1、BS ISO9924-3:2009ICS 83.060NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDRubber and rubber products Determination of the composition ofvulcanizates anduncured compounds bythermogravimetry Part 3: Hydrocarbon rubbers,halogenated rubbers and polysiloxanerubbers
2、after extractionThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 31 October2009 BSI 2009ISBN 978 0 580 58343 8Amendments/corrigenda issued since publicationDate CommentsBS ISO 9924-3:2009National forewordThis British Standard is the UK implementat
3、ion of ISO 9924-3:2009.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/23, Test methods for rubber and non-black compoundingingredients.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport t
4、o include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.BS ISO 9924-3:2009Reference numberISO 9924-3:2009(E)ISO 2009INTERNATIONAL STANDARD ISO9924-3First edition2009-03-15Ru
5、bber 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 la composition des vulcanisats et d
6、es mlanges non vulcaniss par thermogravimtrie Partie 3: Caoutchoucs hydrocarbons, caoutchoucs halogns et caoutchoucs polysiloxanes aprs extraction BS ISO 9924-3:2009ISO 9924-3:2009(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file m
7、ay 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 policy. The ISO Central Secretariat acc
8、epts 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 care has been taken to ensure that t
9、he 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, no part of this publication may be
10、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 postale 56 CH-1211 Geneva 20 Tel. + 41
11、 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 9924-3:2009ISO 9924-3:2009(E) ISO 2009 All rights reserved iiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Principle. 2 4 Reagents 2 5 Appa
12、ratus 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 Calculation of the mass change from curves 4 8.3
13、 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 9924-3:2009ISO 9924-3:2009(E) iv ISO 2009 All rights reserved
14、Foreword 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 body interested in a subject for which a t
15、echnical 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 Electrotechnical Commission (IEC) on all matters
16、 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 by the technical committees are circulate
17、d 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 rights. ISO shall not be held responsible
18、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 products Determination of the composition
19、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 rubbers, halogenated rubbers and polysiloxan
20、e rubbers after extraction BS ISO 9924-3:2009INTERNATIONAL STANDARD ISO 9924-3:2009(E) ISO 2009 All rights reserved 1Rubber and rubber products Determination of the composition of vulcanizates and uncured compounds by thermogravimetry Part 3: Hydrocarbon rubbers, halogenated rubbers and polysiloxane
21、 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 of the user to establish appropriate safet
22、y 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 hazard. Reference should be made to appro
23、priate 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 establishes the “fingerprint” of the tested ma
24、terial. 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 hydrocarbon backbones (NR, BR, SBR, IIR, EPDM, ACM
25、, 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, CM, CO, ECO, etc.) or containing nitroge
26、n (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 with a polysiloxane backbone (VMQ, etc.) a
27、nd 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 referenced document (including any amendments) app
28、lies. ISO 1407, Rubber Determination of solvent extract ISO 23529, Rubber General procedures for preparing and conditioning test pieces for physical test methods BS ISO 9924-3:2009ISO 9924-3:2009(E) 2 ISO 2009 All rights reserved3 Principle A weighed test portion is heated following a pre-set progra
29、mme 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 constituent. The loss in mass as a function of tempe
30、rature 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 (ppm). 4.2 Dry air, with no detectable trace o
31、f 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 basic components of an analyser are listed
32、 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 temperatures from room temperature to approximat
33、ely 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, allowing heating rates to be controlled from
34、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 cm3/min to 250 cm3/min. 5.1.8 Data acquisition and processing system. 6 Preparation of samples 6
35、.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 9924-3:2009ISO 9924-3:2009(E) ISO 2009 All rights reserved 36.2 Extraction of sa
36、mples 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 w1. 6.3 Test portion After extraction (6.2), prepare a test portion of 8 mg 3 mg cut into a single piece. NOTE T
37、he 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 rubbers; b) procedure B for polysiloxane and fluorocarbon
38、 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 Description of the procedures Table 1 gives details of the op
39、erating 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 temperature under nitrogen min 0 5 Cooling under nitrogen
40、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 to 850 Maintenance time at the final temperature u
41、nder 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 9924-3:2009ISO 9924-3:2009(E) 4 ISO 2009 All rights reserved7.3 Test procedures 7.3
42、.1 Connect the apparatus and adjust (5.1.6) the gas flow to a rate between 20 cm3/min and 250 cm3/min (5.1.7). Set the parameters according to the chosen process. The recommended flow rate is 100 cm3/min. 7.3.2 Before the test, ensure that the pan (5.1.4) or the crucible is clean and empty. 7.3.3 Cl
43、ose 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 6.3 in the pan or the crucible and weigh it under the condi
44、tions specified in 7.3.3. Record the mass, m0. 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. 8 Expression of results 8.1 Recordings Make two different
45、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 compound ingredients. 8.2 Calculation of the mass change from c
46、urves 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 0A, 1A, 2A, and 3A, corresponding to the closest points to return to zero of the derived function.
47、Note these points on the main curve of mass change. Report A0, A1, A2, and A3on the ordinate and read the corresponding masses m0, m1, m2, and m3, where m0is the initial mass of the test piece; m1is the mass of the test piece remaining after pyrolysis; m2is the mass of the test piece remaining after
48、 pyrolysis and carbon black combustion; m3is the mass of the residue yield. The percentage mass fraction loss, w2, due to pyrolysis is given by: 0120100mmwm= (1) BS ISO 9924-3:2009ISO 9924-3:2009(E) ISO 2009 All rights reserved 5The percentage mass fraction loss, w5, due to carbon black combustion i
49、s given by: 1250100mmwm= (2) The percentage mass fraction loss, w7, due to partial or total decomposition of mineral components is given by: 2370100mmwm= (3) The percentage mass fraction, w8, corresponding to the residue yield, is given by: 380100mwm= (4) The sum of the percentage mass fractions, w2+ w5+ w7+ w8, shall correspond to 100 % (not including the analytical errors). NOTE These operations can be calculated by computer. 8.3 Interpretation 8.3.1 General A simple interpretatio
