1、BS ISO 3858:2008ICS 83.040.20NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDRubber compoundingingredients Carbonblack Determinationof light transmittanceof toluene extractThis British Standardwas published underthe authority of theStandards Policy andStrategy C
2、ommittee on 30September 2008 BSI 2008ISBN 978 0 580 63602 8Amendments/corrigenda issued since publicationDate CommentsBS ISO 3858:2008National forewordThis British Standard is the UK implementation of ISO 3858:2008. Itsupersedes BS ISO 3858:2004 which is withdrawn.The UK participation in its prepara
3、tion was entrusted 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 contrac
4、t. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.BS ISO 3858:2008Reference numberISO 3858:2008(E)ISO 2008INTERNATIONAL STANDARD ISO3858Third edition2008-09-15Rubber compounding ingredients Carbon black Determination
5、of light transmittance of toluene extract Ingrdients de mlange du caoutchouc Noir de carbone Dtermination de la transmittance spectrale de lextrait tolunique BS ISO 3858:2008ISO 3858:2008(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 2008 All rights reserved. Unless otherwise specified, no part of this publication
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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 2008 All rights reservedBS ISO 3858:2008ISO 3858:2008(E) ISO 2008 All rights reserved iiiForeword ISO (the International Organization for Standardization) is a worldwide federation of n
11、ational 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. Inter
12、national 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. International Standards are drafted in accordance with the
13、 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 voting. Publication as an International Standard requires approval by
14、 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 such patent rights. ISO 3858 was prepared by Technical Committee ISO/
15、TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry. This third edition cancels and replaces the second edition (ISO 3858:2004), of which it constitutes a minor revision, the main purpose of which was to remove the pulverization stage
16、for pelletized samples (6.2 in ISO 3858:2004) from the sample preparation procedure. BS ISO 3858:2008BS ISO 3858:2008INTERNATIONAL STANDARD ISO 3858:2008(E) ISO 2008 All rights reserved 1Rubber compounding ingredients Carbon black Determination of light transmittance of toluene extract WARNING Perso
17、ns 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 health practices and to ensure comp
18、liance with any national regulatory conditions. 1 Scope This International Standard specifies a method for the determination of the light transmittance of the toluene extract from carbon black for use in the rubber industry, as a means of measuring the discolouration caused by the extractable matter
19、. The light transmittance value provides an estimate of the degree of discolouration caused by the toluene-extractable matter present on the surface of the carbon black. This method may not be applicable to carbon blacks with a high extractable-matter content. 2 Normative references The following re
20、ferenced 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) applies. ISO 1124, Rubber compounding ingredients Carbon black shipment sa
21、mpling procedures ISO 1126:2006, Rubber compounding ingredients Carbon black Determination of loss on heating ISO/TR 9272, Rubber and rubber products Determination of precision for test method standards 3 Principle A sample of the carbon black is dried and a test portion weighed out and mixed with a
22、 measured volume of toluene at room temperature. The mixture is filtered and a portion of the filtrate transferred to an absorption cell. The light transmittance of the filtrate is measured against pure toluene at a set wavelength using a spectrophotometer. 4 Reagent 4.1 Toluene, analytical reagent
23、grade, C.A.S. No. 108-88-3. BS ISO 3858:2008ISO 3858:2008(E) 2 ISO 2008 All rights reserved5 Apparatus Ordinary laboratory equipment, plus the following: 5.1 Analytical balance, accurate to 0,1 mg. 5.2 Oven, preferably of the gravity-convection type, capable of temperature regulation within 1 C at 1
24、25 C and temperature uniformity within 5 C. 5.3 Spectrophotometer, with a tungsten filament lamp, 20 nm maximum spectral passband width, capable of measuring percent transmittance at a wavelength of 425 nm. The instrument shall be of the high-resolution prism or grating type, eliminating the use of
25、an optical filter. The instrument shall be operated in accordance with the manufacturers operating manual for optimum performance. Some instruments may require the use of a constant-voltage transformer in the electricity circuit in order to compensate for voltage variations of more than 4 V. NOTE Cu
26、rrent types of photometer could be used. However, they usually differ in passband width from the specified one, and they may give different transmittance results. Proper calibration of such instruments over the whole transmittance range against a high-resolution spectrophotometer (of a passband widt
27、h of 2 nm at 425 nm, for example) is recommended for possible corrections of the readings. 5.4 Absorption cells, with parallel sides polished flat to within 10 nm. The internal distance between the parallel faces shall be 10 mm 0,05 mm. NOTE 1 If the cell used does not have an optical path length of
28、 10 mm, the transmittance which would be obtained with a 10 mm cell is given by the equation 10 0 1010 20log log 2LL= + (1) where 0is the percentage transmittance through a 10 mm cell; is the percentage transmittance observed through the cell used; L is the optical path length, in millimetres, of th
29、e cell used. NOTE 2 Absorption cells may differ in their transmittance. It is recommended that the same absorption cell be used for adjustment of the spectrophotometer as for the actual measurements. 5.5 Conical flasks, capacity 100 cm3or 125 cm3, with ground-glass stoppers. 5.6 Graduated cylinder,
