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Hkkjrh; ekud IS 286 : 2018

Indian Standard

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( rhljk iqujh{k.k )

Methods of Sampling and

Test for Soaps
( Third Revision )

ICS 71.100.40

© BIS 2018

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BUREAU OF INDIAN STANDARDS
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MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI-110002
www.bis.org.in www.standardsbis.in

September 2018 Price Group 11

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Soaps and Other Surface Active Agents Sectional Committee, CHD 25

FOREWORD
This Indian Standard ( Third 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.
This standard was first published in 1951 and subsequently revised in 1966 and 1978. During 1978 revision the
procedure for determination of matter insoluble in alcohol has been elaborated. Provision has been made for
calculation of total fatty matter while determining combined alkali and total anhydrous soap. Similarly provision
has also been made for calculation of neutral sodium silicate content while determining alkaline silicates. For
determination of glycerol content in soaps a concentration of 6 percent of sodium periodate in place of 2 percent
hitherto prescribed has been included which improves the repeatability of the method. An alternate method for
estimation of rosin acids without the use of β-naphthalene sulphonic acid has been added. An additional method
for determination of free carbonated alkali has been included. Amendment No. 1 has been incorporated in this
revision.
This standard is intended to facilitate the introduction of uniform methods of sampling and analysis of soaps. It is
a necessary adjunct to the Indian Standards on individual materials.
During this revision, Amendment No.1, 2, 3, 4 and 5 have been incorporated and also the referred standards have
been updated.
The Committee responsible for the preparation of the standard is given at Annex C.
The methods given in this standard substantially correspond to the following standards of the International
Organization for Standardization (ISO) :
ISO 456 : 1973 Analysis of soap. Determination of free caustic alkali.
ISO 457 : 1976 Analysis of soap. Determination of chlorides.
ISO 672 : 1978 Analysis of soaps. Determination of moisture and volatile matter.
ISO 673 : 1981 Analysis of soaps. Determination of content of ethanol — insoluble matter.
ISO 684 : 1974 Analysis of soaps. Determination of total free alkali.
ISO 685 : 1975 Analysis of soaps. Determination of total alkali.
ISO 1066 : 1975 Analysis of soaps. Determination of glycerol content — Titrimetric method
ISO 1067 : 1974 Analysis of soaps. Determination of unsaponifiable and unsaponified matter.
In reporting the result of a test or analysis made in accordance with this standard, if the final value, observed or
calculated, is to be rounded off, it shall be done in accordance with IS 2 : 1960 ‘Rules for rounding off numerical
values (revised)’. The number of significant places retained in the rounded off value should be the same as that of
the specified value in this standard.
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IS 286 : 2018

Indian Standard
METHODS OF SAMPLING AND
TEST FOR SOAPS
( Third Revision )
1 SCOPE although they actually solidify over a range of
temperature.
1.1 This standard prescribes methods of sampling and
test for soaps. 3.1.8 Total Anhydrous Soap — It represents the fatty
acids existing in soap in combination with alkali.
1.2 Should there be any discrepancy between the
requirements of this standard and the one for an NOTE — Sometimes total anhydrous soap is determined by
individual material specification, the latter shall prevail. deducting the value for moisture and volatile matter from the
mass of soap. This is not a precise method even for genuine
2 REFERENCES soaps and is certainly not applicable to built and filled soaps.

The standards listed in Annex B contains provisions 3.1.9 Total Fatty Matter — It includes substances
which, through reference in this text, constitute soluble in ether under the conditions of the test, such
provisions of this standard. At the time of publication, as fatty and rosin acids present in the combined state
the editions indicated were valid. All standards are as well as unsaponified and unsaponifiable matter.
subject to revision, and parties to agreements based on 3.1.10 Unsaponifiable Matter — It includes substances,
this standard are encouraged to investigate the such as the higher aliphatic alcohols, sterols, colouring
possibility of applying the most recent editions of the materials and hydrocarbons, which may be present in
standards given in Annex B. soap and which are not capable of being saponified by
caustic alkali but are soluble in ordinary fat solvents.
3 TERMINOLOGY
3.1.11 Unsaponified Matter — It is the neutral fat
3.1 For the purpose of this standard, the following (unsaponified, neutral glycerides) present in soap.
definitions, in addition to those given in IS 7597 shall apply.
4 SAMPLING
3.1.1 Combined Alkali — It is the alkali present in soap
in combination with saponifiablc matter. 4.1 General Precautions
3.1.2 Free Fatty Acid — It is the free (uncombined) In drawing, preparing, storing and handling samples, the
fatty acid present in soap and is expressed as percent following precautions and directions shall be observed.
by mass as oleic acid. 4.1.1 Samples shall be taken in a protected place, not
3.1.3 Free Caustic Alkali — It is the free (uncombined) exposed to damp air, dust or soot.
caustic alkali present in soap. 4.1.2 The sampling instruments shall be clean and dry
when used.
3.1.4 Iodine Value (Wijs) — It is the number of grams
of iodine absorbed per 100 grams of the mixed fatty 4.1.3 The samples, the material being sampled, the
and rosin acids obtained from soap. sampling instruments and the containers for samples
shall be protected from adventitious contamination.
3.1.5 Matter Insoluble in Alcohol — It comprises most
of the alkaline salts, such as talc, carbonates, borates, 4.1.4 The samples shall be placed in clean and dry glass
silicates and phosphates, as well as sulphates and starch, containers. The size of the sample containers shall be such
which are insoluble in alcohol under the conditions of that the latter are almost completely filled by the sample.
the test. 4.1.5 Each container shall be scaled air-tight after filling
3.1.6 Moisture and Volatile Matter — It includes and suitably marked.
moisture and any other material contained in soap 4.1.6 The samples shall be stored in such a manner
volatile under the conditions of the test. that the temperature of the material does not vary unduly
3.1.7 Titre — It is the highest temperature reached when from the ambient temperature, and that they are
the mixed fatty and rosin acids obtained from soap are protected from light.
crystallized under the conditions of the test. 4.2 Scale of Sampling
3.1.7.1 Titre is generally taken to represent the 4.2.1 Lot
solidification point of the mixed fatty and rosin acids,
In a single consignment, all the packages containing
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IS 286 : 2018

soap of the same type, grade and form, and drawn from 4.3.1.3 Liquid soaps
the same batch of manufacture, shall continue a lot. If From each one of the packages selected as in 4.2.2 draw
the consignment consists of packages containing soaps at random one or more containers. The material in the
of different types, grades and forms, packages containers so chosen shall be nearly thrice the quantity
containing soaps of the same type, grade, form and required for the purpose of test as indicated in 4.4. This
batch of manufacture shall be grouped together and material shall then be mixed thoroughly to give the gross
each such group shall constitute a separate lot. sample for the package.
4.2.2 For ascertaining the conformity of the lot to the 4.3.2 Test Samples
requirements prescribed in the relevant standard, tests
4.3.2.1 Segregate carefully the gross samples (see 4.3.1)
shall be carried out for each lot separately. The number
of bars, tablets, flakes, chips, powders and liquid soaps.
n of packages to be selected for drawing the samples From the gross samples representing each form of soap,
shall depend upon the size N of the lot, and shall be in take a small but equal quantity of material and mix it
accordance with Table 1. thoroughly with a composite sample which should be
4.2.3 The packages shall be selected at random and, to of a size sufficient to carry out triplicate testing for all
ensure randomness of selection, random number tables the characteristics specified under 4.4.2. The composite
shall be used. In case such tables are not available, the samples representing each form of soap shall be divided
following procedure may be adopted: into three equal parts — one for the purchaser, another
‘Starting from any package, count all the packages for the supplier and the third for the referee.
in one order as 1, 2, 3, etc, up to r and so on, where 4.3.2.2 The remaining portion of the material in each
r is the integral part of N/n ( N being the lot size and one of the gross samples shall be divided into three
n the number of packages to be selected ). Every rth equal parts, each forming an individual sample. One
package thus counted shall be withdrawn to give a set of individual samples representing the n-packages
sample for the purpose of test.’ selected shall be for the purchaser, another for the
supplier and the third for the referee.
4.3 Preparation of Test Samples
4.3.2.3 All the individual and composite samples shall
4.3.1 Gross Samples
be transferred to separate containers. These containers
4.3.1.1 Bars and tablets shall then be sealed air-tight with stoppers and labelled
From each one of the packages selected as in 4.2.2 draw with full identification particulars.
at random a number of bars or tablets from different 4.3.3 Referee Samples
parts of the package. The material so drawn from a
The referee sample, consisting of a composite sample
package shall be nearly equal to thrice the quantity
and a set of n-individual samples, shall bear the seals
required for the purpose of test as indicated in 4.4. The
of both the purchaser and the supplier and shall be kept
bars or tablets selected shall be run through a suitable
at a place agreed to between the two. This shall be used
chopper. The disintegrated material thus obtained from
in case of any dispute.
the chopper shall be mixed thoroughly to give the gross
sample for the package. 4.4 Number of Tests
4.3.1.2 Flakes, chips and powders 4.4.1 Tests for the determination of important
From each one of the packages selected as in 4.2.2 draw characteristics, as specified in the relevant material
at random one or more cartons. The material in the carton specification, shall be conducted on each of the
so chosen shall be nearly thrice the quantity required for individual samples separately.
the purpose of test as indicated in 4.4. This material shall 4.4.2 Tests for the determination of all the remaining
then be disintegrated, if necessary, and mixed thoroughly characteristics in the material specification shall be
to give the gross sample for the package. conducted on the composite sample.
Table 1 Scale of Sampling
(Clause 4.2.2)
No. of Packages in the Lot No. of Packages to be Selected
N n
(1) (2)
4 to 15 3
16 to 40 4
41 to 65 5
66 to 110 7
111 and above 10
NOTE — When the size of the lot is 3 packages or less, the number of packages to be selected and the criteria for judging the
conformity of the lot to the specification shall be as agreed to between the purchaser and the supplier.

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IS 286 : 2018

4.5 Criteria for Conformity 5 DETERMINATION OF MOISTURE AND

VOLATILE MATTER
4.5.1 For Individual Samples
5.1 General
For each of those characteristics which have been
determined on the individual samples, the mean ( x ) Two methods, namely, (a) the oven method, and (b)
and the range (R) of the test results shall be calculated the distillation method, are employed. The oven method
as follows: gives the moisture and volatile matter content
the sum of test results determined by drying the material in an air-oven at a
Mean ( x ) = specified temperature. The distillation method gives
number of test results
only the moisture content determined by measuring the
Range (R) = The difference between the maximum and volume of water distilled over when boiled under reflux
the minimum value of the test results. with xylene or toluene.
a) If the specification limit for the characteristic is 5.1.1 Applicability
given as a minimum, the value of the expression The oven method is generally applicable to all soaps,
( x – KR) shall be calculated from the relevant though, for the following classes of soaps, the
test results [ see also 4.5.1(d) ]. If the value so distillation methodis to be preferred:
obtained is greater than or equal to the minimum
a) Soaps containing appreciable amounts of
limit, the lot shall be declared as conforming to
sodium silicate;
the requirement of that characteristic.
b) Soaps obtained from linseed oil and other
b) If the specification limit for the characteristic is oxidizing oils which absorb oxygen and are
given as a maximum, the value of the expression likely to gain in mass towards the end of the test
( x + KR) shall be calculated from the relevant if the oven method is used. Nevertheless, if the
test results [ see also 4.5.1(d) ]. If the value so oven method is used, the drying should be carried
obtained is less than or equal to the maximum out either in an inert atmosphere or in vacuum;
limit, the lot shall be declared as conforming to c) Soaps containing an appreciable amount of
the requirement of that characteristic. glycerol, especially those manufactured by the
c) If the characteristic has two-sided cold process or by the semi-boiled process,
specification limit, the values of the which usually give high results by the oven
expressions ( x – KR ) and ( x + KR )shall be method; and
calculated from the relevant test results [ see d) Soaps containing sodium hydrogen carbonate,
also 4.5.1(d) ]. If the values so obtained lie perfume, ammonia, alcohol, carbolic acid and
between the two specification limits, the lot persalts.
shall be declared as conforming to the 5.1.2 In case of dispute, moisture content shall be
requirement of that characteristic. determined by the distillation method.
d) The value of the factor K referred to in 4.5.1
[(a) to (c) ] shall be chosen in accordance with 5.2 Oven Method
Table 2, depending upon the acceptable quality 5.2.1 Procedure
level ( that is, the percentage of non-conforming Accurately weigh 5.00 ± 0.01 g of the material in a
package that could reasonably be tolerated). petri dish, about 6 to 8 cm in diameter and about 2 to 4
Table 2 Values of K for Achieving Different cm in depth, and dry to constant mass in an air-oven at
Acceptable Quality Levels a temperature of 105 ± 2°C. Cool in a desiccator and
[Clause 4.5.1(d)] weigh. Constant mass shall be considered to have been
attained when successive heating for 1 h period shows
Acceptable Quality Level Value of K a difference of not more than 0.1 percent in the net loss
Not more than 3 percent defectives 0.4 in mass.
Not more than 1.5 percent defectives 0.5
Not more than 0.5 percent defectives 0.6 5.2.2 Calculation
Moisture and volatile matter content, percent by mass
4.5.2 For Composite Sample
= 100
For declaring the conformity of the lot to the requirements
of all other characteristics determined on the composite where
sample, the test results for each of the characteristics shall m = loss in mass in g of the material after drying,
satisfy the relevant requirement given in the material and
specification. M = mass in g of the material taken for the test.

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IS 286 : 2018

5.3 Distillation Method front of the condenser when the lower water
5.3.1 Apparatus — The apparatus consists of a glass connection is to the left, the finish shall be
flask heated by suitable means and provided with a either smooth or fire-polished. When inserted
reflux condenser discharging into a trap and connected into the trap, the tip of the condenser shall be
to the flask. The connections between the trap and the 6 to 7 mm above the surface of the liquid in
condenser and the condenser and the flask should be the trap after distillation conditions have been
interchangeable ground-glass joints. The trap serves established. The nominal dimensions of the
to collect and measure the condensed water and to joint D are given below:
return the solvent to the flask. The assembly of the Nominal Dia of Nominal Dia of Nominal Length
apparatus is shown in Fig. 1, and the various Large End of Small End of of Ground Zone
components are described below: Ground Zone Ground Zone Measured
a) Flask — a 500 to 1 000-ml flask of the shape mm mm Axially
shown in Fig. 1, made of hard resistant glass, mm
well annealed and as free as possible from 18.8 16.2 26
striae and similar defects.
c) Receiver — also called the trap, made of hard
b) Condenser — a water-cooled reflux-type glass
resistant glass, well annealed and as free as
condenser of the design and dimensions shown
possible from striae and similar defects,
in Fig. 1A. The only mandatory dimensions
provided with ground-glass joints, with the
for the condenser are the external diameters
shape, dimensions and tolerances given in Fig.
of the inner tube and of the jacket, which shall
1B and 1C; consisting essentially of the upper
be 16 to 17 mm and 23 to 25 mm respectively.
chamber, together with the tube and the ground
The joints A and B should be neatly finished
joint leading to the flask, and the graduated
as shown in Fig. 1A, particularly the bore at
tube. The receivers shall be of two sizes,
B shall have the minimum disturbance. The
namely, 2 ml capacity and 10 ml capacity
shoulder above the cone of joint D shall be
(see Fig. 1B and 1C ). The mandatory
elongated as shown in Fig. 1A to avoid a sharp
dimensions and tolerances for the receivers
re-entrant shape which may restrict the free
shall be as given in Table 3.
flow of liquid down the inner wall. The cone
shall be extended beyond the length The shoulder of the upper chamber of the
appropriate to the joint D, and the lower end receiver immediately below the conical joint
ground inclined at an angle of approximately shall be finished square as shown in Fig. 1B
60 to the axis. The drainage tip shall be at the and 1C. The graduated portion of the receiver

F IG. 1 TYPICAL ASSEMBLY OF DEAN AND STARK APPARATUS

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IS 286 : 2018

All dimensions in millimetres.

