BS ISO 9924-3-2009 Rubber and rubber products - Determination of the composition of vulcanizates and uncured compounds by thermogravimetry - Hydrocarbon rubbers halogenate.pdf

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1、BS ISO 9924-3:2009 ICS 83.060 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Rubber and rubber products Determination of the composition of vulcanizates and uncured compounds by thermogravimetry Part 3: Hydrocarbon rubbers, halogenated rubbers and polysiloxan

2、e rubbers after extractionThis British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2009 BSI 2009 ISBN 978 0 580 58343 8 Amendments/corrigenda issued since publication Date Comments BS ISO 9924-3:2009 National foreword This British Standard

3、is the UK implementation of ISO 9924-3:2009. The UK participation in its preparation was entrusted to Technical Committee PRI/23, Test methods for rubber and non-black compounding ingredients. A list of organizations represented on this committee can be obtained on request to its secretary. This pub

4、lication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations.BS ISO 9924-3:2009Reference number ISO 9924-3:2009(E) ISO 2009INTERNATIONAL STANDARD IS

5、O 9924-3 First edition 2009-03-15 Rubber and rubber products Determination of the composition of vulcanizates and uncured compounds by thermogravimetry Part 3: Hydrocarbon rubbers, halogenated rubbers and polysiloxane rubbers after extraction Caoutchouc et produits base de caoutchouc Dtermination de

6、 la composition des vulcanisats et des mlanges non vulcaniss par thermogravimtrie Partie 3: Caoutchoucs hydrocarbons, caoutchoucs halogns et caoutchoucs polysiloxanes aprs extraction BS ISO 9924-3:2009 ISO 9924-3:2009(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with

7、 Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobes licensing po

8、licy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. Every

9、 care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2009 All rights reserved. Unless otherwise specified

10、, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case p

11、ostale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2009 All rights reservedBS ISO 9924-3:2009 ISO 9924-3:2009(E) ISO 2009 All rights reserved iii Contents Page Foreword iv 1 Scope . 1 2 Normative references

12、 . 1 3 Principle. 2 4 Reagents 2 5 Apparatus 2 6 Preparation of samples 2 6.1 Conditioning of samples 2 6.2 Extraction of samples. 3 6.3 Test portion . 3 7 Procedure 3 7.1 General. 3 7.2 Description of the procedures. 3 7.3 Test procedures 4 8 Expression of results . 4 8.1 Recordings 4 8.2 Calculati

13、on of the mass change from curves 4 8.3 Interpretation. 5 8.4 Expression of results . 6 9 Test report . 7 10 Precision 7 Annex A (informative) Recommended procedures. 8 Annex B (informative) Examples of thermogram 9 Annex C (informative) Precision . 14 Bibliography . 16 BS ISO 9924-3:2009 ISO 9924-3

14、:2009(E) iv ISO 2009 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member bo

15、dy 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, also take part in the work. ISO collaborates closely with the International Electrot

16、echnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted b

17、y the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent ri

18、ghts. ISO shall not be held responsible for identifying any or all such patent rights. ISO 9924-3 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 2, Testing and analysis. ISO 9924 consists of the following parts, under the general title Rubber and rubber pr

19、oducts Determination of the composition of vulcanizates and uncured compounds by thermogravimetry: Part 1: Butadiene, ethylene-propylene copolymer and terpolymer, isobutene-isoprene, isoprene and styrene-butadiene rubbers Part 2: Acrylonitrile-butadiene and halobutyl rubbers Part 3: Hydrocarbon rubb

20、ers, halogenated rubbers and polysiloxane rubbers after extraction BS ISO 9924-3:2009 INTERNATIONAL STANDARD ISO 9924-3:2009(E) ISO 2009 All rights reserved 1 Rubber and rubber products Determination of the composition of vulcanizates and uncured compounds by thermogravimetry Part 3: Hydrocarbon rub

21、bers, halogenated rubbers and polysiloxane rubbers after extraction WARNING Persons using this part of ISO 9924 should be familiar with normal laboratory practice. This part of ISO 9924 does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility

