1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 28343:2010Rubber compoundingingredients Process oils Determination of glasstransition temperature by DSCBS ISO 28343:2010 BRITISH STANDARDNational forewordThis British Sta
2、ndard is the UK implementation of ISO 28343:2010.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/23, Test methods for rubber and non-blackcompounding ingredients.A list of organizations represented on this committee can beobtained on request to its secretary.This publ
3、ication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 59106 8ICS 83.040.20Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the au
4、thority of theStandards Policy and Strategy Committee on 30 September 2010.Amendments issued since publicationDate Text affectedBS ISO 28343:2010Reference numberISO 28343:2010(E)ISO 2010INTERNATIONAL STANDARD ISO28343First edition2010-09-01Rubber compounding ingredients Process oils Determination of
5、 glass transition temperature by DSC Ingrdients de mlange du caoutchouc Huiles de mise en uvre Dtermination de la temprature de transition vitreuse par DSC BS ISO 28343:2010ISO 28343:2010(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this
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8、 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 2010 All rights reserved. Unless otherwise specified, no part of this publication
9、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 postale 56 CH-1211 Geneva 20 Te
10、l. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2010 All rights reservedBS ISO 28343:2010ISO 28343:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Terms and definitions .1 4 Reagen
11、ts and materials 1 5 Apparatus.2 6 Storage and laboratory conditions2 7 Calibration2 8 Sampling.2 9 Procedure.3 10 Expression of results3 11 Test report4 Annex A (informative) Determination of Tgfrom the point of inflection5 Annex B (informative) Precision data .7 Bibliography8 BS ISO 28343:2010ISO
12、28343:2010(E) iv ISO 2010 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 memb
13、er 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, also take part in the work. ISO collaborates closely with the International Ele
14、ctrotechnical 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 adop
15、ted by 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 pate
16、nt rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 28343 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry. BS ISO 28343:2010INTERNATIONAL STANDARD
17、ISO 28343:2010(E) ISO 2010 All rights reserved 1Rubber compounding ingredients Process oils Determination of glass transition temperature by DSC WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all of the
18、safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. 1 Scope This International Standard specifies a method for the determination, by differential
19、scanning calorimetry (DSC), of the glass transition temperature, Tg, of process oils used in rubber compounding. NOTE The same oils are used as extender oils for synthetic rubbers. 2 Normative references The following referenced documents are indispensable for the application of this document. For d
20、ated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 1382, Rubber Vocabulary ISO 3170, Petroleum liquids Manual sampling ISO 11357-1:2009, Plastics Differential scanning calorimetry (DSC) Part 1
21、: General principles 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 1382 and ISO 11357-1 and the following apply. 3.1 Tgglass transition temperature approximate midpoint of the temperature range over which the glass transition takes place NOTE For t
22、he purposes of this International Standard, the glass transition temperature is defined as the point of inflection of the DSC curve. The point of inflection corresponds to the calculated maximum of the first-derivative curve. 4 Reagents and materials 4.1 Dry helium gas, purity 99,999 % or in accorda
23、nce with the differential scanning calorimeter manufacturers instructions. 4.2 If helium is not available, use dry nitrogen gas (purity 99,999 % or in accordance with the differential scanning calorimeter manufacturers instructions). BS ISO 28343:2010ISO 28343:2010(E) 2 ISO 2010 All rights reserved5
24、 Apparatus 5.1 Differential scanning calorimeter, equipped with a liquid-nitrogen cooling system so that a temperature of around 150 C can be attained. Two types of instrument can be used: a “heat-flow” analyser1), in which the temperature of the test sample is increased or decreased and the variati
25、on in the flow of heat emitted or received by the sample is monitored; a “power-compensation” analyser2), in which the temperature of the test sample is increased or decreased and the energy necessary to keep the sample at the programmed temperature is monitored. 5.2 Sample pans and lids, made of al
26、uminium, with a volume of about 40 l, suitable for use with the analyser. 5.3 Suitable press, to seal the pans. 5.4 Analytical balance, accurate to 0,1 mg. 6 Storage and laboratory conditions Store the oil sample in a suitable ventilated laboratory cupboard. Prepare the sample pan under an extractio
27、n hood. The DSC instrument should be operated in a laboratory kept at standard conditions as specified in the instrument manufacturers manual. 7 Calibration Temperature calibration shall be carried out in the desired temperature range in accordance with the equipment manufacturers instructions or in
28、 accordance with ISO 11357-1:2009, Clause 8. The heating rate, the type of purge gas and the purge gas flow rate need to be the same for calibration as for the measurement of a test sample. 8 Sampling Carry out sampling in accordance with ISO 3170. 1) Examples of suitable heat-flow analysers are the
29、 Mettler Toledo DSC 821 and DSC 822, the TA Instruments DSC 2920 and the Netzsch DSC 204. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of these instruments. 2) An example of a suitable power-compensation analyser
