1、Designation: D3265 13aStandard 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.1. Scope1.1 This test method covers the determination of the tintstrength of carbon black relative to an industry tint referenceblack (ITRB).1.2 The values stated in SI u
3、nits 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 standard to establish appro-priate safety and health p
4、ractices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD4483 Practice for Evaluating Precision for Test MethodStandards
5、 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(zinc oxide) and a liquid vehicle (soybean oil epoxide) toproduce a black or gray paste. This p
6、aste 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 thereflectance of the ITRB prepared in the same manner. The tintstrength of the tested sample is expres
7、sed as units of thereflectance of the ITRB divided by the reflectance of thesample and multiplied by 100, when calibration and standard-ization in Section 8 is performed with the original ITRB ormultiplied by 101.34 when ITRB2 is used in the calibrationand standardization step.4. Significance and Us
8、e4.1 For the broad range of commercial rubber grade carbonblacks, 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. Therefore, differences in tint stre
9、ngth withingrades of carbon black may reflect differences other thanparticle size.NOTE 1This test method was developed primarily for the character-ization of N100, N200, and N300 series carbon blacks.4.2 Tint strength values within the carbon black industryhave been developed using a Hoover Muller a
10、pparatus which isused to prepare carbon black-zinc oxide pastes. A new mixingapparatus, SpeedMixer3(DAC 150 FVZ), and a correspondingprocedure have been extensively studied within D24 andshown to provide equivalent tint strength for all carcass or softblacks and most tread blacks with the exception
11、of highersurface area N100 types and specialty blacks. Therefore, it isthe responsibility of the user of this alternate apparatus toensure their products will adequately disperse. Disputes arisingbetween a user and producer should be resolved using theHoover Muller apparatus until ASTM develops adeq
12、uateprecision statements.4.3 The term ITRB is used in the entire text for both, theoriginal ITRB, used as the first reference material for tinttesting, but which is now used up, and the successor referencematerial, ITRB2. Wherever required, like in calculations whereit is crucial to differentiate be
13、tween the original ITRB andITRB2, this will be clearly mentioned in the text of the testprocedure.1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.21 on Carbon BlackSurface Area and Related Properties.Current editio
14、n approved Nov. 1, 2013. Published November 2013. Originallyapproved in 1973. Last previous edition approved in 2013 as D3265 13. DOI:10.1520/D3265-13A.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMSta
15、ndards volume information, refer to the standards Document Summary page onthe ASTM website.3SpeedMixer is a registered trademark of FlackTek Inc., 1708 Highway 11,Bldg. G, Landrum, SC 29356. http:/Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. Uni
16、ted States15. Apparatus5.1 Analytical Balance, with a sensitivity of 60.1 mg.5.2 Automatic Muller.4,55.3 Photometric Instrument, capable of detecting differ-ences in the amount of light reflectance between shades ofgray.5,6The instrument is to be operated following the manu-facturers instructions fo
17、r optimum performance.5.4 Oven, Gravity-Convection Type, capable of 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.
18、), two, flexible,tapered.5.7 Syringe, 5-cm3, automatic refilling, 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,5,70.076 mm (0
19、.003 in.) in depth.5.9.1.2 Polished Glass Plate, approximately 760 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.5,85.10 Desiccator.5.11 SpeedMixer (DAC 150 FVZ), PP15 cups and holder.5,95.12 IKA A-10 Analytical Mill, A-14 SS cutter, A
20、-18 cham-ber reducer.5,105.13 5 mm Glass Grinding Beads.5,116. Reagents 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 Ameri
21、can Chemical Society,where such specifications are available.12Other 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.136.3 Plasticizer, soybean oi
22、l epoxide.5,14,156.4 Denatured Alcohol, for cleaning purposes.6.5 Zinc Oxide, Industry Tint Zinc Oxide.5,166.6 ASTM D24 Standard Reference Blacks.5,177. Sampling7.1 Samples of shipments shall be taken in accordance withPractices D1799 and D1900.8. Calibration and Standardization8.1 Standard PastesPr
23、epare pastes of the ITRB, following9.2 9.3.2 for the following masses, prepare the 0.1000-gHoover Muller paste or the 0.1200-g SpeedMixer paste induplicate:Industry Tint Reference BlackCalibration TintUnitsHoover MullerPastesSpeedMixerPastes0.0900 g 0.1080 g 90.00.1000 g 0.1200 g 100.00.1100 g 0.132
24、0 g 110.00.1200 g 0.1440 g 120.00.1300 g 0.1560 g 130.0NOTE 2Optionally, 0.1400 and 0.1500 g of Hoover Muller paste or0.1680 and 0.1700 g of SpeedMixer paste may be added in the standard-ization step when samples with tint results above 130 tint units are tested.4The sole source of supply of the Hoo
25、ver Automatic Muller, Model M5, knownto the committee at this time is Hoover Color Corp., P.O. Box 218, State Highway693, Hiwassee, VA 24347.5If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-atio
26、n at a meeting of the responsible technical committee,1which you may attend.6The 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
27、 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 nolonger commercially available. Instructions are the same for all Hunter Miniscantypes.The Densicron reflectometer, though no longer commercially availabl
28、e, may beused for the test. For instructions, see Test Method D3265 01.7The 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:/.8The sole source of supply of the Tint Roller Spreader, Model 1
29、A, known to thecommittee at this time is Titan Specialties, Inc., P.O Box 2316, Pampa, TX79066-2316.9The 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:/10The sole source of supply of the apparatus (Part
30、#EW-04301-00) known to thecommittee at this time is Cole-Parmer Instrument Company, 625 East Bunker Court,Vernon Hills, IL 60061. http:/11The 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:/12Reag
31、ent Chemicals, American 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 Pharmacopeiaan
32、d National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.13The 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
33、.14The sole source of supply of Paraplex G-62, Chemical Abstracts RegistryNumber 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, IL60638. (Minimum order is 5 gal and order should state “Refer to ASTM D3265.