FIG. 1A CONDENSER

shall be cylindrical throughout its length. The axis of the tube. The graduation marks shall
bottom of the graduated tube of the 2-ml be confined to the cylindrical portion of the
receiver shall be sealed, the end of the tube tube and there shall be no evident
being approximately hemispherical in shape. irregularity in their spacing. In these
The graduated scales on the receivers shall be receivers the numbered graduation marks
numbered and subdivided as shown in Fig. 1B shall be carried completely round the tube,
and 1C. The graduation marks shall be fine, the shortest ones half-way round it and those
cleanly etched permanent lines of uniform of intermediate length approximately two-
thickness lying in plane at right angles to the thirds of the way round the tube, projecting

All dimensions in millimetres.

FIG. 1B 2-ml RECEIVER

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IS 286 : 2018

All dimensions in millimetres.

FIG. 1C 10-ml RECEIVER

equally at each end beyond the shortest fully shut-off position, shall not exceed the
graduation marks. figure given in Table 3.
The capacity corresponding to any graduation Each receiver shall have permanently and
mark is defined as the volume of water at legibly marked on it:
27°C, expressed in millilitres, required to fill
the graduated portion to that mark at 27°C, 1) the abbreviation ‘ml’ ,
the axis of the graduated portion being vertical 2) the inscription ‘27°C’ to indicate that the
and the lowest point of the water meniscus receiver is graduated for content at 27°C,
being set on the graduation mark. In the case and
of the 10-ml receiver, the volume of the bore 3) the identification number on the key.
of the stopcock key and that of the jet below
the stopcock shall not be included as part of d) Heat Source — The source of heat may be
the measured volume. either an oil-bath or an electric heater provided
The error at any point on the receiver scale, with a sliding rheostat or other means of heat
as also the difference between the errors at control. The temperature of oil in the bath
any two points on the scale shall not exceed should not be very much higher than the
the figures given for the receivers in Table 3. boiling point of xylene or toluene, whichever
solvent is used.
For the 10-ml receiver, the stopcock shall be
of the 2-mm oblique bore having the general e) Copper Wire — long enough to extend through
design shown in Fig. 1B and 1C. The rate of the condenser, with one end twisted into a
leakage, tested with the stopcock free from spiral. The diameter of the spiral should be
grease, the barrel and the key wetted with such that it fits snugly within the graduated
water, the receiver filled initially with water portion of the receiver and yet may be moved
to the top of the scale and the key in either up and down.

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IS 286 : 2018

Table 3 Mandatory Dimensions and Tolerances for Receiver

(Clause 5.3.1)
Sl Characteristic Receiver
No.
2-ml 10-ml
(1) (2) (3) (4)
i) Volume, equivalent to smallest subdivision 0.05 ml 0.1 ml
ii) Scale length 95 ± 10 mm 110 ± 10 mm
iii) Length of cylindrical tube above upper graduation mark 10 to 15 mm 10 to 30 mm
iv) Tolerance on capacity ± 0.02 ml ± 0.06 ml
v) Maximum permissible leakage rate of stopcock – 0.004 ml/min

5.3.2 Reagents copper wire up and down in the condenser and receiver
occasionally, thus causing the water to settle at the bottom
5.3.2.1 Potassium dichromate-sulphuric acid cleaning
of the receiver. Reflux until water-level in the receiver
solution
remains unchanged for 30 min; then shutoff the source
5.3.2.2 Xylene or toluene — Saturate the xylene or of heat.
toluene by shaking with a small quantity of water and Flush the condenser with either xylene or toluene, as
distil. Use the distillate for the determination of required, making use of the spiral copper wire to discharge
moisture. any moisture droplets. Immerse the receiver in water at
5.3.3 Procedure — Clean the entire apparatus with about 30°C for at least 15 minutes or until the xylene or
potassium dichromate-sulphuric acid cleaning solution toluene layer is clear; then read the volume of water.
to minimize the adherence of water droplets to the sides 5.3.4 Calculation
of the condenser and the receiver. Rinse thoroughly 100VD
with water and dry completely before use. The quantity Moisture content, percent by mass =
M
of material taken for the test is determined by the where
amount of moisture present ( m/m ), as indicated below: V = volume in ml of water,
D = relative density of water at the temperature
Moisture Range Quantity of Material at which the volume of water is read, and
m/m (Approximately) M = mass in g of the material taken for the test.
Less than 1 percent 50 g
6 DETERMINATION OF MATTER INSOLUBLE
1 to 5 percent 25 g
IN ALCOHOL
Moisture in excess of 5 Proportionately smaller
percent quantity 6.0 General
This method may be used for the approximate
Place the specified quantity of material, accurately determination of these constituents. As these salts are
weighed, in the distillation flask, add 200 ml of xylene not completely insoluble in alcohol, separate portions
or toluene and swirl to mix. Add a few porcelain pieces of soap should be used for accurate determination,
to regulate boiling. Assemble the apparatus and fill the employing specific methods.
receiver with the solvent by pouring it through the
condenser until it begins to overflow into the distillation 6.0.1 Method
flask. Insert a loose cotton plug in the top of the condenser It consists in digesting the material in alcohol and
to prevent condensation of atmospheric moisture within filtering off the residue, which is dried and weighed.
the tube. To ensure that refluxing is under control, wrap
6.1 Reagents
the flask and the tube leading to the receiver with asbestos
cloth. Heat the flask so that the distillation rate is about 6.1.1 Phenolphthalein Indicator — Dissolve 1 g in
100 drops per minute. When the greater part of the water 100 ml of 95 percent rectified spirit.
has distilled over, increase the distillation rate to about 6.1.2 Ethyl Alcohol — conforming to IS 321, or rectified
200 drops per minute and continue until no more water spirit conforming to IS 323, freshly boiled, and neutral
is collected. Purge the reflux condenser occasionally to phenolphthalein.
during the distillation with 5-ml portions of xylene or
toluene to wash down any moisture adhering to the walls 6.2 Procedure
of condenser. The water in the receiver may be made to 6.2.1 Weigh accurately 2 to 10 g of the sample and reflux
separate from xylene or toluene by moving the spiral with 200 ml of freshly boiled ethyl alcohol fitting with a

7
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IS 286 : 2018

suitable reflux condenser on a steam bath until the soap sample of soap, and omitting the addition of barium
is dissolved. Filter into a filter flask through a tared, dried chloride solution and titrate the alcoholic solution with
and counterpoised filter paper or through a tared and standard sodium hydroxide solution. This procedure is
dried Gooch or sintered glass crucible with suction, applicable to pure soaps only.
protecting the solution from carbon dioxide and other
7.4 Calculation
acid fumes during the operation by covering with a watch
glass. The filter paper and Gooch crucible shall be Calculate the percentage of free caustic alkali (as
prepared as per method given under 6.2.2. Wash it several NaOH, KOH and K2O) and free fatty acid (as oleic
times with ethyl alcohol at approximately 60°C till the acid) as follows:
filtrate on dilution with distilled water shows neutrality a) Free caustic alkali (as NaOH), percent by mass
to phenolphthalein, to remove all the alcohol solubles 4VN
=
(preserve the filtrate for 7.2). Dry the filter paper or the M
crucible with the residue at 100 ± 2°C for 3 h and cool. b) Free caustic alkali (KOH), percent by
Weigh the total matter insoluble in alcohol. 5.61VN
mass =
M
6.2.2 Place filter paper in a weighing bottle and dry in an c) Free caustic alkali (as K 2O), percent by
air oven at 105 ± 2°C with cover removed. Remove from 4.71VN
the oven, replace cover, cool to room temperature in a mass =
M
desiccator and weigh. Prepare the Gooch crucible with a where
pad of asbestos fibre. Wash the pad with water, alcohol V = volume in ml of standard sulphuric acid
and ether and then dry to constant mass at 105 ± 2°C, or hydrochloric acid used,
cool to room temperature in a desiccator and weigh. N = normality of standard sulphuric acid or
hydrochloric acid, and
6.3 Calculation
M = mass in g of the material taken for the
m test.
Matter insoluble in alcohol, percent by mass = 100
M d) Free fatty acid, as oleic acid (C18H34O 2),
where 28.5V1 N1
percent by mass =
M
m = mass in g of matter insoluble in alcohol, and where
M = mass in g of the material taken for the test.
V1 = volume in ml of standard sodium
7 DETERMINATION OF FREE CAUSTIC hydroxide solution used,
ALKALI OR FREE FATTY ACID N1 = normality of standard sodium hydroxide
7.0 General solution, and
M = mass in g of the material taken for the test.
The method consists in dissolving the soap in alcohol 8 DETERMINATION OF MATTER INSOLUBLE
and titrating the solution with sulphuric acid or alcoholic IN WATER
sodium hydroxide solution, as the case may be.
8.0 General
7.1 Reagents To determine the matter insoluble in water, the sample
7.1.1 Phenolphthalein Indicator — as in 6.1.1. is extracted with alcohol, filtered and the residue
extracted with hot water.
7.1.2 Ethyl Alcohol — as in 6.1.2.
8.1 Procedure
7.1.3 Standard Sulphuric Acid or Standard
Starting with a fresh sample of soap, proceed as
Hydrochloric Acid — approximately 0.1 N.
described in 6.2, but do not dry or weigh the matter
7.1.4 Standard Sodium Hydroxide Solution — insoluble in alcohol. After filtering and washing the
approximately 0.1 N. residue thoroughly with hot ethyl alcohol, change the
receiver, extract the residue with successive portions
7.1.5 Barium Chloride Solution — 10 percent (m/v).
of water at about 60°C and wash the residue thoroughly
7.2 Procedure for Free Caustic Alkali on the filter paper or in the crucible. Reserve the water
solution for the determination of total alkalinity under
7.2.1 Take the filtrate preserved in 6.2.1. Heat it to boil. 9.2. Dry the filter and the residue at 100 ± 2°C for 3 h
Add about 0.5 ml of phenolphthale in indicator and and cool. Weigh the matter insoluble in water.
titrate with standard sulphuric or hydrochloric acid.
8.2 Calculation
7.3 Procedure for Free Fatty Acid m
Proceed as prescribed under 7.2.1 starting with a fresh Matter insoluble in water, percent by mass = 100
M
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where 10.1.2 Methyl Orange Indicator — Dissolve 0.1 g in

100 ml of water.
m = mass in g of matter insoluble in water, and
10.1.3 Sodium Chloride Solution — saturated.
M = mass in g of the material taken for the test.
10.1.4 Ethyl Ether — See IS 336.
9 DETERMINATION OF TOTAL ALKALINITY
10.1.5 Ethyl Alcohol — as in 6.1.2.
OF MATTER INSOLUBLE IN ALCOHOL
(ALKALINE SALTS) 10.1.6 Standard Sodium Hydroxide Solution —
approximately 0.5 N and carbonate-free.
9.0 General
10.1.7 Standard Hydrochloric Acid — approximately
The matter insoluble in alcohol in the soap is dissolved 0.5 N.
in water and titrated with standard acid using 10.1.8 Phenolphthalein Indicator — as in 6.1.1.
phenolphthalein’ as indicator. Total alkalinity of matter
insoluble in alcohol (alkaline salts) is expressed as 10.2 Procedure
NaOH. 10.2.1 Accurately weigh 5 to 10 g of the sample,
depending upon the anhydrous soap content, and
9.1 Reagents dissolve in 250-ml conical flask by warming in 100 ml
9.1.1 Standard Sulphuric Acid or Hydrochloric Acid — of water. When dissolution is complete, add dilute
approximately 0.5 N. sulphuric acid in slight excess ( as judged by methyl
orange indicator ), insert a small funnel into the neck of
9.1.2 Phenolphthalein Indicator — Dissolve 1 g in the flask, and heat the flask to a temperature not
100 ml of 95 percent of rectified spirit. exceeding 60°C until the fatty acids separate as a clear
9.2 Procedure layer. Add 50 ml of sodium chloride solution and cool.
Transfer quantitatively to a separating funnel, draw off
Titrate the water solution reserved under 8.1 with
the aqueous acid layer into a second separating funnel
standard sulphuric or hydrochloric acid, using
and shake it with three 50-ml portions of ethyl ether.
phenolphthalein indicator.
Dissolve the fatty acids in the ether used for washing
9.3 Calculation the aqueous liquid and extract with 10-ml portions of
water until the extracts are no longer acidic to methyl
Unless otherwise specified or agreed to between the
orange indicator. Mix the water portions used for
purchaser and the supplier, calculate the total alkalinity
washing and shake with 20 ml of ether. Wash this ether
(as NaOH) of matter insoluble in alcohol as follows:
until the wash water is neutral to methyl orange indicator.
Total alkalinity (as NaOH) of matter insoluble in 10.2.2 Mix the ether solutions (if necessary, filter
4VN previously washing the paper with ether) in a suitable,
alcohol, percent by mass =
M weighed vessel, evaporate on a boiling water-bath to a
where volume not less than 50 ml, add 100 ml of ethyl alcohol
and about 0.5 ml phenolphthalein indicator and titrate
V = volume in ml of standard sulphuric or
to exact neutrality with standard sodium hydroxide
hydrochloric acid, solution.
N = normality of standard sulphuric acid, and 10.2.3 Evaporate the alcohol, dry to constant mass in
M = mass in g of the material taken for the test an oven at 105 ± 2°C as in the determination of moisture
under 7. and volatile matter content under 5.1.1.
1 0 D E T E R M I N AT I O N O F C O M B I N E D 10.3 Calculation
ALKALI AND TOTAL ANHYDROUS SOAP 10.3.1 Ascertain the mass of soda soap and calculate
10.0 General as percentage on the mass of the material taken for the
test. This mass of the soda soap includes that of any
Fatty acids in the sample of soap are separated by mineral oil, unsaponifiables and neutral fat which, if
treatment with dilute sulphuric acid and are determined separately, should be deducted from the
quantitatively extracted by ether. The ether extract is results to obtain the true soap. If desired, calculate the
titrated in alcoholic medium with standard sodium combined sodium oxide (Na2O) and deduct from the
hydroxide solution for determining the combined alkali. mass of the soda soap to give the acid anhydrides. For
The total anhydrous soap is determined by evaporating 22
and drying the titrated solution. calculating total fatty matter subtract ( × combined
31
Na2O) from the mass of the soda soap.
10.1 Reagents
10.3.2 If the original soap is a potash soap, combined
10.1.1 Dilute Sulphuric Acid — 1 : 1 ( v/v ).
alkali may be calculated as potassium oxide (K2O).

