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1、BRITISH STANDARD BS 5293-13: 1995 ISO 5435:1994 Sampling and testing carbon black for use in the rubber industry Part 13: Method for determination of tinting strength Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:04:53 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5293-13:1995 This Briti
2、sh Standard, having been prepared under the direction of the Materials and Chemicals Sector Board (I/-), was published under the authority of the Standards Board and comes into effect on 15 February 1995 BSI 09-1999 The following BSI references relate to the work on this standard: Committee referenc
3、e PRI/53 Draft for comment 93/305912 DC ISBN 0 580 23661 7 Committees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Committee PRI/53 Carbon black, upon which the following body was represented: British Rubber Manufacturers Association Amend
4、ments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:04:53 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5293-13:1995 BSI 09-1999i Contents Page Committees responsibleInside front cover National forewordii 1Scope1 2Normative references1 3Princ
5、iple1 4Reagents1 5Apparatus1 6Test conditions1 7Procedure1 8Expression of results4 9Test report4 Figure 1 Slide preparation apparatus for Meeco Colormaster5 List of referencesInside back cover Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:04:53 GMT+00:00 2006, Uncontrolled Copy, (c) BSI
6、BS 5293-13:1995 ii BSI 09-1999 National foreword This Part of BS 5293 has been prepared by Technical Committee PRI/53 and is identical with ISO 5435:1994 Rubber compounding ingredients Carbon black Determination of tinting strength, published by the International Organization for Standardization (IS
7、O). This edition supersedes BS 5923-13:1992 which is withdrawn. The only technical change in this edition is the addition of an extra line (for 0.140 g of carbon black) in Table 1. The Technical Committee has reviewed the provisions of ISO 6809:1989, to which normative references is made in the text
8、, and has decided that they are acceptable for use in conjunction with this standard. A British Standard 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 it
9、self confer immunity from legal obligations. Cross-references International StandardCorresponding British 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 1126:1992BS 5293 Sampling and
10、 testing carbon black for use in the rubber industry Part 5:1992 Method for determination of loss of mass on heating (Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1 to 6, an inside back cover and a back cover. This standard has been
11、updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:04:53 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5293-13:1995 BSI 09-19991 WARNING Persons usin
12、g this International Standard should be familiar with normal laboratory practice. The 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 compliance w
13、ith any national regulatory conditions. 1 Scope This International Standard specifies a method for the determination of the tinting strength of carbon black relative to an industry tint reference black. The method is based on the use of three different commercial instruments. Other instruments may b
14、e used but they shall have at least equivalent performance. NOTE 1Details of the manufacturers of the Erichsen Tint Tester are given in the relevant clause of this International Standard. The Densichron reflectometer and the Meeco Colormaster are no longer available commercially, but the methods are
15、 included for the benefit of users of these instruments. 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 sub
16、ject to revision, and parties to agreements 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 471:, Rubber
17、 Times, temperatures and humidities for conditioning and testing1). ISO 1126:1992, Rubber compounding ingredients Carbon black Determination of loss on heating. ISO 6809:1989, Rubber compounding ingredients Carbon black Standard reference blacks. 3 Principle An industry tint reference black (ITRB) i
18、s mixed with zinc oxide and a liquid plasticizer. The paste obtained is mulled and homogenized, then spread as a layer of regular thickness. Its light reflectance is measured with a reflectometer sensitive to different shades of grey. A test sample is mixed and its light reflectance measured in the
19、same manner and, from the two light reflectance values, the relative tinting strength of the sample is determined. 4 Reagents 4.1 Soyabean oil epoxide, for use as plasticizer, of relative density 0,92 to 0,99. It is essential that the soyabean oil epoxide is maintained above 20 C to prevent turbidit
20、y which leads to erroneous results. 4.2 Industry tint reference black (ITRB)2) 4.3 Zinc oxide, e.g. industry tint zinc oxide (ITZnO)3). Other zinc oxides may be used, provided that they give the same results. 4.4 Standard reference blacks, conforming with the requirements of ISO 6809. 5 Apparatus 5.
