1、Designation: D3265 15aD3265 17Standard Test Method forCarbon BlackTint Strength1This standard is issued under the fixed designation D3265; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in paren
2、theses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the tint strength of carbon black relative to an industry tint reference black(ITRB).1.2 The values state
3、d in SI units are to be regarded as the standard. The values given in parentheses are for information only.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety a
4、nd health practices and determine the applicability of regulatorylimitations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards,
5、 Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1799 Practice for Carbon BlackSampling Packaged ShipmentsD1900 Practice for Carbon BlackSampling Bulk ShipmentsD4483 Practice for Evaluating Preci
6、sion for Test Method Standards in the Rubber and Carbon Black Manufacturing IndustriesD4821 Guide for Carbon BlackValidation of Test Method Precision and Bias3. Summary of Test Method3.1 A carbon black sample is mixed with a white powder (zinc oxide) and a liquid vehicle (soybean oil epoxide) (epoxi
7、dizedsoybean oil, ESO) to produce a black or gray paste. This paste is then spread to produce a surface suitable for measuring thereflectance of the mixture by means of a photo-electric reflectance meter. The reflectance of the tested sample is then comparedto the reflectance of the ITRB prepared in
8、 the same manner. The tint strength of the tested sample is expressed as units of thereflectance of the ITRB divided by the reflectance of the sample and multiplied by 100, when calibration and standardization inSection 100.8 is performed with the original ITRB or multiplied by 101.34 when ITRB2 is
9、used in the calibration andstandardization step.3.2 Correction Factor:3.2.1 When ITRB-2, Paraplex G-62 (made before June 2012) and ZnO lot#8 are used, apply a correction factor of 1.0134 forthe calibration and standardization in Section 8.3.2.2 There should be no correction applied when ITRB is used
10、 with Paraplex G-62 and ZnO Lot#8 or earlier, that is, thecorrection factor is “1”.1 This test method is under the jurisdiction of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.21 on Carbon Black SurfaceArea and Related Properties.Current edition approved No
11、v. 1, 2015May 1, 2017. Published December 2015May 2017. Originally approved in 1973. Last previous edition approved in 2015 asD3265 15.D3265 15a. DOI: 10.1520/D3265-15A.10.1520/D3265-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceast
12、m.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becaus
13、eit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Bar
14、r Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.3 There should be no correction applied in the calculation in Section 10 when using the currently available tint raw materials(see Section 6) for pastes prepared with either ITRB or ITRB2, that is, the correction factor
15、 is “1”.34. Significance and Use4.1 For the broad range of commercial rubber grade carbon blacks, tint strength is highly dependent upon particle size. Tintstrength can be used as an indication of particle size; however, tint strength is also dependent on structure and aggregate sizedistribution. Th
16、erefore, differences in tint strength within grades of carbon black may reflect differences other than particle size.NOTE 1This test method was developed primarily for the characterization of N100, N200, and N300 series carbon blacks.4.2 Tint strength values within the carbon black industry have bee
17、n developed using aAutomatic Muller apparatus which is usedto prepare carbon black-zinc oxide pastes.Anew mixing apparatus, SpeedMixer4 (DAC 150 FVZ), and a corresponding procedurehave been extensively studied within D24 and shown to provide equivalent tint strength for all carcass or soft blacks an
18、d most treadblacks with the exception of higher surface area N100 types and specialty blacks. Therefore, it is the responsibility of the user ofthis alternate apparatus to ensure their products will adequately disperse. Disputes arising between a user and producer should beresolved using the Automat
19、ic Muller apparatus until ASTM develops adequate precision statements.4.3 The term ITRB is used in the entire text for both, the original ITRB, used as the first reference material for tint testing, butwhich is now used up, and the successor reference material, ITRB2. Wherever required, like in calc
