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IS 354-2 (1986): Methods of sampling and test for resins

for paints, Part 2: Special test methods for alkyd resins
[CHD 20: Paints, Varnishes and Related Products]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

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है”
ह
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“Knowledge is such a treasure which cannot be stolen”
 IS : 354 (PART 2) - 1986
Reaffirmed - 2012

Indian Standard
METHODS OF
SAMPLING AND TEST FOR
RESINS FOR PAINTS
PART 2 SPECIALTEST METHODS FOR ALKYD RESINS

( Second Revision )
Second Reprint OCTOBER 2000

UDC 667 621 633 [ 678 674 ] : 620 1

© Copyright 1987

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

Gr 5 February 1987
 AMENDMENT NO. 4 JUNE 2000
TO
IS 354 ( PART 2 ) : 1986 METHODS OF SAMPLING AND
TEST FOR RESINS FOR PAINTS
PART 2 SPECIAL TEST METHODS FOR ALKYD RESINS
( Second Revision )

( Page 13, clause 11.3, line 18 ) — Substitute '(see Notes)' for '(see Note)'.
( Page 13, clause 11.3, Note ) — Substitute the following for the existing:
'NOTES
1 The precipitate is alcoholate and alcohol of crystallization may be driven off on prolonged
heating. However, it is safe to dry up to 60°C for one hour.
2 For pigmented composition, separation of pigment and varnish may be done as per IS 101
(Part 8/Sec 2)‡and volatile matter may be determined as per IS 101 (Part 2/Sec 2)§ before
proceeding further for determination of phthalic anhydride.'

‡Methods of sampling and test for paints, varnishes and related products : Part 8 Tests for pigments
and other solids, Section 2 Pigments and non-volatile matter ( third revision ).

§Methods of sampling and test for paints, varnishes and related products: Part 2 Test on liquid paints
(chemical examination): Section 1 Water content ( third revision ).

( CHD 21 )
Printed at New India Printing Press, Khurja, India
 AMENDMENT NO. 3 OCTOBER 1992
TO
IS 354 ( Part 2 ) : 1986 METHODS OF SAMPLING AND
TEST FOR RESINS FOR PAINTS
PART 2 SPECIAL TEST METHODS FOR ALKYD RESINS
( Second Revision )
( Page 13, clause 11.3, line 10 ) — Insert the words 'followed by an ice
bath' after the words 'running water'.

( CHD 021 )
Printed at New India Printing Press, Khurja, India
 AMENDMENT NO. 2 NOVEMBER 1991
TO
IS 354 ( Part 2 ) : 1986 METHODS OF SAMPLING AND
TEST FOR RESINS FOR PAINTS
PART 2 SPECIAL TEST METHOD FOR ALKYD RESINS
( Second Revision )

( Page 4, clause 4.1, line 2 ) — Substitute 'phenol' for 'phenolphthalein'.

( CHD 021 )

Printed at New India Printing Press, Khurja, India

 AMENDMENT NO. 1 SEPTEMBER 1989
TO
IS : 354 (Part 2) -1986 METHODS OF SAMPLING AND
TEST FOR RESINS FOR PAINTS
PART 2 SPECIAL TEST METHODS FOR ALKYD RESINS
(Second Revision)

(Page 3, clause 0.2, line 7) — Delete the words 'chlorinated rubber'.

(Page 3, clause 0.2, last line) — Delete 'Part 8'.

(CDC 50)

Printed at New India Printing Press, Khurja, India

 IS : 354 ( Part 2 ) - 1986

Indian Standard
METHODS OF
SAMPLING AND TEST FOR
RESINS FOR PAINTS
PART 2 SPECIAL TEST METHODS FOR ALKYD RESINS

( Second Revision )
Raw Materials for Paints Industry Sectional Committee, CDC 50
Chairman Representing
SHRI R. K. MARPHATIA Goodlass Nerolac Paints Ltd, Bombay
Members
S H R I S. S. A N A K A I K A R ( Alternate to
Shri R. K. Marphatia )
SHRI K. M. BANERJEE National Test House, Calcutta
S H R I S. BHATTACHARYYA IEL Ltd, Calcutta
S H R I G. N. T I W A R I ( Alternate )
CHEMIST & METALLURGIST-I Research, Design and Standards Organization
( Ministry of Railways ), Lucknow
ASSISTANT R E S E A R C H O F F I C E R
( CM-II ) ( Alternate )
S H R I M. C. CHOKSI Resins & Plastics Pvt Ltd, Bombay
SHRI O. P. DHAMIJA Export Inspection Council of India, Calcutta
S H R I S. N . D U T T A ( Alternate )
DR A. B. KARNIK Colour-Chem Ltd, Bombay
S H R I M . E. M A R A T H E ( Alternate )
SHRI R. D. KAWATRA Directorate General of Technical Development,
New Delhi
S H R I K U L T A R S I N G H ( Alternate )
SHRI P. R. MALHAN Development Commissioner ( SSI ) ( Ministry of
Industry ), New Delhi
S H R I R . M U K O P A D H Y A Y ( Alternate )
SHRI K. C. M E H T A Indian Oil Corporation Ltd, Faridabad
SHRI B. RAMA M U R T I Travancore Titanium Products Ltd, Trivandrum
D R V . S. V A J A Y A N N A Y A R ( Alternate )
DR R. J. RATHI Sudarshan Chemical Industries Ltd, Pune
S H R I K . L. R A T H I ( Alternate )
S H R I R . R . SEQUEIRA Garware Paints Ltd, Bombay
S H R I C. R . T H U S E ( Alternate )
( Continued on page 2 )

