1、Designation: D3265 15D3265 15aStandard 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.2. Referenced Documents2.1 ASTM Standards:2D1799 Practice for Carbon BlackSampling Packaged ShipmentsD1900 Practice for Carbon BlackSampling Bulk ShipmentsD4483 Practice for Evaluating Precision for Test Method
5、 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) to produce ablack or gray
6、paste. This paste is then spread to produce a surface suitable for measuring the reflectance of the mixture by meansof a photo-electric reflectance meter. The reflectance of the tested sample is then compared to the reflectance of the ITRB preparedin the same manner. The tint strength of the tested
7、sample is expressed as units of the reflectance of the ITRB divided by thereflectance of the sample and multiplied by 100, when calibration and standardization in Section 8 is performed with the originalITRB or multiplied by 101.34 when ITRB2 is used in the calibration and standardization step.4. Si
8、gnificance 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. Therefore, diffe
9、rences 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 been developed us
10、ing aAutomatic Muller apparatus which is usedto prepare carbon black-zinc oxide pastes.Anew mixing apparatus, SpeedMixer3 (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 treadbl
11、acks 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 Automatic Muller appa
12、ratus until ASTM develops adequate precision statements.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 Jan. 1, 2015Nov. 1, 2015. Pub
13、lished February 2015December 2015. Originally approved in 1973. Last previous edition approved in 20142015as D3265 14.D3265 15. DOI: 10.1520/D3265-15.10.1520/D3265-15A.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual
14、Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 SpeedMixer is a registered trademark of FlackTek Inc., 1708 Highway 11, Bldg. G, Landrum, SC 29356. http:/This document is not an ASTM standard and is intended only to provide the user of an
15、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 prior editions as appropriate. In all cases only the current versionof the standard as publish
16、ed 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 States14.3 The term ITRB is used in the entire text for both, the original ITRB, used as the first reference material for tint testing, butw
17、hich 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 the text of the test procedure.5. Apparatus5.1 Analytical Balance, with a sensitivity o
18、f 60.1 mg.5.2 Automatic Muller.4,55.3 Photometric Instrument, capable of detecting differences in the amount of light reflectance between shades of gray.6,5 Theinstrument is to be operated following the manufacturers instructions for optimum performance.5.4 Oven, Gravity-Convection Type, capable of
19、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 150 mm (4 to 6 in.), two, flexible, tapered.5.7 Syringe, 5-cm3, automatic refilling,
20、 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 Applicator,7,5 0.076 mm (0.003 in.) in depth.5.9.1.2 Polished Glass Plate, approximately
21、 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.8,55.10 Desiccator.5.11 SpeedMixer (DAC 150 FVZ), PP15 cups and holder.9,55.12 IKA A-10 Analytical Mill, A-14 SS cutter, A-18 chamber reducer.10,55.13 5 mm Glass Grinding Beads.11,56.
