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है”ह”ह

IS 14925 (2001): Epoxy Resin for Paints [CHD 20: Paints,Varnishes and Related Products]

Indian Standard

EPOXY RESIN FOR PAINTS — SPECIFICATION

ICS 87.060.01

---

0 BIS 2001

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

Price (lroop 4

Raw Materials for Paint Industry Sectional Committee, CHD 21

FOREWORD

This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the RawMaterials for Paint Industry Sectional Committee had been approved by the Chemical Division Council.

Epoxy resin is one of the most important resins used by paint industries in high performance paint application.It may be corrosion resistance or chemical resistance coating.

The need has been felt for preparation of this standard because of excessive usage of epoxy resins in paintformulation.

There is no 1S0 standard and its equivalent available on the subject.

The composition of the technical committee responsible for formulating this standard is given in Annex B.

For the purpose of deciding whether a particular requirement of this standard is complied with, the final value,observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance withIS 2:1960 ‘Rules for rounding off numerical values ( revised )’. The number of significant places retained inthe rounded off value should be the same as that of specified value in this standard.

.

IS 14925:2001

Indian Standard

EPOXY RESIN FOR PAINTS — SPECIFICATION

1 SCOPE

1.1 This Indian Standard prescribes the requirementand methods of sampling and test for epoxy resin usedin paint industry.

2 REFERENCES

2.1 The Indian Standards listed below containprovisions which through reference in. this text,constitute provision of this standard. At the time ofpublication, the editions indicated were valid. Allstandards are subject to revision and parties toagreements based on this standard are encouragedto investigate the possibility of applying the most recenteditions of the standards.

1S No.

354

(Part l): 1987

(Part4): 1986

1303:1983

6667:1972

1070:1992

Title

Methods of sampling and test forresins for paints:

General test methods ( secondrevision )

Special test methods for epoxy resins( second revision )

Glossary of terms relating to paints( second revision)

Glossary of terms used in syntheticresin industry

Specification for reagent grade water(third revision )

3 TERMINOLOGY

3.1 For the purpose of this standard definitions givenin IS 354 ( Part 1 ), IS 1303, IS 6667 and thefollowing shall apply.

3.2 Ambient Temperature

It is a temperature between 21“C and 38”C.

3.3 Epoxide Equivalent

The mass of an epoxide compound, in grams, whichcontains one mole ofepoxide group.

4 CLASSIFICATION

4.1 A condensation product of epichlorohydrin andbispheneol A in alkaline condition, which leads toformation of epoxy group containing resins. These resins

shall have differentmolecularweight or epoxy equivalentweight depending on stochiometric ratios of abovementioned reactants. The manufacturer shall declaremolecular distribution and average molecular weight.

4.2 Depending upon the applications in paint systemepoxy resins can be classified into three types basedon average molecular weight or epoxy equivalent weightwhen determined through the method specified inAnnex A, alongwith physical state of resin.

Physical AverageState Molecular

Weight

Type A Liquid 360-380

Type B Low molecularweight, solid

Grade 1 900

Grade 2 1400

Type C High molecularweight, solid

Grade 1

Grade 2

5 REQUIREMENTS

5.1 Epoxy resin shallspecified in Table 1.

5.2 Keeping Quality

2900

3750

EpoxyEquivalent

Weight

180-200

425-550

850-1000

1700-2300

2400-3500

comply with the requirements“

The material when stored in normal storage conditionat the ambient temperature shall retain its property foratleast 12 months from the date of manufacture asprescribed in Table 1.

6 FORM OF SUPPLY

6.1 Epoxy resin shall supply as 100 percent solids orany other percentage solution in any suitable solventas agreed to between the manufacturer and thepurchaser.

7 PACKING AND MARKING

7.1 Packing

The material shall be packed in sound, clean WI drycontainers as agreed to between the manu filc[urcr WIthe purchaser.

1

&-u-

1S 14925:2001~:

Table 1 Requirement for Epoxy Resins

( Clauses 5.1 and5.2 ) ,--i

slNo.

(1)

i)

ii)

iii)

iv)

v)

vi)

Characteristics Type A Type B Type C Method of Test, Rcf to !

