BS ISO 6209-2009 en_1814 Rubber compounding ingredients - Carbon black - Determination of solvent-extractable material《橡胶配料成分.炭黑.溶剂萃取物质的测定》.pdf

1、BS ISO 6209:2009 ICS 83.040.20 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Rubber compounding ingredients Carbon black Determination of solvent-extractable materialThis British Standard was published under the authority of the Standards Policy and Strategy

2、 Committee on 31 August 2009 BSI 2009 ISBN 978 0 580 59261 4 Amendments/corrigenda issued since publication Date Comments BS ISO 6209:2009 National foreword This British Standard is the UK implementation of ISO 6209:2009. It supersedes BS 5293-16:1990 which is withdrawn. The UK participation in its

3、preparation was entrusted to Technical Committee PRI/50, Rubber - Raw, natural and synthetic, including latex and carbon black. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions

4、 of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations.BS ISO 6209:2009Reference number ISO 6209:2009(E) ISO 2009INTERNATIONAL STANDARD ISO 6209 Fourth edition 2009-07-15 Rubber compounding ingredients Carbo

5、n black Determination of solvent- extractable material Ingrdients de mlange du caoutchouc Noir de carbone Dtermination des matires extractibles par les solvants BS ISO 6209:2009 ISO 6209:2009(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy,

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10、0 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 6209:2009 ISO 6209:2009(E) ISO 2009 All rights reserved iii Contents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Principle. 1 4 Extracti

11、on solvent. 1 5 Apparatus and material 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 6209:2009 ISO 6209:2009(E) iv ISO 2009 All rig

12、hts 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 body interested in a subject f

13、or 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 Electrotechnical Commission (IEC) on

14、 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 by the technical committees a

15、re 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 rights. ISO shall not be held

16、responsible for identifying any or all such 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)

17、, which has been technically revised. The 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 6209:2009 INTERNATIONAL STANDARD ISO 6209:2009(E) ISO 2009 All rights reserved 1 Rubber compounding ingredient

18、s Carbon black Determination of solvent-extractable 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 us

19、er to establish appropriate safety and health 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 the

20、y are not biologically active. They can, however, 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 dete

21、rmination of the solvent-extractable material 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 editio

22、n cited applies. For undated references, the 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

23、Principle A test portion is extracted for 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 pre

24、liminary drying, such materials will not be 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 pur

25、poses, or both. However, carbon black with 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-rela

26、ted legislation. BS ISO 6209:2009 ISO 6209:2009(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 cm 3receiver flask, a jacketed Soxhlet extractor and a condenser as show

27、n in Figure 1. The extraction cup has a capacity of 15 cm 3to 30 cm 3 . 5.1.2 Type 2 extraction apparatus, comprising a 500 cm 3receiver 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 cm 3

28、to 30 cm 3 . 5.2 Other apparatus and material 5.2.1 Extraction thimbles, of 15 cm 3to 30 cm 3capacity, 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 ex

29、tracted with solvent and dried before use. 5.2.2 Distillation 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, o

30、r glass wool, solvent-washed and dried. 5.2.5 Analytical 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 dry

31、ing. Dry approximately 20 g of the carbon black sample 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

32、 be dried at a temperature higher than that specified, 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 6209:2009 ISO 6209:2009(E) ISO 2009 All rights reserved 3Key 1 34/35 jo

33、int 2 extraction cup (15 cm 3to 30 cm 3capacity) 3 24/29 joint 4 receiver flask (150 cm 3capacity) Figure 1 Type 1 extraction apparatus BS ISO 6209:2009 ISO 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 cm 3to 30 cm 3capac

34、ity) 5 receiver flask (500 cm 3capacity) a170 mm nominal. Figure 2 Type 2 extraction apparatus BS ISO 6209:2009 ISO 6209:2009(E) ISO 2009 All rights reserved 5 7 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

35、 0,1 mg to obtain the mass of carbon black. Close the opening with 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 ne

36、arest 0,1 mg and pour in 100 cm 3of solvent (Clause 4). 7.3 Place 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

37、per hour. Allow the extraction to proceed for 8 h to 8,5 h. 7.4 Turn 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 int

38、o a suitable vessel, retaining no more than 5 cm 3in the receiver 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

39、remaining solvent by passing a gentle stream of clean, dry air into 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 sol

40、vent and the same type of extraction apparatus as used for the determination, 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: ( ) 21 0 100 mmm m where m 0is the mass

41、, in grams, of the test portion (see 7.1); m 1is the mass, in grams, of the empty receiver flask (see 7.2); m 2is 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

42、:2009 ISO 6209:2009(E) 6 ISO 2009 All rights reserved9 Test report The test 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)

43、the results obtained for each determination and their arithmetic mean; f) the date(s) of the determinations. BS ISO 6209:2009 ISO 6209:2009(E) ISO 2009 All rights reserved 7 Annex A (informative) Precision of the test method An interlaboratory test programme (ITP) was carried out with three laborato

44、ries. The results are given in Table A.1. Table A.1 Results of the ITP after an 8 h extraction Material Number of participating laboratories Number of replicates Average value s rr ( r) s RR ( 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 repe

45、atability, in measurement units; (r) is the repeatability, in percent (relative); s ris the repeatability standard deviation; R is the reproducibility, in measurement units; (R) is the reproducibility, in percent (relative); s Ris the reproducibility standard deviation. BS ISO 6209:2009 ISO 6209:200

46、9(E) 8 ISO 2009 All rights reservedBibliography 1 ISO 383, Laboratory glassware Interchangeable conical ground joints BS ISO 6209:2009BS ISO 6209:2009 ISO 6209:2009(E) ICS 83.040.20 Price based on 8 pages ISO 2009 All rights reserved BS ISO 6209:2009 This page has been intentionally left blankBS ISO

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