reflux under a water condenser.
dissolves the methylene blue salt of the detergent. The During the first 5 to 10 minutes, the solution will
mixture is titrated with a cationic -active agent, which, thicken and tend to foam strongly; control this by
after it has combined with all the free anionic Temoving the source of heat and swirling the contents
detergent, begins to displace methylene blue from the of the flask. In order to avoid excessive foaming,
salt. The end-point is taken when sufficient instead of refluxing, the solution may be left, on a
methylene
blue has been displaced into the aqueous layer to boiling water bath or one hour. After 10 minutes the
produce phases of equal colour intensity. As the solution clarifiesthe foaming ceases. Reflux for 1% h.
reaction is not stoichiometric, it is essential to carry Remove the source of heat,
cool the flask and carefully
out standardization using a known anionic rinse the condenser with 30 ml of ethanol followed by
detergent
similar in nature to the unknown. water. Add a few drops of phenolphthalein solution
and titrate with standard sodium hydroxide solution.
NOTE-Hypochlorites and sulphites interfere with detection of
the end point and should be destroyed by the addition of ferrous Carry out a blank test by titrating 25 ml of sulphuric
sulphate and hydrogen peroxide respectively. acid solution (1.0 N) with standard sodium
hydroxide
solution.
C-3 APPARATUS
Purity of the sodium lauryl
C-3.1 Volumetric Flasks- 1 000, 500 and 250 ml.
2884 (V-V%) N
sulphate, percent by mass=
C-3.2 Stoppered Graduated Cylinder - 100 ml.
where
M
C-3.3 Graduated Cylinder- 50 mi V,= volume in ml of standard sodium
C-3.4 Burette- 25 ml.
hydroxide solution used for the sample,
C-3.5 Pipette 10 ml. volume in ml of standard sodium
C-3.6 Beaker- 250 ml.
hydroxide solution used for the blank,
N, normality of standard sodium hydroxide
C-4 REAGENTS solution , and
M = mass in g of sodium lauryl sulphate under
C-4.1 Chloroform-Chemically pure.
test.
C-4.2 Sulphuric Acid
C-4.5.2 Procedure
5N solution. Carefully add 134 ml of sulphuric acid
Weigh to the nearest 1 mg, between 1.14 and 1.16 g
(relative density 1.84) to 300 ml of water and dilute to of sodium lauryl sulphate and dissolve in 200 ml of
litre.
water. Transfer to a ground-glass stoppered, I litre
one-mark volumetric flask and dilute to the mark with
water
 IS 4956: 2002

Calculate the molarity, T, of the solution by means of C-S PROCEDURE

the formula:
C-5.1 Standardization of Benzethonium Chloride
Solution
Purny, percentby
mass
7,
288.4x100 C-5.1.1 Pipette 10 ml of standard sodium laury!
sulphate solution (see C-4.5) into a 100-ml graduated
where cylinder provided with a glass stopper. Add 15 ml of
M, = mass in g of sodium lauryl sulphate taken. chloroform and 25 ml of methylene blue reagent 1
C-4.6 Standard Benzethonium Chloride Solution cylinder. Shake well. The chloroform layer (lower)
shall be coloured blue or greenish blue.
0.004 M. Weigh to the nearest I mg between 1.75 g
and 1.85 g of benzethonium chloride and dissolve in C-5.1.2 Add from the burette benzethonium chloride
solution slowly, initially in portions of 0.2 ml. After
water. Transfer to a ground-glass stoppered 1-litre one
mark volumetric flask and dilute to the mark with each addition, stopper the cylinder, shake well and
water.
allow the phases to separate. Initially the chloroform
phase will be coloured blue or greenish blue. Towards
NOTES the end the colour would start migrating to the aqueous
1 In order to prepare a 0.004 M solution, dry the benzethonium
layer. Note the reading at which the colour intensity
chloride at 105'C, weigh 1.792 to the nearest, I mg, dissolve in
water and dilute to I litre. While drying take care not to raise the
in both the phases is the same when viewed under
temperature beyond 105C standard conditions of light, for example, against a
2 Other cationic reagents, such as cetyl trimethyl ammonium white porcelain tile under normal daylight.
bromide and benzalkonium chloride, give results identical to those
obtained using benzethonium chioride. However, these tests have C-5.1.3 Calculate the molarity of benzethonium
not been carried out in sufficient number to make it possible to chloride solution, T2, as follows:
state that the results will be identical no matter what the product
analysed: for that reason, if benzethonium chloride is not avail
able it is permitted to use another reagent provided that this is
stated in the test report. However, in case of doubt and always in
where
T
case ofa dispute, only benzethonium chloride should be used.

