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IS 4511-3 (1987): Methods of Test for Styrene-butadiene Rubber (SBR) Latices, Part 3: Determination of Volatile Unsaturates [PCD 13: Rubber and Rubber Products]
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IS : 4511 ( Part 3 ) - 1987 Indian Standard METHODS OF TEST FOR STYRENE-BUTADIENE RUBBER ( SBR ) LATICES
PART 3 DETERMINATION OF VOLATILE UNSATURATES
[SBRL:8]
( First Revision )
Rubber Sectional Committee, PCDC 14
Chairman Reprcscnting SHRI LALIT MOHAN JAM>.~DAB Cosmos India Rubber Works Pvt Ltd, Bombay
Members SHRI SATISH ABRAHAX Padinjarekara Agencies Ltd, Kottayam SHRI 0. P. AGARWAL Transasia Carpets Ltd, Sikandrabad SXRI J. N. JEA ( Alternate ) SHRI A. K. BANDYOPADRAYA Ministry of Defence ( DGI ) SHRI V. BHATTACHARYA ( Aftcrnate ) DR B. BANERJEE Carbon and Chemicals India Ltd, Cochin Da D. BANERJEE Escon Consultants Pvt Ltd, Calcutta DR P. S. BHARGAVA IEL Ltd, Chemicals Division, Calcutta SI~RI N. C. SAMAJDAR ( Alternate ) DR S. N. CHAI @ Cofiydght 1987 BUREAU OF INDIAN STANDARDS This publication is protected under the In&an Copyriqht Acf ( 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 : 4511 ( Part 3 ) - 1987 ( Continuedfrom page 1 ) Members Representing SERI K. J, JOSEPH The Plantation Corporation of Kerala Ltd, Kottayam SRRI K. T. VER~HESE ( Aldernate) SHRI K. N. KOSHY M. M. Rubber Co Ltd, Madras SHRI N. SUBRAnfANrAN ( Alternate ) SHRI P. K. MADHAVA MENON Thirumbadi Rubber Co Ltd, Mokkam SHRI M. PUSHKARAK SHAN ( Alternate ) SHRI A. K. MALLIK Indian Petrochemicals Corporation Ltd, P.O. Petro- chemicals, Vadodara SHRI GOPAL KRISHNAN ( Allernatc ) SHRI D. W. MCCRIRICK Association of Planters of Kerala, Cochin SHRI P. K. MENON ( Alternate) SHRI P. K. MENON United Planters Association of Southern India, Coonoor SHRI E. B. UNNI ( Alternate ) SHRI P. F. MILLER Directorate -General of Supplies & Disposals, New Delhi DR W. MILLNS Indian Rubber Manufacturers Research Association, Thane SHRI N. B. FE~ADE ( Alternate ) SH%~ R. R. PANDIT Bayer ( India ) Ltd, Bombay SHRI D. J. BARUCHA ( Alternate ) SHRI S. A. PASHA London Rubber Co ( India ) Ltd, Madras SERI R. KRISHNAN ( Alternate ) SEiRl i% G. PAUL Arakkunnam Cooperative Rubber Marketing Society Ltd, P.O. Arakkunnam SHXI A. RAJAMANI Auto;o$;e,hyre Manufacturers’ Association. e SHRI A. GEORGE JOHN ( Alternate ) Dn S. K. RAY Tyre Corporation of India Ltd, Calcutta SERI S. B. SAREAR ( Alternate) REPRESENTATIVE Ministry of Defence ( R & D ) SHRI H. C. PERTI ( Alfernate ) SHRI S. V. SARMA Travancore Rubber & Tea Co Ltd. Trivandrum SERF C. S. KRIBHNASWAMY ( Alternate ) SHRI A. SEN Dunlop India Ltd, Calcutta SHRI K. S. LOCANATHAN ( Alfernate ) SRRI RAJINDER SINQH State Trading Corporation of India Ltd, Bombay SHRI 0. P. ARORA ( Affernatr ) DR E. V. THOMAS Rubber Research Institute of India, Kottayam DR M. G. KUMARAN ( Alternate ) DR E. V. TROMAS Rubber Board, Kottayam DR N. M. MATEEW ( Alternate ) SRRI M. S. SAXENA, Director General, BIS ( Ex-o@io Member ) Director ( P & C ) Secretary SHRI DILEEP KUMAR Assistant Director ( P & C ), BIS ( Contirtued on page 11 ) IS : 4511 ( Part 3 ) - 1987 Indian Standard METHODS OF TEST FOR STYRENE-BUTADIENE RUBBER ( SBR ) LATICES PART 3 DETERMINATION OF VOLATILE UNSATURATES [SBRL:8] (First Revision ) 0. FOREWORD 0.1 This Indian Standard ( Part 3 ) ( First Revision ) was adopted by the Indian Standards Institution on 27 February 1987, after the draft finalized by the Rubber Sectional Committee had been approved by the Petroleum, Coal and Related Products Division Council. 