21、1 Analytical balance, accurate to 0,1 mg. 5.2 Automatic muller 5.3 Oven, capable of being maintained at 105 C 2 C or 125 C 2 C. 5.4 Flexible palette knives, preferably tapered, of stainless steel, 100 mm to 150 mm long. 5.5 Syringe, automatic filling, accurate to 0,02 cm3. 5.6 Light-measuring instru
22、ment, sensitive to variations in light reflectance of shades of grey (see under appropriate procedure). 5.7 Paste application apparatus (see under appropriate procedure). 6 Test conditions The test should preferably be carried out under standard temperature and humidity conditions as specified in IS
23、O 471, i.e. 23 C 2 C and (50 5) % relative humidity or 27 C 2 C and (65 5) % relative humidity. 7 Procedure 7.1 Preparation of pastes 7.1.1 Dry the ITZnO (4.3) and carbon black in accordance with ISO 1126. Just sufficient ITRB (4.2) should be dried, as re-drying on a future occasion is not recommend
24、ed. 7.1.2 Weigh the required amount of carbon black or ITRB (see 7.1.10 and 7.1.11) to the nearest 1 mg (crushing of pelleted carbon blacks is beneficial). Weigh 3,750 g 1 mg of the ITZnO. 1) To be published. (Revision of ISO 471:1983 and ISO 1826:1981) 2) ITRB is available from Degussa Carbon Black
25、 Corporation, 1034 S. Broadway, Akron, Ohio 44311, USA. 3) ITZnO is available from Titan Specialties Inc., SWY 152W, P.O. Box 2316, Pampa, Texas 79066-2316, USA. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:04:53 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5293-13:1995 2 BSI 09-1999 7
26、.1.3 Using the syringe (5.5), place 2,2 cm3 of the plasticizer (4.1) in the centre of the lower glass plate of the automatic muller (5.2). 7.1.4 Place the ITZnO and carbon black in the centre of the pool of plasticizer. 7.1.5 Mix the three materials thoroughly with the palette knife (5.4). 7.1.6 Set
27、 the muller to a pressure of 0,017 MPa between the plates (445 N force when using 18,4 cm diameter plates), by placing the extra masses, supplied with the instrument, on the arm. Close and mull for 25 revolutions. 7.1.7 Open the plates, scrape the upper plate with a palette knife to remove as much p
28、aste as possible and transfer it to the lower plate. Then, with the lower plate rotating, use the palette knife to spread the paste to a flattened circle on the plate, and work all the paste to the centre. Repeat this step twice more. 7.1.8 Repeat steps 7.1.6 and 7.1.7 three times, i.e. for a total
29、of four 25 revolutions. 7.1.9 Remove the paste to a clean smooth surface. Pastes should be tested immediately (in no case shall they be kept for more than 24 h). 7.1.10 For calibration, prepare pastes in duplicate using the masses of carbon black in Table 1. Table 1 7.1.11 For determinations of tint
30、ing strength of test samples, prepare duplicate pastes with 0,100 g of N 100 to N 400 series carbon blacks; 0,200 g of N 500 to N 700 series carbon blacks. 7.2 Individual procedures Instructions are given relating to different types of commercial instrument (5.6). Other instruments may be used provi
31、ded that they have similar performance. All instruments shall be operated in accordance with the manufacturers instructions. 7.2.1 Measurements using the Erichsen Tint Tester 7.2.1.1 Apparatus NOTE 2For general details, see 5.1 to 5.5. 7.2.1.1.1 Erichsen Tint Tester4), model 517 or 527. NOTE 3Model
32、527 has a specially designed head which keeps the paste off the lens. 7.2.1.1.2 Film applicator, 0,08 mm gauge depth, to give 0,04 mm wet film thickness. 7.2.1.1.3 Glass plate, approximately 750 mm 500 mm 10 mm. 7.2.1.2 Calibration 7.2.1.2.1 Switch on the instrument and adjust in accordance with the
33、 manufacturers instructions. Clean the glass plate (7.2.1.1.3) with a tissue to remove any dust particles or film. Using a clean palette knife (5.4), place a portion of one of the mulled pastes with 100 % calibration tint value (7.1.10) at the top edge of the glass plate and smear it almost to the b
34、ottom edge. Using the film applicator (7.2.1.1.2), draw down the paste to the bottom edge in about 2 s to 3 s. 7.2.1.2.2 Place the reflectometer head on the drawdown on the paste. Adjust the meter to read 3,0 for at least three readings, all taken at 75 mm or more from the top of the drawdown. If th
35、e results are variable, gather up the paste and make another drawdown. 7.2.1.2.3 Make a duplicate drawdown of the duplicate paste as in 7.2.1.2.1. Without altering the setting, take three readings from the duplicate paste. If the results are variable, gather up the paste and make another drawdown. T
