IS : 354 (Part 2) - 1986

(Reaffirmed 1997)
Edition 3.4
(2000-06)

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

( Second Revision )
(Incorporating Amendment Nos. 1, 2, 3 & 4)

UDC 667.621.633 [678.674] : 620.1

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

Price Group 5
 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
SHRI S. S. ANAKAIKAR ( Alternate to
Shri R. K. Marphatia )
SHRI K. M. BANERJEE National Test House, Calcutta
SHRI S. BHATTACHARYYA IEL Ltd, Calcutta
SHRI G. N. TIWARI ( Alternate )
CHEMIST & METALLURGIST-I Research, Design and Standards
ASSISTANT RESEARCH OFFICER Organization (Ministry of Railways),
(CM-II), ( Alternate ) Lucknow
SHRI M. C. CHOKSI Resins & Plastics Pvt Ltd, Bombay
SHRI O. P. DHAMIJA Export Inspection Council of India, Calcutta
SHRI S. N. DUTTA ( Alternate )
DR A. B. KARNIK Colour-Chem Ltd, Bombay
SHRI M. E. MARATHE ( Alternate )
SHRI R. D. KAWATRA Directorate General of Technical
SHRI KULTAR SINGH ( Alternate ) Development, New Delhi
SHRI P. R. MALHAN Development Commissioner (SSI) (Ministry
SHRI R. MUKOPADHYAY ( Alternate ) of Industry), New Delhi
SHRI K. C. MEHTA Indian Oil Corporation Ltd, Faridabad
SHRI B. RAMA MURTI Travancore Titanium Products Ltd,
DR V. S. VAJAYAN NAYAR ( Alternate ) Trivandrum
DR R. J. RATHI Sudarshan Chemical Industries Ltd, Pune
SHRI K. L. RATHI ( Alternate )
SHRI R. R. SEQUEIRA Garware Paints Ltd, Bombay
SHRI C. R. THUSE ( Alternate )
( Continued on page 2 )

© BIS 2002
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.
IS : 354 (Part 2) - 1986

( Continued from page 1 )

Members Representing
DR G. K. SINGHANIA Ministry of Defence (R & D)
SHRI I. K. LOOMBA ( Alternate )
SHRI S. K. SRIVASTAVA Oil Technologists’ Association of India,
SHRI SURENDRA GANG ( Alternate ) Kanpur
SHRI M. S. SULTANIA Ministry of Defence (DGI)
SHRI R. S. SENGAR ( Alternate )
DR R. B. TIRODKAR Asian Paints (India) Ltd, Bombay
SHRI V. M. NATU ( Alternate )
SHRI T. K. VISWANATHAN Addisons Paints & Chemical Ltd, Madras
SHRI K. R. SANTHANAN ( Alternate )
SHRI P. M. VYAS Indian Paint Association, Calcutta
SHRI D. K. ROY ( 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
SHRI M. C. CHOKSI Resins & Plastics Pvt Ltd, Bombay
Members
ASSISTANT RESEARCH OFFICER (CM-II) Ministry of Railways
SHRI S. K. ASTHANA Ministry of Defence (DGI)
SHRI S. S. KATIYAR ( Alternate )
SHRI V. S. BHAKRE Hindustan Ciba Geigy, Bombay
SHRI V. H. DESAI ILAC India Ltd, Bombay
SHRI S. MITRA ( Alternate )
SHRI S. C. JAIN Goodlass Nerolac Paints Ltd, Bombay
SHRI V. M. NATU Asian Paints (India) Ltd, Bombay
DR A. V. RAO ( Alternate )
SHRI S. V. R. SEKHAR Reichold Chemicals India Ltd, Madras
SHRI JANKIRAMAN ( Alternate )
SHRI G. N. TIWARI IEL Limited, Calcutta
DR S. D. YADAV Chowgule & Co (Hind) Pvt Ltd, Bombay
SHRI V. M. NACHANE ( 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.
Subsequently, 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 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

