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है”ह”ह

IS 13360-6-14 (2004): Plastics - Methods of Testing, Part6: Thermal Properties, Section 14: Standard Test Method forCoefficient of Linear Thermal Expansion of Plastics between-30°C and 30°C with a Vitreous Silica Dilatometer [PCD 12:Plastics]

IS 13360 (Part 6/See 14) :2004

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Indian Standard

PLASTICS — METHODS OF TESTINGPART 6 THERMAL PROPERTIES

Section 14 Standard Test Method for Coefficient of Linear Thermal Expansion of PlasticsBetween –30°C and 30”C with a Vitreous Silica Dilatometer

ICS 83.080.01

0 BIS 2004

BUREAU OF IN DIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

Septenber 2004 Price Group 2

Plastics Sectional Committee, PCD 12

FOREWORD

This Indian Standard (Part 6/See 14) was adopted by the Bureau of Indian Standards, after the draft finalizedby the Plastics Sectional Committee had been approved by the Petroleum, Coal and Related Products DivisionCouncil.

The test method covered in this standard is intended to provide a means of determining the coefficient of linearthermal expansion of plastics which are not distorted or indented by the thrust of the dilatometeron the specimen.For materials that may indent (see 4.4). The specimen is placed at the bottom of the outer dilatometer tube withthe inner one resting on it. The measuring device, which is firmly, attached to the outer tube is in contact withthe top of the inner tube and indicates variations in the length of the specimen with changes in temperature.Immersing the outer tube in a liquid bath or other controlled temperature environment maintained at the desiredtemperature brings about temperature changes.

While preparing this standard, considerable assistance has been derived from ASTM D 696-1998 ‘Standard testmethod for coefficient of linear thermal expansion of plastics between –30°C and 30°C with a vitreous silicadilatometer’ issued by the American Society for Testing and Materials (ASTM), USA.

The composition of the Committee responsible for formulation of this standard is given in Annex A

For tropical countries like India, the standard temperature and the relative humidity shall be taken as 27 t 2°Cand 65 f 5 percent respectively.

In reporting the results of a test or analysis made in accordance with this standard, if the final value, observedor calculated, is to be rounded off, it shall be done in accordance with IS 2: 1960 ‘Rules for rounding offnumerical values (revised)’.

IS 13360 (Part 6/See 14): 2004

Indian Standard

PLASTICS — METHODS OF TESTINGPART 6 THERMAL PROPERTIES

Section 14 Standard Test Method for Coefficient of Linear Thermal Expansion of PlasticsBetween –30°C and 30°C with a Vitreous Silica Dilatometer

1 SCOPE

1.1 This standard (Part 6/See 14) describes a methodfor determination of the coefficient of linear thermalexpansion for plastic materials having coefficients of

expansion greater than 1 x 10+ “C by use of a vitreoussilica dilatometer.

NOTE — At the test temperatures and under the stressesimposed, the plastic materials shall have a negligible creep orelastic strain rate or both, in so far as these properties wouldsignificantly affect the accuracy of the measurements.

1.2 This test method shall not be used formeasurements on materials having a very lowcoefficient of expansion (less than 1 x 10+ “C).

2

NOTES1 For materials having very low coefficient of expansion,interferometer or capacitance techniques are recommended.2 The thermal expansion of a plastic is composed of a reversiblecomponent on which are superimposed changes in length due tochanges in moisture content, curing, loss of plasticizer orsolvents, release of stresses, phase changes and other factors.This test method is intended for determining the coefficient oflinear thermal expansion under the exclusion of these factors asfar as possible. In gerreral, it will not be possible to exclude theeffect of these factors completely. For this reason, the testmethod can be expected to give only an approximation to thetrue thermal expansion.

SIGNIFICANCE AND USE

The coefficient of linear thermal expansion, ctbetweentemperatures TI and Tz for a specimen whose length isLo at the reference temperature, is given by thefollowing equation:

u = (L2 – L1)/[~(Tz – Tl)] = AL/~AT

where, L.l and Lz are the specimen lengths attemperatures 7’1and Tz respective y. u is, therefore,obtained by dividing the linear expansion per unitlength by the change in temperature.

