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IS/ISO 1066 (1975): Analysis of Soaps - Determination of

Glycerol Content - Titrimetric Method [CHD 25: Chemical]

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IS/ISO 1066 : 1975

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Indian Standard
ANALYSIS OF SOAPS DETERMINATION OF
GLYCEROL CONTENT TITRIMETRIC METHOD

ICS 71.100.40

BIS 2013

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
January 2013

Price Group 2

Soaps and Other Surface Active Agents Sectional Committee, CHD 25

NATIONAL FOREWORD
This Indian Standard which is identical with ISO 1066 : 1975 Analysis of soaps Determination of
glycerol content Titrimetric method issued by the International Organization for Standardization (ISO)
was adopted by the Bureau of Indian Standards on the recommendation of the Soaps and Other Surface
Active Agents Sectional Committee and approval of the Chemical Division Council.
The text of ISO Standard has been approved as suitable for publication as an Indian Standard without
deviations. Certain conventions are, however, not identical to those used in Indian Standards. Attention is
particularly drawn to the following:
a) Wherever the words International Standard appear referring to this standard, they should be read
as Indian Standard.
b) Comma (,) has been used as a decimal marker while in Indian Standards, the current practice is
to use a point (.) as the decimal marker.
In this adopted standard, reference appears certain International Standards for which Indian Standards
also exist. The corresponding Indian Standards which are to be substituted in their respective places are
listed below along with their degree of equivalence for the editions indicated:
International Standard

Corresponding Indian Standard

1)

ISO/R 385 Laboratory glassware

Burettes
ISO/R 6482) Laboratory glassware
Single volume pipettes
ISO/R 10423) Laboratory glassware
one-mark volumetric flasks

IS 1997 : 2008 Laboratory glassware

Burettes (third revision)
IS 1117 : 1975 Specification for onemark pipettes (first revision)
IS 915 : 2006 One-mark volumetric
flasks Specification (second
revision)
4)
ISO/R 1773 Laboratory glassware IS 1381 (Part 1) : 2003 Laboratory
Narrow-necked boiling flasks
glassware Narrow-necked boiling
flasks (second revision)

Degree of Equivalence
Identical
Technically
Equivalent
do

Identical

The technical committee has reviewed the provisions of the following International Standards referred
in this adopted standard and has decided that they are acceptable for use in conjunction with this
standard:
International Standard
ISO 2272 : 1989
ISO 607 : 1980

Title
Surface active agents Soaps Determination of low contents of free
glycerol by molecular absorption spectrometry
Surface active agents and detergents Methods of sample division

The applicable standard atmospheric conditions (SAC) for Indian conditions are 27 2C and
65 5 percent relative humidity and shall be observed while using this Indian Standard.
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).

1)
2)
3)
4)

Since
Since
Since
Since

published
published
published
published

as
as
as
as

ISO 385 : 2005.

ISO 648 : 2008.
1042 : 1998.
ISO 1773 : 1997.

INTERNATIONAL

ISO 10664975
(E)
IS/ISO
1066 : 1975

STANDARD

Indian Standard
ANALYSIS OF SOAPS DETERMINATION OF
GLYCEROL CONTENT TITRIMETRIC METHOD
Analysis of soaps - Determination of glycerol content Titrimetric method
1 SCOPE
This International
Standard specifies a titrimetric
method
for the determination
of the glycerol content of commercial
soaps, excluding compounded products.
2

FIEL0

Sodium hydroxide,

2 N Solution.

5.6

Sodium hydroxide,

0,05 N Solution.

5.7 Sodium
hydroxide,
Solution, carbonate free.

REFERENCES

ISO 2272, Surface active agents - Analysis

Determination
of low contents
of free
Spec tropho tome tric me thod.

of soaps glycerol
-

5.8

volumetric

Sodium Periodate Solution, prepared as follows

PRINCIPLE

of the soap with sulphuric

acid, and
Decomposition
extraction
of the fatty
acids with light Petroleum.
Oxidation of the glycerol by periodic acid to formic acid
and titration
of the formic
acid
and formaldehyde,
produced, using a pH meter.
REAGENTS

The reagents used shall be of recognized

and shall have the following properties.

analytical

purity

5.1 Distilled water, from which carbon dioxide has been

removed by boiling for 15 min and cooling in a vessel
protected from atmospheric carbon dioxide.
5.2

Light Petroleum,

5.3

1,2-Ethanediol,

5.4

Sulphuric

1)

For a glycerol

2)

In preparation.

boiling

range between 40 and 60 C.