22、of the user to establish appropriate safety and health practices to ensure compliance with any regulatory conditions. CAUTION Certain procedures specified in this part of ISO 9924 may involve the use or generation of substances, or the generation of waste, that could constitute a local environmental

23、 hazard. Reference should be made to appropriate documentation on safe handling and disposal after use. 1 Scope This part of ISO 9924 specifies a thermogravimetric method for the determination of the main constituents of rubber compounds such as elastomer(s), carbon black and mineral filler. It esta

24、blishes the “fingerprint” of the tested material. However, the result does not always correspond exactly to the theoretical formula of the rubber. This method applies to raw or compounded rubbers, vulcanized and unvulcanized, after preliminary extraction. This method applies to rubbers with hydrocar

25、bon backbones (NR, BR, SBR, IIR, EPDM, ACM, AEM, etc.) used alone or as mixtures. For the mixtures, the polymer content corresponds to the total rubber, and it is not usually possible to identify individual polymers. This method applies to rubbers with halogenated hydrocarbon backbones (CR, CSM, FKM

26、, CM, CO, ECO, etc.) or containing nitrogen (NBR, HNBR, NBR/PVC, etc.), as well as to their mixtures. However, these rubbers often form carbonaceous residues which interfere with the analysis. Application of an appropriate procedure minimizes these interferences. This method also applies to rubbers

27、with a polysiloxane backbone (VMQ, etc.) and to rubbers not listed above. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenc

28、ed document (including any amendments) applies. ISO 1407, Rubber Determination of solvent extract ISO 23529, Rubber General procedures for preparing and conditioning test pieces for physical test methods BS ISO 9924-3:2009 ISO 9924-3:2009(E) 2 ISO 2009 All rights reserved3 Principle A weighed test p

29、ortion is heated following a pre-set programme in a known atmosphere. Initial pyrolysis in an inert atmosphere (nitrogen) is followed by combustion in an oxidizing atmosphere. Generally, the reactions that generate mass variations are decompositions, oxidations, or reactions volatilizing a constitue

30、nt. The loss in mass as a function of temperature indicates a quantitatively usable thermogram which is characteristic of the material. 4 Reagents 4.1 Nitrogen of minimal purity 99,995 % mass fraction, with an oxygen content of less than 10 mg/kg (ppm) and hydrocarbon content less than 1,5 mg/kg (pp

31、m). 4.2 Dry air, with no detectable trace of oil. The air used may be reconstituted nitrogen and oxygen of purity minimum 99,5 % mass fraction. In some cases, pure oxygen may be used. 5 Apparatus 5.1 Thermogravimetric analyser. 5.1.1 General. Various types of analyser are commercially available. The

32、 basic components of an analyser are listed in 5.1.2 to 5.1.8. 5.1.2 Thermogravimetric balance, comprising a microbalance provided with a pan made from a nonoxidizable material, that can weigh up to 50 mg, is readable to the nearest 1 g, and equipped with an oven capable of being maintained at tempe

33、ratures from room temperature to approximately 1 000 C. 5.1.3 Appropriate enclosure allowing the sample to be kept under a specified atmosphere. 5.1.4 Pan or crucible of size suitable to accommodate the sample and small enough to reduce the influence of buoyancy. 5.1.5 Temperature-control system, al

34、lowing heating rates to be controlled from 10 C/min to 50 C/min. 5.1.6 Gas selector allowing successive introduction of the inert gas and oxidizing gas while controlling the flow rate. 5.1.7 Measurement equipment for gas flow rate in the range 10 cm 3 /min to 250 cm 3 /min. 5.1.8 Data acquisition an

35、d processing system. 6 Preparation of samples 6.1 Conditioning of samples Test samples should be conditioned in standardized laboratory conditions of temperature and humidity in accordance with ISO 23529. These conditions are preferred, but are not mandatory. BS ISO 9924-3:2009 ISO 9924-3:2009(E) IS

36、O 2009 All rights reserved 3 6.2 Extraction of samples A preliminary extraction of plasticizers and additives shall be performed in accordance with ISO 1407 using the appropriate solvent. Conventionally, the amount of extract is denoted w 1 . 6.3 Test portion After extraction (6.2), prepare a test p