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 tolerance 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 This edition 3.4 incorporates Amendment No. 1 (September 1989),
Amendment No. 2 (November 1991), Amendment No. 3 (October 1992)
and Amendment No. 4 (June 2000). Side bar indicates modification of
the text as the result of incorporation of the amendments.
0.5 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 Test — Heat 1 g of resin with 2 to 3 g of phenol
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.
NOTE — 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 (Part 2) - 1986
5. IDENTIFICATION OF ROSIN IN ALKYD RESINS
5.0 Outline of the 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 sulphuric
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/mass 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.
Volume of solvent
Percent tolerance = ----------------------------------------------------------------- × 100
Volume of resin sample
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.
Mass of solvent added
Percent tolerance = ------------------------------------------------------------- × 100
Mass of resin taken
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
unsaponifiable 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
previously tared G 4 sintered glass crucible. Wash the precipitate with
benzene-alcohol mixture until the washings are not alkaline to
phenolphthalein. Avoid suction of air through the precipitate as the
crystals are hygroscopic. Pour about 25 ml of ether and filter. 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

*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 (Part 2) - 1986
portions of water, 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
extractions, 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:
2 M –M 1
Total fatty acids, percent by mass = ------------------------ × 100
M
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
8
 IS : 354 (Part 2) - 1986
formaldehyde 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 formaldehyde 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 : 266-1977¶) 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 hydroxide 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.
NOTE 1 — The 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.
NOTE 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 ( V 1 – V ) N × 0.023 015
( A ), percent by mass = ----------------------------------------------------------------- × 100
M×F
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

( V 1 – V 2 ) N × 0.092 06
b) Glycerol, percent by mass ( B ) = -------------------------------------------------------------- × 100
M×F
where
V1 = 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 and 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 the Method — Monopentaerythritol reacts with
benzaldehyde to form dibenzal, a crystalline compound, and
determination 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
( M 2 + 0.026 9 ) × 43.6
Monopentaerythritol P, percent by mass = ------------------------------------------------------------
-
M1 × F
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
including 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
condenser 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 running water followed by an ice bath. 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 Notes ). Cool to room temperature in a desiccator and weigh.
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.

*Specification for absolute alcohol ( revised ).

†Specification for ether ( second revision ).
‡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 ).
13
IS : 354 (Part 2) - 1986
11.4 Calculation
1 M × 0.513 6
Phthalic anhydride, percent by mass = ----------------------------------- × 100
M2
where
M1 = mass in g of the precipitate obtained, and
M2 = mass in g of the material taken for test.
12. DETERMINATION OF PHTHALIC ANHYDRIDE CONTENT
IN ALKYDS CONTAINING OTHER DIBASIC ACIDS
12.0 Outline of the Method — The method is based on
spectrophotometry. 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.
*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
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
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
M 1 × 0.323
Phthalic anhydride, percent by mass = ----------------------------- × 100
M2
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 Method — 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 Apparatus
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.
15
IS : 354 (Part 2) - 1986
13.1.4 Drying Oven — with thermostatic control to operate
at 80 ± 5°C.
13.2 Reagents
13.2.1 Benzene — conforming to IS : 1840-1961*.
13.2.2 Benzene-Alcohol Mixture — Mix equal volumes of benzene
(conforming 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
phenolphthalein 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

*Specification for benzene, reagent grade.

†Specification for rectified spirit ( revised ).
‡Specification for ether ( second revision ).

16
 IS : 354 (Part 2) - 1986
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 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, M 1 – ( V × N × 0.280 )
percent by mass = ----------------------------------------------------------- × 100
M2
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
suspected, an arbitrary factor 0.216 shall be used, and this fact shall be reported
with the test result.

17
Bureau of Indian Standards
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promote harmonious development of the activities of standardization, marking and quality
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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 by Technical Committee : CDC 50 and amended by
CHD 21

Amendments Issued Since Publication

Amend No. Date of Issue
Amd. No. 1 September 1989
Amd. No. 2 November 1991
Amd. No. 3 October 1992
Amd. No. 4 June 2000

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