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1、BRITISH STANDARD BS 5293-15: 1991 ISO 3858-2: 1990 Sampling and testing carbon black for use in the rubber industry Part 15: Method for determination of light transmittance of toluene extract for product evaluation Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:03:18 GMT+00:00 2006, Uncon
2、trolled Copy, (c) BSI BS 5293-15:1991 This British Standard, having been prepared under the direction of the Plastics and Rubber Standards Policy Committee, was published under the authority of the Standards Board and comes into effect on 31 May 1991 BSI 10-1999 First published as BS 5293:1976 First
3、 published as BS 5293-15 May 1991 The following BSI references relate to the work on this standard: Committee reference PRM/53 Draft for comment 90/45390 ISBN 0 580 19585 6 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Plastics and Rub
4、ber Standards Policy Committee (PRM/-) to Technical Committee PRM/53, upon which the following body was represented: British Rubber Manufacturers Association Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:03:18 GMT+00:00 2006, Uncon
5、trolled Copy, (c) BSI BS 5293-15:1991 BSI 10-1999i Contents Page Committees responsibleInside front cover National forewordii 1Scope1 2Normative references1 3Principle1 4Reagent1 5Apparatus1 6Sample preparation2 7Condition of test2 8Procedure2 9Expression of results3 10Test report3 Publication(s) re
6、ferred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:03:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5293-15:1991 ii BSI 10-1999 National foreword This Part of BS 5293 has been prepared under the direction of the Plastics and Rubber Standards Policy Committee and
7、is identical with ISO 3858-2:1990, “Carbon black for use in the rubber industry Determination of light transmittance of toluene extract Part 2: Method for product evaluation” published by the International Organization for Standardization (ISO). This Part of BS 5293 is part of a revision of BS 5293:
8、1976 as a multipart standard, Parts of which are identical to ISO standards. This Part of BS 5293 supersedes 5.6 of BS 5293:1976, which will be amended accordingly. BS 5293-14 describes a similar photometric method which is more rapid and where pellets of carbon black are not crushed. A British Stan
9、dard does not purport to include 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. Cross-references International StandardCorresponding Br
10、itish Standard ISO 471:1983BS 903 Physical testing of rubber Part A35:1985 Temperatures, humidities and times for conditioning and testing of test pieces (Identical) ISO 1126:1985BS 5293 Sampling and testing carbon black for use in the rubber industry Part 5:1988 Method for determination of loss of
11、mass on heating (Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1 to 4, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the
12、amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:03:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5293-15:1991 BSI 10-19991 1 Scope This part of ISO 3858 specifies a method for the determination of the light transmittance of the toluene extract
13、from carbon black for use in the rubber industry, as a means of measuring the discoloration caused by the extracted matter, as is required in product evaluation. The degree of discoloration is quantitatively measured by means of a spectrometer. This method is not applicable to carbon blacks with hig
14、h toluene extracts. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this part of ISO 3858. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements
15、 based on this part of ISO 3858 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 471:1983, Rubber Standard temperatures, humidities and times
16、for the conditioning and testing of test pieces. ISO 1126:1985, Rubber compounding ingredients Carbon black Determination of loss on heating. 3 Principle Drying of the carbon black and weighing of a test portion. Mixing with a measured volume of toluene at room temperature. Filtration of the mixture
17、 and transfer of the filtrate to an absorption cell. Measurement of the light transmittance of the filtrate against pure toluene at a set wavelength using a spectrometer. 4 Reagent 4.1 Toluene, analytical reagent grade. 5 Apparatus Ordinary laboratory equipment and 5.1 Analytical balance, accurate t
18、o at least 0,01 g. 5.2 Oven, capable of maintaining a temperature of 105 C 2 C or 125 C 2 C. 5.3 Spectrometer, giving direct readings of light transmittance at 425 nm. The spectrometer shall be of the high-resolution prism or grating type eliminating the use of an optical filter. The passband shall
19、be within 10 nm. A constant-voltage transformer shall be inserted into the supply circuit if the voltage is known to vary by more than 4 V. NOTE 1Current types of colorimeter may differ in passband width and may therefore give different transmittance results. The results may be more comparable if su
20、ch colorimeters are calibrated over the whole of the useful transmittance range against the same high-resolution spectrometer, for example one having a passband which is narrower than 2 nm at the 425 nm central wavelength, and the readings corrected using the calibration curve thus produced for each
21、 colorimeter. 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 (see notes 2 and 3). NOTE 2Cylindrical cells of inner diameter 10 mm 0,05 mm may give different results from parallelepipedic cells. If used,
22、 it is recommended that they be calibrated against a parallelepipedic cell over the whole of their useful transmittance range and that corrections be taken from the calibration curve thus produced. NOTE 3If the cell used does not have an optical path length of 10 mm, the transmittance which would be