C-4.7 Phenolphthalein Solution

T molarity of sodium lauryl sulphate
solution, and
Dissolve 1 g of phenolphthalein in 100 mg of V volume in ml of benzethonium chloride
95 percent (v/v) ethanol. solution added.

C-4.8 Methylene Blue Solution C5.2 Determination of Active Ingredient

Proceed as described in C-5.1, taking 10 ml of the
0.005 percent. Dissolve .05 g of methylene blue, 50 g
sample solution (C-4.9) instead of sodium lauryl
of sodium sulphate and 6.8 ml of concentrated
sulphate solution.
sulphuric acid in water and make up the volume to
I litre with water. C-5.3 Calculation

C-4.9 Sample Solution Calculate the active ingredient as sodium alkyl

benzene sulphate as foliows:
Weigh a suitable quantity of the sample containing
100 to 160 mg of anionic active matter per 100 ml of
solution. About 1gofsodium alkyl benzene sulphonate 342 V7 x S
Active ingredient, percent by mass
or 3 g of the sample having around 20 percent anionic M2
active matter content per 500 ml of the solution is
suitable. where

V=volume in ml of benzethonium chloride

solution added,
T molarity of benzethonium chloride
DThe full name of this chemical is benzyl dimethyl2-12-p(1,1,3,3-
solution (see C-5.1.3),
tetramethyl-butyl) phenoxy-ethoxy] ethyl ammonium chloride, mono-
M, = mass in g of the sample taken, and
hydrate (CH,), C.CH,.C.(CH,), C,H,CH,.OCH, OCH,
CH,N(CH,), CH,C,H,I' CF H,O. 342 molecular mass of sodium alkyl benzene
it is commercially sold under the name 'Hyamine 1622 sulphonate taken for calculation.

5
 IS 4956: 2002

ANNEX D
[Table 1, SI No. (i) and Clause C-1]
DETERMINATION OF MOLECULAR MASS OF
SULPHONIC ACID OR SODIUM SALT OF SULPHONIC ACID

D-1 APPARATUS bath for about 2 minutes. Stir and break up any hard
D-1.1 Beakers- 150 ml and 1 000 ml lump with a glass rod flattened at one end. Allow the
capacity. solid matter to settle and decant the hot alcoholic
D-1.2 Buchner Flask-500 ml capacity, fitted with solution through a sintered glass filter funnel fitted to
a sintered
glass filter funnel (porosity 4). a Buchner flask to which suction is
applied. Repeat
the alcoholic digestion in a similar manner with 5
D-1.3 Evaporating Basin
further consecutive 30 ml portions of boiling ethyl
D-1.4 Separating Funnel- 1 000 ml alcohol. Filter each extract in turn through the same
capacity.
sintered glass funnel and finally, wash the residue
D-1.5 Steam-Bath
several times with hot ethyl alcohol to remove all the
D-1.6 Wide-Mouthed Flat-Bottomed alcohol soluble. Evaporate the combined filtrate to a
200 ml capacity.
Flask simall bulk in an evaporating dish and transfer it to a
separating funnel. Rinse the evaporating dish once
D-1.7 Air-Oven- to maintain a temperature of
with 50 ml of 96 percent ethyl alcohol and then four
100 + 1°C, with temperature control device.
times with 50 ml portions of water. Add each wash in
D-2 REAGENTS turn to the separating funnel. Add 150 ml of diethyl
ether, swirl gently to ensure adequate mixing, and
D-2.1 Caustic Soda Solution- 10 percent
(mv). allow the two phases to separate. Run off the aqueous
D-2.2 Ethyl Alcohol-30 percent, 96 percent, and alcoholic layer into a second separating funnel, and
absolute (vv). extract twice with 75 ml portions of diethyl ether.
Transfer the aqueous alcoholic phase into a beaker,
D-2.3 Diethyl Ether and combine the three ether extracts.