© Copyright 1987
BUREAU OF INDIAN STANDARDS
This publication is protected under the Indian Copyright Act ( XIV of 1957 ) and
reproduction in whole or in part by any means except with written permission of the
publisher shall be deemed to be an infringement of copyright under the said Act.

1
IS : 354 ( Part 2 ) - 1986
( Continued from page 1 )

Members Representing
D R G . K . SINGHANIA Ministry o f Defence ( R & D )
S H R I I. K. LOOMBA ( Alternate )
SHRI S. K. SRIVASTAVA Oil Technologists' Association of India, Kanpur
S H R I S U R E N D R A G A N G ( Alternate )
S H R I M. S. SULTANIA Ministry of Defence ( DGI )
S H R I R. S. SENGAR ( Alternate )
DR R. B. TIRODKAR Asian Paints ( India ) Ltd, Bombay
S H R I V . M . N A T U ( Alternate )
SHRI T. K. VISWANATHAN Addisons Paints & Chemical Ltd, Madras
S H R I K. R. S A N T H A N A N ( Alternate )
SHRI P. M. V Y A S Indian Paint Association, Calcutta
S H R I D. K. R O Y ( Alternate )
SHRI SATISH CHANDER, Director General, BIS ( Ex-officio Member )
Director ( Chem )
Secretary
SHRI M. M. MALHOTRA
Deputy Director ( Chem ), BIS

Resins Subcommittee, CDC 50 : 4

Convener
S H R I M. C. C H O K S I Resins & Plastics Pvt Ltd, Bombay
Members
ASSISTANT RESEARCH OFFICER Ministry of Railways
( CM-II )
S H R I S. K. ASTHANA Ministry of Defence ( DGI )
S H R I S. S. K A T I Y A R ( Alternate )
S H R I V. S. BHAKRE Hindustan Ciba Geigy, Bombay
SHRI V. H. DESAI ILAC India Ltd, Bombay
S H R I S. M I T R A ( Alternate )
S H R I S. C. J A I N Goodlass Nerolac Paints Ltd, Bombay
SHRI V. M. NATU Asian Paints ( India ) Ltd, Bombay
D R A . V . R A O ( Alternate)
S H R I S. V. R. S E K H A R Reichold Chemicals India Ltd, Madras
S H R I J A N K I R A M A N ( Alternate )
SHRI G. N. T I W A R I IEL Limited, Calcutta
DR S. D. YADAV Chowgule & Co ( Hind ) Pvt Ltd, Bombay
S H R I V. M. N A C H A N E ( Alternate )

2
 IS : 354 ( Part 2 ) - 1986

Indian Standard
METHODS OF
SAMPLING AND TEST FOR
RESINS FOR PAINTS
PART 2 SPECIAL TEST METHODS FOR ALKYD RESINS

(Second Revision)

0. FOREWORD
0.1 This Indian Standard ( Part 2 ) ( Second Revision ) was adopted by
the Indian Standards Institution on 18 August 1986, after the draft
finalized by the Raw Materials for Paints Industry Sectional Committee
had been approved by the Chemical Division Council.
0.2 This standard was originally published in 1952 covering methods
of sampling and general test methods mainly for natural resins. Subse-
quently, an Indian Standard for method of sampling and test for natural
and synthetic resins was published as Part 2 of the above standard in
1971. These two parts were amalgamated and revised in 1976. This
revision has been necessitated as more and more newer synthetic resins
like polyamides, polyvinyls, chlorinated rubber and emulsion polymers
are being manufactured and used in the country. While revising the
standard, the Committee felt it appropriate to publish this standard in
various parts, as indicated below:
Part 1 General test methods
Part 2 Special test methods for alkyd resins
Part 3 Special test methods for phenolic resins
Part 4 Special test methods for epoxy resins
Part 5 Special test methods for polyamide resins
Part 6 Special test methods for amine resins
Part 7 Special test methods for determination of monomer content
in acrylic or vinylacatate containing polymers and emulsions
Part 8 Special test methods for chlorinated rubber

3
IS : 354 ( Part 2 ) - 1986

0.3 In this standard ( Part 2 ), the test methods covered in 17.1 to 17.7
of IS : 354-1976* have been included. In addition to above, methods
of test for identification of resin, fineness on Hegmann gauge and toler-
ance to solvent have been added. Methods of tests for chemically
modified alkyds will also form a part of this standard as and when
made.
0.4 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†.