20、ulations where it is crucial todifferentiate between the original ITRB and ITRB2, this will be clearly mentioned in the text of the test procedure.5. Apparatus5.1 Analytical Balance, with a sensitivity of 60.1 mg.5.2 Automatic Muller.5,65.3 Photometric Instrument, capable of detecting differences in
21、 the amount of light reflectance between shades of gray.7,6 Theinstrument is to be operated following the manufacturers instructions for optimum performance.5.4 Oven, Gravity-Convection Type, capable of temperature regulation within 61C at 125C (62F at 257F) and temperatureuniformity within 65C (69F
22、).5.5 Reflectance Standards, as required for each reflectance instrument for checking calibration.5.6 Spatulas, 100 to 150 mm (4 to 6 in.), two, flexible, tapered.5.7 Syringe, 5-cm3, automatic refilling, reproducible to 60.02 cm3.5.8 Wiping Tissue, absorbent and lint free.5.9 Paste Application Appar
23、atusAny one of the following groups of equipment may be used:5.9.1 Apparatus for Film Drawdown Method:5.9.1.1 Film Applicator,8,6 0.076 mm (0.003 in.) in depth.5.9.1.2 Polished Glass Plate, approximately 760 by 500 by 10 mm (30 by 20 by 0.375 in.).5.9.2 Apparatus for Roller Spreader Method:5.9.2.1 T
24、int Roller Spreader.8,5Tint Roller Spreader.9,65.10 Desiccator.3 In 2013 issues were reported when using Paraplex G-62 purchased after June 2012 and ZnO Lot#10.AnASTM task group investigated the issues and found the followingraw materials acceptable for Tint testing:1) ESO: Paraplex G-62 purchased b
25、efore June 2012 or currently available GreenChem Greenflex 7170, lot 590911X24, and2) zinc oxide Lot#8 or earlier, and currently available ZnO lot#11.It is highly recommended to only use these raw materials identified as acceptable as other sources may lead to unacceptable differences in the test re
26、sults. The tint taskgroup has determined that Paraplex G-62 with lot numbers that begin with the digit 5 and zinc oxide lots 9 and 10 are suspect and may not give acceptable results.When using the new raw materials for tint testing some differences may be observed with various grades of carbon black
27、 compared with historical data. For this reasonit is the responsibility of the manufacturer to identify any such differences, and if necessary, revise any specifications between producer and user.4 SpeedMixer is a registered trademark of FlackTek Inc., 1708 Highway 11, Bldg. G, Landrum, SC 29356. ht
28、tp:/5 The following instruments have been found satisfactory for this test method: Hoover Automatic Muller, Model M5, Hoover Color Corp., P.O. Box 218, State Highway693, Hiwassee, VA 24347. Automatic Pigment Muller JEL 25/53-II, J. Engelsmann AG, Frankenthaler Str. 137 141, 67059 Ludwigshafen, Germa
29、ny, www.engelsmann.de.6 If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1 which you may attend.7 The following instruments have been foun
30、d satisfactory for this test method: Erichsen Tint Tester 527, available from T. J. Bell, Inc., 1340 HomeAve.,Akron, OH 44310,and Hunter MiniScan EZ, available from Hunter Associates Laboratory, Inc., 11491 Sunset Hills Road, Reston, Virginia 20190-5280.The Hunter MiniScan XE or XE Plus may still be
31、 used for the test, but are no longer commercially available. Instructions are the same for all Hunter Miniscan types.The Densicron reflectometer, though no longer commercially available, may be used for the test. For instructions, see Test Method D3265 01.8 The sole source of supply of the FilmAppl
32、icator, Catalog No.AR-5257, known to the committee at this time is Byk-Gardner, 9104 Guilford Rd., Columbia, MD 21046.http:/.9 The sole source of supply of the Tint Roller Spreader, Model 1A, known to the committee at this time is Titan Specialties, Inc., P.OP.O. Box 2316, Pampa, TX79066-2316.D3265
33、1725.11 SpeedMixer (DAC 150 FVZ), PP15 cups and holder.10,65.12 IKA A-10 Analytical Mill, A-14 SS cutter, A-18 chamber reducer.11,65.13 5 mm Glass Grinding Beads.12,66. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is i
34、ntended all reagentsshall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where suchspecifications are available.13 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purityto permit its use with
