Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public.

इंटरनेट मानक

“!ान $ एक न' भारत का +नम-ण”Satyanarayan Gangaram Pitroda

“Invent a New India Using Knowledge”

“प0रा1 को छोड न' 5 तरफ”Jawaharlal Nehru

“Step Out From the Old to the New”

“जान1 का अ+धकार, जी1 का अ+धकार”Mazdoor Kisan Shakti Sangathan

“The Right to Information, The Right to Live”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता है”Bhartṛhari—Nītiśatakam

“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 4518-2 (1971): Methods of test for styrene-butadienerubbers, Part II: Determination of solvent extract and oilcontent [PCD 13: Rubber and Rubber Products]

IS : 4518 ( Part II ) - 1971

Indiun Standard METHODS OF TEST

FOR STYRENE-BUTADIENE RUBBERS

PART II DETERMINATION OF SOLVENT EXTRACT AND OIL CONTENT

( Second Reprint NOVEMBER 1996 )

UDC 678.746.22-136.22 : 543 : 542.61

0 Copyright 1972

BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DEiHI 110002

Gr3 May 1972

IS I 4518 ( Part II,) - 1971

Indian Standard METHOPS OF .TEST

FOR STYRENE-BUTADIENE RUBBERS PART II DETERMINATION OF SOLVENT EXTRACT

AND OIL CONTENT

Rubber Sectional Committee, CDC 42

Chairman

SHRI LALIT MOHAN JAMNADAS

Vice-Chairman

SHRI P. P. M~KHERJEE

Members

SHRI S. C. NANDY ( Altemute to Shri P. P. Mukherjee )

SHRI V. K. BHASKARAN NAIR SHRI K. C. ANANTH ( Alternate )

DR M. L. BHAUMIK

SHRI J. C. CHALY

Representing

The Cosmos India Rubber Works Pvt Ltd, Bombay

Bata Shoe Co Pvt Ltd, Calcutta

Rubber Research Institute of India, Kottayam

Indian Rubber Manufacturers’ Research Association, Bombay

Arakkunnam Co-operative Rubber Marketing Society Ltd, Arakkunnam ( Keraia )

SHRI B. H. DALAL SHRI M. KUMARAN ( Altemute )

DR D. K. DAS SHRI A. GHOSH ( Alternate )

SHRI S. L. GANDHI

Ministry of Defence ( DGI )

National Test House, Calcutta

Ministry of Defence ( R & D ) SHRI M. G. BHARGAWA ( Alternate )

SHRI P. K. MADHAVA MXNON DR K. N. MODAK

Peirce Leslie & Co Ltd,. Coimbatore Indian Rubber Indnstnes Association, Bombay

SHRI B. B. SANGTANI ( Altemnte) SHRI S. MUKHERJEE Assoga;:nntiof Rubber Manufacturers in India,

SHRI L. N. SATHIA ( Alternate ) SKRI P. MUKUNLA MENON Rubber Board, Kottayam SHRI K. K. NAIR Plantation Corporation of Kterala Ltd, Kottayam

SHRI K. A. PAUL ( Alternate ) .%IRI hf. AI. PATEL Synthetiu & Chemicals Ltd, Bombay

SHRI V. C. NANAVATI ( A&mate ) SHRI R. H. PAYLOR Association of Planters of Kerala, Kottayam SHRI K. M. PHILIP Madras Rubber Factory, Madras SHRI D. RAGHUNATH DR N. V. C. RAO

National Chemical Laboratory ( CSIR), Poona Direrrt;elzenflill of Techmml Development,

SHRI K. C. SEKAR Padinjearekara Agencies ( Pvt ) Ltd. Kottayam

( Continued on page 2 )

BUREAU OF INDIAN STANDARDS MANAK T~HAvAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

IS : 4518 ( Part II ) - 1971

( Continuedfrom fiage 1 )

Members Representing

SHRIS.SUBRAM.~NIAN Kanyakumari Distt Planters’ Association, Nagersoil SHRI A. L. N. RAMANATHAN

