1、Designation: D 1512 05Standard Test Methods forCarbon BlackpH Value1This standard is issued under the fixed designation D 1512; 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 indi
2、cates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 These test methods, Test Method ABoiling Slurry andTest Method BSonic Slurry, a
3、re used to indicate the pH ofthe carbon black surface by measuring the pH of water incontact with the carbon black.NOTE 1The pH of the carbon black is often used in this industry toindicate the relative acidity or alkalinity of carbon black and will be usedin the remainder of these test methods to d
4、escribe this property.NOTE 2Test Method A and Test Method B do not always give thesame results.1.2 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.1.3 This standard does not purport to address all of thesafety concerns, if any, asso
5、ciated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 1799 Practice for
6、 Carbon BlackSampling PackagedShipmentsD 1900 Practice for Carbon BlackSampling Bulk Ship-mentsD 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesE70 Test Method for pH of Aqueous Solutions With theGlass Electrode3. Significance an
7、d Use3.1 The pH level of a carbon black is known to affect thevulcanization of some rubber compounds.TEST METHOD ABOILING SLURRY4. Apparatus4.1 pH Meter, (digital is recommended) having an accuracyof 60.05 pH and equipped with a combination electrode andRNC connector.4.2 Container, stainless steel o
8、r copper, 125 cm3or larger.4.3 Hot Plate.4.4 High Speed Mill, Mixer or Mortar and Pestle.4.5 Beakers, glass, 100 cm3graduated with watch glasses.5. Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall confo
9、rm to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the
10、determination.5.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type 1 in Specification D 1193.5.3 Distilled Water, high purity.5.4 Buffer Solutions, pH of 4.00, 7.00, and 10.00.5.5 Acetone, reagent grade.6. Sampling6.1 Samples s
11、hall be taken in accordance with PracticesD 1799 or D 1900.1These test methods are under the jurisdiction of ASTM Committee D24 onCarbon Black and are the direct responsibility of Subcommittee D24.31 onNon-Carbon Black Components of Carbon Black.Current edition approved Dec. 15, 2005. Published Janu
12、ary 2006. Originallyapproved in 1975. Last previous edition approved in 2000 as D 1512 95 (2000).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 Docum
13、ent Summary page onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.
14、K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7. Calibration7.1 Calibrate the pH meter using buffer solutions ac
15、cordingto manufacturers instructions.8. Procedure8.1 Pulverize pelleted or lumpy carbon black to a finepowder, using either the high speed mixer or mortar and pestle.8.2 Weigh5gofcarbon black into a 100 cm3glass beaker.8.3 Add 50 cm3of boiling, distilled water prepared in astainless steel beaker and
16、 2 to 3 drops of acetone to facilitatewetting of the sample.NOTE 3A stainless steel beaker is used to eliminate contaminationduring boiling.8.4 Cover the glass beaker with a watch glass and boil themixture for 15 min, but do not allow all the liquid to evaporate.8.5 Let the mixture cool to room temp
17、erature in an atmo-sphere free from chemical fumes which might contaminate thesample.8.6 Standardize the pH meter with the buffer solutions.Rinse the electrode with distilled water and wipe clean aftereach test.8.7 Place the electrode in the sludge, rotate gently inalternate directions until a const
18、ant pH is obtained, and recordthe pH to the nearest 0.05 unit.NOTE 4Refer to Test Method E70for a definition of pH and a highlydetailed 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. Re
19、port9.1 Report the following information:9.1.1 Proper identification of the sample,9.1.2 Result obtained, 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 inaccordance with Practice D 44
20、83. Refer to this practice forterminology and other statistical details.10.1.2 The precision results in this precision and biassection give an estimate of the precision of this test methodwith the materials used in the particular interlaboratory pro-gram described below. The precision parameters sho
21、uld not beused for acceptance or rejection testing of any group ofmaterials without documentation that they are applicable tothose particular materials and the specific testing protocols ofthe test method.Any appropriate value may be used from Table1.10.1.3 A type 1 inter-laboratory precision progra
22、m wasconducted as detailed in Table 1. Both repeatability andreproducibility represent short term (daily) testing conditions.The testing was performed using two operators in eachlaboratory performing the test once on each material on each oftwo days (total of four tests).10.1.4 The results of the pr
23、ecision calculations for this testare given in Table 1. The materials are arranged in ascending“mean level” order.10.1.4.1 RepeatabilityThe pooled absolute repeatability,r, of this test has been established as 0.40 pH units. Any othervalue in Table 1 may be used as an estimate of repeatability, asap
24、propriate. The difference between two single test results (ordeterminations) found on identical test material under therepeatability conditions prescribed for this test will exceed therepeatability on an average of not more than once in 20 casesin the normal and correct operation of the method. Two
25、singletest results that differ by more than the appropriate value fromTable 1 must be suspected of being from different populationsand some appropriate action taken.NOTE 5Appropriate action may be an investigation of the test methodprocedure or apparatus for faulty operation or the declaration of as