50 % (V/V)

acid, approximately

content

Dissolve, at room temperature,

60 + 0,5 g of sodium
Periodate (NalOJ,
minimum
purity 99,8 %, in distilled
water containing 120 ml of approximately
0,l N sulphuric
acid Solution. Dilute to 1 1.
If the Solution is turbid, filter it through a glass filter
of porosity 16 to 40 Pm, and place it in a brown glass
bottle, which should be kept stoppered and in the dark.

Ordinary

Standard

6 APPARATUS

ISO . . . , Soaps - Sampling. 2)

4

0,125 N

OF APPLICATION

This method is applicable to soaps with glycerol contents

equal to or greater than 0,5 % (m/m)l ). This method is not
applicable in the presence of organic compounds containing
more than two hydroxyl groups on adjacent carbon atoms.
3

5.5

laboratory

apparatus, and in particular

6.1

Beakers, capacity 250 and 600 ml.

6.2

Separating funnels, capacity 250 ml.

6.3 One-mark
volumetric
flasks,
capacity
250 ml,
complying with the requirements of class A of ISO/R 1042.
6.4 Burette,
capacity
50 ml,
complying
with
the
requirements of class A of ISO/R 385. The drainage time
shall be not less than 90 s for 50 ml.
6.5 Fiat-bottomed
500 mI, complying

or round-bottomed
with the requirements

flask, capacity
of lSO/R 1773.

6.6 Pipette,
capacity
50 ml,
complying
with
the
requirements
of class A of ISO/R 648, with a stated
drainage time in Order to ensure delivery of a constant
volume.

aqueous Solution.
6.7 Variable-Speed
paddles.

7 N Solution.

of less than 0,5 % (m/m),

the method

specified

in ISO 2272

should

stirrer (preferably

magnetic)

with glass

be used.

ISO1066-1975(E)
IS/ISO 1066 : 1975

6.8

pH meter fitted

with

The pH meter shall be calibrated

buffer solutions :
-

potassium

hydrogen

[c,H,(COOK)(COOW],

8.4

a glass electrode.
by means of two Standard

phthalate
0,05 M

Solution,

pH 4,00

at 20 OC;
disodium tetraborate
decahydrate
[Na2Bq07.10H20],
0,Ol M Solution,

pH 9,22

8.1

according

PROCEDURE

IO g of the laboratory

Blank test

Decomposition

under the same conditions

as the test
soap, with 100 ml of the water (5.1).
2 O,l, as specified
in 8.5, but carry
to pH 6,5 + 0,l.

of soap and removal

of fatty

50

12 to 16

75

8to

12

100

6to

150

4to

200
250

Draw off the aqueous layer into a third separating funnel,

extract
it a third time with 50 ml of the Iight Petroleum,
Shake, and allow to settle. Draw off the aqueous layer into
a 250 ml one-mark volumetric
flask (6.3).
Combine
the ethereal extracts and wash them
time with about 50 ml of the water.

twice,

each

Combine the washings with the acid Solution in the 250 ml

one-mark volumetric
flask and dilute to the mark with the
water (5.1).

A naked

flame

must not be used for heating

If the amount
is less than
taken
for determination
recommended,
the results obtained
will be too high and
If the amount
taken for determination
is
lack precision.
greater than that recommended,
the results obtained will be
low. If the result obtained does not fall within the expected
range, as set out in the table, repeat the determination
on
another
al iquot Portion.
For glycerol
contents
less than
2,5 % (m/m),
reduce the volume of the sodium Periodate
Solution to 25 ml.
8.5

acids

Add about
IO ml of the sulphuric
acid Solution
(5.4),
Shake, and allow to cool. After cooling, add about 100 ml
of the light Petroleum
(5.2), Shake, and allow the layers to
separate.
Draw
off
the aqueous
layer into a second
separating funnel, extract it again with about 50 ml of the
light Petroleum,
Shake and allow to settle.

2
2

16 to 20

Test Portion

Dissolve the test Portion in 100 ml of the hot water (5.1).

When dissolution
is complete,
transfer quantitatively
into a
separating
funnel
(6.2), rinsing the beaker with a little of
the water.

1)

ml

iess than 4

Carry out a blank test

itself, without
adding
Adjust the pH to 8,l
out the final titration
8.3

to be taken for determination

at 20 C.

