1、Designation: D3265 171Standard 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 parentheses i
2、ndicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEEditorially corrected footnote 15 in August 2017.1. Scope1.1 This test method covers the determination of the tintstrength of carbon black relative to an industry ti
3、nt referenceblack (ITRB).1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this
4、standard to establish appro-priate safety, health and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decisio
5、n on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon B
6、lackSampling Bulk Ship-mentsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD4821 Guide for Carbon BlackValidation of Test MethodPrecision and Bias3. Summary of Test Method3.1 A carbon black sample is mixed with a white powder(zi
7、nc oxide) and a liquid vehicle (epoxidized soybean oil, ESO)to produce a black or gray paste. This paste is then spread toproduce a surface suitable for measuring the reflectance of themixture by means of a photo-electric reflectance meter. Thereflectance of the tested sample is then compared to the
8、reflectance of the ITRB prepared in the same manner. The tintstrength of the tested sample is expressed as units of thereflectance of the ITRB divided by the reflectance of thesample and multiplied by 100.3.2 Correction Factor:3.2.1 When ITRB-2, Paraplex G-62 (made before June2012) and ZnO lot#8 are
9、 used, apply a correction factor of1.0134 for the calibration and standardization in Section 8.3.2.2 There should be no correction applied when ITRB isused with Paraplex G-62 and ZnO Lot#8 or earlier, that is, thecorrection factor is “1”.3.2.3 There should be no correction applied in the calcula-tio
10、n in Section 10 when using the currently available tint rawmaterials (see Section 6) for pastes prepared with either ITRBor ITRB2, that is, the correction factor is “1”.34. Significance and Use4.1 For the broad range of commercial rubber grade carbonblacks, tint strength is highly dependent upon par
11、ticle size. Tintstrength can be used as an indication of particle size; however,tint strength is also dependent on structure and aggregate size1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.21 on Carbon BlackSurfa
12、ce Area and Related Properties.Current edition approved May 1, 2017. Published May 2017. Originallyapproved in 1973. Last previous edition approved in 2015 as D3265 15a. DOI:10.1520/D3265-17E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at s
13、erviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3In 2013 issues were reported when using Paraplex G-62 purchased after June2012 and ZnO Lot#10. An ASTM task group investigated the issues and found thefollowing raw m
14、aterials acceptable for Tint testing:1) ESO: Paraplex G-62 purchased before June 2012 or currently availableGreenChem 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
15、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 digit5 and zinc oxide lots 9 and 10 are suspect and may not give acceptable results.When using the new raw materials for tint testing s
16、ome differences may beobserved with various grades of carbon black compared with historical data. For thisreason it is the responsibility of the manufacturer to identify any such differences,and if necessary, revise any specifications between producer and user.Copyright ASTM International, 100 Barr
17、Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommen
18、dations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1distribution. Therefore, differences in tint strength withingrades of carbon black may reflect differences other thanparticle size.NOTE 1This test method was developed primarily for the character-ization of N
19、100, N200, and N300 series carbon blacks.4.2 Tint strength values within the carbon black industryhave been developed using a Automatic Muller apparatuswhich is used to prepare carbon black-zinc oxide pastes.Anewmixing apparatus, SpeedMixer4(DAC 150 FVZ), and a corre-sponding procedure have been ext
20、ensively studied within D24and shown to provide equivalent tint strength for all carcass orsoft blacks and most tread blacks with the exception of highersurface area N100 types and specialty blacks. Therefore, it isthe responsibility of the user of this alternate apparatus toensure their products wi