35、out lessening the accuracy of the determination.6.2 Industry Tint Reference Black.146.3 Plasticizer, soybean oil epoxide.15,166.4 Denatured Alcohol, for cleaning purposes.6.5 Zinc Oxide, Industry Tint Zinc Oxide.17,6.6 ASTM D24 Standard Reference Blacks.18,7. Sampling7.1 Samples of shipments shall b
36、e taken in accordance with Practices D1799 and D1900.8. Calibration and Standardization8.1 Standard PastesPrepare pastes of the ITRB, following 9.2 9.3.2 for the following masses, prepare the 0.1000-gAutomatic Muller paste or the 0.1200-g SpeedMixer paste in duplicate:Industry Tint Reference Black C
37、alibration TintUnitsAutomaticMuller PastesSpeedMixerPastes0.0900 g 0.1080 g 90.00.1000 g 0.1200 g 100.00.1100 g 0.1320 g 110.00.1200 g 0.1440 g 120.00.1300 g 0.1560 g 130.0NOTE 2Optionally, 0.1400 and 0.1500 g ofAutomatic Muller paste or 0.1680 and 0.1800 g of SpeedMixer paste may be added in the st
38、andardizationstep when samples with tint results above 130 tint units are tested. The modified standardization should only be used for samples exceeding 130 tint units.8.2 Erichsen Tint Tester 527:8.2.1 Turn on the power switch and allow for 30 min warm-up.8.2.2 Place the reflectance head on the bla
39、ck calibration panel and adjust the digital readout to 0.00 using the “zero” controlpotentiometer.8.2.3 Following Section 9, prepare the paste drawdown for reflectance measurement.8.2.4 Use one of the 0.1000-g Automatic Muller or 0.1200-g SpeedMixer ITRB pastes of 8.1 to set the instrument to read 3
40、.00using the calibration control potentiometer.10 The sole source of supply of the SpeedMixer known to the committee at this time is FlackTek Inc., 1708 Highway 11, Bldg. G, Landrum, SC 29356.http:/11 The sole source of supply of the apparatus (Part #EW-04301-00) known to the committee at this time
41、is Cole-Parmer Instrument Company, 625 East Bunker Court,Vernon Hills, IL 60061. http:/12 The sole source of supply of glass grinding beads known to the committee at this time is Quackenbush Co., Inc., 6711 Sands Rd., Crystal Lake, IL 60014.http:/13 Reagent Chemicals, American Chemical Society Speci
42、fications , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Con
43、vention, Inc. (USPC), Rockville, MD.14 The original ITRB is depleted and therefore no longer commercially available. However, any available stocks of original ITRB may still be used. The successor of theoriginal ITRB is ITRB2. ITRB2 was commercialized in 2012.15 The sole source of supply of Paraplex
44、 G-62,the epoxidized Chemical Abstracts Registry Numbersoybean oil 12768-71-7, known to the committee at this time is C. P.Hall Co., Technical Center, Customer Service Department, 5851 West 73rd St., Chicago, IL 60638. (Minimum order is 5 gal and order should state “Refer to ASTMD3265.”)Balentine En
45、terprises, Inc., dba Laboratory Standards and Technologies, 227 Somerset St., Borger, TX 79007, .16 Supporting data (on the shelf life of this material) have been filed at ASTM International Headquarters and may be obtained by requesting Research ReportRR:D24-1004.17 The sole source of supply of Ind
46、ustry Tint Zinc Oxide known to the committee at this time is Balentine Enterprises, Inc., dba Laboratory Standards and Technologies,227 Somerset St., Borger, TX 79007, .18 The sole source of supply of ASTM D24 Standard Reference Blacks known to the committee at this time is Laboratory Standards and
47、Technologies, 227 Somerset St.,Borger, TX 79007.D3265 1738.2.5 Determine the reflectivity on the remaining 0.1000-g Automatic Muller or 0.1200-g SpeedMixer ITRB paste. Thisreflectance reading must be from 2.99 through 3.01 for the duplicate pastes to be considered acceptable.8.2.6 If the duplicate 0
48、.1000-g Automatic Muller or 0.1200-g SpeedMixer pastes are acceptable, the two duplicate pastes areblended together using a spatula, and the instrument is set to read 3.00 using the calibration control potentiometer.8.2.7 If the duplicate pastes are unacceptable, prepare another 0.1000-g Automatic M
49、uller or 0.1200-g SpeedMixer pastefollowing 9.2 9.3.2, and follow 8.2.5.8.2.8 Determine the reflectance value for all of the remaining ITRB pastes of 8.1.8.2.9 Calculate the tint strength of the standard pastes as follows:Tint Units53.00/S 3100 (1)where:S = reflectance value of sample.8.2.10 Calculate a regression of the standard values (y value) on the measured values (x value) by using the least squaresmethod.8.2.11