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10.3.3 If the soap shows an excess of free acid, proper applied as given. In such cases, the filtrate obtained in
corrections should be made in calculating the combined the determination of total matter insoluble in alcohol
alkali in the original soap. A blank test should be made under 6.2.1 may be used. Evaporate the alcohol on a
on the sodium hydroxide or potassium hydroxide steam-bath, and proceed according to the instructions
solution for neutral salts and correction made, if given under 10.3.1 and 10.3.2.
necessary, by exactly neutralizing 20 ml of the standard
sodium hydroxide solution with standard hydrochloric 11 DETERMINATION OF CHLORIDES
acid, using phenolphthalein indicator. Evaporate the
11.0 General
neutral solution on a water-bath and dry to constant
mass at 105 ± 2°C. From the mass of the residue subtract This method determines the chlorides in the sample
the mass of sodium chloride (NaCl) calculated from and is applicable to all soaps and soap products,
the amount of hydrochloric acid used up. This including those containing synthetic detergents. From
difference will be due to neutral salts which should be an aqueous solution of soap, the fatty acids are
calculated per ml of the caustic solution. precipitated as insoluble calcium soaps by the addition
of calcium nitrate solution. This precipitate is washed
10.3.4 To obtain the value for total anhydrous soap, deduct
free of chlorides and the chlorides in the washings and
the neutral salt calculated from the volume in ml of sodium
filtrate estimated by titration with standard silver nitrate
hydroxide used for titration from the mass of the residue
solution, using potassium chromate as indicator.
obtained after titrating the fatty acids and drying.
10.3.5 Use the following formulae in making the 11.1 Reagents
calculations:
11.1.1 Calcium Nitrate Solution — neutral, chloride-
VNE
a) Combined alkali, percent by mass = free and containing 20 percent ( m/v ) of calcium nitrate
M crystals [ Ca ( NO3 )2, 4H2O ].
where
11.1.2 Methyl Orange Indicator — Dissolve 0.1 g in
V = volume in ml of standard sodium
100 ml of 95 percent rectified spirit.
hydroxide solution required for the
material; 11.1.3 Dilute Nitric Acid — approximately 1 N.
N = normality of standard sodium hydroxide 11.1.4 Potassium Chromate Indicator — Dissolve 5 g
solution; of potassium chromate ( K2CrO4 ) in 100 ml of water.
E = 4.00, 3.10 or 4.71, depending upon
11.1.5 Standard Silver Nitrate Solution —
whether the result is to be expressed as
approximately 0 1 N.
sodium hydroxide (NaOH), sodium
oxide (Na2O) or potassium oxide ( K2O) 11.1.6 Calcium Carbonate or Magnesium Carbonate
respectively; and
11.2 Procedure
M = mass in g of the material taken for the
test. 11.2.1 Weigh accurately about 10 g of the sample and
dissolve in hot water in a 250-ml tall form beaker, add
b) Total anhydrous soap, percent by mass =
20 ml of the calcium nitrate solution, mix thoroughly,
100 ( m − KV )
–U cool and filter into a one-mark 250-ml volumetric flask.
M Wash the filter free from chlorides using water allowing
where
the washing to run into the flask. Shake the flask and
m = mass in g of the soda soap;
the contents and dilute to the mark.
K = correction, grams of neutral salts per
millilitre of standard sodium hydroxide 11.2.2 Take 100 ml of the solution, neutralize to
solution; methyl orange indicator with dilute nitric acid, add
V = volume in ml of standard sodium pitch of calcium or magnesium carbonate and titrate
hydroxide solution; with silver nitrate solution, using potassium chromate
M = mass in g of the material taken for the solution as indicator. Carry out a blank determination
test; and using the same quantity of all reagents but except the
U = unsaponified and unsaponifiable matter sample.
present, percent by mass (see 12).
11.3 Calculation
10.4 For soaps containing a large amount of soluble
silicates and other builders, and soap products a) Chlorides (as NaCl), percent by mass
containing a high percentage of finely divided material 14.6 ( S − B ) N
=
insoluble in water, the procedure under 10.2 cannot be M

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b) Chlorides (as KCl), percent by mass and acidity, calculated as oleic acid, is subtracted from
18.65 ( S − B ) N the mass of the residue.
=
M
where 12.1 Reagents

S = volume in ml of standard silver nitrate 12.1.1 Sodium Bicarbonate — solid.

solution required for the material, 12.1.2 Ethyl Alcohol — conforming to IS 321,
B = volume in ml of standard silver nitrate 95 percent (by volume) or rectified spirit conforming
solution required for the blank, to IS 323, redistilled.
N = normality of standard silver nitrate
12.1.3 Ethyl Alcohol — or rectified spirit, redistilled
solution, and
and diluted with water to give 50 percent (v/v) solution.
M = mass in g of the material taken for the test.
12.1.4 Ethyl Alcohol — or rectified spirit, redistilled
12 DETERMINATION OF UNSAPONIFIED AND and Muted with water to give 10 percent ( v/v ) solution.
UNSAPONIFIABLE MATTER
12.1.5 Sodium Hydroxide Solution — approximately
12.0 General 0.1 N.
The soap sample is dissolved in 50 percent alcohol and 12.1.6 Standard Sodium Hydroxide Solution —
extracted with petroleum ether. The ether extract is approximately 0.02 N.
washed free from soap and the residue obtained after
evaporating the solvent is weighed. This will contain 12.1.7 Petroleum Ether — The solvent shall be of the
unsaponifiable and unsaponified matter. To make a pentane type, containing a minimum amount of
correction for any fatty acids which may have been isopentane, and isohexane. The nonvolatile evaporation
formed due to the hydrolysis of soap, the residue is residue shall be not more than 0.001 percent (m/v) and
dissolved in alcohol and titrated with standard alkali, the material shall comply with the following additional
requirements:

a) Distillation test Initial boiling point 35° to 38°C

Dry flask end point 52° to 60°C
Distilling under 54°C, Min 95 percent
Distilling under 40°C, Max 60 percent
b) Relative density at 15.5°/15.5°C 0.630 to 0.660
c) Colour Water white
d) Doctor test Sweet
e) Copper strip corrosion test Non-corrosive
f) Unsaturated compounds Only traces permitted
g) Residue in distilling flask Neutral to methyl orange
h) Blotter strip odour test Odourless within 12 minutes
j) Aromatic compounds No nitrobenzene odour
k) Saponification value, Min 1.0 mg of potassium hydroxide per 100 m
GHGDG'L

12.2 Procedure separating funnel, washing with about 50 mi of

50 percent ethyl alcohol followed by two 10-ml
12.2.1 Accurately weigh about 5 g of the sample, place
portions of petroleum ether. Add 50 ml of petroleum
it in a 250-ml conical flask or beaker containing
ether, shake vigorously for one minute and allow to
approximately 0.1 g of sodium bicarbonate and dissolve
settle until both the layers are clear. Draw off completely
in 100 ml of 50 percent ethyl alcohol. Warm and shake
the lower aqueous layer into another separating funnel
to effect solution, keeping the temperature under 60°C.
of 500 ml capacity.
Transfer any undissolved residue to a Gooch crucible
with an asbestos pad or to a funnel using an asbestos 12.2.2 Repeat the extraction at least six times, using
pad deposited on a perforated porcelain disc. Wash 50 ml of petroleum ether each time. Wash the combined
three times with hot 50 percent ethyl alcohol. Wash petroleum ether extracts, first with a mixture of 15 ml
with a small amount of petroleum ether to remove any of sodium hydroxide solution and 15 ml of 95 percent
traces of unsaponified and unsaponifiable matter. ethyl alcohol and then at least thrice with 25-ml portions
Transfer the entire filtrate and washings to a 500- ml of 10 percent ethyl alcohol, shaking vigorously each

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IS 286 : 2018

time, until the wash water does not show any pink colour is then dried and weighed.
to phenolphthalein. Transfer the petroleum ether 13.1 Reagents — Besides all the reagents listed
extracts to a beaker and evaporate the petroleum ether under 12.1, the following solution is required.
on a steam-bath with the help of a current of air.
13.1.1 Potassium Hydroxide Solution — 50 percent
12.2.3 Test the residue for solubility by treating with (m/v).
50 ml of petroleum ether at room temperature. Filter
the insoluble residue, if any, and collect the filtrate and 13.2 Procedure
washings into a tared flask. Evaporate and dry in the Accurately weigh 5 g of the sample and place in a 200-
same manner on a steam-bath and, finally, in an air- ml conical flask. Add 30 ml of 95 percent ethyl alcohol
oven at 100° to 10l°C for 30 minutes. Weigh and return and 5 ml of potassium hydroxide solution and boil for
to the oven, reweighing at 15-minutes intervals until one hour under a reflux condenser. Transfer to a
constant mass is reached. Take up the residue in 50 ml separating funnel and wash with 95 percent ethyl
of 95 percent ethyl alcohol neutralized to alcohol. Complete the transfer, first with warm and then
phenolphthalcin indicator and titrate to the same colour with cold water, until the total volume is about 80 ml.
as that of the original neutral alcohol with 0.02 N Repeat the process with a small quantity of petroleum
standard sodium hydroxide solution. ether. Cool to room temperature and add 50 ml of
12.2.4 Make a blank test on the petroleum ether by petroleum ether. Then proceed with the extraction as
evaporating 250 ml of the ether with about 0.25 g of outlined under 11.2. Weigh the residue.
stearin or some other hard fat previously brought to
constant mass by heating and drying as in the actual 13.3 Calculation
determination. The blank should not exceed a few Unsaponifiable matter, percent 100 ( M − M )
milligrams. Deduct the value for the blank on the by mass = 1 2

petroleum ether from the mass before calculating the where M 3

unsaponified and unsaponifiable matter.

M1 = mass in g of the residue,
12.3 Calculation M2 = mass in g of the fatty acids (see 11.3.1), and
Calculate the fatty acids as oleic acid (C18H34O2) M3 = mass in g of the material taken for the test.
equivalent of the 0.02 N standard sodium hydroxide
13.3.1 Correct for fatty acids and express the result as
solution used in the titration under 12.2.3, deduct this
percentage of the mass of the material taken for the test.
from the mass of the residue and express as percentage
of the mass of the material taken for the test. 14 DETERMINATION OF UNSAPONIFIED
12.3.1 Mass of fatty acids in the extract, as oleic acid MATTER
= 0.282 5 VN
14.1 Calculation
where From the percentage of total unsaponified and
V = volume in ml of 0.02 N standard sodium unsaponifiable matter determined under 12, deduct the
hydroxide solution, and percentage of unsaponifiable matter obtained under 13
and report the difference as percentage of unsaponified
N = normality of 0.02 N standard sodium
matter.
hydroxide solution.
12.3.2 Unsaponified and unsaponifiable matter, percent 15 DETERMINATION OF ROSIN
100 ( M 1 − M 2 ) 15.0 General
by mass = M3 Two methods for estimation of rosin have been
where prescribed. The method given in 15.1 shall be used as
M1 = mass in g of the residue, referee method and that given in 15.2 shall be used for
routine analysis. The latter method is applicable when
M2 = mass in g of the fatty acids (see 11.3.1), and rosin acids content is not more than 15 percent of total
M3 = mass in g of the material taken for the test. fatty matter.
13 DETERMINATION OF UNSAPONIFIABLE 15.1 Referee Method
MATTER
15.1.1 Reagents
13.0 General
15.1.1.1 Dilute sulphuric acid — 30 percent ( m/v )
The alcoholic solution of the sample is refluxed with obtained by cautiously adding 16 ml of sulphuric acid,
potassium hydroxide solution and extracted with relative density 1.84 ( conforming to IS 266 ), to 70 ml
petroleum ether, when cold. The petroleum ether extract of water.

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15.1.1.2 Beta-naphthalene sulphonic acid solution — rosin acids actually present is one less than the
Dissolve 40 g of the reagent in one litre of chemically percentage of rosin acids found experimentally.
pure, absolute methyl alcohol.
15.1.3.2 Rosin in fatty acids, percent by mass,
15.1.1.3 Standard alcoholic potassium hydroxide corrected = Rosin in fatty acids, percent by mass,
solution — approximately 0.2 N, in 95 percent (m/v) uncorrected – 1.0.
ethyl alcohol or in rectified spirit (see IS 323),
NOTES
accurately standardized. As alcohol is volatile, frequent
1 The mean equivalent mass of the rosin acids is taken as 346.
restandardization is necessary.
2 When the quantity of rosin, expressed as percent by mass, is
15.1.1.4 Phenolphthalein indicator — same as in 6.1.1. less than 5 in the soaps, the results by this method are not so
accurate as with soaps containing higher rosin content. This
15.1.2 Procedure method is also liable to give erroneous results with certain types
of carbolic soaps containing high boiling tar acids and with
15.1.2.1 Dissolve 10 to 50 g of the sample in about other germicidal soaps, for example, soaps containing
500 ml of hot water. Add 10 to 50 ml of dilute sulphuric hexachlorophene.
acid to split the soap, keep in a steam-bath until the
15.1.4 Liebermann-Storch Test
fatty matter separates as a clear layer and siphon off
the lower aqueous acid layer. Add 300 ml of hot water, In all cases where the rosin content is found to be less
boil gently for a few minutes and siphon off the aqueous than 5 percent, the actual presence or absence of rosin
layer. Repeat the washing with hot water several times should be checked qualitatively by the Liebermann-
until the wash liquor is free of mineral acids. Complete Storch test, described below.
the acidification and washing in as short a period as
15.1.4.1 Reagents
possible, keeping the beaker covered to prevent
oxidation of the acids. Remove the mixture of rosin a) Acetic anhydride — pure.
and fatty acids by means of a dry pipette, filter through b) Dilute sulphuric acid — relative density 1.53.
one or two thicknesses of filter paper, and dry at 105 ±
2°C for 45 to 60 min. 15.1.4.2 Procedure

15.1.2.2 Weigh accurately 2 g of the mixture of fatty Transfer 1 to 2 ml of the sample of fatty acids to a test-
and rosin acids into an esterification flask and add 25 tube, treat with 5 to 10 ml of acetic anhydride and warm
ml of beta-naphthalene sulphonic acid solution. Boil on a steam-bath. After cooling, pour 1 to 2 ml into a
gently under a reflux condenser for 30 minutes, adding white porcelain dish and allow a drop or two of
a few glass beads to ensure smooth boiling. Cool the sulphuric acid to run down the side of the vessel. If
contents of the flask and titrate immediately with rosin is present, a fugitive violet colouration changing
standard alcoholic potassium hydroxide solution, using to a brownish tinge is immediately produced at the
0.5 ml of phenolphthalein indicator. The end point is margin of contact of the reagents. Check the test with a
reached when pink colour persists for 30 seconds. sample of fatty acids to which a small amount of rosin
has been added.
15.1.2.3 Conduct simultaneously a blank determination
with 25 ml of the esterifying agent alone. 15.2 Method for Routine Analysis of Rosin Acids
15.1.3 Calculation 15.2.0 General
Rosin in fatty acids, percent 34.6 ( S − B) N Applicable to fatty matter containing not more than 15
by mass, uncorrected = percent rosin acids.
M
where 15.2.1 Apparatus
S = volume in ml of standard alcoholic 15.2.1.1 Conical flask, 250 ml, of chemically resistant
potassium hydroxide solution required for glass with a standard taper 24/40neck.
the material, 15.2.1.2 Condenser, water-cooled with joint fitting the
B = volume in ml of standard alcoholic flask given in 15.2.1.1.
potassium hydroxide solution required for
the blank, 15.2.1.3 Separatory funnel, 500 ml, pear-shape, fitted
N = normality of alcoholic potassium hydroxide, with a glass stopper.
and 15.2.1.4 Burette
M = mass in g of the material taken for the test. 50 ml capacity with 0.1 ml divisions.
15.1.3.1 The method described in 15.1.2 gives results 15.2.2 Reagents
approximately one percent higher than the amount of
rosin actually present. Consequently, the percentage of 15.2.2.1 Dilute sulphuric acid — 30 percent (m/v)