The nature of most plastics and construction of thedilatometer make –30°C to +30”C a convenienttemperature range for linear thermal expansionmeasurements of plastics. This range covers thetemperatures in which plastics are most commonlyused. Where testing outside of this temperature rangeor when linear thermal expansion characteristics of a~articular plastics are not known through thistemperature range, particular attention shall be paid to

the factors mentioned (see 1.2 Notes) and specialpreliminary investigations by thermo-mechanicalanalysis for the location of transition temperatures,may be required to avoid excessive error.

Other ways of locating phase changes or transitiontemperatures using the dilatometer itself may beemployed to cover the range of temperatures inquestion by using smaller steps than 30”C or byobserving-the rate of expansion during.a steady rise intemperature of the specimen. Once such a transitionpoint has been located, a separate coefficient ofexpansion for a temperature range below and abovethe transition point shall be determined. Forspecification and comparison purposes, the range from–30”C to +30°C (provided it is known that notransition exists in this range) shall be used.

3 APPARATUS

3.1 Fused Quartz Tube Dilatometer, suitable forthis test method is illustrated in Fig. 1. A clearance ofapproximately 1 mm is allowed between the inner andouter tubes.

3.2 Device for measuring the changes in length (dialgauge, LVDT, or the equivalent) is freed on themounting fixture so that its position may be adjustedto accommodate specimens of varying length(see 4.2). The accuracy shall be such that the error ofindication will not exceed ~ 1.0 pm for any lengthchange. The weight of the inner silica tube plus themeasuring device reaction shall not exert a stress ofmore than 70 kPa on the specimen so that the specimenis not distorted or appreciably indented.

3.3 Scale or Caliper, capable of measuring theinitial length of the specimen with an accuracy of* 0.5 percent.

3.4 Controlled Temperature Environment, tocontrol the temperature of the specimen. Arrange thebath so a uniform temperature is assured over thelength of the specimen. Means shall be provided forstirring the bath and for controlling its temperaturewithin f 0.2°C at the time of the temperature andmeasuring device readings.

1

IS 13360 (Part 6/See 14): 2004

THREADED

DIAL GAGEGRAD. IN.001 MM

(.0001 IN.)c

TFOR RECORDING

I L.V.D.T.

JUSTING

t Jgw

BLOCK

/I-J

- VITREOUS SILICA ROD

= VITREOUS SILICA TUBE

– SPECIMEN50 MM(2 IN.)– 125 MM(5in.) LG.

-15 MM(.5901N.)

FIG. 1 QUARTZ-TUBEDILATOMETER

NOTE —If a fluid bath is used, it is preferable and not difficultto avoid contact between the bath liquid and the testspecimens. If such contact is unavoidable, take care to select afluid that will not affect the physical properties of the materialunder test.

3.5 Thermometer or Thermocouple — The bathtemperature shall be measured by a thermometer orthermocotrple capable of an accuracy of + O.l“C.

4 TEST SPECIMENS

4.1 The test specimens may be prepared bymachining, molding or casting operations underconditions, which give a minimum of strain oranisotropy. If anisotropy is suspected on the samplescut the specimens along the principal axes ofanisotropy and the coefficient of linear thermalexpansion shall be measured on each set of specimens.Annealing of the specimens may remove anisotropyeffects due to processing or preparation.

4.2 The specimen length shall be between 50 mm and125 mm.

NOTE — If specimens shorter than 50 mm are used, a loss insensitivity results. If specimens greatly longer than 125 mm areused, the temperature gradient along the specimen may becomedifficult to controt, within the prescribed limits. The length usedshatl be governed by the sensitivity and range of the measuringdevice, the extension expected and the accuracy desired.Generally speatdng the longer the specimen and the moresensitive the measuring device, the more accurate will k thedetermination if the temperature is well controlled.

4.3 The cross-section of the test specimen may beround, square, or rectangular and shall fit easily intothe measurement system of the dilatometer withoutexcessive play on the one hand or friction on the other.The cross-section of the specimen shall be largeenough so that no bending or twisting of the spec~menoccurs. Convenient specimen cross-sections are12.5 mm x 6.3 mm, 12.5 mm x 3 mm, 12.5 mm indiameter or 6.3 mm in diameter. If exce-ssive play isfound with some of the thinner specimen, guidesections may be cemented or otherwise attached to thesides of the specimen to fill out the space.

