BS ISO 9113:2019 BSI Standards Publication Plastics — Polypropylene (PP) and propylene-copolymer thermoplastics — Determination of isotactic index bsi.BS 150 9113-2019 BRITISH STANDARD National foreword ‘This British Standard isthe UK implementation of S0.9113:2019. “The UK participation ints preparation was entrusted to Technical Committee PRI/#2, Thermoplastic materials. Alist of organizations represented on this comamittse can be obtained on request toits secretary. ‘This publication does not purport to include all the necessary provisions ‘ofa contract. Users are responsible for its correct application (© The British Standards Institution 2019 Published by BSI Standards Limited 2019 |ISBN'978.0 580 928604 1s 83,080.20 Compliance with a British Sta logal obligations. ‘This British Standard was published under the authority ofthe Standards Policy and Strategy Commitee on 30 june 2018. 1rd cannot confer Immunity fram, Amendments/corrigenda Issued since publication Date ‘Text aflectedBS 180 9113:2019 INTERNATIONAL Iso STANDARD 9113 Second edition 3019.07.09 Plastics — Polypropylene (PP) and propylene-copolymer thermoplastics — Determination of isotactic index Plasciques — Thermoplastiquesd base de polypropylene (PP) et de copolymeres de propylene ~ Détermination denice disotacticté Reference mamber 1s09118:2019(8) :BS 180 9113:2019 180 9113:2019(8) ee © 1s0 238, naned mSwtaered ‘sees eare Uk hr sel fr of pte maybe aed tert yo Giiptay sans eletrnc or mecca aan at ma ors trae eae pt ‘exer rman cb eqn moter te aurea or BO mer bd omy Gedo andoentd -cr401 (150 2019- AghaContents Foreword Scope Normative references ‘Terms and definitions Apparatus, Procedure 5.1 Preparation of the sample 52 Detormination 6 Caleulation and expression of results 7 Caleulation of isotactic index (1) 8 Testreport, Bibliography. (0130 2019-allghs reserved Bs 1S0 9113:2019 180 9113:2019,Bs 150.9113:2019 180 9113:2019 Foreword {50 {the international Organization for Standardization) is aworktwide federation afnational standards ‘bodies (ISO member bodies). Tho work of preparing International Standards is normally carried out through 180 technical committees: Each member body interested in a subject for which a technical ‘committee has been established has the right to be represented on that committee. International ‘organizations, governmental and non-governmental, in liaison with ISO, aso take part in the work. 150 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of lectrovechnical standardization ‘The procedures used to develop this document and those intended for its further maintenance are ‘described i the ISO/IEC Directives, Part I In particular, the diferent approval criteria needed forthe Lifierent types of IS0 documents should be nated. This document was drafted in accordance with the ‘editorial rules of the ISO/IEC Directives, Part2 (see winveisa.ora/ditectives) ‘Attention is drawn to the possiblity that some of the elements of this document may be the subject of patent rights 180 shall not be beld responsible for identifying any or all such patent rights Detalls of [Bry patent rights identified during the development ofthe dacument will be in the Introduction and/or ‘onthe ISO list of patent declarations recelved (see sewso.ore/patent). ‘Any trade name used in this document is information given forthe convenience of users and does not ‘constitute an endorsement. For an explanation of the yoluntary nature of standards, the meaning of 1SO specific terms and ‘expressions related to conformity assessment, as well as information about ISO's adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see wwritiso, ‘This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 9, Thermoplastic material “This second edition cancels and replaces the first edition (ISO 9113:1986), of which it constitutes a rminor revision. The changes compared to the previous edition are as flows: the normative references have been updat — the mandatory Clause. has been added and the subsequent clauses have been renumbered = minor editorial ehanges have been applied ‘Any feedback or questions on this document should be directed tothe user's national standards body. A ‘complete listing ofthese bodies can be found at ww.s0.org/members. htm w (0150 2019-Aleighs roseBs 150 9113:2019 INTERNATIONAL STANDARD 10 9113:2019 Plastics — Polypropylene (PP) and propylene-copolymer thermoplastics — Determination of isotactic index 1 Scope This document specifies a method for determining the percentage of matter which can be extracted from crystalline propylene plastics by boiling n-heptane under standard conditions of testing, Istactic Index is determined by conventional chemical extraction as an absolute method. ‘This method provides for the identification and coding of types H, Band propylene plastics according to130.19069-10 This method is suitable only for base polymers and is not applicable for mixtures, This method starts with sold propylene plastics in the form of particles of specified Fineness. 2 Normative references ‘There are no normative references inthis document. 3. Terms and definitions No terms and definitions are isted inthis document. 