1. SCOPE
1.1 This standard ( Part 2 ) prescribes the methods of test for alkyd
resins used in paints and enamels.
2. TERMINOLOGY
2.1 For the purpose of this standard ( Part 2 ), the definitions given in
IS : 1303-1963‡ and IS : 6667-1972§ shall apply.
3. SAMPLING
3.1 Representative samples of the alkyd resins shall be drawn as
prescribed in 3 of Part 1 of this standard.
4. IDENTIFICATION
4.0 The resin shall be identified by the qualitative tests given below.
4.1 Phenolphthalein T e s t — Heat 1 g of resin with 2 to 3 g of
phenolphthalein and 10 drops of concentrated sulphuric acid ( see IS : 266-
1977|| ) in a test tube until an orange or brownish-orange melt forms
( see Note ). After the melt has cooled, extract with water, dilute to
1 000 ml and make alkaline with sodium hydroxide solution. Formation
of pink colour confirms phthalate and alkyd resin.
N O T E — Too high a temperature or too much acid or too long heating may char
the melt.
4.2 Resorcinol Test — Heat about 0.5 g of resin with 2 to 3 times the
quantity of resorcinol for several minutes. Cool and extract with boiling
water. Dilute to 50 to 100 ml with water. Make alkaline with dilute
sodium hydroxide solution. A green fluorescence indicates phthalate and
alkyd resin.
*Methods of sampling and test for resins for paints ( first revision ).
†Rules for rounding off numerical values ( revised ).
‡Glossary of terms relating to paints ( second revision ).
§Glossary of terms used in synthetic resin industry.
||Specification for sulphuric acid ( second revision ).
4
 IS : 354 ( P a r t 2 ) - 1986

5. IDENTIFICATION OF ROSIN IN ALKYD RESINS

5.0 Outline of t h e Method — Presence of rosin is qualitatively
determined by any of the following methods.
5.1 Liebermann-Starch Test — Dissolve sample by warming/boiling
in acetic anhydride. Cool to room temperature. Take one or two ml
of this solution in white porcelain dish. Add a drop of sulphuric acid
( sp gr 1.43 ). The presence of violet colour indicates the presence of
rosin in the sample.
5.2 Nichel Modification of Liebermann-Starch Test — Dissolve
5 ml of sample ( 0.1 to 0.5 g ) in 3 ml of chloroform. Add 5 ml sul-
phuric acid ( sp gr 1.56-1.58 ) and shake thoroughly. The yellow
chloroform will float. After it has become clear, add acetic anhydride
drop by drop, the chloroform layer will be coloured violet in presence of
trace of rosin. By repeated vigorous shaking, the sulphuric acid layer
dissolves the colouring matter and takes on a crimson to purple red
colour.
6. DETERMINATION OF FINENESS ON HEGMANN GAUGE
6.0 Outline of the Method — This test prescribes a method of
estimating the fineness of the solution.
6.1 Apparatus
6.1.1 Hegmann Gauge
6.2 Procedure — Place a few drops in the groove of the Hegmann
gauge and draw the same along the decreasing thickness direction. The
point along the groove at which continuous bitty appearance starts is
read in terms of micron scale on the side.
7. DETERMINATION OF TOLERANCE TO SOLVENT
7.0 General — This test prescribes the extent to which alkyd resins can
be diluted. Usually, it is carried out either on volume/volume basis or
mass/volume basis or mass/mats basis.
7.1 Apparatus
7.1.1 Graduated Test Tube
7.1.2 Beaker
7.1.3 Glass Rod
7.2 Procedure
7.2.1 Volume/Volume Basis — 1.2 ml of solution of resin is transferred
directly into a graduated test tube without touching the sides, and the
solvent, for tolerance test, is gradually added in small shots with
5
IS : 354 ( Part 2 ) - 1986
immediate shaking to mix the contents of the test tube. The addition is
continued till a slight haze is obtained in the solution. The volume of
solvent added is noted.

Percent tolerance =

7.2.2 Mass/Volume Basis — Method is similar to the above but a

weighed quantity of the resin in a graduated cylinder is diluted as above
with the solvent, for tolerance. Stop addition when the solution turns
hazy. The volume of liquid added is read out from the graduations.
7.2.3 Mass/Mass Basis — In a weighed beaker of suitable capacity with
a glass rod, weigh accurately 10 g of the alkyd sample. Place the
beaker on a white surface with a black dot so that the dot can be seen
through the alkyd solution. Add the solvent for thinning and stir after
every addition with the glass rod. Add solvent till the dot disappears
due to haze in solution. Reweigh the beaker with solution. Find out
the weight of solvent added.