0.2 Test methods for rubber latex had been originally covered in the following Indian Standards: For natural rubber latex IS : 3708 ( Part 1 )-1966* IS : 3708 ( Part 2 )-1968t For styrene butadiene rubber latex IS : 4511 ( Part 1 )-1967% Since some of the test methods covered in above standards were common, the concerned committee had decided some years ago to unify and publish a separate series of methods of test which would be appli- cable to all types of latices - natural as well as synthetic. Accordingly, the following six test methods had been covered under IS : 9316: IS : 9316 Methods of test for rubber latex: Part l-1 979 Determination of surface tension Part 2-1979 Determination of viscosity -*Methods of test for natural rubber latex: Part 1 Dry rubber content, sludge content, density, total alkalinity, KOH-number, mechanical stability, volatile fatty acid number, pH, total nitrogen, total copper, total iron, total manganese and total ash. +Methods of test fornatural rubber latex, Part 2. *Methods of test for styrene-butadiene rubber ( SBR ) latices: Part 1 Determination of dry polymer, pH, density, residual styrene, bound styrene and soap content. 3 IS : 4511 ( Part 3 ) - I987 Part 3- 1979 Determination of coagulum content Part 4-1979 Determination of total solids content Part 5-1979 Drawing of samples Part 6-1982 Determination of @I 0.2.1. As a result of further rethinking on the subject, it has now been decided to re-designate the test methods common to natural and synthetic rubber latices as RL series; test methods for natural rubber latex, as NRL series and test methods for styrene-butadiene rubber latex as SBRL series. Consequently, test methods for rubber latex have been rationa- lized into the following three series: a) IS : 9316 Unified methods of test applicable to both natural and synthetic rubber latices - RL series; b) IS : 3708 Methods of test applicable to natural rubber latex - NRL series; and c) IS : 4511 Methods of test applicable to styrene-butadiene rubber latex - SBRL series. 0.3 The existing Indian Standards under IS : 3708 ( Parts l* and 2t ), IS : 4511 ( Part 1$ ) and IS : 9316 ( Parts 1 to 6 ) are being gradually replaced by separate standards under the above three series, designated by the appropriate NRL, SBRL, or RL series, respectively. 0.3.1 The methods covered under NRL : 13 NRL : 14 and NRL : 15 of IS 3708 ( Part 1 )-1966 are now being covered under the RL series in IS : 93 16 ( under revision ) . 0.4 In order to facilitate cross-reference, it has been decided to retain the original discrete SBRL series numbers assigned to various test methods in IS : 4511 ( Part l$ ), in the revised parts of IS : 4511. 0.4.1 For proper referencing of the existing test methods and the new methods under revision, a statement showing corresponding methods is given in Appendix A. 0.5 In preparing the above series, the need to align the test methods with the corresponding IS0 standards/DIS/DP wherever available has also been takeninto account for updating the test methods. In the prepara- tion of this standard, assistance has been derived from the following publication: I’Methods of test for natural rubber latex: Part 1 Dry rubber content, sludge content, density, total alkalinity, KOH-number! mechanical stability, volatile fatty acid number, pH, total nitrogen, total copper, total non, total manganese and total ash. tMethods of test for natural rubber latex, Part 2. SMethods of test for styrene butadiene rubber ( SBR ) latex: Part 1 Determination of dry polymer, pH, density, residual styrene, bound styrene and soap content. 