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obtained by cautiously adding 16 ml of sulphuric acid, of sodium sulphate solution. The last washing should
relative density 1.84 (see IS 266), to 70 ml water. not react pink to methyl orange indicator. After
removing the last wash, drain the contents separatory
15.2.2.2 Methanol, 99.5 percent.
funnel into a 500-ml conical flask. Rinse the funnel
15.2.2.3 Sulphuric acid, relative density 1.84 with 20 ml of ether and add the rinsings to the flask.
(see IS 266 LR Grade).
15.2.3.5 Add 20 ml of ethyl alcohol and 1 ml of
15.2.2.4 Sodium sulphate solution, 10 percent. Dissolve phenolphthalein indicator. Titrate to the appearance of
100 g of anhydrous sodium sulphate (Na2SO4) in water. a pink-red colour using 0.2 N alcoholic potassium
15.2.2.5 Petroleum ether, 40-60. hydroxide solution if the rosin acid content is less than
5 percent and 0.5 N if more than 5 percent.
15.2.2.6 Methyl orange indicator — Dissolve 0.1 g of
methyl orange in 100 ml of water. NOTE — For highly coloured samples it will be difficult to
identify the accurate end point using phenolphthalein as
15.2.2.7 Ethyl alcohol, neutral 95 percent ethyl alcohol, indicator. In this case, to the ether extract of 15.2.3.4, add 5 to
6 g of activated charcoal and swirl the flask for 2 to 3 min.
or neutral denatured alcohol.
Filter the solution through a filter paper. Add mixed indicator
15.2.2.8 Phenolphthalein indicator— Dissolve 1 g of for sharper end point, the colour change is from yellow to blue.
Mixed indicator is the mixture of 6 parts of thymol blue and
phenolphthalein in 100 ml of methanol. 1 part of cresol red. This mixture is violet at pH 8.4, blue at
15.2.2.9 Standard alcoholic potassium hydroxide pH 8.3 and rose at pH 8.2.
solution (0.2 N or 0.5 N) — Dissolve 11.2 g of potassium 15.2.4 Calculation
hydroxide ( preferably in pellet form ) for a 0.2 N solution
or 28.0 g for 0.5 N solution in methanol. Dilute to 1 litre Calculate the percentage of rosin acids as follows:
with methanol. Standardize to ± 0.001 N. The Rosin acids, 1.031 × V × N × 30.2
standardized solution should be protected against percent by mass = – 0.74
evaporation and absorption of carbon dioxide from air, M
of soap
and should be restandardized frequently.
where
15.2.3 Procedure
V = volume of standard potassium hydroxide
15.2.3.1 Weigh 40 ± 0.1 g soap sample and dissolve in solution used in titration; in ml;
500 ml of hot water. Add 40 ml of dilute sulphuric acid N = normality of potassium hydroxide solution
to split the soap, keep in a steam bath until the fatty used;
matter separates as a clear layer and siphon off the lower
aqueous acid layer. Add 300 ml of hot water. Boil gently M = mass of the soap sample taken for analysis
for a few minutes and siphon off the aqueous layer. in g; and
Repeat the washing with hot water several times until 0.74= concentration factor.
the wash liquor is free of mineral acids. Complete the NOTE — If the calculated value of rosin acids comes out in
acidification and washing in as short period as possible, negative, it shall be reported as nil.
keeping the beaker covered to prevent oxidation of the 15.2.4.1 Further to above, the rosin acids content based
acids. Remove the mixture of rosin and fatty acids by on Total Fatty Matter (TFM) may be calculated using
means of a dry pipette, filter through two thicknesses the following formula:
of filter paper of size 40 micron, and dry at 105 ± 2oC
for 45-60 min. Dissolve the entire mass in 100 ml Rosin acids, percent by mass of TFM
methanol in a 250 ml conical flask. Swirl the flask to Percentage of rosin acid based on soap × 100
dissolve the oil and add a clean boiling chip. =
TFM percentage
15.2.3.2 Add slowly 5 ml of sulphuric acid while swirling
16 DETERMINATION OF TOTAL FATTY
the flask vigorously. Connect the flask to the condenser,
MATTER
apply heat, and reflux the contents for 10 minutes.
15.2.3.3 Cool the flask to room temperature with cold 16.0 General
water. Add 250 ml of sodium sulphate solution to a he soap split by dilute sulphuric acid is extracted by
500 ml separatory funnel. Pour the contents of the flask ethyl ether as in the determination of combined alkali
into the funnel and complete quantitative transfer of and the ether extract evaporated. The residue is treated
the contents of the flask with 100 ml of petroleum ether. with acetone, evaporated and estimated.
15.2.3.4 Thoroughly shake the mixture in the funnel.
16.1 Procedure
Allow to settle, draw off the salt layer and discard. Wash
contents of the funnel twice again with 250 ml portions Follow the method given in 10.2.1 until the combined

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IS 286 : 2018

ether extract is free from acid or the wash water is with one end bent in the form of a loop of 19 mm outside
neutral to methyl orange indicator. Mix the ether diameter. The upper end may be formed to suit stirring
solution (if necessary, filter previously washing the with hand or attached to a mechanical stirrer.
paper with ether) in a suitable, weighed vessel. Distil
17.1.5 Laboratory Thermometer — range up to 150°C.
off the ether slowly on a steam-bath, and, to the residue,
add 5 ml of acetone. (In order to minimize the risk of 17.1.6 Titre Thermometer — with the following
loss during distillation, the flask should not be more characteristics:
than half full of ether at any stage.) Warm the flask on
a) Type — etched stem glass.
the steam-bath for about one minute, remove it from
the bath and then, while imparting a rotatory motion to b) Liquid — mercury.
the flask hold it at an angle of 45°, direct a current of c) Filling above liquid — evacuated or nitrogen
dry air into its mouth for about one min, thereby gas.
removing the bulk of acetone. Place the flask in a air d) Temperature range — –2°C to 68°C.
oven at about 90°C for 10 min, remove it from the oven e) Subdivisions — 0.2°C.
and blow with air as before for about 15 s. Allow the f) Total length — 385 to 390 mm.
flask to cool and weigh. Return the flask to the steam-
g) Stem diameter — 6 to 7 mm.
oven for another 10 min and blow for 15 s. Allow to
cool and reweigh. Repeat the process until the h) Stem construction — Plain or lens front. The
difference between two consecutive weighings is less cross-section of the lens front type shall be
than 0.005 g. such that it will pass through an 8-mm ring
gauge but will not enter a 5-mm slot gauge.
16.2 Calculation j) Bulb diameter — from 5.5 mm to not greater
M1 than the diameter of the stem.
Total fatty matter, percent by mass = 100 M
2 k) Bulb length — 15 to 25 mm.
where
m) Distance from the bottom of the bulb to –2°C
M1 = mass in g of the fatty matter, and mark — 50 to 60 mm.
M2 = mass in g of the material taken for the test. n) Distance from 68°C mark to the top of the
NOTE — With soaps containing fatty acids, having more than thermometer — 20 to 35 mm.
about 20 percent of fatty acids of molecular mass 200 or below, p) Length of unchanged capillary between the
there is some risk of loss by volatilization if heating in the oven
is unduly prolonged. In such cases, it may be preferable to
highest graduation mark and the expansion
convert the total fatty acids into sodium soaps by titrating with chamber — 10 mm.
ethanolic sodium hydroxide as in 10.2.2 and 10.2.3, drying the q) Expansion chamber — to permit heating to
soaps and calculating the total fatty matter. Allowance must be
made for any trace of neutral salts found to be present in the
at least 85°C.
sodium hydroxide solution. r) Top finish — Glass ring.
s) Longer graduation lines — at each 1°C mark.
17 DETERMINATION OF TITRE OF TOTAL
FATTY ACIDS t) Graduations numbered — at zero and at each
multiple of 2°C.
17.0 General u) Immersion — 10 mm. A line shall be attached
The sample of soap is decomposed with dilute sulphuric around the stem, 45 mm from the bottom of
acid and the fatty acid layer separated. The the bulb.
solidification point of this material is determined under v) Maximum scale error permitted at any
prescribed conditions. point — 0.2°C.
w) Standardization — The thermometer shall be
17.1 Apparatus standardized at the ice point and at intervals
17.1.1 Low Form Beaker — of 2-litre capacity, to serve of approximately 20 deg, for the condition of
as a water-bath. 45 mm immersion, and for an average stem
temperature of the emergent mercury column
17.1.2 Wide Mouth Bottle — of 450-ml capacity, height of 25 deg.
190 mm and inside diameter of neck 38 mm.
17.2 Reagents
17.1.3 Test-Tube — 100 mm in length and 25 mm in
diameter, with an etched mark extending around the 17.2.1 Dilute Sulphuric Acid — 30 percent ( m/v )
tube at a distance of 57 mm from the bottom. obtained by cautiously adding 16 ml of concentrated
sulphuric acid, relative density 1.84 (see IS 266), to
17.1.4 Stirrer — made of stainless steel or Monel metal 70 ml of water.

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17.2.2 Acetone — pure ( see IS 170). iodide and the liberated iodine estimated by titration
with sodium thiosulphate solution.
17.3 Procedure
18.1 Apparatus
17.3.1 Preparation of Fatty Acids
An engraved stem thermometer, calibrated between
Dissolve approximately 50 g of the sample in 500 ml 10°C and 65°C in 0.1 deg intervals and with 0°C point
of hot water contained in a 1 000-ml beaker. Add marked on the stem, is recommended. The thermometer
sufficient dilute sulphuric acid until the solution is shall have an auxiliary reservoir at the upper end, a
distinctly acidic to methyl orange and place in a boiling length of about 370 mm and a diameter of about 6 mm.
water-bath until the fatty acids collect as a clear layer
at the top. Remove the aqueous acid ( lower ) layer 18.2 Reagents
with a siphon, add 300 ml of hot water, place in the 18.2.1 Acetic Acid — glacial, 99 percent, having a
boiling water-bath for a few minutes, and again remove melting point of 14.8°C and free from reducing
the queous acid layer with a siphon. impurities. Determine the melting point and test the
Wash the fatty acids thrice in this manner. Complete acetic acid for reducing impurities as follows:
the acidification and washing in as short a period as
a) Melting point determination — Fill a test-tube,
possible, keeping the beaker covered to prevent
15 cm long, about two-thirds with acetic acid,
oxidation of fatty acids. After the last wash, allow the
and insert the thermometer described in 18.1
fatty acids to settle for a few minutes and then decant
through a cork stopper fitting the test-tube.
them carefully. Filter through one or two thicknesses
The amount of acid should be at least double
of filter paper, introduce into a conical flask and add
the quantity required to cover the bulb of the
10 ml of acetone. Close the flask with an air-tight cork,
thermometer when the bottom of the latter is
carrying a glass tube. Immerse the flask in boiling water
12 mm from that of the test-tube. Suspend this
and apply suction from a water pump until bubbling
tube within a larger test-tube through a cork.
ceases. Remove the cork and dry the flask at 105 ±
Cool the acid by immersing the assembly in
2°C for at least half an hour.
ice water until the temperature is 10°C,
17.3.2 Determination of Titre withdraw the assembly from the ice water, stir
the acid vigorously for a few moments, thereby
Adjust the temperature of the water-bath to 20 ± 1°C
causing the super-cooled liquid to crystallize
for all samples having titres of 35°C or higher, and to
partially and giving a mixture of liquid and
15 to 20°C below the titre point for all samples with
solid acid. Take thermometer readings every
titres below 35°C. Place the fatty acids, prepared as
15 seconds and consider as true melting point
prescribed in 17.3.1, in the test-tube up to the etched
that temperature at which the reading remains
mark and insert the titre thermometer in the centre of
constant for at least 2 min.
the sample. Suspend it at such a height that the
immersion mark coincides with the top of the sample b) Test for reducing impurities ( potassium
of fatty acids. When the titre test thermometer reads permanganate test ) — Dilute 2 ml of acetic
about 10°C above the expected titre value, set the acid with 10 ml of water, add 0.1 ml of 0.1 N
stirrer moving in a vertical manner at the rate of about potassium permanganate solution and
100 complete up-and-down motions per minute. maintain at 27 ± 2°C. The test shall be taken
Continue stirring until the temperature remains as having been satisfactory if pink colour is
constant for 30 s. Stop stirring when the temperature not discharged at the end of two hours.
begins to rise, remove the stirrer or raise it out of the 18.2.2 Carbon Tetrachloride or Chloroform — The
sample and observe the increase in temperature. Titre reagent shall be inert to Wijs solution.
point is the highest temperature indicated by the
18.2.3 Standard Sodium Thiosulphate Solution —
thermometer during this rise. Duplicate determinations
Dissolve pure sodium thiosulphate crystals (Na2S2O3.
should agree within 0.2°.
5H2O) in water, which has been well boiled to free it
18 DETERMINATION OF IODINE VALUE from carbon dioxide, in proportion so that 24.83 g of
(WIJS ) sodium thiosulphate is contained in one litre of the
solution. Let this solution stand for about two weeks
18.0 General
before standardizing. Standardize with pure re-
A known quantity of fatty acids prepared as for the titre sublimed iodine or potassium iodate. The solution will
test is treated in carbon tetrachloride or chloroform be approximately 0.1 N and it is better to leave it as it
medium with a known excess of iodine monochloride is after determining its exact normality instead of
solution in glacial acetic acid ( Wijs solution). The attempting to adjust it to exactly 0.1 N strength.
excess iodine monochloridc is treated with potassium Preserve in a dark-coloured stock bottle with a guard

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IS 286 : 2018

tube filled with soda lime. The strength of the solution Pipette 5 ml of this, add 10 ml potassium
should be checked occasionally. A few drops of iodide solution (10 percent) and titrate with
chloroform may be added to the solution for better 0.1 N sodium thiosulphate solution, using
preservation. starch solution as indicator. Adjust the volume
18.2.4 Starch Solution — Make a paste of 0.5 g of soluble of the solution till it is 0 2 N.
starch in cold water, pour it into 100 ml of boiling water, 18.3 Procedure
boil for 5 min, cool and bottle. The solution should be
18.3.1 It is essential that all the glass apparatus used in
prepared afresh every two or three days.
this experiment should be perfectly clean and dry.
18.2.5 Potassium Iodide Solution — Prepare fresh
18.3.2 Prepare the fatty acids as prescribed
solution by dissolving 10 g of potassium iodide, free
under 17.3.1.
from potassium iodate, in 90 ml of distilled water.
18.3.3 Weigh in a small glass tube an appropriate
18.2.6 Wijs Iodine Monochloride Solution — Prepare quantity of the fatty acids as indicated in Table 4. Drop
this solution by one of the following three methods, the tube into a clean, dry 500-ml glass-stoppered bottle,
and store in a glass-stoppered bottle in cool place, to which 25 ml of carbon tetrachloride have been added,
protected from light: and agitate to dissolve the contents. Add 25 ml of Wijs
a) From iodine — Dissolve 13 g of iodine in one solution and replace the glass stopper after wetting with
litre of acetic acid using gentle heat, if potassium iodide solution.
necessary, and determine the strength by
Swirl for intimate mixing and allow 10 stand for 30
titration with standard sodium thiosulphate
minutes in a dark place. Carry out a blank test
solution. Set aside 50 to 100 ml of the solution
simultaneously under similar experimental conditions.
and introduce dry chlorine gas into the
After 30 minutes, add 20 ml of potassium iodide
remainder until the characteristic colour
solution and 100 ml of water and titrate the liberated
change occurs and the halogen content is
iodine with standard sodium thiosulphate solution,
nearly doubled as ascertained again by
swirling the system continuously to avoid any local
titration. If the halogen content has been more
excess until the yellow colour just disappears. Add 0.5
than doubled, reduce it by adding the requisite
ml of starch solution and continue the titration until
quantity of iodine-acetic acid solution. A slight
the blue colour disappears.
excess of iodine does no harm, but avoid an
excess of chlorine. 18.4 Calculation
Example : (B − S )N
Iodine value = 12.69
If the titration of 20 ml of original iodine- M
acetic acid solution requires 22 ml of standard where
sodium thiosulphate, 20 ml of the finished B = volume in ml of standard sodium
Wijs solution should require between 43 and thiosulphate solution required for the blank,
44 ml (and not more than 44 ml ) of the same
S = volume in ml of standard sodium
sodium thiosulphate solution.
thiosulphate solution required for the
b) From iodine trichloride — Dissolve 8 g of iodine material,
trichloride in approximately 450 ml of glacial N = normality of standard sodium thiosulphate
acetic acid. Dissolve separately 9 g of iodine in solution, and
450 ml of glacial acetic acid, heating if necessary.
Add gradually the iodine solution to iodine M = mass in g of the material taken for the test.
trichloride solution until the colour has changed Table 4 Mass of Fatty Acids for Iodine Value
to reddish brown. Add 50 ml more of iodine Determination
solution and dilute the mixture with glacial acetic ( Clause 18.3.3 )
acid till 10 ml of the mixture is equivalent to 20
Expected Mass in g Weighing
ml of standard sodium thiosulphate solution Iodine Value Accuracy
when the halogen content is estimated by titration Maximum Minimum
in the presence of an excess of potassium iodide (1) (2) (3) (4)
and water. Heat the solution to 100°C for 20 <3 — 10.00 0 ± 0.001 0
minutes and cool. Prevent access of water vapour 5 6.346 0 5.077 0 ± 0.000 5
in preparing the solution. 10 3.173 0 2.538 4 ± 0.000 2
c) From iodine monochloride — Dissolve 10 ml 60 0.528 3 0.423 1 ± 0.000 1
100 0.317 3 0.253 8 ± 0.000 1
of iodine monochloride in about 800 ml of
glacial acetic acid and shake vigorously.