% (m/m)

Weigh, to the nearest 0,Ol g, about

Sample into a 250 ml beaker (6.1).
8.2

Portion

The best conditions

for the determination
of glycerol using
50 ml of the sodium Periodate Solution (5.8) are obtained
when the aliquot Portion on which the test is to be carried
out contains between 0,3 and 0,5 g of glycerol. The volume
of the aliquot
Portion
be taken for the determination
is
shown in the following
table :

SAMPLING

Laboratory
samples shall be prepared and stored
to the procedures specified in ISO . . .

Aliquot

Determination

Introduce
the aliquot Portion to be tested into the 500 ml
flask
(6.5).
Boill)
the Solution
gently
for
5 min to
expel any carbon dioxide
and light Petroleum
that may
be present.
Allow to cool with a carbon dioxide
trap in
Transfer
the al iquot
Portion
the neck of the flask.
quantitatively
into a 600 ml beaker (6.1). If the volume
of liquid
in the beaker is too small to permit
adequate
stirring,
add a sufficient
quantity
of the water
(5.1).
lf the pH of the Solution
is less than 3, insert the glass
electrode
(6.8) and Start the stirrer (6.7). Add, drop by
drop, the 2 N sodium hydroxide
Solution (5.5) until the pH
is 3, then add, drop by drop, the 0,05 N sodium hydroxide
Solution (5.6) until the pH is 8,l f. 0,l.
Pipette
exactly
50 ml (or 25 ml, as appropriate)
of the
sodium Periodate Solution (5.8) into the Solution.
Mix the
Solution
thoroughly
with the aid of the stirrer, cover the
flask with a watch-glass and.leave for 30 min in the dark at
room
temperature
(below 35 C).
When
30 min
have
elapsed, add IO ml sf the 1,2-ethanediol
Solution (5.3) and
mix weil. Cover again with the watch-glass
and leave for
20 min in the dark at room temperature
(below 35 C).

because of the risk of combustion

of flammable

ISO 10664975 (El

IS/ISO 1066 : 1975

Then titrate,
using the pH meter (6.8), with the 0,125
sodium hydroxide
Solution (5.7) until a pH of 8,l + 0,l
reached. Note the volume used, to the nearest 0,05 ml.

EXPRESSION
Method

9.1

N
is

OF RESULTS

9.2

Repeatability

The maximum
differente
between
the results
of two
determinations
carried
out simultaneously
or in rapid
succession
by the same analyst,
in tests carried
out by
23 laboratories
on a Sample containing
2,7 % (m/m)
of
glycerol, was 0,04 %.

of calculation
9.3

The glycerol
the formula

content,

0,092 1 x(V,

is given,

as a percentage

- V*) XTX-x

-- 2302xTx(V,
V. xm

250
Vo

The maximum
differente
between the results of two tests
in different
laboratories
on the Sample containing
2,7 %
(m/m) of glycerol, in tests carried out by 23 laboratories,
was 0,2 %.

100
m

- V2)
10

in millilitres,
VO is the volume,
taken for the determination;

of the aliquot

Portion
I

VI is the volume,
hydroxide
Solution

in millilitres,
of the 0,125 N sodium
(5.7) used for the determination;

V2 is the volume,
hydroxide
Solution

in millilitres,
of the 0,125 N sodium
(5.7) used in the blank test;

T is the exact
hydroxide
Solution

normality
(5.7);

Reproducibility

by mass, by

of

the

0,125

is the mass, in grams, of the test Portion.

sodium

TEST

REPORT

The test report

shall include

the following

in formation
necess ary
a) all
iden tificati on of the Sample;
b)

the method

c)

the results obtained;

d)

the test conditions;

for

particulars
the

:
complete

used;

details
not
specified
in this
e) any
operational
International
Standard
or optional,
as weil
as all
incidents likely to have influenced
the results.

Bureau of Indian Standards

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harmonious development of the activities of standardization, marking and quality certification of goods
and attending to connected matters in the country.
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Enquiries relating to copyright be addressed to the Director (Publications), BIS.
Review of Indian Standards
Amendments are issued to standards as the need arises on the basis of comments. Standards are also
reviewed periodically; a standard along with amendments is reaffirmed when such review indicates that
no changes are needed; if the review indicates that changes are needed, it is taken up for revision. Users
of Indian Standards should ascertain that they are in possession of the latest amendments or edition by
referring to the latest issue of BIS Catalogue and Standards: Monthly Additions.
This Indian Standard has been developed from Doc No.: CHD 25 (1699).
Amendments Issued Since Publication
______________________________________________________________________________________
Amendment No.
Date of Issue
Text Affected
______________________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
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