1、Designation: D3265 171D3265 17aStandard 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 pare
2、ntheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1 NOTEEditorially corrected footnote 15 in August 2017.1. Scope1.1 This test method covers the determination of the tint strength of carbon black relative to an
3、industry tint reference black(ITRB).1.2 The values stated 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
4、 user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability ofregulatory limitations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in th
5、e Decision on Principles for the Development of International Standards, 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 fo
6、r Carbon BlackSampling Bulk ShipmentsD4483 Practice for Evaluating Precision 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 whi
7、te powder (zinc oxide) and a liquid vehicle (epoxidized soybean oil, ESO) toproduce a black or gray paste. This paste is then spread to produce a surface suitable for measuring the reflectance of the mixtureby means of a photo-electric reflectance meter. The reflectance of the tested sample is then
8、compared to the reflectance of the ITRBprepared in the same manner. The tint strength of the tested sample is expressed as units of the reflectance of the ITRB dividedby the reflectance of the sample and multiplied by 100.3.2 Correction Factor:3.2.1 When ITRB-2, Paraplex G-62 (made before June 2012)
9、 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 with Paraplex G-62 and ZnO Lot#8 or earlier, that is, thecorrection factor is “1”.1 This test method is under the jurisdictio
10、n 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 May 1, 2017Sept. 1, 2017. Published May 2017October 2017. Originally approved in 1973. Last previous edition approved in 2015201
11、7 asD3265 15a.D3265 171. DOI: 10.1520/D3265-17E01.10.1520/D3265-17A.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM w
12、ebsite.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. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult pr
13、ior 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 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.3 There should be no correction appli
14、ed 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 is “1”.34. Significance and Use4.1 For the broad range of commercial rubber grade carbon blacks, tint strength is hig
15、hly 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. Therefore, differences in tint strength within grades of carbon black may reflect differences other than particle size.N
16、OTE 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 been developed using aAutomatic Muller apparatus which is usedto prepare carbon black-zinc oxide pastes.Anew mixing appar
17、atus, 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 and most treadblacks with the exception of higher surface area N100 types and specialty blacks. Therefore, it is the res
18、ponsibility of the user ofthis alternate apparatus to ensure their products will adequately disperse. Disputes arising between a user and producer should beresolved using the Automatic Muller apparatus until ASTM develops adequate precision statements.4.3 The term ITRB is used in the entire text for
19、 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 calculations where it is crucial todifferentiate between the original ITRB and ITRB2, this will be clearly mentioned in th
20、e 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 the amount of light reflectance between shades of gray.7,6 Theinstrument is to be operated following the manufacturer
21、s 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).5.5 Reflectance Standards, as required for each reflectance instrument for checking calibration.5.6 Spatulas, 100 to
22、 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 ApparatusAny one of the following groups of equipment may be used:5.9.1 Apparatus for Film Drawdown Method:5.9.1.1 Film App
23、licator,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 Tint Roller Spreader.9,65.10 Desiccator.3 In 2013 issues were reported when using Paraplex G-62 purchased after June 20
24、12 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 before June 2012 or currently available GreenChem Greenflex 7170, lot 590911X24, and2) zinc oxide Lot#8 or earlier, and currently available ZnO
25、 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 results. 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 susp
26、ect 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 compared with historical data. For this reasonit is the responsibility of the manufacturer to identify any such differences, and if necessary
27、, revise any specifications between producer and user.4 SpeedMixer is a registered trademark of FlackTek Inc., 1708 Highway 11, Bldg. G, Landrum, SC 29356. http:/5 The following instruments have been found satisfactory for this test method: Hoover Automatic Muller, Model M5, Hoover Color Corp., P.O.
28、 Box 218, State Highway693, Hiwassee, VA 24347. Automatic Pigment Muller JEL 25/53-II, J. Engelsmann AG, Frankenthaler Str. 137 141, 67059 Ludwigshafen, Germany, www.engelsmann.de.6 If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your co
29、mments will receive careful consideration at ameeting of the responsible technical committee,1 which you may attend.7 The following instruments have been found satisfactory for this test method: Erichsen Tint Tester 527, available from T. J. Bell, Inc., 1340 HomeAve.,Akron, OH 44310,and Hunter MiniS
30、can 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 used for the test, but are no longer commercially available. Instructions are the same for all Hunter Miniscan types.The Densicron reflectome
31、ter, 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 FilmApplicator, 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
32、 of supply of the Tint Roller Spreader, Model 1A, known to the committee at this time is Titan Specialties, Inc., P.O. Box 2316, Pampa, TX 79066-2316.D3265 17a25.11 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 Gl
33、ass Grinding Beads.12,66. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended all reagentsshall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where suchspe
34、cifications are available.13 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purityto permit its use without lessening the accuracy of the determination.6.2 Industry Tint Reference Black.146.3 Plasticizer, soybean oil epoxide.15,166.4 Denatured Alc
35、ohol, for cleaning purposes.6.5 Zinc Oxide, Industry Tint Zinc Oxide.176.6 ASTM D24 Standard Reference Blacks.187. Sampling7.1 Samples of shipments shall be taken in accordance with Practices D1799 and D1900.8. Calibration and Standardization8.1 Standard PastesPrepare pastes of the ITRB, following 9
36、.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 Calibration 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 1
37、20.00.1300 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 standardizationstep when samples with tint results above 130 tint units are tested. The modified standardization should only be used for samples ex
38、ceeding 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 black calibration panel and adjust the digital readout to 0.00 using the “zero” controlpotentiometer.8.2.3 Following Section 9, prepare the paste dr
39、awdown 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 3.00using the calibration control potentiometer.8.2.5 Determine the reflectivity on the remaining 0.1000-g Automatic Muller or 0.1200-g SpeedMixer
40、 ITRB paste. Thisreflectance reading must be from 2.99 through 3.01 for the duplicate pastes to be considered acceptable.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
41、 of the apparatus (Part #EW-04301-00) known to the committee at this time 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
42、Lake, IL 60014.http:/13 Reagent Chemicals, American Chemical Society Specifications , 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 th
43、e United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, 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.
44、 ITRB2 was commercialized in 2012.15 The sole source of supply of the epoxidized soybean oil (Greenflex 7170) known to the committee at this time is Balentine Enterprises, Inc., dba Laboratory Standardsand Technologies, 227 Somerset St., Borger, TX 79007, .16 Supporting data (on the shelf life of th
45、is 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 Industry Tint Zinc Oxide known to the committee at this time is Balentine Enterprises, Inc., dba Laboratory Standards and Technologies,227 Some
46、rset 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 Technologies, 227 Somerset St.,Borger, TX 79007.D3265 17a38.2.6 If the duplicate 0.1000-g Automatic Muller or 0.1200-g SpeedMixer pastes are
47、 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 Muller or 0.1200-g SpeedMixer pastefollowing 9.2 9.3.2, and
48、 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 me
49、asured values (x value) by using the least squaresmethod.8.2.11 The measured tint strength of all subsequent samples is corrected by substituting each measured value into this linearequation and calculating the corrected value for the tint strength.8.2.12 New regression coefficients are determined periodically, typically on a monthly basis.NOTE 3Proper paste preparation and regression may be validated by analyzing