4 IS : 4511 ( Part 3 ) - 1987 IS0 2008-1980 Rubber latex, styrene-butadiene - Determination of volatile unsaturates. International Organization for Standardiza- tion. 0.5.1 In the first edition of IS : 2008-1972 Methods for determination of both volatile unsaturates and residual styrene in styrene.butadiene rubber latices were prescribed. On review of IS0 2008 the method for volatile unsaturates was retained but the ultra-violet spectrophotometric method for residual styrene was withdrawn as it was not sufficiently specific to styrene and was little used. Accordingly, IS0 2008-1980 ( revised ) covers volumetric method for volatile unsaturates only. A gas chromatographic method specific to residual styrene is expected to form the subject of a future international standard. 0.5.2 Originally the method of determination of residual styrene ( volatile unsaturates ) in styrene-butadiene rubber latex was published as SBRL : 8 of IS : 4511 ( Part I )- 1967 covering two methods, namely volumetric and UV spectrophotometric method. In accordance with the latest international thinking, the Committee decided to include only the volumetric method and accordingly the caption of the test method has been amended to ‘Determination of volatile unsaturates’. However, the Committee is not convinced of the non-specificity of the spectro- photometric method. Accordingly, it has been decided to carry out the inter-laboratory investigation for generation of comparative data on the two test methods, namely volumetric and spectrophotometric method using samples, specially admixed with known quantities of residual styrene to establish the repeatability and reproducibility as well as the specificity of the UV spectrophotometric method. 0.6 In reporting the results 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 3 ) prescribes a method for the determination of volatile unsaturates in styrene-butadiene rubber latices. 1.2 This method measures, in addition to residual styrene, other unsaturates such as butadine dimer. 2. OUTLINE OF THE METHOD 2.1 Methanol is added to a test portion and the mixture is distilled. Potassium bromide-bromate solution is added to the distillate followed by potassium iodide. The liberated iodine is titrated with so&urn thiosulphate. *Rules for rounding off numerical values ( wised ). 5 IS : 4511 ( Part 3 ) .- 1987 3. APPARATUS 3.1 Dean and Stark-Distillation Apparatus - Including a distillation flask of capacity 500-ml and a 25-ml receiver, or equivalent distillation apparatus with ground glass joints. 3.2 Iodine Flask - 250-ml capacity. 4. REAGENTS 4.1 Methanol Reagent - Methanol containing 100 mg/kg ( 100 ppm ) of p-tert butyl catechol or an equivalent polymerization inhibitor. 4.2 Standard Potassium Bromide - Potassium Bromate Solution - 0.1 N. Dissolve 2784 g of potassium bromate ( KBrOs ) and 10.0 g of potassium bromide ( KBr ) in water and dilute to 1 000 ml in a volumetric flask. 4.3 Sulphuric Acid Solution - 18 percent ( m+n ). 4.4 Potassium Iodide Solution - 10 percent ( m/m ). 4.5 Standard Sodium Thiosulphate Solution - 0.1 N. 4.6 Starch Indicator Solution 5. PROCEDURE 5.1 Weigh 25.0 k 0.2 g of latex into the distillation flask. Add 25 ml _ of water and 25 ml of the methanol reagent to the test portion. Distil the mixture, adjusting the rate of control frothing, and collect the first 25 ml of distillate in the receiver. 