2

4.4 Cut the ends of the specimens flat andperpendicular to the length axis of the specimen.Protect the ends against indentation by means of flat,thin steel plates cemented or otherwise firmly attachedto them before the specimen is placed in thedilatometer. These plates shall be 0.3 to 0.5 mm inthickness.

5 CONDITIONING

5.1 Conditioning

Condition the test specimens at 27 * 2°C and 65 f 5percent relative humidity for not less than 40 h priorto test unless otherwise specified in the relevantproduct specification. In cases of disagreement, thetolerances shall be tl°C and t2 percent relativehumidity.

5.2 Test Conditions

Conduct tests in the standard laboratory atmosphere of27 f 2°C and 65 i 5 percent relative humidity, unless

otherwise specified in the relevant productspecification. In cases of disagreement, the tolerancesshall be * 1°C and t 2 percent relative humidity.

6 PROCEDURE

6.1 Measure the length of two conditioned specimensat room temperature to the nearest 25 ~m with the scaleor caliper (see 3.3).

6.2 Cement or otherwise attach the steel plates to theends of the specimen to prevent indentation (see 4.4).Measure the new lengths of the specimens.

6.3 Mount each specimen in a dilatometer. Carefullyinstall the dilatometer in the –30°C controlledenvironment. If liquid bath is used, make sure the topof the specimen is at least 50 mm below the liquid levelof the bath. Maintain the temperature of the bath inthe range from –32°C to –28 i 2°C until thetemperature of the specimen along the length isconstant as denoted by no further movement indicatedby the measuring device over a period of 5 to 10 min.Record the actual temperature and the measuringdevice reading.

6.4 Without disturbing or jarring the dilatometer,change to the +30”C bath, so that the top of thespecimen is at least 50 mm below the liquid level ofthe bath. Maintain the temperature of the bath in therange from 28°C to 32 * 0.2°C until the temperatureof the specimen along the length is constant as denotedby no further movement indicated by the measuringdevice over a period of 5 to 10 min. Record the actualtemperature and the measuring device reading.

6.5 Without disturbing or jarring the dilatometer,change to –30°C and repeat the procedure given in 6.3.

NOTE — It is convenient to use alternately two baths at theproper temperatures. Great care shall be taken not to disturb theapparatus during the transfer of baths. Tall thermos bottles havebeen successfully used. The use of two baths is preferred

IS 13360 (Part 6/See 14) :2004

because tlrk shall reduce the time required to bring the specimento the desired temperature. The test shall be conducted in asshort a time as possible to avoid changes in physical propertiesduring long exposures to high and low temperatures that mightpossibly take place.

6.6 Measure the final length of the specimen at roomtemperature.

6.7 If the change in length per degree of temperaturedifference due to heating does not agree with thechange in len@h per degree due to cooling within 10percent of their average, investigate the cause of thediscrepancy and, if possible, eliminate. Repeat the testuntil agreement is reached.

7 CALCULATION

7.1 Calculate the coefficient of linear thermalexpansion over the temperature range used as follows:

a = AL/LoAT

wherea=

AL =

~.

AT =

average coefficient of linear thermalexpansion, per “C,change in length of test specimen due toheating or to cooling,length of test specimen at room temperature(AL and La being measured in the sameunits), andtemperature differences, “C, over which thechange in the length of the specimen ismeasured.

The values of a for heating and for cooling shall beaveraged to give the value to be reported.

NOTE — Correction for thermal expansion of silica is4.3 x 10-7 “C. If requested, this value should be added to the

calculated value to compensate for the expansion of the

appamtus equivalent to the length of the specimen. If thickmetal plates are used, appropriate correction may also bedesirable for their thermal expansions.

8 REPORT

8.1 The report shall include the following:

a)

b)c)d)e)

f)

g)

h)

3

Designation of material, including name ofmanufacturer and information on compositionwhen known;Method of preparation of test Specimen;Form and dimensions of test specimen;Type of apparatus used;.Temperatures between which the coefficientof linear thermal expansion has been deter-mined;Average coefficient of linear thermal expan-sion, per ‘C, for the two specimens tested;Location of phase change or transition pointtemperature, if this is in the range of tempera-tures used; andComplete description of any unusualbehaviour of the specimen, for example,differences of more than 10 percent inmeasured values of expansion and contraction.