(2)

Colour ( on ‘Gardner’Max

Viscosity

a) As such at 25°* 0.05°C ( Cps )

(3) (4) (5) (6) (7) (8)

scale ), 3 4 4 4 6—

Grade 1 Grade 2 Grade 1 Grade 2 Annex Cl No. of IS

~

,,,,

(9)<

6.2 ofIs 354 I~

( Part 1 )

8000- — — — — —

15000

b) 40 percent in butyl carbitol — 80-170 470-750 1 600-34004000-1 I 000

at 25 + 0.5°C ( cps )

c) 50 Percent in 1 : 1 mix- — 100-150 — — —ture of O. Xylene/D.A.A.at 25 + 0.5°C ( cps )

Softening point ( ball and — 60-70°C 90- IOO”C 117-127°C 130-145°C

ring )

Epoxide equivalent g/nYole 180-200 425-550 850- I 000 I 700-2300 2400-3 500 A

Hydrolyzable chlorine 0.5 0.2 0.2 0.2 0.2

content by mass, Max

Relaive density (at ’27 ● 2“C) 1.15-1.20 — — — —

8.1 or 8.4of 1s 354( Part I )

10.1ofIs 354

( Part I )

6 of IS 354( Part 4 )

7 Ofls 354[ Part I )

7.2 Marking

The containers shall be marked with the followinginformation:

a) Name and type of the material;

b) Type and grade;

c) Mass of the material;

d) Month and year of manufacturer;

e) Batch No. or lot No. in code or otherwise; and

t) Name of the manufacturer and/or anyrecognized trade-mark.

7.2.1 BIS Certl~cation Marking

The product may also be marked with the StandardMark.

7.2.1.1 The use of the Standard Mark is governed bythe provisions of the Bureau of Indian Standards Aet,1986 and the Rules and Regulations made thereunder.The details of conditions under which the licence forthe use of the Standard Mark may be granted tomanufacturers or producers maybe obtained from theBureau of Indian Standards.

8 QUALITY OF REAGENTS

8.1 Unless specified otherwise pure chemicals anddistilled water (IS 1070 ) shall be used.

NOTE— ‘Pure chemicals’ shall r,,ean chemical that donot contain impurity which affect the results of the analysis.

9 SAMPLING

9.1 Representativesamplesof the material shall be drawnas prescribed in 3 of IS 354 ( Part 1 ).

2

IS 14925:2001

ANNEX A

[ Clause 4.2 and Table 1, S1 No. (iv) ]

“METHOD OF DETERMINATION OF EPOXIDE EQUIVALENT OF EPOXY COMPOUNDS

A-1 PRINCIPLE

A-1.1 Method A

Epoxide groups react with nascent hydrogen bromideproduced by the action of a standard 0.1 mol/1solutionof perchioric acid on tetraethylammonium bromide. Theend-point is determined either by using crystal violetas indicator or, for dark-coloured products, by apotentiometric method. This method is recommendedfor normal reactive epoxy resin.

A-1.2 Method B

The amino nitrogen of the epoxyamine is titrated witha standard solution of perchloric acid. The value thusobtained is used as a correction in the calculation ofthe epoxide equivalent as obtained in Method A. Thismethod is recommended for slow reactive epoxy resin.

NOTE — Safety goggles and safety screen maybe usedwhile carrying out tests through the above methods.

A-2 REAGENTS

A-2.1 Acetic Acid, Glacial — Conform ingto1S625.

A-2.2 Acetic Anhydride

A-2.3 Suitable Solvent for Solution of the Sample—for example chloroform, dibutyl phthalate,chlorobenzene.

A-2.4 Potassium Hydrogen Phthalate — Dry thepotassium hydrogen phthalate for 2 h at 120”C beforeuse.

A-2.5 Crystal Violet, Indicator Solution — Dissolve100 mg of crystal violet in 100 ml of acetic acid.

A-2.6 Perchloric Acid, 0.1 mol/1 StandardSolution — To 8.5 ml ofa 70 percent (m/m) aqueoussolution of perchloric acid, add 300 ml of acetic acidfollowed by 20 ml of acetic anhydride. Dilute to 1 Iitrewith acetic acid and mix thoroughly,

Standardize this solution by titrating it against 200 mgof potassium hydrogen phthalate dissolved in 50 mlof acetic acid, using the crystal violet indicator solution( see Note 1 ).