23、 obtained with a 10 mm cell is given by the equation where NOTE 4Absorption cells may differ in their transmittance. It is recommended that the same absorption cell be used for adjustment of the spectrometer as for the actual measurements. 5.5 Conical flasks, capacity 100 cm3 or 125 cm3, with ground
24、-glass stopper. 5.6 Graduated cylinder, capacity 50 cm3, graduated in divisions of 1 cm3. 5.7 Pulverizer, i.e. mortar and pestle, high-speed blade mixer or equivalent. 5.8 Filter funnels, 75 mm inside diameter at top, made of chemically resistant glass. 5.9 Filter paper, 150 mm diameter, free from m
25、atter extractable by toluene, and capable of retaining all the carbon black. E0is the percentage transmittance through a 10 mm cell; Eis the percentage transmittance observed through the cell used; lis the optical path length, in millimetres, of the cell used. lg0 10 l -lg 20 l - -2+= Licensed Copy:
26、 sheffieldun sheffieldun, na, Mon Dec 04 16:03:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5293-15:1991 2 BSI 10-1999 5.10 Beakers, capacity 50 cm3 or 100 cm3, with pouring lip. 6 Sample preparation 6.1 Pulverize pelletized samples using the mortar and pestle or equivalent (5.7). 6.2 Dry approx
27、imately 4 g of the pulverized carbon black sample for 1 h at a temperature of either 105 C 2 C or 125 C 2 C in accordance with ISO 1126. Allow 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 tempera
28、ture higher than that specified, nor dried using infra-red lamps, as some of the extract may be driven off, thus affecting the results. 7 Conditions of test The test shall be carried out under standard conditions, as given in ISO 471, of 23 C 2 C and (50 5) % relative humidity or 27 C 2 C and (65 5)
29、 % relative humidity. The reagent and apparatus shall be kept in the test environment for a time sufficient to reach ambient temperature before being used. IMPORTANT Toluene is a hazardous and toxic material, therefore this test shall be carried out in a fume cupboard with suitable fume extraction.
30、Any motor, fan, etc., shall be spark proof. The cupboard shall also be free from other fumes or vapours which might contaminate the reagent or equipment used and therefore affect the results. 8 Procedure WARNING All recognized health and safety precautions shall be taken when using the procedure spe
31、cified in this part of ISO 3858. Carbon blacks may contain polynuclear aromatic compounds, some of which are known carcinogens. These 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 par
32、t of ISO 3858. Care should be taken to avoid skin contact with solvent extracts from such carbon blacks. 8.1 Allow the spectrometer (5.3) to warm up for at least 10 min before adjustment (see 5.4, note 4). Filter approximately 30 cm3 of toluene (4.1) into a conical flask (5.5) and stopper the flask.
33、 Pour a portion of the toluene into a beaker (5.10) and rinse an absorption cell (5.4) three times with 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. Fill the cell
34、 with the filtered toluene and dry the out-side of the cell with optical lens tissue. Place the cell in the spectrometer and adjust the instrument to 100 % transmittance using a wavelength of 425 nm. 8.2 Weigh out 2 g 0,01 g of the pulverized and dried carbon black and transfer this test portion to
35、a conical flask (5.5). If the capacity of the absorption cell makes it necessary, use a larger test portion; add 10 cm3 of toluene for each additional gram of carbon black. 8.3 Using the graduated cylinder (5.6), pour 20 cm3 0,5 cm3 of filtered toluene into the conical flask containing the test port
36、ion and stopper the flask. 8.4 Within 5 s after adding the toluene, shake the mixture by hand for (60) s. Alternatively, a mechanical shaker, capable of vigorous shaking at a rate of approximately 240 shakes per minute, may be used. 8.5 Immediately after swirling, filter the mixture through the filt
37、er paper (5.9) into a second conical flask (5.5) and stopper the flask. If there is evidence of any trace of carbon black in the filtrate, discard and repeat. Change the filter paper for each test portion. 8.6 Rinse the absorption cell three times, each time using approximately 1 cm3 of the filtrate
38、 from 8.5 and emptying the cell. 8.7 Fill the absorption cell to the top with the filtrate from 8.5 and dry the outside of the cell with optical lens tissue. 8.8 Place the cell in the adjusted spectrometer (see 8.1) and read the percentage transmittance at a wavelength of 425 nm. 8.9 Rinse the absor
39、ption cell with clean toluene immediately after each determination. +5 0 Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:03:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5293-15:1991 BSI 10-19993 9 Expression of results The reading obtained in 8.8 is the light transmittance of the tolue
40、ne extract, expressed as a percentage, for an optical path length through the filtrate of 10 mm at a wavelength of 425 nm, with reference to pure toluene. Round off the result to the nearest 1 %. 10 Test report The test report shall include the following information: a) a reference to this part of I
41、SO 3858; b) all details necessary for full identification of the sample; c) all details necessary for identification of the spectrometer used; d) the drying temperature used; e) the result obtained; f) the date of the test. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:03:18 GMT+00:00 20
42、06, Uncontrolled Copy, (c) BSI 4 blank Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:03:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5293-15:1991 BSI 10-1999 Publication(s) referred to See national foreword. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:03:18 GMT+00:00 20
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