Percent tolerance =

8. DETERMINATION OF FATTY ACIDS

8.0 Outline of the Method — The resin is refluxed with alcoholic
potassium hydroxide and filtered. The filtrate collected and the un-
saponifiable and volatile matter are extracted with ether. The aqueous
extract is acidified to pH 2, cooled to room temperature and fatty acids
present are extracted with ether. The ether extract is evaporated, dried
and weighed. The determination is not applicable for alkyd resins
containing modifying agents like urea, phenol, melamine, rosin and
styrene.
8.1 Apparatus
8.1.1 Beakers — of 150- and 400-ml capacities.
8.1.2 Filter Flask
8.1.3 Funnel — long stem, 75 mm diameter.
8.1.4 Flask and Condenser — 500-ml, long-necked, fitted with a reflux
condenser. The joints between the flask and the condenser shall be
ground-glass joints.
8.1.5 Guard Tube — of soda-lime.
8.1.6 Nitrogen Gas Supply
8.1.7 Separating Funnels — three, of 500-ml capacity each.

6
 IS : 354 ( Part 2 ) - 1986

8.1.8 Drying Oven — Vacuum type, controlled thermostatically to

maintain a temperature of 60 ± 2°C.
8.2 Reagents
8.2.1 Alcohol-Benzene Mixture — Mix 1 volume of absolute alcohol
( see IS : 321-1964* ) with 3 volumes of benzene ( see IS : 1840-1961† ).
8.2.2 Benzene — conforming to IS : 1840-1961†.
8.2.3 Ether
8.2.4 Hydrochloric Acid — relative density 1.16, conforming to IS : 265-
1976‡.
8.2.5 pH Indicator Papers — universal type.
8.2.6 Alcoholic Potassium Hydroxide Solution
8.2.7 Sodium Sulphate — anhydrous, conforming to IS : 255-1982§.
8.3 Procedure
8.3.1 Weigh sufficient resin or resin solution to yield 0.8 to 1.2 g of
potassium alcohol phthalate into a long-necked flask. Add 50 ml of
benzene. Warm, if necessary, over a hot water-bath to dissolve. Add
60 ml of alcoholic potassium hydroxide and fit the reflux condenser.
Place the flask in water-bath, immersing to the level of contents of the
flask. Gradually, raise the temperature and reflux for 1½ h. At the end
of this period, remove the flask from bath and wash the inside of the
condenser with a few millilitres of alcohol-benzene mixture. Remove
the condenser, close the flask with soda-lime guard tube and cool in
running water. Cool and filter immediately and quickly through pre-
viously tared G 4 sintered glass crucible. Wash the precipitate with
benzene-alcohol mixture until the washings are not alkaline to phenol-
phthalein. Avoid suction of air through the precipitate as the crystals
are hygroscopic. Pour about 25 ml of ether and filler. Transfer the
filtrate and washings to a 500-ml beaker using water. Concentrate on
steam bath to a volume of nearly 25 ml under a blanket of nitrogen gas
to avoid oxidation of fatty acids. Transfer the solution to a 500-ml
separating funnel with the aid of water and add 300 ml of water and
10 ml of alcohol. Extract the unsaponifiable matter and volatile thinners
with successive 50-ml portions of ether, combining the ether extracts in the
first separating funnel and using the other two for successive extractions
( see Note ). Wash the ether extracts with three 10-ml poitions of water,

*Specification for absolute alcohol ( revised ).

†Specification for benzene, reagent grade.
‡Specification for hydrochloric acid ( second revision ).
||Specification for sodium sulphate, anhydrous ( technical grade ) ( second revision )

7
IS : 354 ( P a r t 2 ) - 1986

adding water to the main aqueous phase. Discard the combined ether
extracts.
NOTE — If the layers do not separate distinctly, draw the aqueous layer carefully
and add 2 to 3 ml of alcohol to the emulsion phase. Swirl gently to break emulsion
and draw the aqueous layer. This procedure may be repeated on subsequent extrac-
tions, if necessary.
8.3.2 Acidify the aqueous phase with hydrochloric acid, cooling while
addition is carried out and bring the solution to pH 2. Cool the mixture
to room temperature and extract the fatty acids with successive 25 ml
portions of ether until a colourless extract is obtained, combining the
ether extracts in the first funnel and using the others for subsequent
extractions. Wash the combined ether extract with water until it is free
from mineral acids as revealed by indicator paper. Preserve the aqueous
phase for polyol determination ( see 9 and 10 ). Dry the combined ether
extract in the separating funnel by the addition of anhydrous sodium
sulphate. Filter the ether extract through rapid low ash filter paper and
collect the filtrate into a previously weighed 150-ml beaker containing a
few pieces of porcelain bits and previously weighed to the nearest 1 mg.
The ether extract should be decanted from the top opening of the
separating funnel. Evaporate the ether portion-wise by placing the
beaker and its contents on the water-bath. Cover the filter funnel with
a watch-glass during evaporation and maintain an inert atmosphere
over beaker by passing nitrogen gas. Remove last portions of fatty acids
from sodium sulphate by washing with small amounts of ether until a
colourless extract is obtained. Remove the final traces of fatty acids
from filter paper with small portions of ether.
8.3.3 Complete the evaporation of fatty acid-ether solution on the
steam-bath while maintaining nitrogen atmosphere. Remove final traces
of ether by heating for successive 20 minutes period in vacuum oven
at 60°C until constant mass is obtained.
8.4 Calculation — Calculate total fatty acids content as follows:

Total fatty acids, percent by mass =

where
M2 = mass in g of the beaker plus residue,
M1 = mass in g of the beaker, and
M = mass in g of the material taken for test.
9. DETERMINATION OF GLYCEROL AND ETHYLENE
GLYCOL
9.0 Outline of the Method — The method covers the determination
of glycerol and ethylene glycol in alkyd resins and resin solutions. Other
polyhydric alcohols that can be oxidized by periodic acid to formaldehyde
8
 IS : 354 ( Part 2 ) - 1986

or formic acid or both, will interfere with the determination of glycerol

and ethylene glycol. Urea, melamine and phenolic resins interfere.
Glycerol and ethylene glycol are determined by adding periodic acid to
the aqueous extract obtained in the determination of fatty acids ( 8.3 ).
This is titrated against standard sodium hydroxide and further with
standard thiosulphate after titrating the iodine liberated by addition of
potassium iodide. The primary hydroxyl groups of ethylene glycol and
glycerol are oxidized to formaldehyde by periodic acid; the secondary
hydroxyl group of glycerol is oxidized to formic acid. By acidimetric
and iodometric titration, the proportions of formic acid and formalde-
hyde may be determined and calculated to glycerol and ethylene glycol
by algebraic equations.
9.1 Apparatus
9.1.1 Burettes — of 50- and 100-ml capacities, conforming to IS : 1997-
1982*.
9.1.2 Pipettes — of 20- and 50-ml capacities ( see IS : 1117-1975† ).
9.1.3 Beakers — two, each of 400-ml capacity ( see IS : 2619-1971‡ ).
9.1.4 Long-Necked Flask — four, each of 1 000-ml capacity.
9.1.5 Volumetric Flasks — two, each of 100-ml capacity ( see IS : 915-
1975§ ).
9.1.6 Graduated Cylinder — 10-ml capacity.
9.2 Reagents
9.2.1 Methyl Purple Indicator — 0.1 percent.
9.2.2 Periodic Acid — Dissolve 11 g of periodic acid crystals in water
and dilute to 1 000 ml. Store the solution in brown bottles.
9.2.3 Potassium Iodide Solution — Dissolve 200 g of potassium iodide in
water and dilute to 1 000 ml.
9.2.4 Standard Sodium Hydroxide Solution 0.1 N.
9.2.5 Standard Sodium Thiosulphate Solution — 0.2 N.
9.2.6 Starch Solution
9.2.7 Sulphuric Acid — 1 : 5 ( v/v ). Mix one volume of concentrated
sulphuric acid ( conforming to IS : 266-l977|| ) with 5 volumes of water.
*Specification for burettes ( second revision ).
†Specification for one-mark pipettes ( first revision ).
‡Specification for glass beakers ( first revision ).
§Specification for one-mark volumetric flasks ( first revision ).
||Specification for sulphuric acid ( second revision ).

9
IS : 354 ( Part 2 ) - 1986

9.3 Procedure — Transfer the aqueous phase obtained from the fatty
acid determination ( 8.3 ) to a 400-ml beaker and evaporate to reduce
to a volume of 60 ml. During evaporation, keep the mouth of the beaker
covered with a watch-glass. Cool to room temperature and filter through
a rapid filter paper into a 100-ml volumetric flask, make up to mark
and homogenize by shaking. Pipette 20 ml into a 1 000-ml long-necked
flask. Add a few drops of indicator and neutralize with sodium hydr-
oxide solution. Add exactly 50 ml of periodic acid into the flask,
stopper and swirl well to mix the contents thoroughly. Simultaneously,
prepare two blanks containing 20 ml of water and allow to attain the
room temperature. Add to the aliquots of the sample and the blank,
100 ml of water and 3 drops of methyl purple indicator and titrate
against standard sodium hydroxide. To another aliquot of the filtered
solution, add 150 ml of water, 30 ml of potassium iodide solution and
25 ml of sulphuric acid. Titrate the solution against standard sodium
thiosulphate solution to faint iodine colour. Add about 5 ml of starch
solution and finish the titration with the disappearance of blue colour
( see Note 2 ). Carry out a blank under similar conditions with all
reagents except the sample.
N O T E 1 — T h e aliquot should be so chosen, if possible, that 15 to 20 percent of
periodic acid is consumed during oxidation, considerable periodic acid is required to
complete the oxidation and in case more than 20 percent is consumed, the results
should be disregarded and a smaller aliquot taken. On the other hand, too small an
aliquot is not advisable, for in such a situation, the difference between titration and
blank is small.

N O T E 2 — If the end-point is not stable, add water and titrate to a stable end
point.