Use 4 to 6 drops of the crystal violet indicator solutionand continue the titration until a stable green colouris obtained. Note the temperature, r~,of the solutionof perch loric acid at the time of standardization( see Note 2 ). The concentration, C, in mol/1 of the

standard perchloric acid solution, is given by theformula:

~= mVX0.20422

where

m = is the mass ( in g ) of potassium hydrogenphthalate, and

V= is the volume ( in ml ) of perchloric acid usedin the titration.

NOTES

1 If a potentiometric method is used, it is necessary to

standardize the perchloric acid in the same way as usedfor the test.

2 The use of a correction factor is necessary if thetemperature of the perchloric acid at the time of itsstandardization is different from that at the time of thetest. This is because of the significant coefficient ofexpansion of the standard perchloric acid solution ( 1.07x 103 ‘C-l ), which corresponds to a volume variation of0.1 percent “C.

A-2.7 Tetraethylammonium Bromide ReagentSolution – Dissolve 100 g of tetraethylammoniumbromide in 400 ml of acetic acid. Add a few drops ofthe crystal violet indicator solution; if it changes colour,bring it back to the original colour with the perchloricacid standard solution.

NOTE — For some epoxy compounds of low reactivity,the use of tetrabutylammonium iodide is advised, eitheras the solid or as a 10 percent solution in chloroform; inthis case, light should be excluded as much as possible.Solutions of tetrabutyl ammonium iodide in chloroformare unstable and should be freshly prepared for eachtitration.

A-3 APPARATUS

A-3.1 Balance — Accurate to within 0,1 mg.

A-3.2 Conical Flask — 100 ml or 200 ml, with groundglass neck and ground glass stopper.

A-3.3 Micro-burette — Of capacity 10 ml.

A-3.4 Magnetic Stirrer — With polytetrafluor-ethylene-coated bar.

A-3.5 Thermometer—Calibrated to permit temperaturemeasurements to within= 0.1 ‘C.

A-3.6 Pipette, One-mark, 10 ml Capacity —Conforming to IS I 117.

In addition the following apparatus is rcquirtd if a

3

.

@,—

IS 14925:2001

potentiometric end-point is to be used.

A-3.7 pH-millivoltmeter — Preferably of thecompensating type.

A-3.8 Glass and Calomel Reference Electrodes—The electrode system shall have a salt bridge of lithiumchloride in glacial acetic acid. If the electrodes arenot in constant use, wash the glass electrode withbutanone, rinse with water, soak the electrode for atleast 10 min in a solution of dilute hydrochloric acid( 9 ml of hydrochloric acid made up to 100 ml withwater ) and rinse again with water and butanone.

If the electrodes are in constant use, it is sufficient tosoak the electrodes in water between carrying out tests.

A-4 PROCEDURE

A-4.1 Method A

Weigh into the flask, to the nearest 0.2 mg, a quantityof samplecontainingfrom0.6 millimolesto 0.9 millimolesof epoxide groups. ( This corresponds to a mass ofbetween 0.6 x EE mg and 0.9 x EE mg, where EE is theepoxide equivalent of the epoxide compound. )

Add 10 ml of the solvent chosen for solution of thesample; then dissolve the sample by stirring and, ifnecessary, heat slightly. Cool the solution to roomtemperature. Add 20 ml of the acetic acid and, withthe pipette, 10 ml of the tetraethylammonium bromidereagent. Then add 4 to 6 drops of the crystal violetindicator solution.

Titrate with the standard perchloric acid solutionimmediately, in a closed system while stirring thecontents of the flask’by means of the magnetic stirrer.Continue the titration until a stable green colour isobtained.

Note the temperature, r, of the standard perchloric acidsolution.

At the same time carry out a blank test, omitting thesample.

If a potentiometric end point is used, carry out the aboveprocedure using the electrodes and omitting theindicator solution. Take the mid-point of the inflectionon the titration curve as the end point.

A-4.2 Method B

Follow the procedure for Method A, including theblank test. Also carry out a second test with the sample,but without the addition of the tetraethylammoniumbromide reagent.