30、capacity 50 cm3, graduated in divisions of 1 cm3, or automatic dispenser, bottle type. 5.7 Filter funnel, 75 mm inside diameter at top, made of chemically resistant glass. 5.8 Filter paper, 150 mm diameter, free from matter extractable by toluene and capable of retaining all the carbon black. 5.9 Be
31、akers, capacity 50 cm3or 100 cm3, with pouring lip. 5.10 Wiping paper, lint free, or optical lens tissue. 5.11 Cotton swabs. 5.12 Fume hood, fully enclosed on three sides, with suitable fume extraction and spark-proof fan and motor. 5.13 Safety container, to discard the used toluene and carbon black
32、 extracts. BS ISO 3858:2008ISO 3858:2008(E) ISO 2008 All rights reserved 36 Sample preparation 6.1 Samples shall be taken in accordance with ISO 1124. 6.2 Dry approximately 4 g of the carbon black sample for 1 h at a temperature of 125 C in the oven (5.2) as specified in ISO 1126:2006, method 1. All
33、ow to cool to ambient temperature in a desiccator. Keep the dried sample in the desiccator until ready for testing. Carbon black shall not 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 re
34、sults. NOTE Drying is optional for blacks, such as thermal blacks, which are produced by a “dry” process. 7 Conditions of test The test shall be carried out under standard conditions of 23 C 2 C and (50 5) % or 27 C 2 C and (65 5) % relative humidity. The reagent and apparatus shall be kept in the t
35、est environment for a time sufficient to reach ambient temperature before being used. IMPORTANT Toluene is a hazardous material, therefore this test shall be carried out in a fume hood with suitable fume extraction. Any motor, fan, etc. shall be spark-proof. The hood shall also be free from other fu
36、mes or vapours which might contaminate the reagent or equipment used and therefore affect the results. 8 Procedure 8.1 Standardization of spectrophotometer 8.1.1 Allow the spectrophotometer (5.3) to warm up for the length of time specified in the instrument operating manual. 8.1.2 Set the wavelength
37、 of the instrument at 425 nm. Check the zero reading of the instrument and adjust if necessary. 8.1.3 Place a filter paper (5.8) in a funnel (5.7) and filter approximately 30 cm3of toluene (4.1) into a conical flask (5.5), and stopper the flask. 8.1.4 Pour a portion of the filtered toluene into a be
38、aker (5.9). 8.1.5 With the heIp of the beaker pouring lip, rinse an absorption cell (5.4) three times with the filtered toluene, filling to approximately one-third full each time. Handle the absorption cell on the ground-glass sides only. Do not touch the smooth, clear sides with the fingers. 8.1.6
39、Fill the cell with filtered toluene and wipe the outside surfaces thoroughly with wiping paper or optical lens tissue (5.10), while holding the cell in front of a suitable Iight source for proper inspection. The contents of the cell shall be free of any contaminant, such as lint particles, which mig
40、ht cause light scattering and influence the results. lf necessary, clean the inside surface with a cotton swab (5.11), or wipe again the outside until perfectly clean. If cleaning of the internal cell surface is necessary, restart the procedure as in 8.1.5. 8.1.7 Place the absorption cell in the spe
41、ctrophotometer, and adjust the instrument to read 100 % transmittance at a wavelength of 425 nm. BS ISO 3858:2008ISO 3858:2008(E) 4 ISO 2008 All rights reserved8.2 Sample testing 8.2.1 Except for N990, N991, N907 and N908 carbon blacks, weigh out 2 g 0,01 g of the dried carbon black and transfer thi
42、s test portion to a conical flask (5.5). For N990 and N991 carbon blacks, weigh out 5,0 g 0,01 g of black; for N907 and N908 carbon blacks, weigh out 3,0 g 0,01 g of black. 8.2.2 Using the graduated cylinder or automatic dispenser (5.6), add 20 cm3 0,5 cm3of toluene to the conical flask containing t
43、he test portion and stopper the flask (for N990 and N991 add 50 cm3 0,5 cm3of toluene, for N907 and N908 add 30 cm3 0,5 cm3of toluene). If necessary, larger quantities of test portion and toluene may be used, but they shall remain in the ratio of 10 cm3of toluene for every 1 g of carbon black. 8.2.3
44、 Within 5 s of adding the toluene, shake the mixture vigorously by hand for 60 s to 65 s. Alternatively, a mechanical shaker, capable of vigorous shaking at a rate of about 240 shakes per minute, may be used. 8.2.4 lmmediately after shaking, filter the mixture with a funnel (5.7) and a filter paper
45、(5.8) into a second conical fIask (5.5), and stopper the flask. lf there is evidence of any trace of carbon in the filtrate, discard it, and repeat. Change the filter paper for each test portion. WARNING Carbon blacks may contain polycyclic aromatic compounds, some of which are known carcinogens. Th
46、ese compounds, when present, are so strongly bound to the carbon black that they are biologically inactive, but they may be removed by the procedure specified in this standard. Care should be taken to avoid skin contact with solvent extracts from carbon blacks. 8.2.5 Using an absorption cell matchin
47、g in transmittance the one used in 8.1.5, or if possible the same cell, repeat with the filtrate (see 8.2.4) the operations described in 8.1.4 to 8.1.6. 8.2.6 Place the absorption cell in the standardized (see 8.1) spectrophotometer, and record the percentage transmittance at the 425 nm wavelength t
48、o the nearest 1 %. 8.2.7 Rinse the absorption cell with clean toluene (4.1) immediately after each determination. 8.2.8 lf possible, correct the transmittance values given by the spectrophotometer in accordance with the Note to 5.3 and Note 1 to 5.4 and record the result to the nearest 1 %. 9 Precis
49、ion and bias 9.1 Precision and bias information have been obtained from an interlaboratory test programme carried out in accordance with ISO/TR 9272. 9.2 The results give an estimate of the precision as described below. The precision parameters shall 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 testing protocols that include this test method. 9.3 A Type 1 interlaborato