9.4 Calculation — Calculate the percentage of glycerol and ethylene

glycol as follows:
a) Glycerol and ethylene glycol
( A ), percent by mass =

where
V1 = volume in ml of standard sodium thiosulphate solution
required for blank,
V = volume in ml of standard sodium thiosulphate solution
required for sample,
N = normality of standard sodium thiosulphate solution,
M = mass in g of the material taken for test, and
F = aliquot in g fraction of the solution used.

10
 IS : 354 ( Part 2 ) - 1986

b) Glycerol, percent by mass (B ) =

where
V 1 = volume in ml of standard sodium hydroxide solution
used for titration of the sample,
V2 = volume in ml of standard sodium hydroxide solution
required for blank,
N = normality of the standard sodium hydroxide solution,
M = mass in g of the sample taken for test, and
F = aliquot fraction.
c) Ethylene glycol, percent by mass = 1.348 ( A — B )
NOTE — In practice, samples containing no ethylene glycol have given values of
up to one percent aud hence samples giving ethylene glycol values of 1 percent or less
should be considered as having no ethylene glycol.

10. DETERMINATION OF PENTAERYTHRITOL

10.0 Outline of t h e Method — Monopentaerythritol reacts with
benzaldehyde to form dibenzal, a crystalline compound, and determina-
tion carried out gravimetrically.
10.1 Apparatus
10.1.1 Beakers — 100-ml capacity.
10.1.2 Pipettes
10.1.3 Desiccator
10.1.4 Oven — capable of maintaining a temperature of 105°C.
10.2 Reagents
10.2.1 Benzaldehyde-Methanol Reagent — Add 100 ml of methanol
( conforming to IS : 517-1967* ) to 20 ml of benzaldehyde.
10.2.2 Hydrochloric Acid — conforming to IS : 265-1976†.
10.2.3 Methanol-Water Mixture — 1 : 1 ( v/v ). Mix equal volumes of
methanol and water. Store one-fourth of the solution in refrigerator
and the remainder at room temperature.
*Specification for methanol ( methyl alcohol ) ( first revision ).
†Specification for hydrochloric acid ( second revision ).

11
IS : 354 ( Part 2 ) - 1986

10.3 Procedure — Transfer an aliquot of the solution ( 9.3 ) containing

0.15 to 0.55 g of pentaerythritol to a 100-ml beaker. Reduce the volume
of the solution over a water-bath to about 5 ml. To the hot solution,
add 15 ml of benzaldehyde-methanol reagent and 12 ml of hydrochloric
acid Mix well and let stand at room temperature for about 15 minutes,
swirling occasionally to prevent the precipitate from sticking to the
bottom of the beaker. Place the beaker in an ice-bath for about an hour
and maintain the temperature at 0 to 2°C. Remove the beaker from ice-
bath and filter the contents immediately through a weighed fritted glass
crucible of medium porosity. Rinse the beaker with 25 ml of cold
methanol-water mixture ( 10.2.3 ) and add to crucible. Continue to
transfer and wash the precipitate with about 100 ml of methanol-water
mixture at 20 to 25°C as follows:
Disconnect suction or vacuum, pour 10 ml of the methanol-
water mixture from beaker to crucible and stir the precipitate to get
a homogenous slurry, using a short flat-end glass rod. Start
filtering using suction or vacuum. Repeat washing thus about six
times. Finally wash the precipitate and rinse the walls of the
crucible with 30 ml of methanol-water mixture. Filter completely
and dry the precipitate at about 105°C for about 2 hours. Cool in a
desiccator and weigh.
10.4 Calculation

Monopentaerythritol P, percent by mass =

where
M2 = mass in g of the precipitate,
M1 = mass in g of the material taken for test, and
F = the aliquot fraction taken for determination.
NOTE — The percentage of monopentaerythritol may be converted to percentage
of commercial monopentaerythritol on the assumption that the commercial grade
contains 85 percent monopentaerythritol, using the following formula:
Commercial monopentaerythritol, percent by mass = P/0.85, where P is the value
obtained in 10.4.

11. DETERMINATION OF PHTHALIC ANHYDRIDE

11.0 Outline of the Method — The method covers the determination
of phthalic anhydride content in alkyds and alkyd resin solutions includ-
ing those containing styrene. The material is refluxed with alcoholic
potassium hydroxide solution and phthalic anhydride precipitated as
potassium alcohol phthalate and determined gravimetrically.