CH~rrX4a ( Afternote ) SHRI K. C. THOMAS Rubber Dealers’ Association, Kottayam

SHRI T. D. MATHEW ( Altemute ) SHRI M. M. VARCHESE United Planters’ Association of Southern India,

Coonoor SHRI M. M. MUTHIAH ( Alkmate )

SHRI D. DAS &PTA, Director General, IS1 ( Ex-oficio Member ) Director ( Chem )

Secretary

SHRI SATISH CHANDER

Deputy Director ( Chem ), ISI

Methods of Testing Subcommittee, CDC 42 : 1

SHRI V. K. BHASKARAN NAIR SHRI K. C. ANENTH (Alternate)

DR S. N. CHAKRAVAR~ SHRI R. R. PANDIT ( Alternate )

DR D. K. DPS SHRI A. GHOSH ( Alternate )

SHRI W. G. DESAI Da A. S. GHAG ___._. _. _ SHRI P. D. KHEMKA

Indian Rubber Regenerating Co Ltd, Thana Monsanto Chemicals of India Pvt-Ltd, Bombay The Cosmos India Rubber Works Pvt Ltd, Bombay

SHRI PULIN L. KINAR~WALA ( Alternate ) SHRI P. K. MADHAVA MENON Peirce Leslie & Co Ltd. Coimbatore SHRI N. S. NAGARAJA RAO L. G. Balakrishnan & Bros Pvt Ltd, Coimbatore

Rubber Board, Kottayam

Bayer ( India ) Ltd, Bombay

National Test House, Calcutta

SHRI MURARI ~ARMAICAR ( Altematc) SHRI M. M. PATEL Synthetics & Chemicals Ltd, Bombay

SHRI P. P. MAHALINGAM ( Alternate ) SHRI L. N. SATHIA Dunlop India Ltd, Calcutta

SHRI I. DANIEL ( Al&mute ) SHRI K. C. SEKAR Pandinjarekara Agencies ( Pvt ) Ltd, Kottayam

2

IS : 4518 ( Part II ) - 1971

Indian Standard METHODS OF TEST

FOR STYRENE-BUTADIENE RUBBERS PART II DETERMlNATiON OF SOLVENT EXTRACT

AND OIL CONTENT

0. FOREWORD

0.1 This Indian Standard ( Part II ) was adopted by the Indian Standards Institution on 29 October 1971, after the draft finalized by the Rubber Sectional Committee had been approved by the Chemical Division Council.

0.2 Part I of this standard covers the methods of test for determination of the following:

a) Volatile matter by mill method ( SBR : 1 ) and mill oven method (SBR : 2 ),

b) Total ash ( SBR : 3 ),

c) Organic acid content ( SBR : 4 ),

d) Soap content ( SBR : 5 ),

e) Antioxidants ( SBR : 6 ),

f) Bound styrene ( SBR : 7 ), and

g) Mooney viscosity ( SBR : 8 ).

0.3 The methods prescribed in this standard take into consideration the recommendations of International Synthetic Rubber Producers Association. Besides, assistance has also been derived from ,ASTM Designation D 1416-67 T ‘ Chemical analysis of synthetic elastomers ( solids tyrene- butadiene copolymers ) ’ issued by the American Society for Testing and Materials and Draft IS0 Recommendation No. 1407 ‘Determination of solvent extract in natural and synthetic rubber’ issued by International Organization for Standardization.

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*.

*Rules for rounding off numerical values ( revised ).

3

IS : 4518 (Part II ) - 1971

1. SCOPE.

1.1 This standard prescribes the methods of test for determining solvent extract rubbers.

( SBR : 9 ) and oil content ( SBR : 10 ) of raw styrene-butadiene

2. QUALITY OF REAGENTS

2.1 Unless otherwise, specified ‘pure chemicals’ and distilled water ( see IS : 1070-1960* ) shall be employed in tests.

NOTE - ‘ Pure chemicals ’ shall mean chemicals that do not contain impurities which affect the result of analysis.