5.2 Transfer the distillate to the iodine flask and rinse the condenser and receiver into the iodine flask with 20 ml of the methanol reagent. If desired, the distillate may be collected in the iodine flask. From a burette add 20 ml of the potassium bromide-potassium bromate solution and cool the solution~to 27 f 2°C. Rapidly add 15 ml of the sulphuric acid solution, stopper the flask, slrake, and add water to the funnel lips as a vapour seal. If no yellow cOlour remains after allowing the flask to stand for at least one minute, add successive 10 ml portions of the bromide-bromate solution until a slight yellow colour persists for one min after the addition. Make the additions by running the solution from the burette into the funnel lip and lifting the stopper so that the solution enters the flask around the stopper. Wash the funnel lip with water in the same manner and seal with water. After the final addition of the bromide-bromate solution, add 10 ml of the potassium iodide solution to the funnel lip and lift the stopper to allow the solution to enter the flask around the stopper. Shake the flask and contents and titrate the liberated iodine with the sodium thiosulphate solution to G IS : 4511 ( Part 3 ) - 1987 a faint yellow colour. Add 1 ml of the indicator solution and continue the titration with the sodium thiosulphate solution until the solution is colourless. 5.3 Carry out a blank test by repeating the procedure, but using 25 ml of water in place of the test portion. 6. CALCULATION 6.1 Calculate the percentage of volatile unsaturates as follows: Volatile unsaturates ( as stprene ), percent by mass = 0.208 x .N ( V, - I’2 ) where fl = normality of the sodium thiosulphate solution; VI = volume, in ml, of sodium thiosulphate solution used in the blank test; and V2 = volume, in ml, of sodium thiosulphate solution used in the determination. APPENDIX A ( Clause 0.4.1 ) TAB&E SHOWING CORRESPONDENCE OF THE VARIOUS METHODS OF TEST CONVERTED IN THE EXISTING IS : 9316 ( PARTS 1 TO 5 )-1979, IS : 9316 ( PART 6 )-1982, IS : 3708 ( PART 1 )-1966, IS : 3708 ( PART 2 )- 1968, IS : 4511 ( PART 1 )-1967 WITH THE REVISION/PROPOSED REVISION OF IS : 9316, IS : 3708 AND IS : 4511 EXISTING TEET METHODS PROPOSED REVWONS REMARKS ~~~~~_~_~~~~_h~_~~_,_~___-_~ Test Method IS No. Part ( Series) ’ IS No. Series . (1) (2) (3) (4) (5) (6) RL SERIES Determination of surface IS : 9316-1979 Part 1 IS : 9316 Part 1 ( RL:l ) co tension Determination of viscosity IS : 9316-1979 Part 2 iS : 9316 Part 2 ( RL:2 ) Determination of coagu- TS : 9316-1979 Part 3 IS : 9316 Part 3 ( RL:3 ) lum content Determination of total IS : 9316-1979 Part 4 IS : 9316 Part 4 ( RL:4) 1 solids content [Under Drawing of samples IS : 9316-1979 Part 5 IS : 9316 Part 56 (RL:5)( RL:6 ) [ ?zi- Determination of PH IS : 9316-1982 Part 6 J Determination of total IS : 3708-1966 Part 1 (NRL:I3) IS : 9316 Part 7 ( RL:7 ) copper Determination of total IS : 3708-1966 Part 1 (NRL:14) IS : 9316 Part 8 (RL:8 1 iron Determination of total IS : 3708-1966 Part 1 (NRL:15) JS : 9316 Part 9 ( RL:9 > manganese NRLZSERIES Determination of dry IS : 3708-1966 Part 1 ( NRL:I ) IS : 3708-1985 Part 1 ( NRL: 1) rubber content Determination of sludge IS : 3708-1966 Part 1 ( NRL:5 ) IS : 3708- 1985 Part 2 ( NRL:5 ) content Determination of density IS : 3708-1966 Part 1 (NRL:6 ) IS : 3708-1985 Part 3 ( NRL:6 ) Determination of total IS : 3708-1966 Part I ( NRL:7 ) IS : 3708-1985 Part 4 ( NRL:7 ) alkalinity Determination of KOH- IS : 3708-1966 Part 1 ( NRL:8 ) IS : 3708-1985 Part 5 ( NRL:8 ) number Determination of mech- IS : 3708-1966 Part 1 ( NRL:9 ) IS : 3708-1985 Part 6 ( NRL:9 ) co anical stability Determination of vola- IS : 3708-1966 Part 1 (NRL:lO ) IS : 3708-19136 Part 7 ( NRL:IO ) tile fatty acid number Determination of total IS : 3708-1966 Part 1 ( NRL:12 ) 1S : 3708 Part 8 ( NRL:12 ) nitrogen 5: Determination of total IS : 3708-1966 Part 1 (NRL:16) IS : 3708-l 986 Part 9 ( NRL: 16 ) 2 ash 2 Determination of boric, IS : 3708-1968 Part 2 ( NRL:17 ) IS : 3708-1986 Part 10 ( NRL:17 ) ,’ acid r+$ Determination of IS : 3708-1968 Part 2 (NRL:18 ) IS : 3708-1386 Part 11 (NRL:18) w magnesium V I Y 6 ( Continued) 3 TABLE SHOWING CORRESPONDENCE OF THE VARIOUS METHODS OF ; TEST CONVERTED IN THE EXISTING IS : 9316 ( PARTS 1 TO 5 )-1979, .. IS : 9316 ( PART 6 )-1982, IS : 3708 ( PART 1 )-1966, IS : 3708 ( PART 2 )- 6 c1 1968, IS : 4511 ( PART 1 )-1967 WITH THE REVISION/PROPOSED m REVISION OF IS : 9316, IS :3708 AND IS : 4511 - Cord h w EXISTING TEST METHODS PROPOSEDREVISIONS REMARKS $ cc r------h___-_-----_-~ ~---_-_*_-_~--~ W Test Method IS No. Part (Series) IS No. Series V (0 (2) (3) (4) (5) (6) i SBRL SERIES 2 Determination of dry IS : 4511-1967 Part 1 ( SBRL:l ) IS : 4511-1986 Part 1 ( SBRL:l ) polymer -. Determination ofdensity TS : 4511-1967 Part 1 ( SBRL:6 ) IS : 4511 Part 2 ( SBRL:6 ) E; Determination of vola- IS : 4511-1967 Part 1 ( SBRL:8 ) IS : 4511 Part 3 ( SBRL:8 ) tile unsaturates Determination of bound IS : 451 I-1967 Part 1 ( SBRL:9 ) IS : 4511 Part 4 ( SBRL:9 ) styrene Determination of soap IS: 4511-1967 Part 1 (SBRL:lO) IS : 4511 Part 5 ( SBRL: 10 ) content Determination of high- - - IS : 4511 Part 6 ( SBRL: 11 ) speed mechanical stability 1s : 4511 ( Part 3 ) - 1987 ( Continued from page 2 ) , Methods of Testing Subcommittee, PCDC 14 : 1 Convener Representing SHRI S. K. MUSTAFI Modi Rubber Ltd, Modipuram Members SRRI ABHIK CRA~TERJI ( Altcrnalc to Shri S. K. Mustafi ) SHRI SATISH ABRAHAM Padinjarekara Agencies Ltd, Kottayam SHRI P. S. BALASUBRAMANIAM L. G. Balakrishnan & Bros Ltd, Coimbatore SHRI S. KUMAR ( Alternate ) SHRI A.N. BHATTACHARYA Union Commercial and Industrial Co Pvt Ltd, Calcutta SHRI B. PANJA ( Alternate ) SHRI J. CHATTERJEE Andrew Yule & Co Ltd, Calcutta SHRI A. K. BISWAS ( Alternate ) :SHRI P.K. CHATTERJEE Bayer ( India ) Ltd, Bombay SHRI D. J. BARUCHA ( Alternate ) SERI H. C. CHOPRA Synthetics and Chemicals Ltd, Bombay DR R. N. MEHROTRA ( Alternate ) SHRI J. M. GAH~ Directorate General of Technical DeveloDment.. I New Delhi SHRI K. R. GARB Ministry of Defence ( DGI ) SHRI P. L. NAO ( Alternate ) .~HRI C. S. INAYDAR Polyolefins Industries Ltd, Bombay SHRI V. K. SUD ( Alternate ) SHRI A.GEORQE JOHN MRF Ltd, Madras SHRI P. L. KINARIWALA Cosmos India Rubber Works Pvt Ltd, Bombay SHXZIN. M. REQE ( Alternate ) SHRI K. S. LOQANATRAI~ Dunlop India Ltd, Calcutta SHRI J. C. BOSE ( Altcrnate ) SHRI P. K. MADHAVA MENON Thirumbadi Rubber Co Ltd,~Mokkam SHRI A. K. MALLIK Indian Petrochemicals Corporation Ltd, P.O. Petro- chemicals, Vadodara \ DR Y. N. SHARMA ( Alternate , DR W. MILLNS Indian Rubber Manufacturers Research Association, Thane SHRI ASOK MITRA Tyre Corporation of India Ltd, Calcutta DR S. K. RAY ( Alternate ) SHRI P. K. PAIN National Test House, Calcutta SHRI S. C. ROY Bata India Ltd, Calcutta SRRI P. B. GKOSH DASTIDAR 'SHRI s'. ":"e:A::A. Travancore Rubber & Tea Co Ltd, Trivandrum SHRI C. S. KRISXNASWAMY ( AIternatc ) DR E. V. THOMAS Rubber Board, Kottayam DR N. M. MATHEW ( Al’rrnate) 11 INTERNATIONAL SYSTEM OF UNITS ( SI UNITS ) Base Units QUANTITY UrJIT SYMBOL Length metre m Mass kilogram kg Time second s Electric current ampere A Thermodynamic kelvin K temperature Luminous intensity candela cd Amount of substance mole mol Supplementary Units QUANTITY UNIT SYMBOL Plane angle radian rad Solid angle steradian sr Derived Units QUANTITY UNIT SYMBOL DEEINITION Force newton N 1 N = 1 kg.m/sa Energy joule J 1 J = 1 N.m Power watt W 1 W = 1 J/s Flux weber Wb 1 Wb = 1 V.s Flux density tesla T 1 T = 1 Wb/ma Frequenr J hertz Ha 1 Hz = 1 c/s (s-l) Electric cnnductance siemens s 1 S = 1 A/V Electromotive force volt V 1 V=lW/A Pressure, stress Pascal Pa 1 Pa = 1 N/m’