150 and 18 maintain terminological databases for use in standardization atthe following addresses — 150 Online browsing platform: available at hitps,//o wise ra/obp — 18 Blectropedia available at htip//ivwiclectropedi.ong/ 4 Apparatus 4.1. Extractor, typeof which is shown in Figure 1. Any other typeof extractor giving the same results may be used. This extractor shall be suitable for use atthe boiling point of r-heptane. (6 1802019- al npbsreserved 1[so.9113:2019 180 9113:2019, 43._Drying ovens, shall he capable of being maintained at temperatures of 70 “€ + 2 °C and 140°C-£2°C respectively, both of thom provided with vacuum lines of less than 25 kPa 44° Balance, shall be accurate to the nearest 0,000 1g. 45° Grinding mi ‘or equivalent machine 446 Steve. mesh size ofthe sieve shall not be greater than 1 mm. A mesh size of 05 mm £ 0.1 mm is recommended, 5 Procedure 5.1. Preparation of the sample 5.1.1 _ Reduce the propylene plasticsoid matter to particles fine enough to pass through the sieve (4.5). For powrler, flakes, bres or films, grinding and sereening are unnecessary if atleast one dimension i Jess than 0,6 mm. Films shall be cut into small fragments or changed to a crushable forma by molting to the shape of ribbons or smal plaques. 3.1.2 Grind dhe sample a follows. Mic atleast 10 g of the sample with solid carbon dioxide oF liquid ait _atinding mill (4.5) and crush unl reduced to small particles. yen in excess, place tin the After screening, collect the matter which passes through the sieve (J.6) and allow standing at room temperature until iti tested 52. Determination 52.1. Weigh the glass fibre or paper cartridge (4.2), dred to constant mass at 140 °C and cooled to oom temperature in a desiccator. o the nearest 0,000 1 g (mass ma) (See 5.25). ‘Then, fil itwith approximately 5 ofthe sample and place tin the aven (1.3) controlled at 140°C *2°C, unr 25 kPa nitrogen vacuum of less. This means thatthe existing resioual pressure of nitrogen inthe apparatus shall be 25 kPa or lower (see 5.2.6)- Usually, 2 h are sufficient for complete drying and sample annealing, but calibration of the oven efficiency Is recommended to determine the minimum time required to achieve constant mass of the samples. 52.2 Cool the cartridge containing the test portion to room temperature in a desiceator and weigh again to the nearest 0,000 1 g (mass ma). Record the mass of the propylene plastic test portion by difference (mz ~mi)-Then place the cartridge inthe extractor tap (see Figre 1) and estract with belling ‘n-heptane (analytical grade, free from aromatic components) fr 24h (see 5.25 and 52.7) 5.2.3 Regulate the solvent boing rate to give 15 to 25 extractions per hour, using 300 ml of n-heptane mthentasle 5.2.4. After 24 h of extraction, cool the cartridge containing residual polymer to room temperature, carefully wash it with acetone (analytical grade) and dry it in the oven (4.3) controlled at 70°C 2°C, 0 constant mass, under 25 kPa nltogen vacuum o less Usually. 40 6 h are sufficient to reach constant mass but Its recommended that the oven drying ficiency be checked by a preliminary test (01802010 Alligs reserved 3BS 18091132019 180 9113:2019 ‘Weigh the dried cartridge containing the residual polymer tothe nearest 0,000 1 g after cooling ta room temperature in adesicestor (mass m:) (see 2.5) 5.25 I papor cartridges are used, they shall be placed in a glass weighing bottle bofore weighing in ‘rderto avoid the influence of atmospheric humidity absorbed by the paper wall, 52.6. In onder to improve the reproducibility of extraction tests, itis recommended that ground ‘propylene plastic particles be snncaled in oven lor 2 hat 140°C under nitrogen atmosphere to equalize he degree of erystalliaty. 52.7 If powderor crushed garticles aftype H propylene plastic pass through 0.5 mm mesh sieves. 6 h ‘extraction time i allowed (for practical purposes), provided that the relevant results are consistent with those of 24 h extraction, The sandard 24h extraction fs mandatory in the folowing cases: 4) fortype B propylene plastics 1b). incase of dispute concerning the results 6 Calculation and expression of results 6.4 Then-heptane extractah‘e matter 5, expressed as percentage by mass, is given by the Formula (1)> = 5100 o where ‘my Ssthe mas, in grams ofthe cartridge: ‘ma isthe mas, in rams, of te cartridge pls test portion Belare extraction ‘mys the mas. in grams, of te cartridge pls test porn afer extraction. {62 _Recont the value of extractable matter (S) a5 the arithmetic mean (quoted to two significant ‘gares) of the observed values in a duplicate west, provided that they are within +7,5 % of the average, ® where Syandy aro the observed india! value of ¢ s ‘stn anenmetiemean ofthese two values If this condition isnot flied, repeat the test. 7 Calculation of isotactic index (11) Calewlate the Isotactic index tas shown in Formula (3) Isocactie index (It) = 100-8 @ Round off the value of 100 - Sto the nearest unitand report it as the isotactc index the first decimal ligitis 5, round off to the nextiower unit 4 © 502019- Angus reservedbs 180 9113:2019 180 9113:2019 8 Test report ‘The test report shall inchde the folowing information: 4) areference to this document, ie, ISO 9113:2019; 1b) complete identification ofthe product tested; ©) the individual results and the arithmetic moan for mhoptane extractable matter, and the isotacticindex, 4) any umsual features noted during the determination: €)_any operation not specified inthis document or regarded as opticnal. (0180 2019- At ngs reserved 5BS 180.9113:2019, 180 9113:2019 Bibliography [1] 1501905941, Pasties — Polypropylene (PP) moukiing and extrusion materias— Part 1: Designation system and basis for speefieations 6 61502010 allege roc‘This page deliberately left bankBritish Standards Institution (BSI) SOREL tandards-related publication Mier Eroticy Sitesi rie) re oduc About us ‘Reteaye ened na snd een ary ser ‘imation tromeneen coon mee ‘gram oto ae sara cc aan oenmekeroae’ Information on standards ‘tein de nh Pete ep ogo (Sister ert cent ‘mong wna oroxtr ion Sone coe Buying standards ety cre rte ai er Sous omsce wewtscoes on notaries ‘edo ao ean on he Str Bcc pum tapes oreo on Cee nea copsh nbn ‘tan carina soe your ey es core Pe Sa. 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