3. METHOD FOR TAKING OUT SAMPLES

.3.1 The method for taking out samples shall be in accordance ,with the method prescribed in 3 of IS : 4518 ( Part I )-1967t.

Specification for water, distilled quality ( revised ). tMethods of tests for styrene-butadiene rubbers ( SBR ): Part I.

4

lSt4518(PWII)-19’ft

DETERMINATION OF SOLVENT EXTRACT (SBR:9)

0. GENERAL

0.1 Two’ methods~are prescribed here. Method A is based on the method being considered by ISO/TC 45 Rubber, and is recommended as a reference method. Method B is an alternate method and is recommended for routine analysis.

1. SCOPE

1.1 This method is intended to determine the various organic constituents in the rubber as solvent extract. It will give the combined amount of rosin and fatty acids, soaps, oil extenders, defoamer tars, antioxidants and other uncombined organic constituents.

NOTE -The rubber hydrocarbon can alao be estimated by subtracting the sum of the ethanol-toluene azeotrope (ETA) extract. the total ash, and the volatile matter from 100.

METHOD A

2. OUTLINE OF THE METHOD

2.1 A weighed test portion of the rubber is extracted with ethahol-toluene azeotrope solvent in a suitable apparatus. The solvent is distilled off and the residue is dried and weighed.

3. APPARATUS

3.1 Extraction Apparatus -The extraction apparatus is of the reflux type with the condenser placed immediately above the cup which holds the rubber, The cup is situated in the vapour of the boiling solvent and is emptied by a siphon. The apparatus is of glass except in patterns where an extraction cup is suspended from the end of condenser and, in that case, platinum wire is used for the suspension. The apparatus fits together with- out the use of cork, rubber or metal and in such a manner that loss of vapour during extractioh does not exceed 20 percent of the extracting liquid.

3.1.1 Suitable tvnes of apparatus are shown in Fig. 1.

3.2 Filter Paper or Cloth - Acid washed hardened filter paper or nylon cloth of open weave and continuous filaments.

5

1YPE I

175mm MtN

A -joint 34135

TYPE 2

FIG. 1 &cTRACTION APPARATUS

6

IS:4518(PartII)--I971

4. R&AGENTS

4.1 Ethanol-Toluene Azeotrope ( ETA ) - Mix 70 volumes of ethanol (see IS: 321-1964, ) and 30 volumes of toluene ( set IS : 537-1967t). Reflux for four hours over freshly calcined calcium oxide. Distil and collect a middle fraction with a boiling range between 76.2 to 77.2% at atmospheric pressure.

5. PROCEDURE

5.1 Pass the rubber six times between the rolls of a laboratory mill set to a nip not exceeding 0~5 mm. Cut from the sheet a test portion estimated to weigh 3 to 5 g depending on the material to be tested and weigh to the nearest 0.01 g. If it is not possible to pass the sample through the mill, the sample may be cut into pieces less than 1 mm per side. Roll the weighed test portion in filter paper or nylon cloth to form a loose roll from which the rubber cannot fall and so that no part of the rubber is anywhere in contact with any other part of the rubber. Place the roll in the extraction cup ofthe extraction apparatus and pour into the extraction flask sufficient solvent to fill the extraction cup two or three times. Assemble the apparatus and ,adjust the temperature so that the distilled quantity of solvent fills the extraction cup ten to twenty times per hour. The extraction time shall be 16.0 i 0.5 hours. Evaporate off the solvent in a weighed vessel, preferably in the extraction flask, at about 100°C. Dry the flask for two hours at 100 f 2°C in an oven. Cool in a desiccator and weigh to the nearest 0.001 g.

NOTE - The results obtained may be different depending on the method of sample preparation.

6. CALCULATION

6.1 Solvent extract, percent by mass = M %--MI x 100 a

where Ml = mass in grams of the extraction flask and extract, Ma = mass in grams of the extraction flask, and M,= mass in grams of the test portion.