D-2.4 Acetone D-3.2 Take the combined ether extracts in a clean

separating funnel. Wash three times with successive
D-2.5 Phenolphthalein Indicator- 1 percent 50 ml portions of 30 percent ethyl alcohol and then
solution in 95 percent (/v) ethyl alcohol. with successive 50 ml portions of water until the ether
phase is free from alcohol; usually 7 to 10 water washes
D-2.6 Methyl Orange Indicator-0.1 percent
(m/v) are necessary. Combine all the alcoholic and aqueous
Ferric Ammonium
D-2.7
Saturated solution.
Sulphate Indicator- extracts, neutralize to phenolphthalein and evaporate
on a steam-bath until the volume is reduced to about
25 ml. Add an equal volume of absolute alcohol and
D-2.8 Standard Sulphuric Acid- Approximately
0.1 N.
evaporate to dryness. The solution shall remain just
pink to phenolphthalein throughout evaporation. To
D-2.9 Standard Ammonium Thiocyanate Solution ensure that the residue is completely anhydrous, add
- Approximately 0.1 N. 30 ml of absolute alcohol and again evaporate to
dryness. Extract the residue with 30 ml of hot
D-2.10 Standard Silver Nitrate Solution
96 percent ethyl alcohol, stirring and breaking up the
Approximately 0.1 N.
solid matter in the dish with a glass rod. Allow the
D-2.11 Nitrie Acid-Concentrated relative density solid matter to settle and decant the hot alcoholic
1.42. solution through a sintered glass filter funnel fitted to
a Buchner flask to which suction is applied. Extract
D-2.12 Nitrobenzene the residue in the dish with six further consecutive
30 ml portions of hot 96 percent ethyl alcohol. Pass
D-3 PROCEDURE
each extract in turn through the sintered glass filter.
D-3.1 Weigh about 2 g of the material into a 150-ml Finally, wash the residue in the sintered glass filter
beaker. Dissolve in minimum quantity of water and three times with about 20 ml of hot 96 percent ethyl
neutralize with caustic soda solution. Evaporate on a alcohol from the jet of a wash bottle.
steam-bath to almost complete dryness. Digest with
D-3.3 Transfer the filtrate and washings in the
50 ml of 96 percent ethyl alcohol by heating on steam-
Buchner flask to a wide, mouth flat-bottomed flask,
 IS 4956: 2002

evaporate nearly to dryness on a water-bath, and drive carbonates (see D-3.4.1.2), add 2 ml of concentrated
offthe remaining solvent by directinga gentle stream nitric acid and 20 ml of standard silver nitrate solution.
of dry air into the flask whilst continuously rotating Add 3 ml of nitrobenzene and shake vigorously. Titrate
the latter in the water-bath. A thin film of active with standard ammonium thiocyanate solution using
ingredient, easy to dry, is thereby obtained. Add 10 ml ferric ammonium sulphate as indicator.
of acetone, evaporate and remove the last traces of
D-3.4.2.1 Calculation
solvent as described above, cool in a desiccator and
weigh. Heat the flask for not more than 5 minutes in Mass in g of M
an air-oven at temperature of 100 1°C, gently blow sodium chloride 0.058 5(20 N,-V,N,)x
M
=

out with a current of air, cool and re-weigh. Repeat

where
this drying process until the difference between two
successive weighings does not exceed 3 mg. V volume in ml of standard ammonium
thiocyanate solution used,
D-3.4 The extract obtained contains the active
ingredients, some sodium chloride and possible traces N, normality of the standard ammonium
=

of alkali carbonates, which may have passed through thiocyanate solution,

the filter in the presence of the detergent. Find out the N,= normality of the standard silver nitrate
percentage of sodium carbonate and sodium chloride solution,
in the extract as prescribed in D-3.4.1 and D-3.4.2 M, = mass in g of the total extract (see D-3.3),