22、 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 suchspecifications are available
23、.12 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.136.3 Plasticizer, soybean oil epoxide.14,5,154 The following instruments have been fo
24、und 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, Germany, www.engelsmann.de.5 If you are aware of
25、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.6 The following instruments have been found satisfactory for this test method: Erichse
26、n 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 used for the test, but are no longer commer
27、cially 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 01.7 The sole source of supply of the FilmApplicator, Catalog No.AR-5257, known to the com
28、mittee at this time is Byk-Gardner, 9104 Guilford Rd., Columbia, MD 21046.http:/.8 The sole source 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 79066-2316.9 The sole source of supply of the SpeedMixer known t
29、o the committee at this time is FlackTek Inc., 1708 Highway 11, Bldg. G, Landrum, SC 29356.http:/10 The sole source of supply 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:/11 The sole so
30、urce 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:/12 Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not
31、 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 Convention, Inc. (USPC), Rockville, MD.13 The original ITRB is depleted and therefore no longer commerci
32、ally available. However, any available stocks of original ITRB may still be used. The successor of theoriginal ITRB is ITRB2. ITRB2 was commercialized in 2012.14 The sole source of supply of Paraplex G-62, Chemical Abstracts Registry Number 12768-71-7, known to the committee at this time is C. P. Ha
33、ll Co., Technical Center,Customer Service Department, 5851 West 73rd St., Chicago, IL 60638. (Minimum order is 5 gal and order should state “Refer to ASTM D3265.”)D3265 15a26.4 Denatured Alcohol, for cleaning purposes.6.5 Zinc Oxide, Industry Tint Zinc Oxide.16,56.6 ASTM D24 Standard Reference Black
34、s.17,57. 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 9.2 9.3.2 for the following masses, prepare the 0.1000-gAutomatic Muller paste or the 0.1200-g SpeedMixer p
35、aste 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 120.00.1300 g 0.1560 g 130.0NOTE 2Optionally, 0.1400 and 0.1500 g of Automatic Muller paste or 0.1680 and 0
36、.17000.1800 g of SpeedMixer paste may be added in thestandardization step when samples with tint results above 130 tint units are tested. The modified standardization should only be used for samplesexceeding 130 tint units.8.2 Erichsen Tint Tester 527:8.2.1 Turn on the power switch and allow for 30
37、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 drawdown for reflectance measurement.8.2.4 Use one of the 0.1000-g Automatic Muller or 0.1200-g SpeedM
38、ixer 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 ITRB paste. Thisreflectance reading must be from 2.99 through 3.01 for the duplicate pastes to be c
39、onsidered acceptable.8.2.6 If the duplicate 0.1000-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 unacc
40、eptable, prepare another 0.1000-g Automatic 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 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
41、 = 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 The measured tint strength of all subsequent samples is corrected by substituting each measured value into this linearequation and ca
42、lculating 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 at least one SRB tread grade (SRB A-C). After applying thenormalization to the
43、tint pastes and calculation as described in Section 10 the tested SRB samples should be within the accuracy limits given in GuideD4821.8.2.13 Proper calibration and standardization of the equipment, reagents, materials, and method shall be checked on a periodicbasis using ASTM D24 Standard Reference
44、 Blacks. The standard tint strength values and the acceptable test limit of the standardreference blacks may be found in Guide D4821.15 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
45、.16 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 Somerset St., Borger, TX 79007, .17 The sole source of supply of ASTM D24 Standard Reference Blacks known to the committee at th
46、is time is Laboratory Standards and Technologies, 227 Somerset St.,Borger, TX 79007.D3265 15a38.3 Hunter MiniScan:8.3.1 Calibrate the instrument using the black and white tiles.8.3.2 Place the instrument in Setup Mode. Set up instrument with XYZ color scale, D65 illuminant, 10 observer, average amin
47、imum of three readings. (Note that Y corresponds to the lightness/darkness function, and thus represents the information ofinterest).8.3.3 Read each of the ITRB pastes at least three times and record only the average Y value of the three readings. The Y valuefor the 0.1000-g Automatic Muller or 0.12
48、00-g SpeedMixer paste should read approximately 2.60. Calculate the tint strength ofthe ITRB pastes as follows:Tint5I/Y 3100 (2)where:I = reflectance of 0.1000-g Automatic Muller or 0.1200-g SpeedMixer ITRB paste.Y = reflectance value of sample.8.3.4 Follow 8.2.10 8.2.13 to complete the calibration
49、of the Hunter MiniScan.9. Procedure9.1 Paste Preparation:9.1.1 Automatic Muller Paste Preparation:9.1.1.1 Dry the zinc oxide, ITRB, and the carbon black sample(s) for 1 h in the specified oven set at 125 6 1C (257 6 2F).Remove to a desiccator and allow to cool to room temperature.NOTE 4The ITRB must be dried each day a test is performed, preferably at the same time as the tested sample. Dry only the required amount, asthe ITRB should