7. REPORT

7.1 The report shall include the following: a) Proper identification of sample, b) Sample preparation,

*Specification for absolute alcohol ( rcviscd) . tspecification for toluene, pure, nitration grade (JsrSr r&a).

7

IS t 4518 ( Part II ) - 1971

c) Type of extraction apparatus, and d) Result obtained.

8. OUTLINE OF THE METHOD

8.1 Thin, narrow strips of the dried rubber are extracted three times with 100 ml of hot ETA ( see 10.1) solvent for one hour each and rinsed three times with 10 ml portions of ETA solvent. Although two extractions are sufficient for non-pigmented rubbers, three extractions are necessary for oil-masterbatch rubbers. The extracted rubber is boiled with 25 ml of acetone, decanted, and dried. The difference in weight between the original sample and the extracted sample is the weight of ETA extract,

9. APPARATUS

9.1 Asbestos Mat

9.2 Filter Paper

9.3 Hot plate

9.4 WideMouth Flask - 400 to 500 ml capacity.

9.5 Wire Gauze

10. REAGENTS

10.1 Ethanol-Toluene Azeotrope ( ETA-) - Prepare by mixing 70 volumes of ethyl alcohol and 30 volumes of toluene, refluxing the mixture for four hours over calcium oxide and distilling. Discard the first and last portion, keeping only that distillate coming over within a range of 1°C.

NOTE -Distilling may be avoided by using absolute alcohol.

10.2 Acetone - conforming to IS : 170-1966’.

11. PROCEDURE

11.1 Dry the sample in accordance with the method prescribed in ( SBR : 1) nor ( SBR : 2 ) of IS : 4518 ( Part I )-1967t. Sheet it to a thickness of 0.5 mm or less. Cut approximately 6 g of the dried, sheeted material into strips not wider than 10 mm nor longer than 50 mm.

NOTE-Ensure ~that the strips are 0.5 mm or less in thickness in order to secure complete extraction.

*Specification for acetone (J;rst reuision ). tMethods of tests for styrene-butadiene rubbers ( SBR ): Part I.

8

IS : 4518 ( Part II ) - 1971

11.2 Accurately weigh 6 g sample of the dried strips. Add 100 ml of ETA ( see 10.1) solvent to the wide-mouth flask. Add each strip of the weighed sample separately to the flask, swirling the flask after each addi- tion so that each strip is thoroughly wetted with the solvent to avoid sticking. To prevent the sample from sticking to the wide-mouth flask, place a filter paper in the bottom of the flask and use a wire gauze or asbestos mat between the flask and the hot plate. Reflux the contents of the wide-mouth flask on the hot plate for one hour. After refluxing, decant the ETA extract and discard it. Add a second 100 ml portion of the ETA solvent to the rubber sample and reflux again for one hour. Again decant the ETA extract and discard it. Add a third 100 ml portion of the ETA solvent to the rubber sample and reflux again for one hour. For the third time., decant the ETA extract and discard it. Rinse the sample with three successive 10 ml portions of the ETA solvent. Add approximately 25 ml of acetone to the rubber sample remaining in the wide-mouth flask. Heat the acetone to gentle boiling and boil it for approximately 5 minutes. Decant the acetone and transfer the extracted sample to a tared watch‘glass. Dryit to constant weight at 105°C.

NOTE -This can be done in 1 hour at 105“C and 725 mm of vacuum in a vacuum oven.

13. CALCULATION

13.1 ETA extract, percent = 100 (Ml-%) M 1

where

Ml = mass in grams of the original dry sample, and

M, = mass in grams of the extracted sample.

9

IS : 4518 ( Part II ) - 1971

DETERMINATION OF OIL (SBR: IO)

1. SCOPE

CONTENT

1.1 This method covers the estimation of the oil content of oil extended ( SBR)-rubbers and carbon black masterbatches. It is intended for use in checking for uniformity having loading up to 75 -parts per hundred of rubber ( phr).