12
 IS : 354 ( Part 2 ) - 1986

11.1 Apparatus
11.1.1 Flask and Condenser — A 500-ml long-necked flask fitted with a
75-cm long air condenser. The joint between the flask and the conden-
ser shall be a taper ground-glass joint.
11.1.2 Desiccator — with concentrated sulphuric acid as desiccant.
11.2 Reagents
11.2.1 Benzene
11.2.2 Alcoholic Potassium Hydroxide Solution — Dissolve 66 g of potassium
hydroxide in 1 000 ml of absolute alcohol ( conforming to IS : 321-
1964* ).
11.2.3 Ether — anhydrous, conforming to IS : 336-1973†.
11.2.4 Alcohol-Benzene Wash Solution — 1 : 3 ( v/v ).
11.2.5 Hydrochloric Acid – 0.1 N.
11.3 Procedure — Weigh from a closed container, a sample of the resin
or resin solution sufficient to yield 0.8 to 1.2 g of potassium alcohol
phthalate into a 500-ml long-necked flask. Add 150 ml of benzene,
warm if necessary over a water-bath and bring into solution. Add
60 ml of alcoholic potassium hydroxide solution. Reflux for 1½ hours
over a water-bath using the condenser. Remove the flask from the
water-bath, rinse down the inside of the condenser with a few millilitres
of alcohol-benzene wash solution. Remove the condenser and stopper
the flask with soda-lime guard tube and cool the flask by means of runn-
ing water. Filter the contents through a weighed fritted glass crucible,
when cool. Use alcohol-benzene wash solution to transfer the precipitate
completely from the flask to crucible. Wash the precipitate with
successive portions of alcohol-benzene wash solution until a few millilitres
of wash solution shows no signs of alkalinity to phenolphthalein. Do
not allow to draw air through the crystals as they are hygroscopic.
Finally wash the precipitate with 25 ml of ether. Wipe the outside of
the crucible with a clean cloth and place in an oven at 60°C for one hour
( see Note ). Cool to room temperature in a desiccator and weigh.
NOTE — The precipitate is alcoholate and alcohol of crystallization may be driven
off on prolonged heating. However, it is safe to dry up to 60°C for one hour.
11.4 C a l c u l a t i o n

Phthalic anhydride, percent by mass =

where
M1 = mass in g of the precipitate obtained, and
M2 = mass in g of the material taken for test.
*Specification for absolute alcohol ( revised ).
†Specification for ether ( second revision ).
13
IS : 354 ( Part 2 ) - 1986
12. DETERMINATION OF PHTHALIC ANHYDRIDE CONTENT
IN ALKYDS CONTAINING OTHER DIBASIC ACIDS
12.0 Outline of the Method — The method is based on spectrophoto-
metry. It is suitable for the determination of phthalic anhydride
content in alkyds containing dibasic acids like maleic, fumaric, adipic
acids, etc. The material is saponified in alcoholic potassium hydroxide
and benzene and the potassium salt of phthalic acid precipitated. With
the exception of maleic and fumaric acids, other interfering substances
are eliminated by dissolving the precipitate in water, adjusting the pH to
2.5 with nitric acid and filtering. Phthalic acid is then reprecipitated as
non-atoichiometric lead phthalate and calculated to phthalic anhydride,
using a factor obtained when compositions of known purity are
analyzed.
12.1 Apparatus
12.1.1 Flask and Condenser — A 500-ml long-necked flask fitted with
76-cm long air condenser, having tapered ground-glass joint.
12.1.2 Oven
12.1.3 Desiccator — with sulphuric acid as desiccant.
12.2 Reagents
12.2.1 Benzene — anhydrous.
12.2.2 Alcoholic Potassium Hydroxide Solution — same as in 11.2.2.
12.2.3 Ether — anhydrous, conforming to IS : 336-1973*.
12.2.4 Alcohol-Benzene Wash Solution — 1 : 3 ( v/v ).
12.2.5 Glacial Acetic Acid — conforming to IS : 695-1986†.
12.2.6 Methanol — anhydrous, conforming to IS : 517-1967‡.
12.2.7 Lead Acetate Solution — Dissolve 25 g of lead acetate trihydrate
in glacial acetic acid, dilute to 100 ml with acetic acid.
12.2.8 Nitric Acid — 1 : 3 ( v/v ). Mix one volume of nitric acid
conforming to IS : 264-1976§ with 3 volumes of water.
12.3 Procedure — Weigh sufficient amount of material from closed
container into a 500-ml long-necked flask and follow the digestion and
filtration processes as prescribed in 11.3. Then dissolve the contents of
the crucible in 70 ml of water using a filter so as to collect the
washings in a 250-ml beaker. Adjust the pH of the contents to 2.5 by
*Specification for ether ( second revision ).
†Specification for acetic acid ( third revision ).
‡Specification for methanol ( methyl alcohol ) ( first revision ).
§Specification for nitric acid ( second revision ).
14
 IS : 354 ( Part 2 ) - 1986
adding nitric acid. Let stand the contents for 30 minutes and then filter
through a double thickness fine filter paper directly into a 100-ml
volumetric flask ( see Note ). Make up to mark with water, using water
simultaneously to wash the beaker and filter. Stopper the flask and
shake well. Withdraw an aliquot containing not less than 60 mg or not
more than 90 mg of the dissolved salts. Transfer this to a 250-ml long-
necked flask. Dry the contents of the flask in an oven at 60°C. Add 5 ml
of glacial acetic acid, vent the stopper by inserting a paper strip under
one side, and heat in the oven at 60°C for one hour. Add 100 ml of
anhydrous methanol and continue heating in the oven with occasional
agitation until the crystals are completely dissolved. To the hot solution
add from a pipette 2.0 ml of lead acetate solution, agitating while
adding. Return the flask to oven at 60°C for one hour. Remove the
stopper tightly after 30 minutes. Allow to stand for at least 12 hours.
Filter through fritted glass crucible of medium porosity. Wash the flask
with anhydrous methanol and transfer the washings to the filter.
Carefully examine the filtrate. If cloudy, filter again. Dry the crucible
for 1 hour at 105°C, cool in a desiccator and weigh.
NOTE — If the sample does not cloud when acidified, it may be diluted to volume
at once and the filtering omitted.