-IS 13360 (Part 6/See 14) :2004

ANNEX A

( Foreword)

COMMITTEE COMPOSITION

Plastics Sectional Committee, PCD 12

OrganizationBorouge Pvt Ltd, MumbaiAll lndla Plastic Industries Association, Delhi

Central Institute of Plastics Engineering& Technology (CIPET),Chennai

Central Food Technological Research Institute (CITRI), Mysore

Directorate General of Health Services, New Delhi

Gas Authority of India Ltd, Noida

GE Plastics India Limted, Gurgaon

Gharda Chemicals Ltd, Distt Thane

Gujarat State Fertilizers& Chemicals Limited, Vadodara

Haldia Petrochemicals Limited, Kolkata

Indian Centse for Plastics in the Environment, New DelhiIndian Institute of Packaging, Mumbai

Indian Petrochemicals Corporation Lknited, Vadodara

Industrial Toxicology Research Centre (ITRC), Lucknow

Jain Irrigation Systems Ltd, Jalgaon

Machino-Basell India Limited, Gurgaon

Ministry of Defence (DMSRDE), Kanpur

Ministry of Environment& Forests, New Delhi

National Chemical Laboratory, Pune

Reliance Industries Ltd, Mumbai

Saint-Gobain Vetrotex India Ltd, Thimmapur

Shriram Institute for Industrial Research, Delhi

Supreme Petrochem Ltd, Mumbai

VIP Industries Ltd, Nasik

XPROIndia Ltd, Faridabad

BIS Directorate General

Representative(s)SHRIP. R. SINGHVI(Cfrairrnan)SHRIRAW K. AGGARWAL

SHR~V. P, BHARDWAJ(Alternate)DR SUSHILK. VERMA

SHRI S. K. SHARMA(Altemare)DR V. PRAKASH

SHRIK. R. KUMAR(A/?emate)ASSISTANTDIREaOR GENERAL(PFA)

TECHNICALOFFICER(PFA) (Alternate)SHRISHIVAJtBASU

SHRIMANJSHKHANOELWAL(Alternate)SHRIP. V. MURALIMOHAN

SHRIGOPALMAJUMDAR(Ahemare)DR B. K. DESAI

DR H. P. NATU (Alternate)SHRIRAMESHKUMAR

DR 1’. P. SINGH(Alternate)DR SWAPANDHAR

SHRIAMtTAVASANYAL(Alternate)DR A. N. BHATSHRIRAJW DHAR

DR N. G. MOKASHI(Alternate)SHRI A. K. KHERA

SHRIV. C. FRANCIS(Alternate)DR V. P. SHARMA

DR A. K. AGARWAL(Alternare)DR H. C. MRUTHYUNJAYA

SHRIS. B. JOSHI(Alternate 1)SHRIA. P. CHOUOHARY(Alternare II)

SHRISANJEEVKUMARVARSHNEYSHRIDEEPBANERJEE(Alternate)

DR R. K. SINGHSHRIR. K. GUPTA(Alternate)

DR (SHRJMATI)INDRANICHANDRASEKHARANDR U. SMDHARAN(Aftemate)

DR B. D. SARWADEDR P. G. SHUKLA(Alternate)

DRY. B. VASUDEODR U. K. SARCOP(A1/ernate)

SHRI D..H. KASHYAPSHRIM. A. NAEER(Akernate)

DR P. K. KAICKERDR R. K. RAINA(Alternate)

SHRIP. B. RAMANSHRI.ANIMJDHABHIDE(Alternate)

SHRJSIDDHARTHAROYSHSUS. GOPAKUMAR(Alternate)

SHRIC. BHASKARSHRIMANMOHANKRISHAN(Alternate)

SHRJANJANKAR. Director& Head(pCD)[RepresentingDirectorGeneral(JI.&@cio)]

Member SecretarySHRIA. K. BHATNAGAR

Joint Director (PCD), BIS

4

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This Indian Standard has been developed from Doc : No. PCD 12 (1792).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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