1、BS ISO 6209:2009ICS 83.040.20NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDRubber compoundingingredients Carbonblack Determinationof solvent-extractablematerialThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee o
2、n 31 August2009 BSI 2009ISBN 978 0 580 59261 4Amendments/corrigenda issued since publicationDate CommentsBS ISO 6209:2009National forewordThis British Standard is the UK implementation of ISO 6209:2009. Itsupersedes BS 5293-16:1990 which is withdrawn.The UK participation in its preparation was entru
3、sted to TechnicalCommittee PRI/50, Rubber - Raw, natural and synthetic, including latexand carbon black.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are r
4、esponsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.BS ISO 6209:2009Reference numberISO 6209:2009(E)ISO 2009INTERNATIONAL STANDARD ISO6209Fourth edition2009-07-15Rubber compounding ingredients Carbon black Determination of solvent-ex
5、tractable material Ingrdients de mlange du caoutchouc Noir de carbone Dtermination des matires extractibles par les solvants BS ISO 6209:2009ISO 6209:2009(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed bu
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9、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 22 749 01 11 Fax + 41 22
10、749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2009 All rights reservedBS ISO 6209:2009ISO 6209:2009(E) ISO 2009 All rights reserved iiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Principle. 1 4 Extraction solvent. 1 5 Apparatus and material
11、2 5.1 Extraction apparatus 2 5.2 Other apparatus and material 2 6 Sampling 2 7 Procedure 5 8 Expression of results . 5 9 Test report . 6 Annex A (informative) Precision of the test method. 7 Bibliography . 8 BS ISO 6209:2009ISO 6209:2009(E) iv ISO 2009 All rights reservedForeword ISO (the Internatio
12、nal 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 technical committee has been
13、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 of electrotechnical standar
14、dization. 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 circulated to the member bodies for v
15、oting. 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 for identifying any or all s
16、uch patent rights. ISO 6209 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. This fourth edition cancels and replaces the third edition (ISO 6209:1988), which has been technically revised. Th
17、e main changes are as follows: the extraction time has been reduced to 8 h (instead of 16 h); precision data have been included (see Annex A). BS ISO 6209:2009INTERNATIONAL STANDARD ISO 6209:2009(E) ISO 2009 All rights reserved 1Rubber compounding ingredients Carbon black Determination of solvent-ex
18、tractable material WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard 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 safety and hea
19、lth practices and to ensure compliance with any national regulatory conditions. Carbon blacks may contain polycyclic aromatic hydrocarbons, some of which are known carcinogens. These compounds, when present, are so strongly bound to the carbon black that they are not biologically active. They can, h
20、owever, be removed by the procedure specified in this International Standard. Care should therefore be taken to avoid skin contact with solvent extracts from such carbon blacks. 1 Scope This International Standard specifies a method for the quantitative determination of the solvent-extractable mater
21、ial in carbon black for use in the rubber industry. The method is applicable to all types of carbon black. 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, t
22、he latest edition of the referenced document (including any amendments) applies. ISO 1124, Rubber compounding ingredients Carbon black shipment sampling procedures ISO 1126:2006, Rubber compounding ingredients Carbon black Determination of loss on heating 3 Principle A test portion is extracted for
23、8 h. The solvent is then eliminated by evaporation and the extract obtained is weighed. NOTE If the carbon black contains extractable materials which are volatile at the temperature required to eliminate the solvent, or materials which are removed by the preliminary drying, such materials will not b
24、e detected by the procedure specified. This test provides a uniform and precise method for the gravimetric determination of organic-solvent-extractable materials in carbon black. Accuracy and precision are acceptable for most specification or regulatory purposes, or both. However, carbon black with
25、a very low extract (less than 0,02 %) may require a more rigorous extraction procedure. 4 Extraction solvent The solvent used shall be of recognized analytical grade. The use of toluene is recommended as it is the solvent of choice in most food-contact-related legislation. BS ISO 6209:2009ISO 6209:2
26、009(E) 2 ISO 2009 All rights reserved5 Apparatus and material 5.1 Extraction apparatus Use one of the following types of apparatus: 5.1.1 Type 1 extraction apparatus, comprising a 150 cm3receiver flask, a jacketed Soxhlet extractor and a condenser as shown in Figure 1. The extraction cup has a capac
27、ity of 15 cm3to 30 cm3. 5.1.2 Type 2 extraction apparatus, comprising a 500 cm3receiver flask, a condenser and an extraction cup suspended from two hooks on the condenser by clean wire as shown in Figure 2. The extraction cup has a capacity of 15 cm3to 30 cm3. 5.2 Other apparatus and material 5.2.1
28、Extraction thimbles, of 15 cm3to 30 cm3capacity, of sufficiently fine porosity to retain carbon black. They may be made of greaseless paper, cellulose or alundum and shall be of the appropriate size to fit the extraction cup. Thimbles shall be extracted with solvent and dried before use. 5.2.2 Disti
29、llation head and condenser or rotary evaporator. 5.2.3 Gravity-convection oven, capable of maintaining temperatures of 70 C 5 C for drying the extract and 125 C 5 C for drying the carbon black prior to extraction. 5.2.4 Cotton wool, greaseless, or glass wool, solvent-washed and dried. 5.2.5 Analytic
