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1、BRITISH STANDARD BS 5293-7: 2001 ISO 1125:1999 Sampling and testing carbon black for use in the rubber industry Part 7: Method for determination of ash content (ISO title: Rubber compounding ingredients Carbon black Determination of ash) ICS 83.040.20 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERM
2、ITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:05:26 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5293-7:2001 This British Standard, having been prepared under the direction of the Sector Policy and Strategy Committee for Materials and Chemicals, was published unde
3、r the authority of the Standards Policy and Strategy Committee on 7 November 2001 BSI 7 November 2001 ISBN 0 580 38662 7 National foreword This British Standard reproduces verbatim ISO 1125:1999 and implements it as the UK national standard. It supersedes BS 5293-7:1991 which is withdrawn. The UK pa
4、rticipation in its preparation was entrusted to Technical Committee PRI/50, Natural and synthetic rubbers, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement intern
5、ational or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to inclu
6、de all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/Europe
7、an committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, ISO title page, page ii
8、, pages 1 to 4, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:05:26 GMT+00:00 2006, Uncontrolled
9、 Copy, (c) BSI A Reference number ISO 1125:1999(E) INTERNATIONAL STANDARD ISO 1125 Third edition 1999-03-15 Rubber compounding ingredients Carbon black Determination of ash Ingrdients de mlange du caoutchouc Noir de carbone Dtermination du taux de cendres 9991:73925 SBBS 52937:2001 Licensed Copy: sh
10、effieldun sheffieldun, na, Mon Dec 04 16:05:26 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 1125:1999(E) OSI 9991 All irthgs serevr.de lnUess toiwrehse scepifi,de trap on fo this lbupictaino may eb cudorperde tu roziliyna ni de foyb ro mr yna snaem, celetrcino cem rocinaha,l cniltohp gniducoypogni
11、 dna .rehsilbup eht morf gnitirw ni noissimrep tuohtiw ,mliforcim noitazidradnatS rof noitazinagrO lanoitanretnI 65 elatsop esaC 02 evneG 1121-HC dnalreztiwS tenretnIhc.osiosi dnalreztiwS ni detnirP ii Foreword ISO (the International Organization for Standardization) is a worldwide federation of nat
12、ional 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 established has the right to be represented on that committee. Interna
13、tional 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 standardization. Draft International Standards adopted by the technical comm
14、ittees 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. International Standard ISO 1125 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw ma
15、terials (including latex) for use in the rubber industry. This third edition cancels and replaces the second edition (ISO 1125:1990), which has have been technically revised. 9991:73925 SBBS 52937:2001 Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:05:26 GMT+00:00 2006, Uncontrolled Copy,
16、 (c) BSI DRADNATS LANOITANRETNI OSI)E(9991:5211 OSI 1 Rubber compounding ingredients Carbon black Determination of ash 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, a
17、ssociated 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 determining the ash of all types of carbon black for use in t
18、he rubber industry. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agre
19、ements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 1124:1988, Rubber compounding ingredients Carbon
20、black shipment sampling procedures. ISO/TR 9272:1986, Rubber and rubber products Determination of precision for test method standards. 3 Principle An accurately weighed portion of dried sample is ignited in a crucible until all the carbonaceous material is oxidized. The crucible is cooled in a desic
21、cator, weighed, and the percentage of ash calculated. 4 Apparatus 4.1 Muffle furnace, capable of maintaining a temperature of 550 C 25 C (or other required temperature). NOTE The use of a vented furnace would decrease the time of heating to constant mass (see 6.3). 4.2 Porcelain crucible, tall form,
22、 diameter 35 mm, height 30 mm, with lid. The use of the lid on the crucible is optional. If it is not used, this shall be mentioned in the test report. 4.3 Analytical balance, accurate to 0,1 mg. 9991:73925 SBBS 52937:2001 Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:05:26 GMT+00:00 200
23、6, Uncontrolled Copy, (c) BSI ISO 1125:1999(E) ISO 2 4.4 Desiccator. 4.5 Oven, preferably of the gravity-convection type, capable of temperature regulation to within 1 C at 125 C and temperature uniformity to within 5 C. 5 Sampling Carry out sampling in accordance with ISO 1124. 6 Procedure 6.1 Heat
24、 the crucible (4.2), with its lid (if used), in the muffle furnace (4.1) at a temperature of 550 C 25 C for 1 h. Place the crucible (and lid) in the desiccator (4.4). Cool to ambient temperature and reweigh to the nearest 0,1 mg. NOTE If, after cleaning, drying and reweighing at the end of the deter
25、mination (see 6.4), the crucible is stored in a dessicator, step 6.1 is needed only for new crucibles. 6.2 Dry a little more than 2 g of furnace carbon black or a little more than 5 g of thermal or channel carbon black in the oven (4.5) at a temperature of 125 C for 1 h. Allow to cool to room temper