26、ignificant difference in the two materials, samples, etc., which generatedthe two test results.10.1.4.2 ReproducibilityThe pooled absolute reproduc-ibility, R, of this test has been established as 1.65 pH units.Anyother value in Table 1 may be used as an estimate ofreproducibility, as appropriate. T
27、he difference between twosingle and independent test results found by two operatorsworking under the prescribed reproducibility conditions indifferent laboratories on identical test material will exceed thereproducibility on an average of not more than once in 20 casesin the normal and correct opera
28、tion of the method. Two singletest results produced in different laboratories that differ bymore than the appropriate value from Table 1 must besuspected of being from different populations and some appro-priate investigative or technical/commercial action taken.10.2 BiasIn test method terminology,
29、bias is the differ-ence between an average test value and the reference (true) testproperty value. Reference values do not exist for this testmethod since the value or level of the test property isexclusively defined by the test method. Bias, therefore, cannotbe determined.TABLE 1 Precision Paramete
30、rs 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 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 (N32
31、6) 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 1.65D1512052TEST METHOD BSONIC SLURRY11. Apparatus11.1 pH Meter, (digital is recommended) having an accu-racy of 6 0.05 pH and equipped with a combination electrodeand RNC connec
32、tor.11.2 Container, stainless steel or copper, 125 cm3or 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,such as TFE-fluorocarbon.11.5 Beakers, glass, 30 cm3graduated with watc
33、h glasses.12. Reagents12.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are avai
34、lable.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.12.2 Purity of WaterUnless otherwise indicated, refer-ences to water shall be understood to mean reagent water asdefine
35、d by Type 1 in Specification D 1193.12.3 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 PracticesD 1799 or D 1900.14. Procedure14.1 Weigh 1.5 g of carbon black into a 30 cm3beaker.
36、14.2 Insert a magnetic spinbar into the beaker and add 20cm3of distilled water and 2 to 3 drops of acetone to aiddispersion.NOTE 6The water should be boiled in a stainless steel beaker andcooled prior to use to remove dissolved carbon dioxide.14.3 Cover the beaker with a watch glass and insert it in
37、tothe ultrasonic bath which contains water to a depth of 40 mmthat is 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 bythe spinbar, and turn on the sonic power for 3 min to equilibratethe mixture
38、.NOTE 8If a combination ultrasonic stirring bath is not available, usealternate periods of 1 min of ultrasonic agitation and 1 min of magneticspin stirring for a total time of 6 min.14.5 Remove the beaker from the ultrasonic bath, place theelectrode in the aqueous dispersion (slurry), allow a 2-mine
39、quilibration period, then stir the slurry with the electrode andrecord the pH to the nearest 0.05 unit (see Note 4).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
40、 Method B:16.1.1 These precision statements have been prepared inaccordance with Practice D 4483. Refer to this practice forterminology and other statistical details.16.1.2 The precision results in this precision and biassection give an estimate of the precision of this test methodwith the materials
41、 used in the particular interlaboratory pro-gram described below. The precision parameters should not beused for acceptance or rejection testing of any group ofmaterials without documentation that they are applicable tothose particular materials and the specific testing protocols ofthe test method.A
42、ny appropriate value may be used from Table2.16.1.3 A type 1 inter-laboratory precision program wasconducted as detailed in Table 2. Both repeatability andreproducibility represent short term (daily) testing conditions.The testing was performed using two operators in eachlaboratory performing the te
43、st once on each material on each oftwo days (total of four tests).16.1.4 The results of the precision calculations for this testare given in Table 2. The materials are arranged in ascending“mean level” order.16.1.4.1 RepeatabilityThe pooled absolute repeatability,r, of this test has been established
44、 as 0.34 pH units. Any othervalue in Table 2 may be used as an estimate of repeatability, asappropriate. The difference between two single test results (ordeterminations) found on identical test material under the4The sole source of supply of the apparatus known to the committee at this timeis Micro
45、-Star 2000, Inc., 255 Bradwick Dr., Unit 21, Concord, Ontario, Canada L4K1K7. If 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
46、 may attend.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D241023.TABLE 2 Precision Parameters for ASTM D 1512, Carbon Black - pH Value, Method B, (Type 1 Precision)Units pH UnitsMaterial Period Number of Laboratories Mean Le
47、vel 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 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 1.27D151205
48、3repeatability conditions prescribed for this test will exceed therepeatability on an average of not more than once in 20 casesin the normal and correct operation of the method. Two singletest results that differ by more than the appropriate value fromTable 2 must be suspected of being from differen
49、t populationsand some appropriate action taken.NOTE 9Appropriate action may be an investigation of the test methodprocedure or apparatus for faulty operation or the declaration of asignificant difference in the two materials, samples, etc., which generatedthe two test results.16.1.4.2 ReproducibilityThe pooled absolute reproduc-ibility, R, of this test has been established as 1.27 pH units.Anyother value in Table 2 may be used as an estimate ofreproducibility, as appropriate. The difference between twosingle and independent test results found by two o