METHOD A

2. OUTLINE OF THE METHOD

2.1 The ETA extract of the dried rubber is determined. The oil content of the masterbatch ise stimated by subtracting from the ETA extract the total of the ETA soluble constituents other than oil. This difference is an estimate of the oil content.

3. PROCEDURE.

3.1 Determine ETA extract in styrene butadiene rubbers as percent by mass of original dry sample ( A ) in accordance with ( SBR : 9 ).

3.2 Determine organic acid in styrene butadiene rubbers as percent by mass of original dry sample ( B ) in accordance with (SBR : 4) [ see IS : 45 18 ( Part I )-1967* 1.

3.3 Determine soap content in styrene butadiene rubbers as percent by mass of original dry sample ( C ) in accordance with (SBR : 5) [ see IS : 4518 ( Part I )-1967* 1.

3.4 Determine antioxidants in styrene butadiene rubbers as percent by mass of original dry sample ( D ) IS : 4518 ( Part I )-1967*].

in accordance with ( SBR : 6 ) [see

NOTE - If antioxidant/antiozonants ( D ) cannot be determined, the following value may be calculated:

D=-;- x100

where

E = nominal antioxidant added to rubber phrt; and

F = ;n;zrbatch recipe, in parts = 100 + phrt of oil $ phrt of carbon

‘Methods of tests for styrene-butadiene rubbers ( SBR ): Part I. tPart.s per hundred of rubber.

10

IS : 4518 ( Part II ) - 1971

4. CALCULATION

4.1 Oil content percent by mass = A - ( B + C +D )

where

A = ETA extract, percent by mass of the original dry sample;

B = organic acid, percent by mass of the original dry sample;

C = soap, percent by mass of ihe original dry sample; and

D I antioxidant/antiozonant, percent by mass of the original dry sample.

METHOD B

5. OUTLINE OF THE METHOD

5.1 The acetone extract of the dried rubber is determined. The oil content ~of the masterbatch is estimated by subtracting from the acetone extract the total of the acetone soluble co@ituents other than the oil. The difference is an estimate of the oil content.

6. APPARATUS

6.1 Extraction Apparatus - The extraction flask and condenser is of the general type prescribed in ( SBR : 9 ),

6.2 Hot Plate - Surface to maintain a temperature of at least 100°C.

6.3 Vacuum Oven

7. PROCEDURE

7.1 Dry the sample in accordance with the method prescribed in SBR: 1 or ( SBR : 2 ) of IS : 4518 ( Part I )-1967*. Sheet it to a thickness of O-5 mm or less. Cut approximately 6 g of the dried, sheeted matetial into strips not wider than 10 mm and not longer than 50 mm.

NOTE -Ensure that the strips are 0.5 mm or less in thickness in order to secure complete extraction.

7.2 Accurately weigh a 2 g sample of the dried strips. Add 200 ml of acetone to a 400 to 500-ml flask. Add each strip of the weighed sample separately to the flask, swirling the flask after each addition so that peach strip is_ thoroughly wetted with solvent to avoid sticking. To prevent the sample from sticking to the flask, place a filter paper in the bottom of the flask, and use a wire gauze or an asbestos mat between the flask and the hot plate. Reflux the contents of the flask on the hot plate for 30 minutes.

I *Methods of tests for styrene-butadiene rubbers ( SBR ) : Part I.

11

IS : 4518 ( Part II ) - 1971

Decant the acetone extract and discard it, but make sure that all the rubber remains in the flask. Add a second 200 ml portion of acetone to the rubber sample and reflux again for 30 minutes. Decant the acetone ex- tract and discard it, but make sure that all the rubber remafns in the flask. Add a third 200 ml portion of acetone to the rubber sample and reflux again for 30 minutes. For the third time, decant the acetone extract and discard it. Rinse the sample with 10 to 20 ml of acetone. Decant the acetone and transfer the extracted sample to a tared watch glass. Dry the rubber to constant weight in a vacuum oven at 105°C and minimum 685 mm of mercury vacuum. Weigh the dry rubber.