12.4 Calculation

Phthalic anhydride, percent by mass =

where
M1 = mass in g of lead precipitate, and
M2 = mass in g of the material present in the aliquot used.

13. DETERMINATION OF UNSAPONIFIABLE MATTER

13.0 Outline of the M e t h o d — The material is refluxed with sodium
hydroxide and unsaponifiable matter separated, evaporated and
weighed. The method is not applicable to alkyd resins containing
modifying agents like urea, melamine and phenol.
13.1 A p p a r a t u s
13.1.1 Beaker — of aluminium and capacity 125-ml.
13.1.2 Flask and Condenser — same as in 12.1.1.
13.1.3 Separating Funnels — three, each of 500-ml capacity.
13.1.4 Drying Oven — with thermostatic control to operate at
80 ± 5°C.
15
IS : 354 ( Part 2 ) - 1986

13.2 Reagents
13.2.1 Benzene — conforming to IS : 1840-1961*.
13.2.2 Benzene-Alcohol Mixture — Mix equal volumes of benzene ( con-
forming to IS : 1840-1961* ) and ethyl alcohol ( conforming to IS : 323-
1959† ), add 2 drops of phenolphthalein indicator solution and neutralize
to a persistent faint pink colour with sodium hydroxide solution.
13.2.3 Ethyl Alcohol — 95 percent by volume ( conforming to IS : 323-
1959† ).
13.2.4 Ether — conforming to IS : 336-1973‡.
13.2.5 Phenolphthalein Indicator Solution — Dissolve 0.1 g of phenolph-
thalein in 100 ml of 60 percent rectified spirit ( conforming in IS : 323-
1959† ).
13.2.6 Sodium Hydroxide Solution — Dissolve sodium hydroxide in equal
mass of water.
13.2.7 Standard Sodium Hydroxide Solution — 0.02 N.
13.2.8 pH Papers
13.3 Procedure — Weigh sufficient material so as to contain 0.05 to 0.2 g
of unsaponfiable matter into a 200-ml long-necked flask. Add 10 ml of
benzene, and warm to dissolve the sample. Add 50 ml of alcohol, swirl
to mix, add slowly 5 ml of sodium hydroxide solution and 5 ml of water.
Attach the condenser and reflux gently over a water-bath for 2 hours.
Remove from water-bath, cool to room temperature, rinse down the
condenser and joint with water. Transfer the contents of the flask
completely to a separating funnel, using water. Finally, rinse the flask
with three 25-ml portions of ether, adding the ether washings to the
separating funnel. Add sufficient water to bring the volume to 300 ml
and add 10 ml of alcohol. Stopper the separating funnel, shake gently
and allow the layers to separate. Draw off the lower aqueous layer to a
second separating funnel. Continue the extraction of aqueous layer
with successive 20-ml portions of ether until a colourless ether extract is
obtained, combining the ether extractions in the first funnel. Wash the
combined ether extract contained in the first separating funnel with
25 ml of water until the washings are neutral to pH paper. Transfer the
ether extract completely into a 125-ml beaker containing a few porous
bits, weighed previously. Evaporate the ether over a steam-bath
carefully. When all the ether has been removed, transfer the beaker to
an oven previously heated to 80°C. Heat to constant mass, cool to room
temperature in a desiccator and weigh. After weighing, add 50 ml of

*Specification for benzene, reagent grade.

†Specification for rectified spirit ( revised ).
‡Specification for ether ( second revision ).
16
 IS : 354 ( Part 2 ) - 1986
warm benzene-alcohol mixture. Titrate against standard sodium
hydroxide solution to the same persistent faint pink colour as in the
neutralization of benzene-alcohol mixture.
13.4 Calculation
Unsaponifiable matter,
percent by mass =

where
M1 = mass in g of the residue obtained,
V = volume in ml of standard sodium hydroxide used in the
titration,
N = normality of standard sodium hydroxide solution, and
M2 = mass in g of the material taken for test.
NOTE — A factor of 0.280 is used in the equation on the assumption that the acid
is 18 carbon atom fatty acid. If coconut, lauric, or other short chain acids are sus-
pected, an arbitrary factor 0.216 shall be used, and this fact shall be reported with
the test result.

17
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