34、”)15Supporting data (on the shelf life of this material) have been filed at ASTMInternational Headquarters and may be obtained by requesting Research ReportRR:D24-1004.16The sole source of supply of Industry Tint Zinc Oxide known to the committeeat this time is Forcoven Products, Inc., P.O. Box 1556
35、, Humble, TX 77347.17The sole source of supply of ASTM D24 Standard Reference Blacks known tothe committee at this time is Laboratory Standards and Technologies, 227 SomersetSt., Borger, TX 79007.D3265 13a2The modified standardization should only be used for samples exceeding130 tint units.8.2 Erich
36、sen 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 potentiometer.8.2.3 Following Section 9, prepare the paste drawdown forreflectance measurement.
37、8.2.4 Use one of the 0.1000-g Hoover 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 0.1000-gHoover Muller or 0.1200-g SpeedMixer ITRB paste. Thisreflectance reading must b
38、e from 2.99 through 3.01 for theduplicate pastes to be considered acceptable.8.2.6 If the duplicate 0.1000-g Hoover Muller or 0.1200-gSpeedMixer pastes are acceptable, the two duplicate pastes areblended together using a spatula, and the instrument is set toread 3.00 using the calibration control po
39、tentiometer.8.2.7 If the duplicate pastes are unacceptable, prepare an-other 0.1000-g Hoover Muller 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 remain-ing ITRB pastes of 8.1.8.2.9 Calculate the tint strength of the standard p
40、astes 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 method.8.2.11 The measured tint strength of all subsequent samplesis corrected by substituting ea
41、ch 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.8.2.13 Proper calibration and standardization of theequipment, reagents, materials, and method shall be chec
42、kedon 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 S
43、etup Mode. Set up instrumentwith XYZ color scale, D65 illuminant, 10 observer, average aminimum of three readings. (Note that Y corresponds to thelightness/darkness function, and thus represents the informa-tion of interest).8.3.3 Read each of the ITRB pastes at least three times andrecord only the
44、average Y value of the three readings. The Yvalue for the 0.1000-g Hoover Muller or 0.1200-g SpeedMixerpaste should read approximately 2.60. Calculate the tintstrength of the ITRB pastes as follows:Tint 5 I/Y 3100 (2)where:I = reflectance of 0.1000-g Hoover Muller or 0.1200-gSpeedMixer ITRB paste.Y
45、= reflectance value of sample.8.3.4 Follow 8.2.10 8.2.13 to complete the calibration ofthe Hunter MiniScan.9. Procedure9.1 Paste Preparation:9.1.1 Hoover Muller Paste Preparation:9.1.1.1 Dry the zinc oxide, ITRB, and the carbon blacksample(s) for1hinthespecified oven set at 125 6 1C (2576 2F). Remov
46、e to a desiccator and allow to cool to roomtemperature.NOTE 3The ITRB must be dried each day a test is performed,preferably at the same time as the tested sample. Dry only the requiredamount, as the ITRB should not be dried repeatedly.NOTE 4As an optional step in the procedure a carbon black samplem
47、ay be homogenized prior to drying and weighing using either a mortarand pestle or by low-intensity grinding, for example, in a coffee mill.9.1.1.2 Weigh a sample of exactly 0.1000 g of carbon blackinto a weighing dish and then weigh onto the carbon black3.7500 g of zinc oxide. For N500, N600, N700 s
48、eries carbonblacks, weigh exactly 0.2000 g of carbon black and 3.7500 g ofzinc oxide.9.1.1.3 Using the syringe, place 2.20 6 0.02 cm3or, ifpreferred, 2.20 g of plasticizer in the center of the mullingplate.NOTE 5If the use of 2.20 cm3(2.20 g) of plasticizer produces anunmanageable fluid paste, then
49、it is acceptable to use 2.00 cm3(2.00 g) ofplasticizer for both the ITRB standard and the sample.9.1.1.4 Place the zinc oxide and carbon black in the centerof the pool of plasticizer.9.1.1.5 Mix the three materials with a spatula, confiningthem as close to the center as possible; mix until they are wellincorporated. Clean the material from the spatula onto the topmulling plate, maintaining minimum loss of material.9.1.1.6 Set the muller for 25 revolutions with on