8. CALCULATION

8.1 Oil content, percent by mass = lOO(;-*)-(BfC+D)

where

A = mass of the original dry sample;

X = mass of the extracted sample;

B = organic acid, percent by mass ( SBR : 4 );

c = soap, percent by mass ( SBR : 5 ) ; and

_D = antioxidant, percent by mass ( SBR : 6 ).

NOTE - If antioxidant cannot be determined, the following value may be calculated:

D=+ x 100

E = nominal antioxidant added to rubber, phr*; and

F = ;;;rbatch recipe, in parts = 100 + phr* of oil + phr* of carbon

*Parts per hundred of rubber.

12

BUREAU OF INDIAN STANDARDS

Headquarters: Manak Bhavan, 9 Bahadur Shah Zafar Marg, NEW DELHI 110002 Telephones: 323 0131,323 8375,323 9402 Fax :Ql 11 3234062.91 11 3239399

Central Laboratory :

Plot No. 20/Q, Site IV, Sahibabad Industrial Area, Sahibabad 201010

Regional OtTices:

Telegrams : Manaksanstha (Common to all Offices)

Telephone

8-77 00 32

Central : Manak Bhavan, 9 Bahadur Shah Zafar Marg, NEW DELHI 110002 323 76 17

*Eastern : l/14 CIT Scheme Vii M, V.I.P. Road, Manifdola, CALCUTTA 700054 337 66 62

Northern : SC0 335-336, Sector 34-A, CHANDIGARH 160022 60 36 43

Southern : C.I.T. Campus, IV Cross Road, MADRAS 600113 23523 15

fwestern : Manakalaya, EQ, Behind Marol Telephone Exchange, Andheri (East), 832 92 95 MUMBAI 400093

Branch Offices::

‘Pushpak’, Nurmohamed Shaikh Marg, Khanpur, AHMEDABAD 360001

SPeenya Industrial Area, 1st Stage, Bangalore-Tumkur Road, BANGALORE 560056

550 1346

639 49 55

Gangotri Complex, 5th Floor, Bhadbhada Road, T.T. Nagar, BHOPAL 462003 554021

Plot No. 6263, Unit VI, Ganga Nagar, BHUBANESHWAR 751001 40 36 27

Kalaikathir Buildings, 670 Avinashi Road, COIMB~ATORE 641037 21 01 41

Plot No. 43, Sector 16 A, Mathura Road, FARIDABAD 131001 6-26 66 01

Savitri Complex, 116 G.T. Road, GHAZIABAD 201001 6-71 19 96

53/S Ward No.29, R.G. Barua Road, 5th By-lane, GUWAHATI 261003 54 1137

5-8-56C, L.N. Gupta Marg, Nampally Station Road, HYDERABAD 500001 20 10 63

E-52, Chitaranjan Marg, C-Scheme, JAIPUR 302061 37 29 25

117/416 B, Sarvodaya Nagar, KANPUR 206005 21 68 76

Seth Bhawan. 2nd Floor, Behind Leela Cinema, Naval Krrhore Road, 23 8923 LUCKNOW 226001

Patliputra Industrial Estate, PATNA 800013 26 23 05

T.C. No. 14/l 421, University P. 0. Palayam, THIRUVANANTHAPURAM 695034 621 17

Inspection Officer (With Sale Point) : Pushpanjali, 1st Floor, 205-A, West High Court Road, Shankar Nagar Square, 52 51 71

NAGPUR 440010

Institution of Engineers (India) Building 1332 Shivaji Nagar, PUNE 411005 32 36 35

*Sales Office is at 5 Chowringhee Approach, P.O. Princep Street, CALCUTTA 700072

27 1085

fSales Office is at Novelty Chambers, Grant Road, MUMBAI 400007

SSales Office is at ‘F’ Block, Unity Building, Narashimaraja Square, BANGALORE 560002

309 65 28

222 39 71

Printed at Simco Printing Press, Delhi, India