30、al balance, accurate to 0,1 mg. 5.2.6 Heating device, suitable for the extraction apparatus (5.1). 5.2.7 Desiccator. 6 Sampling Carry out sampling in accordance with ISO 1124. Crush all carbon blacks to destroy the pellet configuration before drying. Dry approximately 20 g of the carbon black sample
31、 for 1 h at a temperature of 125 C 5 C in the oven (5.2.3) as specified in ISO 1126:2006, method 1. Allow to cool to room temperature in a desiccator (5.2.7). Keep the dried sample in the desiccator until ready for testing. Carbon black shall not be dried at a temperature higher than that specified,
32、 nor dried using infra-red lamps, as some of the extractable matter may be driven off, thus affecting the results. Take duplicate test portions from this dried sample. BS ISO 6209:2009ISO 6209:2009(E) ISO 2009 All rights reserved 3Key 1 34/35 joint 2 extraction cup (15 cm3to 30 cm3capacity) 3 24/29
33、joint 4 receiver flask (150 cm3capacity) Figure 1 Type 1 extraction apparatus BS ISO 6209:2009ISO 6209:2009(E) 4 ISO 2009 All rights reservedKey 1 34/35 joint 2 two hooks 3 two holes in extraction cup 4 extraction cup (15 cm3to 30 cm3capacity) 5 receiver flask (500 cm3capacity) a170 mm nominal. Figu
34、re 2 Type 2 extraction apparatus BS ISO 6209:2009ISO 6209:2009(E) ISO 2009 All rights reserved 57 Procedure 7.1 Take a test portion of about 10 g from the prepared sample, place it in a weighed thimble (5.2.1) and reweigh to the nearest 0,1 mg to obtain the mass of carbon black. Close the opening wi
35、th a plug of cotton or glass wool (5.2.4). For carbon blacks with a low extractable-material content (less than 0,02 %, for example), the test portion can be increased to 20 g. 7.2 Weigh the clean, dry receiver flask (see 5.1) to the nearest 0,1 mg and pour in 100 cm3of solvent (Clause 4). 7.3 Place
36、 the extraction thimble containing the test portion in the extraction cup, assemble the apparatus (5.1) and adjust the rate of heating of the heating device (5.2.6) so that the distilled solvent fills the extraction cup about 10 times per hour. Allow the extraction to proceed for 8 h to 8,5 h. 7.4 T
37、urn off the heating device, allow the apparatus to cool, then remove the extraction cup and discard the thimble. 7.5 Remove the receiver flask, fit the distillation head and condenser (5.2.2) and distill off the bulk of the solvent into a suitable vessel, retaining no more than 5 cm3in the receiver
38、flask. A rotary evaporator can also be used to remove the solvent. Discard the distilled solvent. 7.6 Allow the apparatus to cool and then disconnect the receiver flask, which now contains the concentrated extract. Remove most of the remaining solvent by passing a gentle stream of clean, dry air int
39、o the flask. 7.7 Dry the flask and its contents for 2 h at 70 C 5 C in the oven (5.2.3), cool to ambient temperature in the desiccator (5.2.7) and weigh to the nearest 0,1 mg. 7.8 Carry out a blank test, using the same quantity of solvent and the same type of extraction apparatus as used for the det
40、ermination, but omitting the test portion. 7.9 Carry out two determinations. 8 Expression of results The solvent-extractable material, expressed as a percentage by mass, is given by the formula: ( )210100mm mm where m0is the mass, in grams, of the test portion (see 7.1); m1is the mass, in grams, of
41、the empty receiver flask (see 7.2); m2is the mass, in grams, of the receiver flask plus the extract after drying (see 7.7); m is the increase in mass, in grams, of the receiver flask during the blank test (see 7.8). BS ISO 6209:2009ISO 6209:2009(E) 6 ISO 2009 All rights reserved9 Test report The tes
42、t report shall contain the following information: a) a reference to this International Standard; b) all details necessary for the identification of the sample; c) the type of extraction apparatus used; d) the solvent used; e) the results obtained for each determination and their arithmetic mean; f)
43、the date(s) of the determinations. BS ISO 6209:2009ISO 6209:2009(E) ISO 2009 All rights reserved 7Annex A (informative) Precision of the test method An interlaboratory test programme (ITP) was carried out with three laboratories. The results are given in Table A.1. Table A.1 Results of the ITP after
44、 an 8 h extraction Material Number of participating laboratories Number of replicates Average value srr (r) sRR (R) N326 3 6 0,074 0,021 0,059 80 0,062 0,175 237 N375 3 6 0,267 0,050 0,142 53 0,084 0,238 89 r is the repeatability, in measurement units; (r) is the repeatability, in percent (relative)
45、; sris the repeatability standard deviation; R is the reproducibility, in measurement units; (R) is the reproducibility, in percent (relative); sRis the reproducibility standard deviation. BS ISO 6209:2009ISO 6209:2009(E) 8 ISO 2009 All rights reservedBibliography 1 ISO 383, Laboratory glassware Int
46、erchangeable conical ground joints BS ISO 6209:2009BS ISO 6209:2009ISO 6209:2009(E) ICS 83.040.20 Price based on 8 pages ISO 2009 All rights reserved BS ISO 6209:2009This page has been intentionally left blank BS ISO6209:2009BSI GroupHeadquarters 389Chiswick High Road,London, W4 4AL, UKTel +44 (0)20
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48、endment or revision. Users of BritishStandards should make sure that they possess the latest amendments oreditions.It is the constant aim of BSI to improve the quality of our products and services.We would be grateful if anyone finding an inaccuracy or ambiguity while usingthis British Standard would inform the Secretary of the technical committeeresponsible, the identity of which can be found on the inside front cover. Tel:+44 (0)20 8996 9000. Fax: +44 (0)20 8996 7400.BSI offers members an individual updating service called PLUS which ensuresthat subscribers automatically receive
