1、Designation: D3265 11D3265 13Standard 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 parent
2、heses 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 stated
3、 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 an
4、d 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 p
6、aste. 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 s
7、ample is expressed as units of the reflectance of the ITRB divided by thereflectance of the sample and multiplied by 100.100, when calibration and standardization in Section 8 is performed with theoriginal ITRB or multiplied by 101.34 when ITRB2 is used in the calibration and standardization step.4.
8、 Significance 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, di
9、fferences 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
10、 using a Hoover 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 treadb
11、lacks 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 Hoover Muller appara
12、tus 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 May 1, 2011Jan. 1, 2013. Publis
13、hed June 2011February 2013. Originally approved in 1973. Last previous edition approved in 20072011 asD3265 07.D3265 11. DOI: 10.1520/D3265-11.10.1520/D3265-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of
14、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 ASTM sta
15、ndard 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 published by AS
16、TM 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, butwhich is
17、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 of 60.1 m
18、g.5.2 Automatic Muller.4,55.3 Photometric Instrument, capable of detecting differences in the amount of light reflectance between shades of gray.5,6 Theinstrument is to be operated following the manufacturers instructions for optimum performance.5.4 Oven, Gravity-Convection Type, capable of temperat
19、ure 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, reprodu
20、cible 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,5,7 0.076 mm (0.003 in.) in depth.5.9.1.2 Polished Glass Plate, approximately 760 by
21、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.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 chamber reducer.5,105.13 5 mm Glass Grinding Beads.5,116. Reagent
22、s 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.12 Othe
23、r 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.,134 The sole source of supply of the Hoover Automatic Muller, Model M5, known to the committe
24、e at this time is Hoover Color Corp., P.O. Box 218, State Highway 693,Hiwassee, VA 24347.5 If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committe
25、e,1 which you may attend.6 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 MiniScan EZ, available from Hunter Associates Laboratory, Inc., 11491 Sunset Hills Road, Reston,
26、 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 reflectometer, though no longer commercially available, may be used for the test. For instructions, s
27、ee Test Method D3265 01.7 The sole source of supply of the Film Applicator, Catalog No. AR-5257, known to the committee 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
28、Titan Specialties, Inc., P.O Box 2316, Pampa, TX 79066-2316.9 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:/10 The sole source of supply of the apparatus (Part #EW-04301-00) known to the committee a
29、t this time is Cole-Parmer Instrument Company, 625 East Bunker Court,Vernon Hills, IL 60061. http:/11 The sole source 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 S
30、ociety 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 the United States Pharmacopeia and NationalFormulary, U.S. Pharm
31、acopeial Convention, Inc. (USPC), Rockville, MD.13 The sole source of supply of Industry Tint Reference Black, an N-330 carbon black, known to the committee at this time is Laboratory Standards and Technologies,227 Somerset St., Borger, TX 79007.original ITRB is depleted and therefore no longer comm
32、ercially available. However, any available stocks of original ITRB may still beused. The successor of the original ITRB is ITRB2. ITRB2 was commercialized in 2012.D3265 1326.3 Plasticizer, soybean oil epoxide.5,14,156.4 Denatured Alcohol, for cleaning purposes.6.5 Zinc Oxide, Industry Tint Zinc Oxid
33、e.5,166.6 ASTM D24 Standard Reference Blacks.5,177. 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-g HooverM
34、uller paste or the 0.1200-g SpeedMixer paste in duplicate:Industry Tint Reference Black Calibration TintUnits AcceptableRangeHoover 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 0.1440 g 120.0 119.0 121.00.13
35、00 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 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
36、paste drawdown for reflectance measurement.8.2.4 Use one of the 0.1000-g Hoover 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 Hoover Muller or 0.1200-g SpeedMix
37、er ITRB paste. This reflectancereading must be from 2.99 through 3.01 for the duplicate pastes to be considered acceptable.8.2.6 If the duplicate 0.1000-g Hoover Muller or 0.1200-g SpeedMixer pastes are acceptable, the two duplicate pastes areblended together using a spatula, and the instrument is s
38、et to read 3.00 using the calibration control potentiometer.8.2.7 If the duplicate pastes are unacceptable, prepare another 0.1000-g Hoover Muller or 0.1200-g SpeedMixer paste following9.2-9.3.2, 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
39、 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 If the measured tint values are not within the guidelines (60.8 % relative of the target tint strength values) given in 8.1,then a regression of the standard values (
40、y value) on the measured values (x value) must be calculated using the least squaresmethod.NOTE 2It is almost always necessary to develop a statistical equation to measure tint strength values.8.2.11 The measured tint strength of all subsequent samples shall then be corrected by substituting each me
41、asured value intothis linear equation and calculating the corrected value for the tint strength.8.2.12 New regression coefficients are determined periodically, typically on a monthly basis.8.2.13 Proper calibration and standardization of the equipment, reagents, materials, and method shall be checke
42、d on a periodicbasis using ASTM D24 Standard Reference Blacks. The standard tint strength values and the acceptable test limit of the standardreference blacks may be found in Guide D4821.8.3 Hunter MiniScan:14 The sole source of supply of Paraplex G-62, Chemical Abstracts Registry Number 12768-71-7,
43、 known to the committee at this time is C. P. Hall 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.”)15 Supporting data (on the shelf life of this material) have been filed at ASTM Internati
44、onal Headquarters and may be obtained by requesting Research ReportRR:D24-1004.16 The sole source of supply of Industry Tint Zinc Oxide known to the committee at this time is Forcoven Products, Inc., P.O. Box 1556, Humble, TX 77347.17 The sole source of supply of ASTM D24 Standard Reference Blacks k
45、nown to the committee at this time is Laboratory Standards and Technologies, 227 Somerset St.,Borger, TX 79007.D3265 1338.3.1 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, averag
46、e aminimum 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 Hoover Muller or 0
47、.1200-g SpeedMixer paste should read approximately 2.60. Calculate the tint strength of theITRB pastes as follows:Tint5I/Y 3100 (2)where:I = reflectance of 0.1000-g Hoover 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
48、of the 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 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 3The ITRB must be
49、 dried each day a test is performed, preferably at the same time as the tested sample. Dry only the required amount, asthe ITRB should not be dried repeatedly.9.1.1.2 Weigh a sample of exactly 0.1000 g of carbon black into a weighing dish and then weigh onto the carbon black 3.7500 gof zinc oxide. For N500, N600, N700 series carbon blacks, weigh exactly 0.2000 g of carbon black and 3.7500 g of zinc oxide.9.1.1.3 Using the syringe, place 2.20 6 0.02 cm3 or