21、ll adequately disperse. Disputes arisingbetween a user and producer should be resolved using theAutomatic Muller apparatus until ASTM develops adequateprecision statements.4.3 The term ITRB is used in the entire text for both, theoriginal ITRB, used as the first reference material for tinttesting, b
22、ut which is now used up, and the successor referencematerial, ITRB2. Wherever required, like in calculations whereit is crucial to differentiate between the original ITRB andITRB2, this will be clearly mentioned in the text of the testprocedure.5. Apparatus5.1 Analytical Balance, with a sensitivity
23、of 60.1 mg.5.2 Automatic Muller.5,65.3 Photometric Instrument, capable of detecting differ-ences in the amount of light reflectance between shades ofgray.7,6The instrument is to be operated following the manu-facturers instructions for optimum performance.5.4 Oven, Gravity-Convection Type, capable o
24、f temperatureregulation within 61C at 125C (62F at 257F) andtemperature uniformity within 65C (69F).5.5 Reflectance Standards, as required for each reflectanceinstrument for checking calibration.5.6 Spatulas, 100 to 150 mm (4 to 6 in.), two, flexible,tapered.5.7 Syringe, 5-cm3, automatic refilling,
25、reproducible to60.02 cm3.5.8 Wiping Tissue, absorbent and lint free.5.9 Paste Application ApparatusAny one of the followinggroups of equipment may be used:5.9.1 Apparatus for Film Drawdown Method:5.9.1.1 Film Applicator,8,60.076 mm (0.003 in.) in depth.5.9.1.2 Polished Glass Plate, approximately 760
26、 by 500 by10 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.5.11 SpeedMixer (DAC 150 FVZ), PP15 cups and holder.10,65.12 IKA A-10 Analytical Mill, A-14 SS cutter, A-18 cham-ber reducer.11,65.13 5 mm Glass Grinding Beads.12,66. Re
27、agents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended allreagents shall conform to the specifications of the Committeeon Analytical Reagents of the American Chemical Society,where such specifications are available.13Ot
28、her grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Industry Tint Reference Black.146.3 Plasticizer, soybean oil epoxide.15,166.4 Denatured Alcohol, for cleaning purposes.4Spee
29、dMixer is a registered trademark of FlackTek Inc., 1708 Highway 11,Bldg. G, Landrum, SC 29356. http:/5The following instruments have been found satisfactory for this test method:Hoover Automatic Muller, Model M5, Hoover Color Corp., P.O. Box 218, StateHighway 693, Hiwassee, VA 24347. Automatic Pigme
30、nt Muller JEL 25/53-II, J.Engelsmann AG, Frankenthaler Str. 137 141, 67059 Ludwigshafen, Germany,www.engelsmann.de.6If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the resp
31、onsible technical committee,1which you may attend.7The following instruments have been found satisfactory for this test method:Erichsen Tint Tester 527, available from T. J. Bell, Inc., 1340 Home Ave., Akron,OH 44310, and Hunter MiniScan EZ, available from Hunter Associates Laboratory,Inc., 11491 Su
32、nset Hills Road, Reston, Virginia 20190-5280.The Hunter MiniScan XE or XE Plus may still be used for the test, but are nolonger commercially available. Instructions are the same for all Hunter Miniscantypes.The Densicron reflectometer, though no longer commercially available, may beused for the test
33、. For instructions, see Test Method D3265 01.8The sole source of supply of the FilmApplicator, Catalog No.AR-5257, knownto the committee at this time is Byk-Gardner, 9104 Guilford Rd., Columbia, MD21046. http:/.9The sole source of supply of the Tint Roller Spreader, Model 1A, known to thecommittee a
34、t this time is Titan Specialties, Inc., P.O. Box 2316, Pampa, TX79066-2316.10The sole source of supply of the SpeedMixer known to the committee at thistime is FlackTek Inc., 1708 Highway 11, Bldg. G, Landrum, SC 29356. http:/11The sole source of supply of the apparatus (Part #EW-04301-00) known to t
35、hecommittee at this time is Cole-Parmer Instrument Company, 625 East Bunker Court,Vernon Hills, IL 60061. http:/12The sole source of supply of glass grinding beads known to the committee atthis time is Quackenbush Co., Inc., 6711 Sands Rd., Crystal Lake, IL 60014.http:/13Reagent Chemicals, American
36、Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.
