1、Designation: D1512 05 (Reapproved 2012)D1512 15Standard Test Methods forCarbon BlackpH Value1This standard is issued under the fixed designation D1512; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A nu
2、mber in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope1.1 These test methods, Test Method ABoiling Slurry and
3、 Test Method BSonic Slurry, are used to indicate the pH of thecarbon black surface by measuring the pH of water in contact with the carbon black.NOTE 1The pH of the carbon black is often used in this industry to indicate the relative acidity or alkalinity of carbon black and will be used in theremai
4、nder of these test methods to describe this property.NOTE 2Test Method A and Test Method B do not always give the same results.1.2 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.1.3 This standard does not purport to address all of
5、 the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Re
6、agent WaterD1799 Practice for Carbon BlackSampling Packaged ShipmentsD1900 Practice for Carbon BlackSampling Bulk ShipmentsD4483 Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing IndustriesE70 Test Method for pH of Aqueous Solutions With the Gla
7、ss Electrode3. Significance and Use3.1 The pH level of a carbon black is known to affect the vulcanization of some rubber compounds.TEST METHOD ABOILING SLURRY4. Apparatus4.1 pH Meter, (digital is recommended) having an accuracy of 60.05 pH and equipped with a combination electrode and RNCconnector.
8、4.2 Container, stainless steel or copper, 125 cm3 or larger.4.3 Hot Plate.4.4 High Speed Mill, Mixer or Mortar and Pestle.4.5 Beakers, glass, 100 cm3 graduated with watch glasses.5. Reagents5.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is in
9、tended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where1 These test methods are under the jurisdiction ofASTM Committee D24 on Carbon Black and are the direct responsibility of Subcommittee D24.31 on Non-Carbon Black
10、Components of Carbon Black.Current edition approved June 1, 2012Jan. 1, 2015. Published November 2012February 2015. Originally approved in 1975. Last previous edition approved in 20052012as D1512 05.D1512 05 (2012). DOI: 10.1520/D1512-05R12.10.1520/D1512-15.2 For referencedASTM standards, visit theA
11、STM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an i
12、ndication 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 is to b
13、e considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1such specifications are available.3 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit
14、 its use without lessening the accuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water as defined byType 1 in Specification D1193.5.3 Distilled Water, high purity.5.4 Buffer Solutions, pH of 4.00, 7.00, and 10.00.5.5
15、Acetone, reagent grade.6. Sampling6.1 Samples shall be taken in accordance with Practices D1799 or D1900.7. Calibration7.1 Calibrate the pH meter using buffer solutions according to manufacturers instructions.8. Procedure8.1 Pulverize pelleted or lumpy carbon black to a fine powder, using either the
16、 high speed mixer or mortar and pestle.8.2 Weigh 5 g of carbon black into a 100 cm3 glass beaker.8.3 Add 50 cm3 of boiling, distilled water prepared in a stainless steel beaker and 2 to 3 drops of acetone to facilitate wettingof the sample.NOTE 3A stainless steel beaker is used to eliminate contamin
17、ation during boiling.8.4 Cover the glass beaker with a watch glass and boil the mixture for 15 min, but do not allow all the liquid to evaporate.8.5 Let the mixture cool to room temperature in an atmosphere free from chemical fumes which might contaminate the sample.8.6 Standardize the pH meter with
18、 the buffer solutions. Rinse the electrode with distilled water and wipe clean after each test.8.7 Place the electrode in the sludge, rotate gently in alternate directions until a magnetic stir bar into the glass beaker and placeon magnetic stir plate (or similar mechanical stirring device) and adju
19、st the stir speed to achieve a continuous uniform slurry.Carefully place the pH electrode into the slurry taking care not to allow the electrode to contact the stir bar. Once a constant pHis obtained, and record the pH obtained record to the nearest 0.05 unit.NOTE 4Refer to Test Method E70 for a def