30、is the PerkinElmer Pyris. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of this instrument. BS ISO 28343:2010ISO 28343:2010(E) ISO 2010 All rights reserved 39 Procedure 9.1 Principle The glass transition temperatur
31、e of the process oil is measured by differential scanning calorimetry. During the glass transition, the specific heat changes. The differential scanning calorimeter is able to detect accurately this change in specific heat, thus allowing the temperature at which the change occurs, Tg, to be determin
32、ed. 9.2 Experimental conditions 9.2.1 Preparation of the pans The mass of sample used, the type of pan and the lid-crimping operation are very important parameters. For each instrument, the manufacturers instructions shall be strictly followed. Use a test sample mass between 5 mg and 15 mg. 9.2.2 Me
33、asurements Adjust the helium (or nitrogen) gas flow in accordance with the instrument manufacturers recommendation. NOTE Typically, a value between 20 ml/min and 50 ml/min is used for either gas. When results obtained by different parties are going to be compared, it is recommended that the same typ
34、e of purge gas be used. Place the test sample in the instrument at room temperature. Raise the temperature to 60 C at a rate of 30 C/min to remove any thermal history of the sample. Cool to 140 C at a rate of 10 C/min and maintain the sample at this temperature for 5 min. Record the thermogram from
35、140 C to 60 C at a heating rate of 20 C/min. 9.2.3 Evaluation The recorded curve is evaluated using equipment-specific software, defining the appropriate limits corresponding to the transition range. The glass transition temperature, Tg, is determined from the point of inflection of the recorded cur
36、ve, which corresponds to the maximum in the first-derivative curve (see Example 1 in Annex A). In cases when the glass transition is followed by a crystallization peak, Tgis also determined from the point of inflection (see Example 2 in Annex A). By agreement between the interested parties, the so-c
37、alled midpoint method may be used to determine Tg. In this case, Tgis measured at the point of intersection of the curve with the straight line equidistant from the two straight lines obtained by extrapolating the baselines before and after the transition. 10 Expression of results Report the tempera
38、ture corresponding to the point of inflection as the glass transition temperature, Tg, expressed in degrees Celsius. BS ISO 28343:2010ISO 28343:2010(E) 4 ISO 2010 All rights reserved11 Test report The test report shall include the following information: a) a reference to this International Standard;
39、 b) all details necessary for the identification of the oil sample(s) tested; c) the mass of the test sample; d) the DSC instrument used name of instrument and type of analyser (“heat flow” or “power compensation”); e) the purge gas used (helium or nitrogen) and the gas flow rate, in millilitres per
40、 minute; f) the value of Tg, in degrees Celsius, together with a copy of the recorded DSC curve; g) details of any operation not included in this International Standard, as well as any observations which could have a bearing on the result; h) the date of the test. BS ISO 28343:2010ISO 28343:2010(E)
41、ISO 2010 All rights reserved 5Annex A (informative) Determination of Tgfrom the point of inflection EXAMPLE 1 No crystallization after the glass transition minC-85,0 -80,0 -75,0 -70,0 -65,0 -60,0 -55,0 -50,0 -45,0 -40,0 -35,0 -30,0 -25,0 -20,0 -15,0 -10,0 -5,0 0,07,2 7,4 7,6 7,8 8,0 8,2 8,4 8,6 8,8
42、9,0 9,2 9,4 9,6 9,8 10,0 10,2 10,4 10,6 10,8 11,0 11,2 11,4minC-85,0 -80,0 -75,0 -70,0 -65,0 -60,0 -55,0 -50,0 -45,0 -40,0 -35,0 -30,0 -25,0 -20,0 -15,0 -10,0 -5,0 0,07,2 7,4 7,6 7,8 8,0 8,2 8,4 8,6 8,8 9,0 9,2 9,4 9,6 9,8 10,0 10,2 10,4 10,6 10,8 11,0 11,2 11,4a231Key 1 first-derivative curve 2 rec
43、orded curve 3 glass transition temperature (inflection point at 43,41 C) aExothermic. Figure A.1 Oil showing no crystallization after the glass transition BS ISO 28343:2010ISO 28343:2010(E) 6 ISO 2010 All rights reservedEXAMPLE 2 Glass transition followed by crystallization minC-90,0 -85,0 -80,0 -75
44、,0 -70,0 -65,0 -60,0 -55,0 -50,0 -45,0 -40,0 -35,0 -30,0 -25,0 -20,0 -15,0 -10,0 -5,0 -0,0 5,0 10,0 15,026,0 26,5 27,0 27,5 28,0 28,5 29,0 29,5 30,0 30,5 31,0minC-90,0 -85,0 -80,0 -75,0 -70,0 -65,0 -60,0 -55,0 -50,0 -45,0 -40,0 -35,0 -30,0 -25,0 -20,0 -15,0 -10,0 -5,0 -0,0 5,0 10,0 15,026,0 26,5 27,
45、0 27,5 28,0 28,5 29,0 29,5 30,0 30,5 31,0a32145Key 1 first-derivative curve 2 recorded curve 3 glass transition temperature (inflection point at 62,73 C) 4 crystallization peak 5 melting aExothermic. Figure A.2 Oil showing crystallization after the glass transition BS ISO 28343:2010ISO 28343:2010(E)
46、 ISO 2010 All rights reserved 7Annex B (informative) Precision data B.1 General The precision of this test method was determined in accordance with ISO/TR 9272. Refer to ISO/TR 9272 for terminology and other statistical details. The precision results merely give an estimate of the precision to be ex
47、pected. The precision parameters should not be used for acceptance/rejection testing of any group of materials without documentation that they are applicable to those particular materials and the specific test protocols that include this test method. An interlaboratory test programme was conducted t
48、o determine a type 1 precision. Both the repeatability and the reproducibility determined represent short-term testing conditions. Eleven laboratories tested one process oil (MES oil). The number of within-laboratory replicates was two and the time span for repeatability was 7 days. Each laboratory
49、carried out two replicates per day. The results of the precision calculations are given in Table B.1. Table B.1 Tgmeasured from inflection point Within-laboratory Between laboratories Material Mean value of TgC srr (r) sRR (R) MES oil 61,11 0,368 1,04 1,7 0,704 1,99 3,3 Number of laboratories: 11, number of replicates: 2. sris the within-laboratory standard deviation; sRis the between-laboratory standard deviation; r is the repeatability, in measurement units; (r) is the re