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19 DETERMINATION OF ALKALINE filter papers in a tared platinum crucible and ignite

SILICATES carefully, first at low temperature to burn off the paper
and then at bright red heat (850°C) over a burner. Cool
19.0 General in a desiccator and weigh. Repeat heating, cooling and
The alkaline silicates present in soaps arc determined weighing to constant mass.
as sodium silicate from the charred residue of the soap
19.4 Calculation
and its water extract.
Sodium silicate (Na2O, 2SiO2),
19.1 Apparatus A
percent by mass = 151.6
where M
19.1.1 Platinum Evaporating Dish — 10-ml capacity.
19.1.2 Platinum Crucible — 30-ml capacity. A = mass in g of the residue, and
19.1.3 Watch Glass M = mass in g of the material taken for the test.
19.1.4 Ashless Filter Papers 19.4.1 Neutral sodium silicate (Na 2O, 3.25SiO 2),
A
percent by mass = 131.8
19.2 Reagents M
19.2.1 Hydrochloric Acid — concentrated, relative where A and M have the same legends as in 19-4.
density 1.16 (see IS 265). 19.5 Referee Method
19.2.2 Hydrofluoric Acid — 48 percent (m/v). For accurate results, moisten the weighed contents of
the crucible ( obtained as prescribed under 19.3.3 ) with
19.2.3 Sulphuric Acid — concentrated, relative density
water, add 10 ml of hydrofluoric acid and 4 drops of
1.84 (see IS 266).
sulphuric acid and evaporate to dryness over a low flame.
19.3 Procedure Ignite as directed previously, cool to room temperature
in a desiccator and weigh. The difference between this
19.3.0 The procedure varies depending upon whether
mass and that of the residue found under 19.3.3 is the
the material contains mineral matter insoluble in water,
mass of the silica.
or not.
19.3.1 When the material contains no mineral matter 20 DETERMINATION OF BORAX
insoluble in water, ignite 1 to 5 g of it [quantity taken 20.0 General
containing not more than 0.2 g of silica (SiO2)], in a Conduct the qualitative test described under 20.1 and,
platinum evaporating dish over a burner at low if the result is positive, proceed with the quantitative
temperature (350 to 400°C). When charred, extract the determination described under 20.2.
water soluble material with water, return the filter paper
and the residue to the platinum dish and continue 20.1 Qualitative Test
ignition to bright red heat (850 to 950°C) till all the 20.1.1 Reagents
carbonaceous material is removed. Continue the water
extract and the residue, and carefully neutralize with a) Turmeric test paper — prepared by
hydrochloric acid, avoiding any loss by spray by impregnating unglazed white paper with the
keeping the dish covered. Finally, add 5 to 10 ml of clear extract obtained by macerating for one
hydrochloric acid in excess. week 10 g of bruised turmeric in 60 ml of
alcohol ( 95 percent by volume ).
19.3.2 When the sample contains mineral matter
b) Potassium iodide solution — 5 percent ( m/v).
insoluble in water, take a portion of the solution
containing not more than 0.2 g of silica (SiO2) after c) Starch solution — perpared as under 18.2.4.
titrating the matter insoluble in alcohol but soluble in d) Dilute sulphuric acid — 1 : 4 by volume.
water as under 9.2 and add 5 to 10 ml of hydrochloric 20.1.2 Procedure — Wet a piece of turmeric test paper
acid. with a few milliliters of filtrate obtained under 19.3.3
19.3.3 Evaporate the acidified solution, obtained as after acidifying the filtrate. A borate or perborate is
prescribed under 19.3.1 or 19.3.2 to dryness on a steam- present if the paper, on drying in air, turns deep brick
bath. Cool the residue and moisten with hydrochloric red. To determine whether the colouration is due to
acid. Add about 25 ml of hot water, heat for a few perborate, dissolve about 2 g of the original analysis
minutes and filter through an ashless filter paper. Wash sample in about 100 ml of potassium iodide solution
thoroughly with water. Evaporate the filtrate to dryness containing 2 ml starch solution. Add 10 ml of dilute
and repeat the above treatment, filtering through a sulphuric acid and stir. A blue solution denotes the
second ashless filter paper. Preserve this filtrate for presence of an oxidizing agent which, with a positive
qualitative tests under 20.1.2 and 21.1.2. Place the two turmeric test, confirms the presence of perborate.

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20.2 Quantitative Test where

20.2.1 Apparatus V = volume in ml of standard sodium hydroxide
a) Platinum evaporating disk — 100-ml capacity. solution required for titration,
b) Round-bottom flask — 250-ml capacity. N = normality of standard sodium hydroxide
solution, and
c) Water-cooled reflux condenser
M = mass in g of the material taken for the test.
20.2.2 Reagents
20.3 Determination of Perborates
a) Fusion mixture — prepared by mixing 200 g 20.3.0 General — Persalt content is determined from
of sodium carbonate with 15 g of powdered the iodine set free when the solution is reacted with
silica. acidified potassium iodide solution. The iodine liberated
b) Ethyl alcohol — 95 percent (v/v). is titrated with standard sodium thiosulphate solution.
c) Dilute hydrochloric acid — 1 : 1 (v/v). This method is applicable even when ethylenediamine
d) Calcium carbonate — powder. tetracetic acid or perfume is present in the soap.
e) Standard sulphuric acid — approximately 1 N. 20.3.1 Reagents
f) Methyl orange indicator — Dissolve 0.1 g in a) Dilute sulphuric acid — 1 : 1 (v/v).
100 ml of water. b) Potassium iodide
g) Standard sodium hydroxide solution — c) Ammonium molybdate solution — 3 percent
approximately 0.1 N, carbon dioxide-free. (m/v).
h) Glycerine — conforming to CP Grade of IS1796 d) Sodium thiosulphate solution — 0.1 N.
j) Phenolphthalein indicator — as in 6.1.1. e) Starch indicator solution
20.2.3 Procedure — Weigh accurately about 10 g of the 20.3.2 Procedure
sample (or about 5 g if more than 5 percent borax is Weigh accurately 2 to 5 g of the sample and transfer to a
present) into a platinum evaporating dish and add 2.15 g 500-ml glass-stoppered bottle. Dissolve in 100 ml water
of fusion mixture and 15 ml of ethyl alcohol. Mix the heated to 37°C and add 2 g of the potassium iodide.
whole with a glass rod and, after washing the rod with a Acidify the solution by adding 10 ml of sulphuric acid.
little ethyl alcohol, evaporate the mixture to dryness on Add 1 ml of ammonium molybdate solution. Allow the
a water-bath. Char the mixture thoroughly and ignite to solution to stand in a dark cupboard for 5 minutes and
fusion over a burner. Cool, extract the residue with titrate the liberated iodine with sodium thiosulphate
boiling water into a round-bottom flask and acidify with solution using starch solution as indicator.
20 ml of dilute hydrochloric acid. An excels of acid is
20.3.3 Calculation
necessary if any phosphates are to be hydrolyzed. Boil
under reflux for 2 h, add a moderate excess of calcium Sodium perborate (NaH2BO4, 3H2O), 0.770T
carbonate and continue boiling vigorously for 20 min. percent by mass =
M
Add a further small amount of calcium carbonate if the where
precipitate is gelatinous. Filter and wash several times T = volume in ml of 0.1 N sodium thiosulphate
with small quantities of water. Transfer the filtrate and solution used, and
washings into a round-bottom flask, and neutralize with
standard sulphuric acid in the presence of methyl orange M = mass in g of the sample taken.
indicator. To the neutral solution, add 0.1 ml of standard 21 DETERMINATION OF PHOSPHATES
sulphuric acid, boil for 5 minutes more, cool the solution
21.0 General
and neutralize with standard sodium hydroxide solution.
Add 50 ml of glycerine to the solution and titrate it with Conduct the qualitative test described under 21.1 and,
standard sodium hydroxide solution in the presence of if the result is positive, proceed with the quantitative
phenolphthalein indicator. After the end point is reached, determination described under 21.2.
add another 10 ml of glycerine and continue the titration 21.1 Qualitative Test
until pink colour appears again. Repeat this until the
21.1.1 Reagents
addition of glycerine causes no further change in the end
point. a) Nitric acid — concentrated, relative density
1.42 (see IS 264).
20.2.4 Calculation
b) Ammonium nitrate solution — 30 percent (m/v).
Borax (as Na2B4O7. 10H2O), VN c) Ammonium molybdate solution — Dissolve
percent by mass = 9.536
M 100 g of molybdic acid in dilute ammonium
hydroxide solution prepared by adding 270 ml

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IS 286 : 2018

of water to 144 ml of concentrated ammonium exceed 100 ml. Collect the solution and the washings in
hydroxide solution. Pour the resulting solution a beaker and neutralize with dilute hydrochloric acid
slowly, with continuous stirring, into 489 ml of using litmus paper as an indicator. Cool and add slowly
nitric acid and 1 148 ml of water. Keep the with constant stirring 15 ml of magnesia mixture for every
mixture in a warm place for several days. Decant decigram of phosphorus pentoxide (P2O5) present. Allow
the solution and make sure that no yellow to stand and add 12 ml of ammonium hydroxide solution
precipitate is deposited on heating to 40°C. (relative density 0.90). After 2 h, filter through a filter
paper and wash the precipitate with ammonium
21.1.2 Procedure
hydroxide solution (1 : 9) until the washings are free from
To 20 ml of the filtrate obtained under 19.3.3, add 2 ml chlorides. Dry and ignite the filter paper, starting at low
of nitric acid and 5ml of ammonium nitrate solution. heat and finishing at bright red heat (about 1 100°C) till
Heat to boiling, add 20 ml of ammonium molybdate the colour of the pyrophosphate is white. Cool to room
solution and allow the solution to stand for 20 min on a temperature and weigh. Repeat ignition, cooling and
steam-bath. If a yellow precipitate forms, a phosphate weighing until constant mass of the precipitated
is present. If metaphosphates or pyrophosphates are magnesium pyrophosphate (Mg2 P2O7) is obtained.
present, add about 10 ml of nitric acid and heat at or
21.3 Calculation
near boiling temperature overnight to convert them to
Calculate the phosphates as phosphorus pentoxide as
orthophosphates before testing as described above.
follows:
m1
21.2 Quantitative Test Phosphorus pentoxide, percent by mass = 63.79 m
2
21.2.1 Reagents
where
a) Dilute hydrochloric acid — 1 : 1 (v/v).
m1 = mass in g of magnesium pyrophosphate, and
b) Ammonium hydroxide solutions — m2 = mass in g of the material corresponding to
concentrated, relative density 0.90, and dilute the aliquot taken for the test.
1 : 9 (v/v).
c) Nitric acid — relative density 1.43 (see IS 264). 22 DETERMINATION OF SULPHATES
d) Ammonium nitrate — solid or 10 percent 22.0 General
solution ( m/v ).
All organic matter in the soap is thoroughly charred,
e) Ammonium molybdate solution — prepared the residue digested with hydrochloric acid and
as described under 21.1.1 (c). extracted with hot water. The solution is filtered and
f) Ammonium chloride — solid. the sulphate determined in the filtrate gravimetrically
g) Magnesia mixture — Dissolve 55 g of as barium sulphate.
magnesium chloride (Mg Cl2, 6H2O ) in water, 22.0.1 This method is applicable only to soaps and soap
and 140 g of ammonium chloride and 130.5 ml products free from sulphonated oils, synthetic
of concentrated ammonium hydroxide detergents and organic compounds containing sulphur.
solution and dilute the mixture to one litre.
22.1 Reagents
21.2.2 Procedure
22.1.1 Hydrochloric Acid — concentrated, relative
Accurately weigh about 2 g of the matter insoluble in density 1.16 (see IS 265).
alcohol or ash and proceed as in the case of determining
alkaline silicates under 19.3. After filtering off the 22.1.2 Barium Chloride Solution — 10 percent.
residue, collect the filtrate and washings and make up to 22.2 Procedure
250 ml in a volumetric flask, concentrating if necessary.
Take out an aliquot corresponding to 0.05 to 0.10 g of Proceed as for the estimation of alkaline silicates
phosphorus pentoxide (P2O5), add a slight excess of under 19.3, igniting and charring either the original
ammonium hydroxide solution ( relative density 0.90 ), sample or the residue left after the removal of alcohol
and dissolve the precipitate with a few drops of nitric soluble matter if highly accurate results are not required.
acid while stirring vigorously. Add 15 g of dry ammonium Collect the filtrates and washings after removal of any
nitrate or a solution containing that amount, heat to 60°C residue, if present, and make up to approximately 200
and test for complete precipitation by the addition of 1 ml. Add 10 ml of hydrochloric acid, boil the solution
to 2 ml of ammonium molybdate solution. Filter and and add hot barium chloride solution drop by drop by
wash with ammonium nitrate solution, redissolve the means of a pipette. Boil for 2 min to coagulate the
precipitate on the filter paper with ammonium hydroxide precipitate and allow to stand and cool for about 4 hours.
solution (relative density 0.90) and wash the filter paper Filter through a tared Gooch crucible or a sintered glass
with hot water. The total volume of liquid should not crucible (G No. 4), wash thoroughly with hot water and
heat at 105 to 110°C to constant mass.
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22.2.1 The addition of 5 ml of a saturated solution of Remove the rod with cake attached to it, rinse with
picric acid after adding 10 ml of hydrochloric acid water and collect the rinsings in the beaker.
accelerates the precipitation of barium sulphate and 23.3.2 Transfer the aqueous phase and washings to a
reduces the standing time from 4 h to about 30 min. 250-ml graduated flask, make up to volume and filter
22.2.2 Excess of barium chloride is necessary to reduce through a filter paper (Whatman No. 540 or equivalent
the solubility of barium sulphate. Precipitation in hot is suitable) into a 100-ml graduated flask. Transfer
solution by the addition of barium chloride in a slow exactly 100 ml of the filtrate into a 500-ml conical flask
stream, with stirring, minimizes mechanical occlusion and make just alkaline with 1 N sodium hydroxide
of barium chloride and gives a course precipitate, which solution. Add about 1 ml excess of hydrochloric acid,
is less soluble in acids. boil gently for three minutes to expel carbon dioxide,
stopper the flask with a soda lime guard-tube and allow
22.3 Calculation to cool in a bath of cold water. When cooled, wash
m down the sides of the flask with carbon dioxide- free
Sulphates (as Na2SO4), percent by mass = 60.86
M water and adjust the pH of the solution to that used for
where final titration by adding 0.05 N sodium hydroxide
m = mass in g of barium sulphate, and solution. Add 25 ml of sodium periodate solution, insert
M = mass in g of the material taken for the test. the guard-tube, swirl and allow the reaction to proceed
23 DETERMINATION OF GLYCEROL for 30 minutes in the dark. Wash down the sides of the
flask with carbon dioxide-free water, add 5 g of ethylene
23.0 General glycol, swirl the flask and allow to stand in the dark for
The glycerol content is estimated from the formic acid a further 20 minutes. Finally, titrate the solution with
produced by its oxidation by a solution of sodium 0.05 N sodium hydroxide solution using the pH meter
metaperiodate. until the pH of the solution is 8.1. Carry out a blank
test at the same time under exactly the same conditions
23.1 Apparatus except that while the pH value is adjusted to 8.1 before
the addition of the periodate solution, the final titration
23.1.1 pH Meter — with glass electrodes.
is carried to the end point of pH 6.5 and not 8.1.
23.2 Reagents NOTE — If a pH meter is not available, use phenol red indicator
(0.05 percent aqueous solution). Titrate blank and test to the
23.2.1 Dilute Sulphuric Acid — 10 percent (m/v). colour change of the indicator (yellow to red). Add 0.3 percent
(expressed on 100 percent glycerol) the observed glycerol result.
23.2.2 Beeswax This is not a reference method.
23.2.3 Sodium Hydroxide Solution — approximately 1 N. 23.4 Calculation
23.2.4 Dilute Hydrochloric Acid — approximately 1 N. 1.1511
Glycerol, percent by mass = (T − T1 )
m
23.2.5 Sodium Hydroxide Solution — 0.05 N, where
accurately standardized against potassium hydrogen
T = volume in ml of 0.05 N sodium hydroxide
phthalate and free from carbonates.
solution required for test,
23.2.6 Sodium Periodate Solution — 6 percent (m/v) T1 = volume in ml of 0.05 N sodium hydroxide
solution in carbon dioxide-free water. solution used for blank, and
23.2.7 Ethylene Glycol m = mass in g of the sample taken.
23.3 Procedure 24 DETERMINATION OF SUGARS
23.3.1 Dissolve 20 g of soap in about 150 ml of water 24.0 General
in a 250-ml beaker, precipitate the fatty acids by adding
The matter insoluble in alcohol is extracted from the
a slight excess of sulphuric acid and allow the beaker
soap with water to which Fehling solution is added.
and its contents to stand either overnight at room
Sugar reduces Fehling solution to red cuprous oxide
temperature or in a steam-bath with frequent stirring
under suitable conditions. From the mass of cuprous
until the fatty acid layer is clear. Add about 10 g of
oxide, the amount of invert sugar is obtained from the
beeswax, stir occasionally to ensure homogeneous
mixing of the fatty acids and the beeswax and leave the Munson and Walker table.
beaker with the glass rod in the bath for a few minutes 24.1 Reagents
until the fatty layer is clear. Remove the beaker from
the bath, keep overnight and warm slightly to obtain 24.1.1 Ethyl Alcohol — 95 percent ( v/v ).
two distinct layers. Cool quickly in running water. 24.1.2 Dilute Sulphuric Acid — 1 : 4 ( v/v ).