37、S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.14The original ITRB is depleted and therefore no longer commercially available.However, any available stocks of original ITRB may still be used. The successor ofthe original ITRB is ITRB2. ITRB2 was commercialized in 2012.15The sole source of su
38、pply of the epoxidized soybean oil (Greenflex 7170)known to the committee at this time is Balentine Enterprises, Inc., dba LaboratoryStandards and Technologies, 227 Somerset St., Borger, TX 79007, www.carbon-.16Supporting data (on the shelf life of this material) have been filed at ASTMInternational
39、 Headquarters and may be obtained by requesting Research ReportRR:D24-1004.D3265 17126.5 Zinc Oxide, Industry Tint Zinc Oxide.176.6 ASTM D24 Standard Reference Blacks.187. Sampling7.1 Samples of shipments shall be taken in accordance withPractices D1799 and D1900.8. Calibration and Standardization8.
40、1 Standard PastesPrepare pastes of the ITRB, following9.2 9.3.2 for the following masses, prepare the 0.1000-gAutomatic Muller paste or the 0.1200-g SpeedMixer paste induplicate:Industry Tint Reference BlackCalibration TintUnitsAutomaticMuller PastesSpeedMixerPastes0.0900 g 0.1080 g 90.00.1000 g 0.1
41、200 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 or0.1680 and 0.1800 g of SpeedMixer paste may be added in the standard-ization step when samples with tint results above 130 tint units are tested.The modifi
42、ed standardization should only be used for samples exceeding130 tint units.8.2 Erichsen Tint Tester 527:8.2.1 Turn on the power switch and allow for 30 minwarm-up.8.2.2 Place the reflectance head on the black calibrationpanel and adjust the digital readout to 0.00 using the “zero”control potentiomet
43、er.8.2.3 Following Section 9, prepare the paste drawdown forreflectance measurement.8.2.4 Use one of the 0.1000-gAutomatic Muller or 0.1200-gSpeedMixer ITRB pastes of 8.1 to set the instrument to read3.00 using the calibration control potentiometer.8.2.5 Determine the reflectivity on the remaining 0
44、.1000-gAutomatic Muller or 0.1200-g SpeedMixer ITRB paste. Thisreflectance reading must be from 2.99 through 3.01 for theduplicate pastes to be considered acceptable.8.2.6 If the duplicate 0.1000-g Automatic Muller or0.1200-g SpeedMixer pastes are acceptable, the two duplicatepastes are blended toge
45、ther using a spatula, and the instrumentis set to read 3.00 using the calibration control potentiometer.8.2.7 If the duplicate pastes are unacceptable, prepare an-other 0.1000-g Automatic Muller or 0.1200-g SpeedMixerpaste following 9.2 9.3.2, and follow 8.2.5.8.2.8 Determine the reflectance value f
46、or all of the remain-ing ITRB pastes of 8.1.8.2.9 Calculate the tint strength of the standard pastes asfollows:Tint Units 5 3.00/S 3100 (1)where:S = reflectance value of sample.8.2.10 Calculate a regression of the standard values (yvalue) on the measured values (x value) by using the leastsquares me
47、thod.8.2.11 The measured tint strength of all subsequent samplesis corrected by substituting each measured value into this linearequation and calculating the corrected value for the tintstrength.8.2.12 New regression coefficients are determinedperiodically, typically on a monthly basis.NOTE 3Proper
48、paste preparation and regression may be validated byanalyzing at least one SRB tread grade (SRB A-C). After applying thenormalization to the tint pastes and calculation as described in Section 10the tested SRB samples should be within the accuracy limits given inGuide D4821.8.2.13 Proper calibration
49、 and standardization of theequipment, reagents, materials, and method shall be checkedon a periodic basis using ASTM D24 Standard ReferenceBlacks. The standard tint strength values and the acceptabletest limit of the standard reference blacks may be found inGuide D4821.8.3 Hunter MiniScan:8.3.1 Calibrate the instrument using the black and whitetiles.8.3.2 Place the instrument in Setup Mode. Set up instrumentwith XYZ color scale, D65 illuminant, 10 obs
