1、Designation: D3265 13aD3265 14Standard 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 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 treadblac
11、ks 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 apparatus
12、 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 Nov. 1, 2013June 1, 2014. Publishe
13、d November 2013July 2014. Originally approved in 1973. Last previous edition approved in 2013 asD3265 13.D3265 13a. DOI: 10.1520/D3265-13A.10.1520/D3265-14.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM
14、 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 standar
15、d 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 ASTM i
16、s 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 now
17、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 mg.5.
18、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 temperature
19、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, reproducibl
20、e 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 500
21、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. Reagents an
22、d 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 Other gr
23、ades 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 committee at
24、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 committee,1 w
25、hich 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, Virg
26、inia 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, see Te
27、st Method D3265 01.7 The sole source of supply of the FilmApplicator, 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 Titan S
28、pecialties, 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 at this
29、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 Society
30、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. Pharmacopeia
31、l Convention, Inc. (USPC), Rockville, MD.13 The original ITRB is depleted and therefore no longer commercially available. However, any available stocks of original ITRB may still be used. The successor of theoriginal ITRB is ITRB2. ITRB2 was commercialized in 2012.D3265 1426.3 Plasticizer, soybean o
32、il 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 with Practices D1799 and D1900.8. Calibration and Standardization8.1 Standard Pastes
33、Prepare pastes of the ITRB, following 9.2 9.3.2 for the following masses, prepare the 0.1000-g HooverMuller paste or the 0.1200-g SpeedMixer paste in duplicate:Industry Tint Reference Black Calibration TintUnitsHoover MullerPastesSpeedMixerPastes0.0900 g 0.1080 g 90.00.1000 g 0.1200 g 100.00.1100 g
34、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 Hoover Muller paste or 0.1680 and 0.1700 g of SpeedMixer paste may be added in the standardizationstep when samples with tint results above 130 tint units are tested. The modified standardization sho
35、uld only be used for samples exceeding 130 tint units.8.2 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
36、Section 9, prepare the 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 Mull
37、er or 0.1200-g SpeedMixer 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, a
38、nd the instrument is set 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 IT
39、RB 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 = 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 ti
40、nt strength of all subsequent samples is corrected by substituting each measured value into this linearequation and calculating 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 re
41、gression may be validated by analyzing at least one SRB tread grade (SRB A-C). After applying thenormalization to the 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 o
42、f the equipment, reagents, materials, and method shall be checked 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 D4821.14 The sole source of supply of Paraplex G-62, Ch
43、emical Abstracts Registry Number 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, IL 60638. (Minimum order is 5 gal and order should state “Refer to ASTM D3265.”)15 Supporting data (on the shelf life of this
44、 material) have been filed at ASTM International 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 su
45、pply of ASTM D24 Standard Reference Blacks known to the committee at this time is Laboratory Standards and Technologies, 227 Somerset St.,Borger, TX 79007.D3265 1438.3 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 inst
46、rument with XYZ color scale, D65 illuminant, 10 observer, average 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 th
47、e three readings. The Y valuefor the 0.1000-g Hoover Muller or 0.1200-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 o
48、f sample.8.3.4 Follow 8.2.10 8.2.13 to complete the calibration 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 desicca
49、tor 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 not be dried repeatedly.NOTE 5As an optional step in the procedure a carbon black sample may be homogenized prior to drying and weighing using either a mortar and pestleor by low-intensity grinding, for example, in a coffee mill.9.1.1.2 Weigh a sample of exactly