26、ature. 6.3 Weigh, to the nearest 0,1 mg, about 2 g of dried furnace carbon black or 5 g of dried thermal or channel black into the crucible tared in 6.1, place in the furnace at a temperature of 550 C 25 C and heat uncovered until constant mass is obtained. Cover with the lid (if used), remove to th
27、e desiccator, and allow to cool to ambient temperature. Weigh to the nearest 0,1 mg. To avoid repeated handling of the crucible, an adequate ashing time shall be established at each test site. IMPORTANT Take the following precautions: a) keep the door of the furnace open about 0,5 cm to admit air to
28、 support the combustion of organic material; b) after the test portion has cooled in the desiccator, admit air slowly to avoid loss of ash from the crucible due to air currents. By mutual agreement between the interested parties, it is permissible to use another ashing temperature such as 750 C 25 C
29、 or 825 C 25 C (subclauses 4.1, 6.1 and 6.3 would have to be adapted accordingly). However, this temperature leads to lower ash contents than the ones obtained at 550 C, and shall not be used for reference purposes. 6.4 Clean the crucible (and lid), dry in the oven (4.5) at 125 C and reweigh to the
30、nearest 0,1 mg. 7 Expression of results The ash is given, as a percentage by mass, by the equation %ash= mm mm 23 10 100 where m0is the mass, in grams, of the crucible (and lid) before the determination; m1is the mass, in grams, of the crucible (and lid) plus the test portion; m2is the mass, in gram
31、s, of the crucible (and lid) plus the ash; m3is the mass, in grams, of the crucible (and lid) after the determination (should be the same as m0). 9991:73925 SBBS 52937:2001 Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:05:26 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISOISO 1125:1999(E)
32、3 8 Precision and bias 8.1 The precision of the method was determined in accordance with ISO/TR 9272. Refer to this document for terminology and other statistical details. 8.2 The precision data given below merely give an estimate of the precision. The precision parameters shall not therefore be use
33、d 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 method. 8.3 A type 1 interlaboratory precision programme was conducted. Both repeatability and reproducibility w
34、ere measured under short-term testing conditions. Ten laboratories tested five carbon black samples (A, B, C, D and E) twice on two different days. Therefore p = 10, q = 5 and n = 4. Difference values were not measured. 8.4 The results of the precision calculations are given in Table 1, with the mat
35、erials arranged in ascending order of the mean ash value. Table 1 Precision data Material Mean ashWithin laboratoryBetween laboratories %srr(r)sRR(R) Black A0,170,0160,04525,4970,0210,06035,188 Black E0,350,0200,05716,1210,0370,01429,663 Black B0,450,0300,08518,9190,0430,12227,067 Black C0,610,0270,
36、07612,4830,0370,10617,445 Black D0,830,0160,0455,6200,0230,0667,961 Pooled or averaged values0,480,020,0613,250,030,0919,63 The symbols are defined as follows: srwithin-laboratory standard deviation; rrepeatability (in measurement units); (r)repeatability (in percent); sRbetween-laboratory standard
37、deviation; Rreproducibility (in measurement units); (R) reproducibility (in percent). 8.5 The precision for the pooled values for the ash may be expressed as follows: 8.5.1 Repeatability: The repeatability r of the result has been established as 0,06 % ash. Two individual test results (or determinat
38、ions) that differ from each other by more than 0,06 % ash shall be considered suspect and dictate that some appropriate investigative action be taken. 8.5.2 Reproducibility: The reproducibility R of the result has been established as 0,09 % ash. Two individual test results (or determinations) produc
39、ed in separate laboratories that differ by more than 0,09 % ash shall be considered suspect and dictate that some appropriate investigative action be taken. 8.6 Bias: In test method terminology, bias is the difference between an average test value and the reference (true) test property value. Refere
40、nce values do not exist for this test method since the value of the test property is exclusively defined by the test method. Bias, therefore, cannot be determined. 9991:73925 SBBS 52937:2001 Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:05:26 GMT+00:00 2006, Uncontrolled Copy, (c) BSI IS
41、O 1125:1999(E) ISO 4 9 Test report The test report shall include the following particulars: a) a reference to this International Standard; b) the results and the units in which they have been expressed; c) any unusual features noted during the determination; d) any operation not included in this Int
42、ernational Standard, or any operation regarded as optional such as the ashing temperature if different from the specified one or the omission of the crucible lid; e) the date of the test. 9991:73925 SBBS 52937:2001 Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:05:26 GMT+00:00 2006, Uncon
43、trolled Copy, (c) BSI BS 52937:19991002:73925 SB Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:05:26 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5293-7: 2001 ISO 1125:1999 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body re
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