A-5 EXPRESSION OF RESULTS

A-5.1 Method A

The epoxide equivalent, EE, in grams per mole, is given

by the formula:

1 000x mEE=

(V, -vo)(l - :;;; )Xc

where

m = is the mass ( in g ) of the test sample;

VO= is the volume ( in ml ) of the standardperchloric acid solution used in the blanktest;

V, = is the volume ( in ml ) of the standardperchloric acid solution used in the test onthe sample;

t = is the temperature ( in 0C ) of the standardperchloric acid solution at the time of tests;

[, = is the temperature ( in ‘C ) of the standardperchloric acid solution at the time ofstandardization; and

C = isthe concentration( inmol/1) of the perchloricacid solution at the time of standardization.

The result is sometimes expressed as epoxide index( in moles of epoxide groups per kg ) calculated asfollows:

1000Epoxide index= —

EEA-5.2 Method B

The epoxide equivalent, EE, in grams per mole, is givenby the formula:

1000xmEE = –1

(V, -VO-V2 m,+(1- &o)xc s

where

tn = is the mass ( in g ) of the test sample;

ml = is the mass ( in g ) of the test sample used inthe second test, that is, without the add itionof the tetraethylammonium bromide reagent;

VO= is the volume ( in ml ) of the standardperchloric acid solution used in the blanktest;

VI = is the volume ( in ml ) of the standardperchloric acid solution used in the first teston the sample;

V2= is the volume ( in ml ) of the standardperchloric acid solution used in the secondtest on the sample, that is, without theaddition of the tetraethylammonium bromidereagent;

t = is the temperature ( in “C ) of the standard

..s

-,‘‘

4

perch loric acid solution at the time of the

tesls;

is the temperature (in ‘C) of the standard

perchloric acid solution at the time of

standardization; and

is tk conccnlmtion (in nlol/1) of the perchloric

acid solution at the time of standardization.

The result is sometimes expressed as epoxide index,expressed in moles of epoxide groups per kilogram,

caicutated as follows:

I 000Epoxide index= —

EE

~.,7

IS 14925:2001w-.

A-6 TEST REPORT,F

~~

d

,$

The test report shall include the following

particulars : - ai,

a) A complete identification of the material tested,

including type, source, manufacturer’s codenumbers etc;

b)

c)

d)

e)

The epoxide equivalent;

The solvent used for solutiol] and the reagentused ifit is not tetraetllylalllllloll itllll bromide:

Whether a visual or potentiometric end-pointwas used; and

Any other factor likely to have affected the

result.

IS 14925:2001

ANNEX B

( F’OrewOrd)

COMMITTEE COMPOSITION

..-

Raw Materials for Paint Industry Sectional Committee, CHD 21

Chairman

D~ R. B. TIROOKAR

Members

SHRI R. SIUNIVASANSHRI E. RAMANATIiAN( Alternate )

SHRI K. P. JAMISOTHARSHtu S. G. SHI:TYE( Alfernafe )

SHRI B. P. MALIKSHIU N. K. RAY ( AJrernme )

DR L. K. ACiAI<WALSHIU K. K. ASTHANA( Ahmate )

SHIU R. N. GHC)SH

SHIU S. C. SRIVASTAVASHRI S. KAMAL KUMAR( Alrernate )

SHIUA. S. S(NXISHIU SURIXH YADAV ( Alternate )

SHIUJASIIIKSINCiH

SHIU N. R. NAKAYANAN( Ahernate )

SHRI KARAM CHAND

SHIU S. S. ANAKAIKARSHIU A. E. PANHALE( Alternate )

DR A. BASUD~ K. V. SUSHAMU( Alternate )

CHAIRMAN,CI!NT~AL TIXHNICAL COMMITIWSHRI N. S. Pwmtim ( Ahernafe )

SHRI BAIIU JACOIJSHRI E. J. ANTO ( Alternate )

SHRI M. S. SULTANIASHRI K. G. NIGAM ( Alternate)

SHRI T. C. SHAMISHIU K. L. BHATIA( Alternate )

CHIIMIST & MUTAI.LURCiIST

D~ B. V. BAPATSHIU M. B. SURVEY( Alternate )

D~ S. K. SAHADR A. N. BANMWI) ( Alfernate )