respectively. and
M, = mass in g of the extract taken for analysis
D-3.4.1 Determination of Alkali Carbonates
in D-3.4.1.
Weigh accurately about 1gofthe extract. Dissolve it D-3.5 Weigh accurately about 1 g of the extract.
in cold water, add a few drops of methyl orange Dissolve in water and make up to 500 ml. Follow the
indicator and titrate with standard sulphuric acid to titration procedure given in C-4.1 taking 10 ml of the
methyl orange end point. solution for titration.
D-3.4.1.1 Calculation
D-4 CALCULATION
Mass in g of sodium carbonate = 0.053 PN, x M
M2 Molecular mass of sodium (100 M - M2)x M
where salt ofsulphonic acid
5xVx Ti
=volume in ml of standard sulphuric acid where
solution used,
M,= percent by mass of sodium carbonate
of the standard sulphuric acid
N normality (see D-3.4.1)
solution, M, = percent by mass of sodium chloride
M, = mass in g of the total extract (see D-3.3),
(see D-3.4.2),
and M = mass in g of the extract taken,
M, = mass in g of the extract taken for analysis.
V = volume in ml of benzethonium chloride
D-3.4.1.2 Reserve the solution for the estimation of solution added, and
chlorides. T= molarity of benzethonium chloride
D-3.4.2 Determination of Chlorides solution.

To the solution remaining after the estimation ofalkali

IS 4956:2002 e
ANNEX E
[Table 1, St No. (ii)]
DETERMINATION OF CLEAR POINT TEMPERATURE

E-I GENERAL E-2.5 Thermometer - Range -10°C to 100°C.

E-1.1 This method is not applicable to materials E-2.6 Cooling Mixture - Iso-propyl alcohol or
showing reverse solubility temperature effect. ethanol to which solid carbon dioxide or ice-salt
mixture is added as required.
E-1.2 The clear point is defined as the temperature at
which the clarification occurs under the conditions of E-3 PROCEDURE
the test.
E-3.1 Place 25 ml ofthe liquid product itself in one of
E-2 APPARATUS the tubes and cool it whilst carefully stirring to avoid
incorporation of air bubbles, until solid material
E-2.1 Beaker-2-litre capacity to serve as a water
bath. separates, and the material under test becomes solid
and opaque.
E-2.2 Wide-Mouthed Bottle -450-ml capacity,
E-3.2 If no solid material separates after cooling up
height 190 mm and inside diameter of neck 38 mm.
to 0°C, the test shall be discontinued and the sample
E-2.3 Test Tube- 10 mm in length and 25 mm in shall be taken as passing the requirement of the test.
diameter.
E-3.3 Ater solid separation has taken place, heat the
E-2.4 Stirrer Made of stainless steel or glass with bath gradually whilst stirring, until the solution
onc end bent in the form of a loop of 19 mm outside becomes clear. Note the temperature at which this
diameter. ocurs and record it as the clear point of the solution.

ANNEX FF
[Table 1, Sl No. (iv)]
DETERMINATION OF pH

F-1 GENERAL dioxide, and shall be protected with soda lime or soda
asbestos while cooling and in storage. The pH of this
pH determination shall be made in an acid-free
water shall be between 6.2 and 7.2 at 30°C. The residue
atmosphere. on evaporation when heated at 105°C for one hour
F-2 APPARATUS shall not exceed 0.5 mg/1.

F-2.1 pH Meter F-3.2 Standard Buffer Solution

Any standard electrometric instrument, equipped with Any two suitable buffer solutions within the pH range
a low sodiunm error glass electrode. The instrument of 9 to 11 at 30°C for calibrating the pH meter.
shall be calibrated and standardized with standard
F-4 PROCEDURE
buffer solution (see F-3.2) before use.
Weigh 10 + 0.001 g of the material and transfer to a
F-2.2 Volumetric Flask- 1 000 ml capacity.
one litre volumetric flask. Partially fill the flask with
F-2.3 Beaker- 100 ml capacity. distilled water and agitate until the sample is
completely dissolved. Adjust the temperature of the
F-3 REAGENTS solution and the distilled water to 30 +0.5°C, and fill
F-3.1 Distilled Water to the calibration mark with distilled water. Stopper
the flask, mix thoroughly, and aliow the solution to
Distilled water shall be boiled thoroughly or purged stand at a temperature of 30°C for two hours ior to
with carbon dioxide-free air to remove carbon dioxide, measuring the pH. Measure the pH of the solution
and shall be protected with soda lime or soda carbon using a glass electrode.