37、ortion of 8 mg 3 mg cut into a single piece. NOTE The preparation of the test portion can influence the kinetics of the phenomena. 7 Procedure 7.1 General Considering the variety of the decomposition modes linked to the nature of polymers, two procedures are defined: a) procedure A for carbon rubber

38、s; b) procedure B for polysiloxane and fluorocarbon rubbers. If procedure A does not result in a thermogram that achieves constant mass at 600 C, procedure B shall apply. A non-exhaustive list of the recommended procedures for each of the various rubber families is given in Table A.1. 7.2 Descriptio

39、n of the procedures Table 1 gives details of the operating steps for procedures A and B. Table 1 Operating steps Step Units Procedure A Procedure B Initial temperature C 35 10 35 10 Heating rate under nitrogen C/min 20 20 Target temperature under nitrogen C 600 800 Maintenance time at target tempera

40、ture under nitrogen min 0 5 Cooling under nitrogen C 600 to 400 800 to 400 Temperature at the change of atmosphere C 400 400 Maintenance time at atmosphere change temperature under air min 2 2 Heating rate under air C/min 20 20 Final temperature under air according to the equipment aC 800 to 850 800

41、 to 850 Maintenance time at the final temperature under air min 10 to 20 10 to 20 aIf procedures do not result in a thermogram that achieves constant mass at final temperature under air, maintain the final temperature condition until constant mass is achieved. BS ISO 9924-3:2009 ISO 9924-3:2009(E) 4

42、 ISO 2009 All rights reserved7.3 Test procedures 7.3.1 Connect the apparatus and adjust (5.1.6) the gas flow to a rate between 20 cm 3 /min and 250 cm 3 /min (5.1.7). Set the parameters according to the chosen process. The recommended flow rate is 100 cm 3 /min. 7.3.2 Before the test, ensure that th

43、e pan (5.1.4) or the crucible is clean and empty. 7.3.3 Close the thermobalance oven (5.1.2), purge with a nitrogen (4.1) flow at the preset rate. Wait until stabilization. Adjust the zero to compensate for the mass of the pan or the crucible. 7.3.4 Place the test piece prepared in accordance with 6

44、.3 in the pan or the crucible and weigh it under the conditions specified in 7.3.3. Record the mass, m 0 . 7.3.5 Conduct the test by following the operating steps specified in Table 1. 7.3.6 At the end of the test, allow the oven to cool to room temperature, open it and clean the pan or the crucible

45、. 8 Expression of results 8.1 Recordings Make two different types of recording to enable the necessary calculations to be made: a) a plot of the percentage variation in mass fraction, w, vs. temperature or time; b) a derivative plot, dw/dT. These will be used to derive the content of the various com

46、pound ingredients. 8.2 Calculation of the mass change from curves An example of a thermogram is given in Figure B.1. The derivative plot shall be used to define particular points on the mass variation plot as follows. Identify on the derivative plot the minima 0 A , 1 A , 2 A , and 3 A , correspondi

47、ng to the closest points to return to zero of the derived function. Note these points on the main curve of mass change. Report A 0 , A 1 , A 2 , and A 3on the ordinate and read the corresponding masses m 0 , m 1 , m 2 , and m 3 , where m 0is the initial mass of the test piece; m 1is the mass of the

48、test piece remaining after pyrolysis; m 2is the mass of the test piece remaining after pyrolysis and carbon black combustion; m 3is the mass of the residue yield. The percentage mass fraction loss, w 2 , due to pyrolysis is given by: 01 2 0 100 mm w m = (1) BS ISO 9924-3:2009 ISO 9924-3:2009(E) ISO

49、2009 All rights reserved 5 The percentage mass fraction loss, w 5 , due to carbon black combustion is given by: 12 5 0 100 mm w m = (2) The percentage mass fraction loss, w 7 , due to partial or total decomposition of mineral components is given by: 23 7 0 100 mm w m = (3) The percentage mass fraction, w 8 , corresponding to the residue yield, is given by: 3 8 0 100 m w m = (4) The sum of the percentage mass fractions, w 2+ w 5+ w 7+ w 8 , shall correspond to 100 % (not in