20、inition of pH and a highly detailed procedure for making pH measurements.8.8 Rinse the electrode with distilled water and wipe clean. Keep the electrode soaking in distilled water when not in use.9. Report9.1 Report the following information:9.1.1 Proper identification of the sample,9.1.2 Result obt
21、ained, reported to the nearest 0.05 unit, and9.1.3 Test Method used, A or B.10. Precision and Bias10.1 Test Method A:10.1.1 These precision statements have been prepared in accordance with Practice D4483. Refer to this practice for terminologyand other statistical details.3 Reagent Chemicals, Americ
22、an Chemical Society 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
23、, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.TABLE 1 Precision Parameters for ASTM D1512, Carbon Black - pH Value, Method A, (Type 1 Precision)Units pH UnitsMaterial Period Number of Laboratories Mean Level Sr r SR RHS Tread Fall 2003 22 6.2 0.15 0.43 0.73 2.07SRB A6 (N134) Fall 2004
24、23 6.5 0.15 0.41 0.53 1.49LS Carcass Spring 2004 26 7.2 0.14 0.39 0.50 1.41SRB C6 (N326) Spring 2003 27 8.5 0.11 0.32 0.50 1.41N774 Fall 2002 19 8.6 0.16 0.45 0.62 1.75Average 7.4Pooled Values 0.14 0.40 0.58 1.65D1512 15210.1.2 The precision results in this precision and bias section give an estimat
25、e of the precision of this test method with thematerials used in the particular interlaboratory program described below. The precision parameters should not be used foracceptance or rejection testing of any group of materials without documentation that they are applicable to those particularmaterial
26、s and the specific testing protocols of the test method. Any appropriate value may be used from Table 1.10.1.3 A type 1 inter-laboratory precision program was conducted as detailed in Table 1. Both repeatability and reproducibilityrepresent short term (daily) testing conditions. The testing was perf
27、ormed using two operators in each laboratory performing thetest once on each material on each of two days (total of four tests).10.1.4 The results of the precision calculations for this test are given in Table 1. The materials are arranged in ascending “meanlevel” order.10.1.4.1 RepeatabilityThe poo
28、led absolute repeatability, r, of this test has been established as 0.40 pH units. Any other valuein Table 1 may be used as an estimate of repeatability, as appropriate. The difference between two single test results (ordeterminations) found on identical test material under the repeatability conditi
29、ons prescribed for this test will exceed therepeatability on an average of not more than once in 20 cases in the normal and correct operation of the method. Two single testresults that differ by more than the appropriate value from Table 1 must be suspected of being from different populations and so
30、meappropriate action taken.NOTE 5Appropriate action may be an investigation of the test method procedure or apparatus for faulty operation or the declaration of a significantdifference in the two materials, samples, etc., which generated the two test results.10.1.4.2 ReproducibilityThe pooled absolu
31、te reproducibility, R, of this test has been established as 1.65 pH units. Any othervalue in Table 1 may be used as an estimate of reproducibility, as appropriate. The difference between two single and independenttest results found by two operators working under the prescribed reproducibility condit
32、ions in different laboratories on identicaltest material will exceed the reproducibility on an average of not more than once in 20 cases in the normal and correct operationof the method. Two single test results produced in different laboratories that differ by more than the appropriate value from Ta
33、ble1 must be suspected of being from different populations and some appropriate investigative or technical/commercial action taken.10.2 BiasIn test method terminology, bias is the difference between an average test value and the reference (true) test propertyvalue. Reference values do not exist for
34、this test method since the value or level of the test property is exclusively defined by thetest method. Bias, therefore, cannot be determined.TEST METHOD BSONIC SLURRY11. Apparatus11.1 pH Meter, (digital is recommended) having an accuracy of60.05 pH and equipped with a combination electrode and RNC