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24.1.3 Ether acid and 200 ml of water and reflux the mixture under
24.1.4 Sodium Hydroxide Solution — approximately 1 N. a water condenser for 2 to 3 h. Cool, add sodium
hydroxide solution until almost neutral and make up to
24.1.5 Modified Fehling’s Solution — Dissolve 34.639
250 ml in a volumetric fiask. Filter and discard the first
g of copper sulphate (CuSO4.5H2O) in water and make 10 ml of the filtrate. Pipette 50 ml of the filtrate and
up to 500 ml. Dissolve 173 g of Rochelle salt (sodium proceed to estimate the amount of invert sugar present
potassium tartrate, NaKC4H4O6, 4H2O) and 50 g of in the aliquot as under 24.2.
sodium hydroxide in water and make up to 500 ml.
Mix equal volumes of the two solutions before use. 25.3 Calculation
24.2 Procedure Use the standard ‘Munson and Walker’ table (see Annex
A) to compute the milligrams of dextrose corresponding
Proceed as in the method for the removal of
the mass of the cuprous oxide (Cu2O) and calculate as
alcoholinsoluble and water-insoluble matter as under 8.
follows:
Use water at 0 to 10°C if starch is to be removed. Take
the water alcohol solutions, evaporate off the alcohol, Starch, percent by mass =
concentrate to 200 ml and add 25 ml of dilute sulphuric
acid. Boil gently for 20 min. Remove the cake of fatty milligramsof dextrose×0.093
acids after cooling and extract with 25 ml of ether to massin g of materialin thealiquot taken for the test
remove the ether-soluble materials. Neutralize the acids
in the aqueous solution with sodium hydroxide solution 26 DETERMINATION OF COMBINED SODIUM
and make up to 500 ml in a volumetric flask. Pipette out AND POTASSIUM OXIDES
50 ml of this solution (to contain less than 0.25 g of 26.0 General
reducing sugars) and add 50 ml of the modified Fehling’s Organic matter in the soap is removed by ashing the
solution. Heat with a flame to start boiling in exactly 4 sample and the residue is digested with hydrochloric
minutes and continue boiling for exactly 2 minutes. Filter acid and potassium precipitated as potassium
immediately through a tared Gooch crucible and wash chloroplatinate. From this potassium oxide is
several times with water at 60°C. Wash the filter paper calculated. Sodium oxide is obtained by subtracting the
finally with 10 ml of ethyl alcohol and 10 ml of ether. percentage of potassium oxide from the percentage of
Dry the crucible in an air-oven at 105 ± 2°C for 30 min, combined alkali.
cool and weigh as cuprous oxide (Cu2O).
26.1 Reagents
24.3 Calculation 26.1.1 Dilute Hydrochloric Acid — 1 : 1 (v/v).
Use the standard ‘Munson and Walker’ table (see Annex 26.1.2 Platinum Solution — Prepare a solution
A) to compute the milligrams of invert sugar containing the equivalent of 0.2 g of metallic platinum
corresponding to the mass of the cuprous oxide (Cu2O) [0.42 g of chloroplatinic acid (H2Pt Cl6) in each 10 ml
formed. Calculate as follows: of solution].
Invert sugar, percent by mass 26.1.3 Ethyl Alcohol — 80 percent (v/v). Dilute 84 ml
milligrams of invert sugar×0.1 of ethyl alcohol, 95 percent by volume, with 16 ml of
= massin g of materialin aliquot taken for the test water.
Sucrose, percent by mass = invert sugar, percent by 26.1.4 Concentrated Hydrochloric Acid — relative
mass × 0.95. density 1.16 (see IS 265).
26.1.5 Ammonium Chloride Solution — To 500 ml of
25 DETERMINATION OF STARCH 20 percent ammonium chloride solution, add 5 to 10 g
25.1 Reagents of pulverized potassium chloroplatinate (K2PtCl6) and
shake at intervals of 6 to 8 h. Allow the mixture to settle
25.1.1 Dilute Hydrochloric Acid — relative density and filter.
1.125, obtained by diluting 100 ml of concentrated
26.2 Procedure
hydrochloric acid, relative density 1.16 (see IS 265)
to 130 ml. Accurately weigh about 10 g of the sample in an
evaporating dish and heat over a burner or in a Muffle
25.1.2 Sodium Hydroxide Solution — approximately
furnace below dull red heat (350 to 450°C) until the
0.5 N.
mass is well carbonized. Cool, leach out the ash with
25.2 Procedure hot water, filter into a 100 ml volumetric flask and wash
Remove the alcohol-soluble matter as under 5 and wash the filter paper with three portions of 5 to 10 ml each
the alcohol-insoluble residue with water at 0 to 10°C. of hot water. Return the filter paper and the residue to
Transfer the wet insoluble matter on the filter paper the evaporating dish and continue heating as before until
into a conical flask, add 20 ml of dilute hydrochloric all carbonaceous matter is burnt off. Add a few drops

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of dilute hydrochloric acid and wash the contents of 5 mole of sodium bromide to one mole of
the dish through a filter paper into the 100 ml sodium bromate.
volumetric flask. Acidify the solution in the volumetric d) Dilute hydrochloric acid — 1 : 1 (v/v).
flask with dilute hydrochloric acid and dilute to 100 e) Potassium iodide solution — 10 percent (v/v).
ml with water. Pipette 10 ml of the solution into a 100 ml
f) Standard sodium thiosulphate solution —
beaker and acidify with a few drops of dilute
approximately 0.1 N.
hydrochloric acid. Add 10 ml of platinum solution and
evaporate on a water-bath to the consistency of a thick g) Starch solution — prepared as under 18.2.4.
paste. Add 5 ml of ethyl alcohol and 0.6 ml of 27.1.2 Procedure
concentrated hydrochloric acid and transfer the
precipitate to a tared Gooch crucible. Accurately weigh about 5 g of the sample and dissolve
in 200 ml of water made alkaline with 10 ml of sodium
Wash with ethyl alcohol until the filtrate is colourless. hydroxide solution. Transfer to a 1 000 ml volumetric
Then wash the residue, 5 or 6 times, with 20 ml portions flask, dilute to 600 ml, add 20 ml of calcium nitrate
of ammonium chloride solution and, finally with ethyl solution, cool and make up to one litre. Filter, reject
alcohol until the filtrate gives no test for chlorides. Dry the first few millilitres of the filtrate and pipette 100
in an air-oven at 105 to 110°C for 30 min, cool and ml into a narrow-mouth stoppered bottle. Add 100 ml
determine the mass of potassium chloroplatinate. of water, 50 ml of sodium bromate-bromide solution
26.3 Calculation and 10 ml of dilute hydrochloric acid. Allow to stand
B for 90 min, add 25 ml of potassium iodide solution and
Potassium oxide (K2O), percent by mass = 193.8 mix well. Titrate the liberated iodine against standard
M
sodium thiosulphate solution using starch as indicator.
Sodium oxide (Na 2 O), percent by mass = A —
Run a blank, using a material known to be free from
[potassium oxide (K2O), percent by mass × 0.658 2 ]
carbolic acid.
where
27.1.3 Calculation
B = mass in g of potassium chloroplatinatc V −v
(K2PtCl6), Carbolic acid, percent by mass = 0.156 7
M
M = mass in g of the material taken for the test, where
and
V = volume in ml of standard sodium
A = combined alkali (as Na2O), percent by mass,
thiosulphate solution required for the blank,
as found under 10.
v = volume in ml of standard sodium
27 DETERMINATION OF CARBOLIC ACID thiosulphate solution required for the test,
AND CRESYLIC ACID and
27.0 General M = mass in g of the material in the aliquot taken
Insoluble metal salts of soap fatty acids are precipitated for the test.
by the addition of calcium nitrate to an aqueous solution
27.2 Cresylic Acid
of the soap and removed by filtration. The cresylic acid
in the alkaline filtrate is brominated by bromine 27.2.1 Reagents — In addition to the reagents
liberated on the addition of a standard sodium bromide- prescribed in 27.1.1 the following reagent is
sodium bromide solution and dilute mineral acid. required:
Excess bromine is determined by adding potassium
a) Standard cresylic acid — a mixture of
iodide and titrating the liberated iodine with standard
35 percent o-cresol, 40 percent m-cresol and
sodium thiosulphate. From this carbolic acid and
25 percent ñ-cresol.
cresylic acid are calculated.
27.2.2 Procedure
27.1 Carbolic Acid
Weigh quickly 0.25 g of standard cresylic acid and add
27.1.1 Reagents immediately 10 ml of sodium hydroxide solution.
a) Sodium hydroxide solution — 10 percent (m/v). Dissolve 5 g of any bar soap free from carbolic acid in
b) Calcium nitrate solution — 20 percent (m/v). water, add the cresylic acid solution and continue as
c) Sodium bromate-bromide solution — Dilute described under 27.1.2.
90 ml of sodium hydroxide solution to 400 ml 27.2.3 Calculation
with water and add liquid bromine until the V −v
Cresylic acid, percent by mass = 5
solution is yellow. Boil the solution until it is V −s
clear, add 5 ml of sodium hydroxide solution where
and make up to 2 litres. The solution contains V = volume in ml of standard sodium
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thiosulphate solution required for the blank, d) Condenser — water cooled, 3- or 4-bulb Allihn
v = volume in ml of standard sodium thiosulphate type, with a jacket about 200 mm long and a
solution required with the sample, and side arm for connecting to the conical flask; and
s = volume in ml of standard sodium e) Mercury manometer.
thiosulphate solution required against 28.1.2 Glass Beads
standard cresylic acid and soap free from
carbolic acid. 28.2 Reagents
28.2.1 Hydrochloric Acid — 0.5 N, accurately
28 DETERMINATION OF CARBONATES
standardized.
28.0 General 28.2.2 Dilute Hydrochloric Acid – 1 : 2 (v/v).
This method determines all of the carbonates as carbon 28.2.3 Alkaline Absorbent Solution — Mix equal volumes
dioxide and is applicable to all soaps and soap products. of 1.0 N sodium hydroxide (carbonate-free) solution and
28.1 Apparatus — The following apparatus is required. 0.1 N barium chloride solution. Allow to settle overnight,
filter and preserve in well-stoppered bottles.
28.1.1 Volumetric Carbonate Apparatus — consisting
of the following and assembled as in Fig. 2. 28.2.4 Magnesium Chloride Solution — 20 percent (m/m ).
a) Evolution or sample flask — round-bottom 28.2.5 Phenolphthalein Indicator — as in 6.1.1.
ring-neck flask of heat resistant glass, of 1 litre 28.2.6 Methyl Orange Indicator — as in 20.2.2(f).
capacity and provided with a two-hole rubber
28.2.7 Trichlorobenzene — 1 : 2 : 4 isomer, boiling
stopper;
point 213°C and relative density 1.47.
b) Dropping funnel — provided with a stopcock
and having stem long enough to reach into the 28.3 Procedure
lowest bulb of the condenser; 28.3.1 Weigh sufficient quantity of the sample into the
c) Conical flask — of heat-resistant glass, 300 ml sample flask to yield about 0.2 g of carbon dioxide. Add
capacity and provided with a one-hole rubber about 400 ml of unboiled water to which have been added
stopper; 2 ml of alkaline absorbent solution to prevent the loss of

F IG. 2 TYPICAL ASSEMBLY OF VOLUMETRIC CARBONATE FOR THE DETERMINATION OF C ARBONATES

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carbon dioxide. Heat the flask on a steam-bath until soap in water and filtered. The water soluble carbonates are
is dissolved and cool until the flask is only slightly warm estimated by absorbing carbon dioxide gas evolved by
to the hand. Add 30 ml of magnesium chloride solution reacting with the acid and expressed as sodium carbonate.
and a few glass beads to prevent bumping.
29.1 Apparatus
28.3.2 Pipette 25 ml of alkaline absorbent solution into
29.1.1 Volumetric Carbonate Apparatus — same as in
the conical flask and assemble the apparatus as shown in
Fig. 2.
Fig. 2. Start the water through the condenser. Apply suction
to the side tube to evacuate the system and reduce the 29.1.2 Glass Beads
pressure to 65 to 85 mm as indicated by the manometer.
29.2 Reagents
CAUTION : Maintain a properly reduced pressure and do not
allow air to enter the system at any time during the test. 29.2.1 Hydrochloric Acid — 0.5 N, accurately
28.3.3 Add dilute hydrochloric acid containing a few standardized.
drops of methyl orange indicator through the dropping 29.2.2 Dilute Hydrochloric Acid — 1 : 2 ( v/v).
funnel until the mixture in the flask is acidic (see Note).
29.2.3 Alkaline Absorbent Solution — same as
Avoid a large excess of acid. Add trichlorobenzene
in 28.2.3.
through the dropping funnel in the proportion of about
1 ml to every 2 g of the sample. 29.2.4 Magnesium Chloride Solution — 20 percent
NOTE — Shake the conical flask at frequent intervals from the (m/m).
time the acid is added until the sample flask and the condenser
29.2.5 Phenolphihalein Indicator — as in 6.1.1.
have been filled with water.