8
 IS 4956 : 2002

ANNEX G
[Table 1, SI No. (v)]
DETERMINATION OF MATTER INSOLUBLE IN WATER

G-1 PROCEDURE G-1.2 Change the receiver, extract the residue with
successive portions of distilled water at about 60°C,
G-1.1 Weigh accurately about 5 g ofthe material into
and wash the residue several times to remove all the
a beaker and digest with 50 ml of ethyl alcohol by
water solubles. Dry the sintered glass funnel with the
heating on a steam-bath for about 2 minutes. Stir and
residue in an air-oven at a temperature of 105 + 2°C
break up any hard lump with a glass rod flattened at
until constant mass is obtained.
one end. Allow the solid matter to settle and decant
the hot alcoholic solution through a sintered glass filter G-1.3 Calculation
funnel fitted to a Buchner flask to which suction is
applied. Repeat the alcoholic digestion in a similar Matter insoluble in water, percent by mass= 100
manner with 5 further consecutive 30 ml portions of M
boiling ethyl alcohol. Filter each extract in turn
Where
through the same sintered glass funnel and, finally,
wash the residue several times with hot ethyl alcohol m = mass in g of the matter insoluble in water,

to remove all the alcohol solubles. and

M mass in g of the material taken for the test.

ANNEX HH
(Clause 7.1)
SAMPLING PROCEDURE FOR SYNTHETIC DETERGENTS

H-1 GENERAL REQUIREMENTS H-1.1.6 The samples shall be stored in such a manner
that the temperature of the material does not vary
drawing, preparing, storing and
H-1.I In handling8 unduly from the normal temperature, and that they
samples, the following precautions shall be observed. are protected from light.
H-1.1.1 Samples shall be taken in a protected place,
not exposed to damp air, dust or soot. H-2 SCALE OF SAMPLING

H-1.1.2 The sampling instruments shall be clean and H-2.1 Lot

dry when used. In a single consignment, all the packages containing

material of the same type, and drawn from the same
H-1.1.3 The samples, the material being sampled, the
sampling instruments and the containers for samples batch of manufacture, shall constitute a lot. If the
shall be protected from adventitious contamination. consignment consists of packages containing
detergents of different types then the packages
H-1.1.4 The samples shall be placed in clean and dry containing detergents of the same type and batch of
glass containers. The sample containers shall be of manufacture shall be grouped together, and each such
such a size that they are almost completely filled by group shall constitute a separate lot.
the sample.
H-2.2 For ascertaining the conformity of the lot to
H-1.1.5 Each container shall be sealed air-tight after the requirements prescribed in this standard, tests shal
filling, and marked with full details of sampling, date be carried out on each lot separately. The number (n)
of sampling, batch or code number, name of ofthe packages to be selected for drawing the samples
manufacturer, and other important particulars of the shall depend upon the size () of the lot and shall be
consignment. in accordance with Table 2.

9
 IS 4956 2002

Table 2 Scale of Sampling H-3.2.2 The remaining portion of the material in each
one of the gross samples shall be divided into three
(Clause H-2.2)
equal parts, each forming an individual sample. One
No of Packages No. of Packages set of individual samples representing the n selected
in the Lot to be Selected packages shall be for the purchaser, another for the
(N) () supplier, and the third for the referee.
() (2) H-3.2.3 Allthe composite and individual samples shall
4 to 15 3 be transferred to separate containers. These containers
16 to 40 shall then be sealed air-tight with stoppers, and
41 to 65 5
labelled with full particulars of identification given
66to 110
in H-1.1.5.
111 and above 10
H-3.3 Referee Samples
NOTE-When the size ofthe lot is 3 packages or less, the number
ofcontainers to be sclccted and the criteria for judging the con- H-3.3.1 The referee samples shall consist of a
formity of the lot to the specification shall be as agreed to between
the purchaser and the supplier. composite sample and a set of n individual samples.
All the containers shall bear the seals of both the
H-2.3 The packages shall be selected at random. In purchaser and the supplier, and shall be kept at a place
order to ensure the randomness of selection, a random agreed to between the two parties.
number table shall be used. For guidance and use of
H-3.3.2 Referee samples shall be used in cases of any
random number tables, IS 4905 may be used.
dispute between the purchaser and the supplier.
In the absence ofa random number table, the following
procedure may be adopted: H-4 NUMBER OF TESTS