35、connector.11.2 Container, stainless steel or copper, 125 cm3 or larger.11.3 Ultrasonic Stirring Bath4, two-position.11.4 Magnetic Spinbars, 4.8 mm (316 in.) or 6.4 mm (14 in.) by 22.4 mm (78 in.) long, coated with a fluorocarbon polymer, suchas TFE-fluorocarbon.11.5 Beakers, glass, 30 cm3 graduated
36、with watch glasses.12. Reagents12.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications
37、 are available.3 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.4 The sole source of supply of the apparatus known to the committee at this time is Micro-Star 2000, Inc.,
38、255 Bradwick Dr., Unit 21, Concord, Ontario, Canada L4K1K7. 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 which you may attend.TABLE
39、2 Precision Parameters for ASTM D1512, Carbon Black - pH Value, Method B, (Type 1 Precision)Units pH UnitsMaterial Period Number of Laboratories Mean Level Sr r SR RHS Tread Fall 2003 15 6.8 0.13 0.38 0.49 1.39SRB A6 (N134) Fall 2004 18 7.1 0.13 0.37 0.36 1.03LS Carcass Spring 2004 16 7.3 0.12 0.35
40、0.43 1.21SRB C6 (N326) Spring 2003 15 8.8 0.10 0.28 0.33 0.93N774 Fall 2002 8 9.1 0.11 0.30 0.59 1.67Average 7.8Pooled Values 0.12 0.34 0.45 1.27D1512 15312.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water as defined byType 1 in Specification
41、 D1193.12.3 Distilled Water, high-purity.12.4 Buffer Solutions, pH of 4.00, 7.00, and 10.00.12.5 Acetone, reagent grade.13. Sampling13.1 Samples shall be taken in accordance with Practices D1799 or D1900.14. Procedure14.1 Weigh 1.5 g of carbon black into a 30 cm3 beaker.14.2 Insert a magnetic spinba
42、r into the beaker and add 20 cm3 of distilled water and 2 to 3 drops of acetone to aid dispersion.NOTE 6The water should be boiled in a stainless steel beaker and cooled prior to use to remove dissolved carbon dioxide.14.3 Cover the beaker with a watch glass and insert it into the ultrasonic bath wh
43、ich contains water to a depth of 40 mm thatis 5 to 10C below ambient temperature.NOTE 7Use small pieces of ice to control bath temperature.14.4 Adjust the magnetic stirrer to give vigorous stirring by the spinbar, and turn on the sonic power for 3 min to equilibratethe mixture.NOTE 8If a combination
44、 ultrasonic stirring bath is not available, use alternate periods of 1 min of ultrasonic agitation and 1 min of magnetic spinstirring for a total time of 6 min.14.5 Remove the beaker from the ultrasonic bath, place the bath and place it on a magnetic stirrer and adjust the stir speed toachieve a con
45、tinuous uniform slurry. Carefully place the pH electrode in the aqueous dispersion (slurry), allow a 2-minequilibration period, then stir the slurry with the electrode and recordslurry taking care not to allow the electrode to contact thestir bar. Measure the pH to the nearest 0.05 unit (seeunits af
46、ter Note 4).an equilibration period of 2 min.14.6 Rinse the electrode with distilled water and wipe clean. Keep the electrode soaking in distilled water when not in use.15. Report15.1 See Section 9.16. Precision and Bias516.1 Test Method B:16.1.1 These precision statements have been prepared in acco
47、rdance with Practice D4483. Refer to this practice for terminologyand other statistical details.16.1.2 The precision results in this precision and bias section give an estimate of the precision of this test method with thematerials used in the particular interlaboratory program described below. The
48、precision parameters should not be used foracceptance or rejection testing of any group of materials without documentation that they are applicable to those particularmaterials and the specific testing protocols of the test method. Any appropriate value may be used from Table 2.16.1.3 A type 1 inter
49、-laboratory precision program was conducted as detailed in Table 2. Both repeatability and reproducibilityrepresent short term (daily) testing conditions. The testing was performed using two operators in each laboratory performing thetest once on each material on each of two days (total of four tests).16.1.4 The results of the precision calculations for this test are given in Table 2. The materials are arranged in ascending “meanlevel” order.16.1.4.1 RepeatabilityThe pooled absolute repeatability, r, of this test has been established as 0.34 pH un