36、hese pastes are acceptable if a reading of 3,0 0,03 is obtained from the duplicate paste. NOTE 4It is beneficial to have the two drawdowns side by side. 7.2.1.2.4 If these pastes are acceptable, blend the two together using a palette knife. 7.2.1.2.5 If the pastes are not acceptable, prepare a furth
37、er paste and determine its reflectance using the same procedure. 7.2.1.2.6 Blend together whichever two of these three pastes do not differ by more than 0,03. 7.2.1.2.7 Determine the reflectance values of the remaining calibration pastes (see 7.1.10), taking three readings from each paste. 7.2.1.2.8
38、 Plot a graph of the average readings versus the calibration tint values or determine the equation to give the best fit. NOTE 5The equation is not necessarily linear. IRTBCalibration tint value g% 0,090 0,100 0,110 0,120 0,130 0,140 90 units 100 units 110 units 120 units 130 units 140 units 4) The E
39、richsen Tint Tester is the trade-name of an apparatus supplied by Erichsen GmbH u. Co KG, 5870 Hemer-Sundwig, Germany. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of the apparatus named. Equivalent products may b
40、e used if they can be shown to lead to the same results. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 16:04:53 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5293-13:1995 BSI 09-19993 7.2.1.2.9 Periodically check the proper calibration and standardization of the equipment, reagents, materia
41、ls and method, as required, using standard reference blacks (4.4). 7.2.1.3 Determination of tinting strength of a test sample 7.2.1.3.1 Prepare duplicate pastes of 100 % calibration tint values as described in 7.1.1 to 7.1.10. 7.2.1.3.2 Prepare the paste and set the instrument to 3,0 as described in
42、 7.2.1.2.1 to 7.2.1.2.6. 7.2.1.3.3 Using the correct mass of the test sample (see 7.1.11), prepare duplicate pastes as described in 7.1.1 to 7.1.9. 7.2.1.3.4 Determine the reflectance values of the pastes containing the test sample, taking three readings with each. 7.2.1.3.5 Determine the tinting st
43、rength of the test sample by using the graph or equation determined in 7.2.1.2.8. 7.2.2 Measurements using the Densichron reflectometer (film drawdown and roller spreader methods) 7.2.2.1 Apparatus NOTE 6For general details, see 5.1 to 5.5. 7.2.2.1.1 Densichron reflectometer, for the film drawdown m
44、ethod. 7.2.2.1.2 Film applicator, 0,08 mm gauge depth, to give 0,04 mm wet film thickness. 7.2.2.1.3 Glass plate, approximately 750 mm 500 mm 10 mm. 7.2.2.1.4 Tint roller spreader, for the roller spreader method. 7.2.2.2 Calibration 7.2.2.2.1 Film drawdown method 7.2.2.2.1.1 Clean the glass plate (7
45、.2.2.1.3) with a tissue to remove any dust particles or film. Using a clean palette knife (5.4), place a portion of one of the mulled pastes with 100 % calibration tint value (7.1.10) at the top edge of the glass plate and smear it almost to the bottom edge. Using the film applicator (7.2.2.1.2), dr
46、aw down the paste to the bottom edge in about 2 s to 3 s. 7.2.2.2.1.2 Set the range switch to 2 and operate with no filter in the reflection head. Use 4,76 mm aperture if head No. 3882A is used. Place the reflectometer head on the drawdown of the paste. Adjust the meter reading to read 80 % for at l
47、east three readings, all taken at 75 mm or more from the top of the drawdown. If the results are variable, gather up the paste and make another drawdown. 7.2.2.2.1.3 Make a duplicate drawdown of the duplicate paste as in 7.2.2.2.1.1. Without altering the setting, take three readings from the duplica
48、te paste. If the results are variable, gather up the paste and make another drawdown. These pastes are acceptable if a reading of 80 0,5 is obtained from the duplicate paste. NOTE 7It is beneficial to have the two drawdowns side by side. 7.2.2.2.1.4 If these pastes are acceptable, blend the two toge
49、ther using a palette knife. 7.2.2.2.1.5 If the pastes are not acceptable, prepare another paste containing 0,100 g of ITRB and check using the same procedure. 7.2.2.2.1.6 Blend together whichever two of these three pastes do not differ by more than 0,5 %. 7.2.2.2.1.7 Determine the reflectance values of the remaining calibration pastes (see 7.1.10), taking three readings from each paste. 7.2.2.2.2 Roller spreader method 7.2.2.2.2.1 Using a clean palette knife (5.4) place a portion of one of the mulled pastes of 100 % cali