28.3.4 Place the small flame of a burner immediately 29.2.6 Methyl Orange Indicator — as in 20.2.2(f).
in contact with the bottom of the sample glass and heat 29.2.7 Trichlorobenzene — same as in 28.2.7.
continuously for 30 minutes. After this, discontinue
heating and pour boiled and cooled (carbon 29.3 Procedure
dioxidefree) water at 50°C through the condenser tube 29.3.1 Weigh accurately 2 to 10 g of the sample and
to fill the flask and the condenser to just below the side digest with 200 ml of freshly boiled ethyl alcohol in a
of the arm of the condenser. covered vessel on a steam-bath until the soap is dissolved.
28.3.5 Disconnect the conical flask, add one millilitre Filter into a filter flask through a counterpoised filter
of phenolphthalein indicator and titrate immediately paper neutral to phenolphthalein, or through a weighed
with 0.5 N hydrochloric acid with vigorous agitation Gooch or sintered crucible with suction, protecting the
until pink colour disappears. Add the acid drop by drop. solution from carbon dioxide and other acid fumes during
If it is not possible to titrate immediately, stopper the the operation by covering with a watch glass. Wash it
flask tightly to guard against entrance of air. several times with hot ethyl alcohol to remove all the
alcohol solubles. After filtering and washing the residue
28.3.6 Conduct a blank determination in order to thoroughly with hot ethyl alcohol, change the receiver,
establish the equivalent of the alkaline absorbent extract the residue with successive portions of water at
solution in terms of 0.5 N hydrochloric acid and also about 60°C and wash the residue thoroughly on the filter
to correct for any carbon dioxide in the reagents. paper or in the crucible.
28.4 Calculation 29.3.2 Then proceed as prescribed in 28.3.1 to 28.3.6.
Carbonate (as CO2), ( B − S ) × N × 2.2 29.4 Calculation
=
percent by mass M
Free carbonated alkali, ( B − S ) × N × 5.3
where as sodium carbonate, =
B = volume in ml of standard hydrochloric acid M
percent by mass
used in the blank,
S = volume in ml of standard hydrochloric acid where
used for the sample, B = volume in ml of standard hydrochloric acid
N = normality of standard hydrochloric acid, and used for the blank,
M = mass in g of the sample taken for the test. S = volume in ml of standard hydrochloric acid
29 DETERMINATION OF FREE CARBONATED used for the sample,
ALKALI N = normality of standard hydrochloric acid
used, and
29.0 General M = mass in g of the sample taken for the
The matter insoluble in alcohol in the soap is dissolved determination of matter insoluble in water.

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ANNEX A
(Clauses 24.3 and 25.3)
MUNSON AND WALKER TABLE FOR CALCULATING DEXTROSE, INVERT SUGAR ALONE,
INVERT SUGAR IN THE PRESENCE OF SUCROSE (0.4 g AND 2 g TOTAL SUGAR ), LACTOSE,
LACTOSE AND SUCROSE (2 MIXTURES) AND MALTOSE (CRYSTALLIZED)*
(APPLICABLE WHEN Cu2O IS WEIGHED DIRECTLY)
(Expressed in Milligrams)

Cuprous Dextrose Invert Invert Sugar Lactose Lactose and Maltose Cuprous
Oxide (D- Sugar and Sucrose Sucrose Oxide
(Cu2O) Glucose) (Cu2O)
0.4 2 1 1 Lac-
Grams Grams (C12H22O11+H2O) Lactose tose (C12H22O11+H2O)
Total Total 4 12
Sugar Sugar Sucrose Sucrose
10 4.0 4.5 1.6 … 6.3 6.1 … 6.2 10
12 4.9 5.4 2.5 … 7.5 7.3 … 7.9 12
14 5.7 6.3 3.4 … 8.8 8.5 … 9.5 14
16 6.6 7.2 4.3 … 10.0 9.7 … 11.2 16
18 7.5 8.1 5.2 … 11.3 10.9 … 12.9 18
20 8.3 8.9 6.1 12.5 12.1 … 14.6 20
22 9.2 9.8 7.0 … 13.8 13.3 … 16.2 22
24 10.0 10.7 7.9 … 15.0 14.5 … 17.9 24
26 10.9 11.6 8.8 … 16.3 15.8 … 19.6 26
28 11.8 12.5 9.7 … 17.6 17.0 … 21.2 28
30 12.6 13.4 10.7 4.3 18.8 18.2 … 22.9 30
32 13.5 14.3 11.6 5.2 20.1 19.4 … 24.6 32
34 14.3 15.2 12.5 6.1 21.4 20.7 … 26.2 34
36 15.2 16.1 13.4 7.0 22.8 22. … 27.9 36
38 16.1 16.9 14.3 7.9 24.2 23.3 … 29.6 38
40 16.9 17.8 15.2 8.8 25.5 24.7 … 31.3 40
42 17.8 18.7 16.1 9.7 26.9 26.0 … 32.9 42
44 18.7 19.6 17.0 10.7 28.3 27.3 … 34.6 44
46 19.6 20.5 17.9 11.6 29.6 28.6 … 36.3 46
48 20.4 21.4 18.8 12.5 31.0 30.0 … 37.9 48
*U.S. Bur. Standards Circ. 44, p. 139. The columns headed ‘Lactose’ and ‘Lactose and Sucrose’ were taken
from ‘Methods of Sugar Analysis and Allied Determinations’ by Arthur Given.
(Continued)

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MUNSON AND WALKER TABLE — (Continued)

(Expressed in Milligrams)

Cuprous Dextrose Invert Invert Sugar Lactose Lactose and Maltose Cuprous
Oxide (D- Sugar and Sucrose Sucrose Oxide
(Cu2O) Glucose) (Cu2O)
0.4 2 1 1 Lac-
Grams Grams (C12H22O11+H2O) Lactose tose (C12H22O11+H2O)
Total Total 4 12
Sugar Sugar Sucrose Sucrose
50 21.3 22.3 19.7 13.4 32.3 31.3 … 39.6 50
52 22.2 213.2 20.7 14.3 33.7 32.6 … 41.3 52
54 23.0 24.1 21.6 15.2 35.1 34.0 … 42.9 54
56 23.9 25.0 22.5 16.2 36.4 35.3 … 44.6 56
58 24.8 25.9 23.4 17.1 37.8 36.6 … 46.3 58
60 25.6 26.8 24.3 18.0 39.2 37.9 … 48.0 60
62 26.5 27.7 25.2 18.9 40.5 39.3 … 49.6 62
64 27.4 28.6 26.2 19.8 41.9 40.6 … 51.3 64
66 28.3 29.5 27.1 20.8 43.3 41.9 … 53.0 66
68 29.2 30.4 28.0 21.7 44.7 43.3 40.7 54.6 68
70 30.0 31.3 28.9 22.6 46.0 44.6 41.9 56.3 70
72 30.9 32.3 29.8 23.5 47.4 45.9 43.1 58.0 72
74 31.8 33.2 30.8 24.5 48.8 47.3 44.2 59.6 74
76 32.7 34.1 31.7 25.4 50.1 48.6 45.4 61.3 76
78 33.6 35.0 32.6 26.3 51.5 49.9 46.6 63.0 78
80 34.4 35.9 33.5 27.3 52.9 51.3 47.8 64.6 80
82 35.3 36.8 34.5 28.2 54.1 52.6 49.0 66.3 82
84 36.2 37.7 35.4 29.1 55.6 53.9 50.1 68.0 84
86 37.1 38.6 36.3 30.0 57.0 55.3 51.3 69.7 86
88 38.0 39.5 37.2 31.0 58.4 56.6 52.5 71.3 88
90 38.9 40.4 38.2 31.9 59.7 57.9 53.7 73.0 90
92 39.8 41.4 39.1 32.8 61.1 59.3 54.9 74.7 92
94 40.6 42.3 40.0 33.8 62.5 60.6 56.0 76.3 94
96 41.5 43.2 41.0 34.7 63.8 61.9 57.2 78.0 96
98 42.4 44.1 41.9 35.6 65.2 63.3 58.4 79.7 93
100 43.3 45.0 42.8 36.6 66.6 64.6 59.6 81.3 100
102 44.2 46.0 43.8 37.5 68.0 66.0 60.8 83.0 102
104 45.1 46.9 44.7 38.5 69.3 67.3 62.0 84.7 104
106 46.0 47.8 45.6 39.4 70.7 68.6 63.2 80.3 106
108 46.9 46.7 46.6 40.3 72.1 70.0 64.4 88.0 108
110 47.8 49.6 47.5 41.3 73.5 71.3 65.6 89.7 110
112 48.7 50.6 48.4 42.2 74.8 72.6 66.7 91.3 112
114 49.6 51.5 49.4 43.2 76.2 74.0 67.9 93.0 114
116 50.5 52.4 50.3 44.1 77.6 75.3 69.1 94.7 116
118 51.4 53.3 51.2 45.0 79.0 76.7 70.3 96.4 118
(Continued)

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MUNSON AND WALKER TABLE — (Continued)

(Expressed in Milligrams)

Cuprous Dextrose Invert Invert Sugar Lactose Lactose and Maltose Cuprous
Oxide (D- Sugar and Sucrose Sucrose Oxide
(Cu2O) Glucose) (Cu2O)
0.4 2 1 1 Lac-
Grams Grams (C12H22O11+H2O) Lactose tose (C12H22O11+H2O)
Total Total 4 12
Sugar Sugar Sucrose Sucrose
190 84.3 87.2 85.6 79.5 128.5 125.1 113.8 156.4 190
192 85.3 88.2 86.6 80.5 129.9 126.4 115.0 158.0 192
194 86.2 89.2 87.6 81.4 131.3 127.8 116.2 159 7 194
196 87.1 90.1 88.5 82.4 132.7 129.2 117.4 161.4 196
198 88.1 91.1 89.5 83.4 134.1 130.5 118.6 163.0 198
200 89.0 92.0 90.5 84.4 135.4 131.9 119.8 164.7 200
202 89.9 93.0 91.4 85.5 136.8 133.2 121.0 166.4 202
204 90.9 94.0 92.4 86.3 138.2 134.6 122.3 168.0 204
206 91.8 94.9 93.4 87.3 139.6 135 9 123.5 169.7 206
208 92.8 95.9 94.4 88.3 141.0 137.3 124.7 171.4 208
210 93.7 96.9 95.4 89.2 142.3 138.6 126.0 173.0 210
212 94.6 97.8 96.3 90.2 143.7 140.0 127.2 174.7 212
214 95.6 98.8 97.3 91.2 145.1 141.4 128.4 176.4 214
216 96.5 99.8 98.3 92.2 146.5 142.7 129.6 178.0 216
218 97.5 100.8 99.3 93.2 147.9 144.1 130.9 179.7 218
220 98.4 101.7 100.3 94.2 149.3 145.4 132.1 181.4 220
222 99.4 102.7 101.2 95.1 105.7 146.8 133.3 183.0 222
224 100.3 103.7 102.2 96.1 152.0 148.1 134.5 184.7 224
226 101.3 104.6 103.2 97.1 153.4 149.5 135.8 186.4 226
228 102.2 105.6 104.2 98.1 154.8 150.8 137.0 188.0 228
230 103.2 106.6 105.2 99.1 156.2 152.2 138.2 189.7 230
232 104.1 107.6 106.2 100.1 157.6 153.6 139.4 191.3 232
234 105.1 108.6 107.2 101.1 159.0 154.9 140.7 193.0 234
236 106.0 109.5 108.2 102.1 160.3 156.3 141.9 194.7 236
238 107.0 110.5 109.2 103.1 161.7 157.6 143.2 196.3 238
240 108.0 111.5 110.1 104.0 163.1 159.0 144.4 198.0 240
242 108.9 112.5 111.1 105.0 164.5 160.3 145.6 199.7 242
244 109.9 113.5 112.1 106.0 165.9 161.7 146.9 201.3 244
246 110.8 114.5 113.1 107.0 167.3 163.1 148.1 203.0 246
248 111.8 115.4 114.1 108.0 168.7 164.4 149.3 204.7 248
250 112.8 116.4 115.1 109.0 170.1 165.8 150.6 206.3 250
252 113.7 117.4 116.1 110.0 171.5 167.2 151.8 208.0 252
254 114.7 118.4 117.1 111.0 172.8 168.5 153.1 209.7 254
256 115.7 119.4 118.1 112.0 174.2 169.9 154.3 211.3 256
258 116.6 120.4 119.1 113.0 175.6 171.3 155.5 213.0 258
(Continued)

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MUNSON AND WALKER TABLE — (Continued)

(Expressed in Milligrams)

