1、Designation: D3265 11Standard 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 in
2、dicates 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 un
3、its 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 pr
4、actices 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 pa
6、ste 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 express
7、ed as units of thereflectance of the ITRB divided by the reflectance of thesample and multiplied by 100.4. Significance and Use4.1 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
8、size; however,tint strength is also dependent on structure and aggregate sizedistribution. 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 N100, N200, and
9、N300 series carbon blacks.4.2 Tint strength values within the carbon black industryhave been developed using a Hoover Muller apparatus which isused to prepare carbon black-zinc oxide pastes. A new mixingapparatus, SpeedMixer3(DAC 150 FVZ), and a correspondingprocedure have been extensively studied w
10、ithin D24 andshown to provide equivalent tint strength for all carcass or softblacks 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 will adequately disp
11、erse. Disputes arisingbetween a user and producer should be resolved using theHoover Muller apparatus until ASTM develops adequateprecision statements.5. Apparatus5.1 Analytical Balance, with a sensitivity of 60.1 mg.5.2 Automatic Muller.4,55.3 Photometric Instrument, capable of detecting differ-enc
12、es in the amount of light reflectance between shades of1This 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 edition approved May 1, 2011. Published June 2011
13、. Originallyapproved in 1973. Last previous edition approved in 2007 as D3265 07. DOI:10.1520/D3265-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards
14、 Document Summary page onthe ASTM website.3SpeedMixer is a registered trademark of FlackTek Inc., 1708 Highway 11,Bldg. G, Landrum, SC 29356. http:/4The sole source of supply of the Hoover Automatic Muller, Model M5, knownto the committee at this time is Hoover Color Corp., P.O. Box 218, State Highw
15、ay693, Hiwassee, VA 24347.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.gray.5,6The instrument is to be operated following the manu-facturers instructions for optimum performance.5.4 Oven, Gravity-Convection Type, capable of temper
16、atureregulation 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, reproduc
17、ible 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 (0.003 in.) in depth.5.9.1.2 Polished Glass Plate, approximately 760 by 500
18、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-18 cham-ber reducer.5,105.13 5 mm Glass Grinding Beads.5,116. Reagents an
19、d 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.12Other grade
20、s 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.5,136.3 Plasticizer, soybean oil epoxide.5,14,156.4 Denatured Alcohol, for cleaning purposes.6.5 Zinc O
21、xide, 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 PastesPrepare pastes of the ITRB, follow-ing 9.2-9.3.2 for the following masses,
22、 prepare the 0.1000-gHoover Muller paste or the 0.1200-g SpeedMixer paste induplicate:Industry Tint Reference BlackCalibration TintUnitsAcceptableRangeHoover MullerPastesSpeedMixerPastes0.0900 g 0.1080 g 90.0 89.3 90.70.1000 g 0.1200 g 100.0 99.2 100.80.1100 g 0.1320 g 110.0 109.1 110.90.1200 g 0.14
23、40 g 120.0 119.0 121.00.1300 g 0.1560 g 130.0 129.0 131.08.2 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 potentiometer.8.2.3 Following
24、 Section 9, prepare the paste drawdown forreflectance measurement.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
25、 or 0.1200-g SpeedMixer ITRB paste. This5If 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 responsible technical committee,1which you may attend.6The following instrument
26、s 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 Sunset Hills Road, Reston, Virginia 20190-5280.The Hunter MiniScan XE or XE P
27、lus 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. For instructions, see Test Method D3265 01.7The sole source of supply of
28、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 1A, known to thecommittee at this time is Titan Specialties, Inc., P.O Box 2316, Pampa, TX79066-2316.9
29、The 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 #EW-04301-00) known to thecommittee at this time is Cole-Parmer Instrument Company, 625 East Bunker C
30、ourt,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:/12Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. F
31、or 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.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.13The sole source of s
32、upply of Industry Tint Reference Black, an N-330 carbonblack, known to the committee at this time is Laboratory Standards and Technolo-gies, 227 Somerset St., Borger, TX 79007.14The sole source of supply of Paraplex G-62, Chemical Abstracts RegistryNumber 12768-71-7, known to the committee at this t
33、ime 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.”)15Supporting data (on the shelf life of this material) have been filed at ASTMInternational Headquarters and may be obtaine
34、d 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, Humble, TX 77347.17The sole source of supply ofASTM D24 Standard Reference Blacks known tothe committee at this time is Lab
35、oratory Standards and Technologies, 227 SomersetSt., Borger, TX 79007.D3265 112reflectance 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 Hoover Muller or 0.1200-gSpeedMixer pastes are acceptable, the two duplicate pastes ar
36、eblended together using a spatula, and the instrument is set toread 3.00 using the calibration control potentiometer.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 reflectan
37、ce value for 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 3 100 (1)where:S = reflectance value of sample.8.2.10 If the measured tint values are not within the guide-lines (60.8 % relative of the target tint strength v
38、alues) givenin 8.1, then a regression of the standard values (y value) on themeasured values (x value) must be calculated using the leastsquares method.NOTE 2It is almost always necessary to develop a statistical equationto measure tint strength values.8.2.11 The measured tint strength of all subseq
39、uent samplesshall then be corrected by substituting each measured valueinto this linear equation and calculating the corrected value forthe tint strength.8.2.12 New regression coefficients are determined periodi-cally, typically on a monthly basis.8.2.13 Proper calibration and standardization of the
40、 equip-ment, reagents, materials, and method shall be checked on aperiodic basis using ASTM D24 Standard Reference Blacks.The standard tint strength values and the acceptable test limitof the standard reference blacks may be found in Guide D4821.8.3 Hunter MiniScan:8.3.1 Calibrate the instrument usi
41、ng the black and whitetiles.8.3.2 Place the instrument in Setup 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
42、of the ITRB pastes at least three times andrecord only the 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 3 100 (2)where:I = reflectance o
43、f 0.1000-g Hoover Muller or 0.1200-gSpeedMixer ITRB paste.Y = reflectance value of sample.8.3.4 Follow 8.2.10-8.2.13 to complete the calibration of theHunter 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(
44、s) for1hinthespecified oven set at 125 6 1C (2576 2F). Remove 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.9.1.1
45、.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 series 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, ifprefe
46、rred, 2.20 g of plasticizer in the center of the mullingplate.NOTE 4If the use of 2.20 cm3(2.20 g) of plasticizer produces anunmanageable fluid paste, then 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 i
47、n 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
48、 25 revolutions with one extra masson the arm equivalent to a force of 445 N (100 lbf) on the plate.Close the plates, raise the mass arm, and start the muller.9.1.1.7 At the end of the 25-revolution cycle, lower the massarm, and open the plates. Scrape the upper plate with a spatulato remove as much
49、 paste as possible, and transfer it to thecenter of the lower plate. Then, with the lower plate rotating,use the spatula to spread the paste to a flattened circle on theplate, then work all of the paste to the exact center. Repeat thisstep two additional times. Clean the material from the spatulaonto the top mulling plate.9.1.1.8 Repeat 9.1.1.6 and 9.1.1.7 three times, for a total offour cycles of 25 revolutions each.9.1.1.9 Remove the paste to a smooth, clean