SHIU DIAWNIXA ACiARWAI.SHIU M. C. SHUKLA( Alfern@e )

SHIU M. M. Gi+OSH

Representing

Asian Paints India Ltd, Mumbai

Addisons Paints and Chemicals Ltd, Chenrmi

Asian Paints ( India ) Ltd, Mumbai

Berger Paints ( India ) Ltd, Kolkata

Central Building Research Institute, Roorkee

Coates of India Ltd, Kolkata

Colour-Chem Ltd, Mumbai

The Development Commissioner ( SS1 ), New Delhi

Ministry of Industry, Department of Industrial Policy and Promotion,New Delhi

Export Inspection Council of India, New Delhi

Goodlass Nerolac Paints Ltd, Mumbai

ICI India Ltd, Kolkatri

Indian Paints Association, Murnbai

The Kerala Minerals and Metals Ltd, Quilon

Ministry of Defence ( DGQA ), Kanpur

Ministry of Defence ( R&D), New Delhi

RDSO, Lucknow

National Organic Chemical Industries Ltd, Mumbai

National Test House, Calcutta

Departmentof Oil and Paint Technology, Kanpur

Shalimar Paints Ltd, Howrah

( Continued on page 7 )

6

IS 14925:2001

( Contimwdfiom page 6 )

Member.r Representing

Stm[M. C. CHOKSI Resins and PlasticsLtd, Mumbai

SHRIS. H. HARSLII.K SudarshanChemical IndustriesLtd, Pune

SHRIP. G. NNK(Ahernate)

SHRI K. RAMAN UNNITHAN Travwrcore Titwrium Products Ltd, Thiruvtrnmrthapuram

DN K. GcJI’INATHANNAll<(A/lerllare)

DR V. K. Vi;RMA Shrimm Institutefor Industrial Research, New Delhi

SHW A. P. SINCiH ( Alternate )

SHRI P. JAYKUMAItAN Dlrectomte General of Supplies and Disposal, New Delhi

SHKI M. A. KHAN ( Alferrmfe )

SHRI VINOD JOSHI Indiwr Small Scale Paint Manufacturers’ Association, Mumbni

SHIU M. B. SATYANAUAYANA Continental Coatings Pvt Ltd, Chennai

REPRIXENTATIW The Indian Turpentine and Rosin Co Ltd, 13areilly

SHIU V. M. NATU Vam Organic Chemicals Ltd, Bhartiagmm, Uttar Pradesh

SHRI LAJINDIX SINLiH, Director General, BIS ( h-officio Member)

Director & Head ( Chem )

Member-Secretary

Dit R. K. S[NtiH

Director (Chem), BIS

Resins Subcommittee, CHD 21:03

Convener

SHRI M. C. CHOKSI

Members

SHRI K. P. JAMUOTKAR

SHRI N1. B. SATYANARAYAN

SHRI G. S. KAMATH

SHIUV. D. Rmmu ( Alternate )

DR K. V. !%SHAORI

Dk A. R. BANOYOPAOHYAYA( Alternate )

SHW D. L. VYAS

SHRI D. L. BHUMKA ( Aherna[e )

Da N. KRISHNAMUI{THY

DR D. S. SITARAMAN ( Ahernnte )

DR SUNH. KUMAR SAHA

SHRI G. N. TEWAIU

DR M. A. .%ENOY

SHRI N. PAREKH

SHRI M. S. SULTANIA

Resins and Plastics Ltd. Mumbai

Asian Paints ( India ) Ltd, Mumbai

Continental Coatings Pvt Ltd, Chennai

Goodlass Nerolac Paints Ltd. Mumbai

ICI India Ltd, Kolkata

Indian Petrochemicals Township, Vadodara

HCT, Hyderabad

National Test House, Kolkata

Punjab Paint Colour rmd Varnish Works, Kanpur

University Department of Chemical Technology ( UDCT ), Mumbai

Noble Synthetics, New Mumbai

Ministry of Defence ( DGQA ), Kanpur

7

.!=4

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i

$’J

harmonious development of the activities of standardization, marking and quality certification of goods and ~:$attending to connected matters in the country. 1.,

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This Indian Standard has been developed from Doc: No. CH D 2 I ( 632 ).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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