'Starting from any package in the lot, count them in H-4.1 Tests for the determination ofcharacteristics of
one order as 1, 2, 3 up to r and so on where r is the active ingredient shall be performed on each of the
integral part of N/n (N being the lot size and n the individual samples .
number of packages to be selected). Every th package H-4.2 Tests for determination of the remaining
thus counted shall be withdrawn to given the required characteristics specified in Table 1 shall be conducted
sample size. on the composite sample.
H-3 PREPARATION OF GROSS SAMPLES, H-5 CRITERIA FOR CONFORMITY
TEST SAMPLES AND REFEREE SAMPLES
H-5.1 For ndividual Samples
H-3.1 Gross Samples
For the characteristics which has been determined on
H-3.1.1 From each one of the packages seiected as the individual samples, the mean (X) and the range
inH-2, draw at random one or more containers so (R) of the test results shall be calculated as follows:
chosen shall be nearly thrice the quantity required for
purposes of test as indicated in H-4. Mean (X) = nC Sum of testresults
Number of test results
H-3.1.1.1 The material from the containers selected
Range (R) = the difference between the maximum
as in H-3.1.! shall be disintegrated, if necessary, and
mixed thoroughly to give the gross sample for the and the minimum value of the test
package. results.
a) The value of the expression (X - KR) shall
H-3.2 Test Samples
be calculated from the relevant test results
H-3.2.1 Segregate carefully the gross samples. From see also H-5.1 (b)]. If the value so obtained
each gross sample, take a small but equal quantity of is greater than or equal to minimum limit,
material and mix it, thoroughly into a composite the lot shall be declared as conforming to the
sample which should be of a size sufficient to carry requirement for that characteristic.
out triplicate testing for all the characteristics
specified b) The value of the factor K referred to
under H-4. The composite samples representing each in H-5.1 (a) shall be chosen in accordance
type of synthetic detergent shall be divided into three with Table 3, depending upon the acceptable
equalparts one for the purchaser, another for the quality level, that is the percentage of non-
supplier, and the third for the referee. conforming packages that may be tolerated
reasonably.

10
 IS 4956 : 2002

Table 3 Value of '** for Achleving H-5.2 For Composite Sample

Different Quality Levels
For declaring the conformity of the lot to the
IClause H-5. 1(b)]
requirements of all the remaining characteristies
Acceptable Quality Level Value of determincd on the composite sample, the test results
for each of the characteristics shall satisfy the relevant
() (2) requirement given in Table 1 of this standard.
Not morc than 3.0 percent defectives 0.4
Not more than 1 S percent defectives 0.5
Not more than 0.5 perccnt defcctives 06

11
 IS 4956: 2002

ANNEXJ

(Foreword)
COMMITTEE COMPOSITION
Soaps and other Surface Active Agents Sectional Committee, CHD 25

Organization Representatve(s)

Drugs Controller General of India, New Delhi DR P.DAsGuPTA (Chairman)

SHRI B. R. WADHAWAN (Alternate)
Association for Consumer Action on Safcty & Hcalth (ACASH), Mumbai
SHRIYoGESHKaMDAR
SHRI N. G. WAGLE (Alternate)
Central Board of Excise & Customs, Ministry of Finance, New Delhi CHIEF CHEMIST
DEPUTY CHEF CHEMIST (Alternate)
Central Pollution Control Board, Delhi DR S. K. GHOSH
Consumer Guidance Society of India (Rcgd), Mumbai SHRI N. G. WAGLE
SHRIMATI R. TALWAI (A lternate)
Consumer Education and Research Centre, Ahmedabad DR C. J. SHsHOO
SHRI SANTOSH YELLORE (4lternate)
Department of Industrial Development, Ministry ofIndustry, New Delhi SHRI SHAISHKUMAR
SHRIB. B. SHARMA (Alternate)
Development Commissioner (Small Scale lIndustries), New Delhi SHRI J.S. REKHI
Directorate General ofSupplies and Disposals (Inspection Wing), New Delhi SHRIP. JAYAKUMARAN
SHRI M. A. KHAN (Alternate)
Federation of Associations of Small Scale Soap & Detergent SHRI SANTOSH KUMAR
Manufacturers of India, Delhi SHRI R.C. Dosn (Alternate)
Godrej Soaps Limited, Mumbai SHRIA. RANGARAJAN
Gujarat Detergent Manufacturers Association, Ahmedabad SHRI S. A. PATEL
SHRI MAHENDRA VYAS (Alternate)
Hindustan Lever Limited, Mumbai DRA.N. BHAT
DRV.R. DANUKA (Alternate)
Indian Soaps and Toilctries Manufacturers Association, Mumbai SHRI V.P. MENON
Karnataka Soaps & Detergents Limited, Bangalore
DRK.B. PATIL
SHRI M.P. NaIK
(Alternate)
Khadi &Village Industries Commission, Mumbai SHRI A. A. WARSI
K.S. Krishnan Associates (P) Limited, New Delhi StRI. K. S. KRISHNAN
SHRI S. KRuSHNAN (4lternate)
Ministry of Defence (DGQA), Kanpur SHRI M. S. SuLTANA
SHRI S. S. SHUKLA (Alternate)
Mumbai Grahak Panchayat, Mumbai SHRI BHMRAo BAGALKOTE
SHRIMATI VASUDHA CHACHAD (Alternate)
Nand Kishore Khanna & Sons, Mumbai SHRI P.P. KHANNA
SHRI A. C. KHANNA (Alernate)
National Test House, Kolkata
SHRI A. KCHAKRAVORTY
SHRI P.K. CHAKRABORTY (Alternate)
Nima Limited, Ahmedabad SHRI K. K. PATEL
SHRI M. A. BHATT (4lternate)
Oil Technologists Association of India, Kanpur DRB.R.GAIKWAD
SHRI P.K.
Procter & Gamble Hygiene & Healthcare (India) Limited, Mumbai
TiWARE(4lternate)
DRARUN VIsttWANATH
SHRIMATI SHWETA PURANDRE (4lternate)
Reliance Industries Limited, Mumbai
REPRESENTATIVE
Research, Design and Standards Organization (Ministry of Railways), Lucknow SHRI A. K. CHOUDHURI