Cuprous Dextrose Invert Invert Sugar and Lactose Lactose and Maltose Cuprous
Oxide (D- Sugar Sucrose Sucrose Oxide
(Cu2O) Glucose) (Cu2O)
0.4 2 1 Lactose 1 Lac-
Grams Grams (C12H22O11+H2O) 4 Sucrose tose (C12H22O11+H2O)
Total Total 12
Sugar Sugar Sucrose
260 117.6 121.4 120.1 114.0 177.0 172.6 156.8 214.7 260
262 118.6 122.4 121.1 115.0 178.4 174.0 158.0 216.3 262
264 119.5 123.4 122.1 116.0 179.8 175.3 159.3 218.0 294
266 120.5 124.4 123.1 117.0 181.2 176.7 160.5 219.7 266
268 121.5 125.4 124.1 118.0 182.6 178.1 161.8 221.3 268
270 122.5 126.4 125.4 119.0 184.0 179.4 163.0 223.0 270
272 123.4 127.4 126.2 120.0 185.3 180.8 164.3 224.6 272
274 124.4 128.4 127.2 121.1 186.7 182.2 165.5 226.3 274
276 125.4 129.4 128.2 122.1 188.1 183.5 166.81 228.0 276
278 126.4 130.4 129.2 123.1 189.5 184.9 168.0 229.6 278
280 127.3 131.4 130.2 124.1 190.9 186.3 169.3 231.3 280
282 128.3 132.4 131.2 125.1 192.3 187.6 170.5 233.0 282
284 129.3 133.4 132.2 126.1 193.7 189.0 171.8 234.6 284
286 130.3 134.4 133.2 127.1 195.1 190.4 173.0 236.3 286
288 131.3 135.4 134.3 128.1 196.5 191.7 174.3 238.0 288
290 132.3 136.4 135.3 129.2 197.8 193.1 175.5 239.6 290
292 133.2 137.4 136.3 130.2 199.2 194.4 176.8 241.3 292
294 134.2 138.4 137.3 131.2 200.6 195.8 178.1 242.9 294
296 135.2 139.4 138.3 132.2 202.0 197.2 179.3 244.6 296
298 136.2 140.5 139.4 133.2 203.4 198.6 180.6 246.3 298
300 137.2 141.5 140.4 134.2 204.8 199.9 181.8 247.9 300
302 138.2 142.5 141.4 135.3 206.2 201.3 183.1 249.6 302
304 139.2 143.5 142.4 136.3 207.6 202.7 184.4 251.3 304
306 140.2 144.5 143.4 137.3 209.0 204.0 185.6 252.9 306
308 141.2 145.5 144.5 138.3 210.4 205.4 186.9 254.6 308
310 142.2 146.6 145.5 139.4 211.8 206.8 188.1 256 3 310
312 143.2 147.6 146.5 140.4 213.2 208.1 189.4 257.9 312
314 144.2 148.6 147.6 141.4 214.6 209.5 190.7 259.6 314
316 145.2 149.6 148.6 142.4 216.0 210.9 191.9 261.2 316
318 146.2 150.7 149.6 143.5 217.3 212.2 193.2 262.9 318
320 147.2 151.7 150.7 144.5 218.7 213.6 194.4 264.6 320
322 148.2 152.7 151.7 145.5 220.1 215.0 195.7 266.2 322
324 149.2 153.7 152.7 146.6 221.5 216.4 197.0 267.9 324
326 150.2 154.8 153.8 147.6 222.9 217.7 198.2 269.6 326
328 151.2 155.8 154.8 148.6 224.3 219.1 199.5 271.2 328

(Continued)

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IS 286 : 2018

MUNSON AND WALKER TABLE — (Continued)

(Expressed in Milligrams)

Cuprous Dextrose Invert Invert Sugar Lactose Lactose and Maltose Cuprous
Oxide (D- Sugar and Sucrose Sucrose Oxide
(Cu2O) Glucose) (Cu2O)
0.4 2 1 1 Lac-
Grams Grams (C12H22O11+H2O) Lactose tose (C12H22O11+H2O)
Total Total 4 12
Sugar Sugar Sucrose Sucrose
330 152.2 156.8 155.8 149.7 225.7 220.5 200.8 272.9 330
332 153.2 157.9 156 9 150.7 227.1 221.8 202.0 274.6 332
334 154.2 158.9 157.9 151.7 228.5 223.2 203.3 276.2 334
336 155.2 159.9 159.0 152.8 229.9 224.6 204.6 277.9 336
338 156.3 161.0 160.0 153.8 231.3 226.0 205.9 279.5 338
340 157.3 162.0 161.0 154.8 232.7 227.4 207.1 281.2 340
342 158.3 163.1 162.1 155.9 234.1 228.7 208.4 282.9 342
344 159.3 164.1 163.1 156.9 235.5 230.1 209.7 284.5 344
346 160.3 165.1 164.2 158.0 236.9 231.5 211.0 286.2 346
348 161.4 166.2 165.2 159.0 238.3 232.9 212.2 287.9 348
350 162.4 167.2 166.3 160.1 239.7 234.3 213.5 289.5 350
352 163.4 168.3 167.3 161.1 241.1 235.6 214.8 291.2 352
354 164.4 169.3 168.4 162.2 242.5 237.0 216.1 292.8 354
356 165.4 170.4 169.4 163.2 243.9 238.4 217.3 294.5 356
358 166.5 171.4 170.5 164.3 245.3 239.8 218 6 296.2 358
360 167.5 172.5 171.5 165.3 246.7 241.2 219.9 297.8 360
362 168.5 173.5 172 6 166.4 248.1 242.5 221.2 299.5 362
364 169.6 174.6 173.7 167.4 249.5 243.9 222.5 301.2 364
366 170.6 175.6 174.7 168.5 250 9 245.3 223.7 302.8 366
368 171.6 176.7 175.8 169.5 252.3 246.7 225.0 304.5 368
370 172.7 177.7 176.8 170.6 253.7 248.1 226.3 306.1 370
372 173.7 178 8 177.9 171.6 255.1 249.5 227.6 307.8 372
374 174.7 179.8 179 0 172.7 256.5 250.9 228.9 309.5 374
376 175.8 180.9 180.0 173.7 257.9 252.2 230.2 311.1 376
378 176.8 182.0 181.1 174.8 259.3 253.6 231.5 312.8 378
380 177.9 183.0 182.1 175.9 260.7 255.0 232.8 314.5 380
382 178.9 184.1 183.2 176.9 262.1 256.4 234.1 316 1 382
384 180.0 185.2 184.3 178.0 263 5 257.8 235.4 317.8 384
386 181.0 186.2 185.4 179.1 264.9 259.2 236.6 319.4 386
388 182.0 187.3 186.4 180.1 266.5 260.5 237.9 321.1 388
390 183.1 188.4 187.5 181.2 267.7 261.9 239.2 322.8 390
392 184.1 189.4 188.6 182.3 269.1 263.3 240.5 324.4 392
394 185.2 190.5 189.7 183 3 270.5 264.7 241.8 326.1 394
396 186.2 191.6 190.7 184.4 271.9 266.1 243.1 327.7 396
398 187.3 192.7 191.8 185.5 273.3 267.5 244.4 329.4 398
(Continued)

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IS 286 : 2018

MUNSON AND WALKER TABLE — (Continued)

(Expressed in Milligrams)

Cuprous Dextrose Invert Invert Sugar Lactose Lactose and Maltose Cuprous
Oxide (D- Sugar and Sucrose Sucrose Oxide
(Cu2O) Glucose) (Cu2O)
0.4 2 1 1 Lac-
Grams Grams (C12H22O11+H2O) Lactose tose (C12H22O11+H2O)
Total Total 4 12
Sugar Sugar Sucrose Sucrose
400 188.4 193.7 192.9 186.5 274.7 268.9 245.7 331.1 400
402 189.4 194.8 194.0 187.6 276.1 270.3 247.0 332.7 402
404 190.5 195.9 195.0 188.7 277.5 271.7 248.3 334.4 404
406 191.5 197.0 196.1 189.8 278.9 273.0 249.6 336.0 406
408 192.6 198.1 197.2 190.8 280.3 274.4 251.0 337.7 408
410 193.7 199.1 198.3 191.9 281.7 275.8 252.3 339.4 410
412 194.7 200.2 199.4 193.0 283.2 277.2 253.6 341.0 412
414 195.8 201.3 200.5 194.1 284.6 278.6 254.9 342.7 414
416 196.8 202.4 201.6 195.2 286.0 280.0 256.2 344.4 416
418 197.9 203.5 202.6 196.2 287.4 281.4 257.5 346.0 418
420 199.0 204.6 203.7 197.3 288.8 282.8 258.8 347.7 420
422 200.1 205.7 204.8 198.4 290.2 284.2 260.1 349.3 422
424 201.1 206.7 205.9 199.5 291.6 285.6 261.4 351.0 424
426 202.2 207.8 207.0 200.6 293.0 287.0 262.7 352.7 426
428 203.3 208.9 208.1 201.7 294.4 288.4 264.0 354.3 428
430 204.4 210.0 209.2 202.7 295.8 289.8 265.4 356.0 430
432 205.5 211.1 210.3 203.8 297.2 291.2 266.6 357.6 432
434 206.5 212.2 211.4 204.9 298.6 292.6 268.0 359.3 434
430 207.6 213.3 212.5 206.0 300.0 294.0 269.3 361.0 436
438 208.7 214.4 213.6 207.1 301.4 295.4 270.6 362.6 438
440 209.8 215.5 214.7 208.2 302.8 296.8 272.0 364.3 440
442 210.9 216.6 215.8 209.3 304.2 298.2 273.3 365.9 442
444 212.0 217.8 216.9 210.4 305.6 299.6 274.6 367.6 444
446 213.1 218.9 218.0 211.5 307.0 301.0 275.9 369.3 446
448 214.1 220.0 219.1 212.6 308.4 302.4 277.2 370.9 448
450 215.2 221.1 220.2 213.7 309.9 303.8 278.6 372.6 450
452 216.3 222.2 221.4 214.8 311.3 305.2 279.9 374.2 452
454 217.4 223.3 222.5 215.9 312.7 306.6 281.2 375.9 454
456 218.5 224.4 223.6 217.0 314.1 308.0 282.5 377.6 456
458 219.6 225.5 224.7 218.1 315.5 309.4 283.9 379.2 458
460 220.7 226.7 225.8 219.2 316.9 310.8 285.2 380.9 460
462 221.8 227.8 226.9 220.3 318.3 312.2 286.5 382.5 462
464 222.9 228.9 228.1 221.4 319.7 313.6 287.8 384.2 464
466 224.0 230.0 229.2 222.5 321.1 315.0 289.2 385.9 466
468 225.1 231.2 230.3 223.7 322.5 316.4 290.5 387.5 468
(Continued)

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IS 286 : 2018

MUNSON AND WALKER TABLE — (Concluded)

(Expressed in Milligrams)

Cuprous Dextrose Invert Invert Sugar Lactose Lactose and Maltose Cuprous
Oxide (D- Sugar and Sucrose Sucrose Oxide
(Cu2O) Glucose) (Cu2O)
0.4 2 1 1 Lac-
Grams Grams (C12H22O11+H2O) Lactose tose (C H O +H O)
12 22 11 2
Total Total 4 12
Sugar Sugar Sucrose Sucrose
470 226.2 232.3 231.4 224.8 323.9 317.7 291.8 389.2 470
472 227.4 233.4 232.5 225.9 325.3 319.1 293.2 390.8 472
474 228.3 234.5 233.7 227.0 326.8 320.5 294.5 392.5 474
476 229.6 235.7 234.8 228.1 328.2 321.9 295.8 394.2 476
478 230.7 236.8 235.9 229.2 329.6 323.3 297.1 395.8 478
480 231.8 237.9 237.1 230.3 331.0 324.7 298.5 397.5 480
482 232.9 239.1 238.2 231.5 332.4 326.1 299.8 399.1 482
484 234.1 240.2 239.3 232.6 333.8 327.5 301.1 400.8 484
486 235.2 241.4 240.5 233.7 335.2 328.9 302.5 402.4 486
488 236.3 242.5 241.6 234.8 336.6 330.3 303.8 404.1 488
490 237.4 243.6 242.7 236.0 338.0 331.7 305.1 403.8 490

ANNEX B
(Clause 2)
LIST OF REFERRED INDIAN STANDARDS

IS No. Title IS No. Title

170 : 2004 Acetone — Specification (fourth 323 : 2009 Rectified spirit for industrial use
revision) — Specification (second revision)
264 : 2005 Nitric acid — Specification (third 336 : 1973 Specification for ether (second
revision). revision)
265 : 1993 Hydrochloric acid — Specification 1070 : 1992 Reagent grade water (third
(fourth revision) revision)
266 : 1993 Sulphuric acid — Specification 1796 : 1977 Specification for glycerine
(third revision) (second revision)
321 : 1964 Specification for absolute alcohol 7597 : 2001 Surface active agents — Glossary
(revised) of terms (first revision)

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IS 286 : 2018

ANNEX C
(Foreword)
COMMITTEE COMPOSITION
Soaps and Other Surface Active Agents Sectional Committee, CHD 25

Organization Representative(s)
Drugs Controller General of India, New Delhi DR G. N. SINGH (Chairman)
SHRI S. DEY (Alternate)
Association for Consumer’s Action on Safety and Health, Mumbai DR YOGESH KAMDAR
SHRI SATYADEV PANDEY (Alternate)
Central Pollution Control Board, Delhi DR M. Q. ANSARI
DR REKHA L. SITASAWAD (Alternate)
Central Revenue Control Laboratory, New Delhi SHRI Y. K. S. RATHORE
SHRI S. C. MATHUR (Alternate)
Colgate-Palmolive (India) Ltd, Mumbai DR SHASHANK POTNIS
SHRI VILAS TULLE (Alternate)
Consumer Education & Research Centre, Ahmedabad MS ANINDITA MEHTA
MS DOLLY S. JANI (Alternate)
Consumer Guidance Society of India, Mumbai DR SITARAM DIXIT
SRI B. V. DESAI (Alternate)
Department of Industrial Policy and Promotion, New Delhi SHRI NAND LAL
Directorate General of Health Services, New Delhi NOMINATION AWAITED
Directorate General of Supplies & Disposals, New Delhi SRI N. K. KAUSHAL
A. K. M. KASHYAP (Alternate)
FASSSDMI, Delhi SHRI SANTOSH KUMAR
SHRI ASEEM GALHOTRA (Alternate)
Godrej Consumers Products Limited, Mumbai SHRI JIMMY DORDI
DR N. M. SUNDER (Alternate)
Harcourt Butler Technological Institute, Kanpur PROF RAKESH TRIVEDI
DR V. K. TYAGI (Alternate)
Hindustan Unilever Limited, Mumbai/Bangalore DR A. SIVAKUMAR
MS VRINDA RAJWADE (Alternate)
ITC Limited, Bangalore DR V. KRISHNAN
DR SURESH RAMAMURTHI (Alternate)
K. S. Krishnan Associates (P) Ltd, Noida SHRI S. KRISHNAN
SHRI KRISHNA MURTHY (Alternate)
Khadi & Village Industries Commission, Mumbai SHRI GULAM HUSSAIN
Ministry of Defence (DGQA), Kanpur SHRI A. K. SHUKLA
SHRI L. THARACHAND (Alternate)
Ministry of Micro Small & Medium Enterprises (MSME), SHRI H. S. BISHT
New Delhi
National Test House, Ghaziabad SHRI M. CHAKRABORTY
DR (SMT) MADHURIMA MISRA (Alternate)
Nirma Limited, Ahmedabad SHRI H. K. PATEL
SHRI ASHISH K. DESAI (Alternate)
Oil Technologist Association of India, Mumbai SHRI ASHOK MAHINDRU
SHRI H. P. SAXENA (Alternate)
Procter & Gamble India, Mumbai MS PRIYANKA BHAT
SHRI GAURAV NANDRAJOG (Alternate)
Voluntary Organization in Interest of Consumer Education (VOICE), SRI M. A. U. KHAN
New Delhi SHRI B. K. MUKHOPADH (Alternate)
In personal capacity (8/308, Rajendra Nagar, Sector 3, Sahibabad SHRI M. MITRA (EX DGQS)
Ghaziabad)
BIS Directorate General DR RAJIV K. JHA Scientist ‘F’ and Head (Chemical)
[Representing Director General (ex-officio)]

Member Secretary
SHRI T. ARIVUDAIYANAMBI
Scientist ‘E’ (Chemical), BIS

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