(Continued onpage 13)

12
 IS 4956: 2002
(Contimed from poge 12)

Orgontcatio Repre sentative(s)

Tata Chemicals, Pithampur REPRESENTATIVE
The Non-Power Soap Manufacturers Association, Mumbai SHRI R.C. DoSHI
SHRI Y. R. Dosm (Alternate)
BIS Directorate General StRI LAINDER SINCGH, Director & Head (Chem)
Representing Director General (Ex-Oficio Member)

Member-Secretary
SHRIMAT CHTTRA GuPTA
Deputy Director (Chem), BIS

Non-Soapy Detergents Subcommittee, CHD 25:2

Nima Limited, Ahmedabad SHRIM. A. BHAT (Convener)
SHRI. K. K. PATEL (A lernate)
Central Board of Excise& Customs, Ministry of Finance, New Delhi CHEF CHEMST
DEuTY CHTEF CHEMST (Alernate)
Consumer Education and Rescarch Ccntre, Ahmedabad Stmu S. YreuoRE
SRDAATI FALaUM MAzUMDAR (Alternate)
Consumer Guidance Socicty of Ihdia (Regd), Mumbai SHRuN.G. WAGLE
SHRI A. R. SHENOY (Alternate)
Department of Industrial Development, Ministry of Industry, New Delhi Str SHAISH KUMAR
StRu B. B. SHARMA (Alternate)
Federation of Associations of Small Scale Soap & Detergent SHRI R.C. DosHH
Manufacturers of India, Delhi SHRI SANTOSHKUMAR{Alternate)
Fena (P) Limited, New Delhi SHRI DALIP JouY
SHRI PRADEEP JoLLY (Alternate)
Godrej Soaps Limited, Mumbai StIRIA. RANGARAJAN
Hindustan Lever lLimited, Mumbai DRA.N. BHAT
DR V. R. DHANUKA (Alernate)
Khadi & Village Industrics Commission, Mumbai CHIEF ExECUumVE OFFICER
SHRI A. A. WARSI (Allernate)
Kopsons Surfactants (P) Limited, Mumbai SHRI S. S. KoPPIKAR
SHRIMATI GITA S. KoPPKAR (Alternate)
Officc of Devclopment Commissioner (Small Scale Industries), New Delhi SHRI S. R. S1NGH
SHRI R. MUKHOPADHYAY (Alternate)
Office of the Textile Commissioner, Mumbai SHRI M.R. MA
SHRI R.A. LAL (Alternate)
Oil Technologists Association of India, Kanpur REPRESENTATVE
Tata Chemicals, Pithampur REPRESENTATVE

13
 C
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developed from Doc No. CHD 25 (910).

Amendments Issued Since Publication

Amend No. Date of lIssue Text Affected

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