1、Designation: D 1506 99 (Reapproved 2007)Standard Test Methods forCarbon BlackAsh Content1This standard is issued under the fixed designation D 1506; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A numbe
2、r in parentheses indicates 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 cover the determination of the ashconte
3、nt of carbon black.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standar
4、d to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificprecautionary statements see Sections 6 and 13.2. Referenced Documents2.1 ASTM Standards:2D 1799 Practice for Carbon BlackSampling PackagedShipmentsD 1900 Prac
5、tice for Carbon BlackSampling Bulk Ship-mentsD 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3. Summary of Test Method3.1 Apre-dried sample (1 h at 125C) is weighed before andafter combustion for 16 h at 550C. The remaining ash
6、isweighed and calculated as a percent of the dried sample.4. Significance and Use4.1 The ash content of a carbon black is the amount ofnon-carbon components present after combustion. Primarycontributants to ash are the manufacturing process water andthe catalyst in the feedstock.Method AMuffle Furna
7、ce Method5. Apparatus5.1 Muffle Furnace, capable of temperature regulation of625C at 550C.5.2 Crucibles:5.2.1 Porcelain Crucible, high-form, size O, rim 35 mm,height 29 mm, capacity 15 cm3, with cover size E.5.2.2 Porous Quartz Fiber Crucible, rim 47 mm, height 14mm, with disk.35.3 Analytical Balanc
8、e, having a sensitivity of 0.1 mg.5.4 Desiccator.5.5 Oven, gravity-convection type, capable of temperatureregulation within 61C at 125C and temperature uniformitywithin 65C.6. Hazards6.1 Precautions:6.1.1 Keep the door of the furnace open about 6 mm toadmit air to support the combustion of organic m
9、aterial.6.1.2 Exert care in removing ashed sample from furnace todesiccator.6.1.3 Always keep the cover on the crucible when transfer-ring it to and from the desiccator to prevent the loss of ash dueto air currents.6.1.4 After the sample has cooled in the desiccator, admit airslowly to avoid loss of
10、 ash from the crucible.7. Sampling7.1 Samples shall 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
11、 edition approved May 1, 2007. Published July 2007. Originally approvedin 1957. Last previous edition approved in 1999 as D 1506 99.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume inform
12、ation, refer to the standards Document Summary page onthe ASTM website.3The sole source of supply of the apparatus (quartz ashing dishes, Part Number303040) known to the committee at this time is CEM Corporation, P.O. Box 200,Matthews, NC 28106. If you are aware of alternative suppliers, please prov
13、ide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.8. Proce
14、dure8.1 Ignite the crucible with cover in the muffle furnace at550 6 25C for 1 h. Place the crucible and cover in thedesiccator. Cool to room temperature and weigh to nearest 0.1mg.8.2 Dry an adequate sample of carbon black for1hinthegravity-convection oven set at 125C in an open container ofsuitabl
15、e dimensions, so that the depth of the black is no morethan 10 mm. Cool and store the sample in a desiccator.8.3 Weigh 2 60.1 g of the dried carbon black into theignited crucible and weigh to the nearest 0.1 mg. Place theuncovered crucible and its cover into the furnace (Note 1)at550C for 16 h (porc
16、elain crucible) or 1.5 h (porous quartzfiber cruciblesee 6.1.1). Cover the crucible containing the ash,remove from the furnace to the desiccator, and allow to cool toroom temperature. Weigh the covered crucible to the nearest0.1 mg. Put the covered crucible back into the desiccator foradditional 0.5
17、 h. Reweigh to the nearest 0.1 mg. Repeat thisweighing process until constant mass is obtained.NOTE 1For carbon blacks with very low ash content (such as highpurity blacks) larger sample mass and longer ashing time may be required.NOTE 2If control testing is done at temperatures exceeding 550C,some
18、volatile salts may be lost from inorganic ash.9. Calculation9.1 Calculate the percent ash to the nearest 0.01 % asfollows:A 5 D 2 B!/C 2 B!# 3 100 (1)where:A = ash, %,B = mass of crucible, g,C = mass of crucible plus the sample, g, andD = mass of crucible plus the ash, g.10. Report10.1 Report the fo
19、llowing information:10.1.1 Proper identification of the sample, and10.1.2 A result obtained from an individual determinationreported to the nearest 0.01 %.11. Precision and Bias11.1 These precision statements have been prepared inaccordance with Practice D 4483. Refer to this practice forterminology
20、 and other statistical details.11.2 The precision results in this precision and bias sectiongive an estimate of the precision of this test method with thematerials used in the particular interlaboratory program de-scribed below. The precision parameters should not be used foracceptance or rejection
21、testing of any group of materialswithout documentation that they are applicable to those par-ticular materials and the specific testing protocols of the testmethod. Any appropriate value may be used from Table 1.11.3 A type 1 inter-laboratory precision program was con-ducted as detailed in Table 2.
22、Both repeatability and reproduc-ibility represent short term (daily) testing conditions. Thetesting was performed using two operators in each laboratoryperforming the test once on each of two days (total of fourtests). A test result is the value obtained from a singledetermination. Acceptable differ
23、ence values were not mea-sured. The between operator component of variation is in-cluded in the calculated values for r and R.11.4 The results of the precision calculations for this test aregiven in Table 1. The materials are arranged in ascending“mean level” order.11.5 RepeatabilityThe pooled relat
24、ive repeatability, (r), ofthis test has been established as 16.0 %. Any other value inTable 1 may be used as an estimate of repeatability, asappropriate. The difference between two single test results (ordeterminations) found on identical test material under therepeatability conditions prescribed fo
25、r 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 1 must be suspected of being from different populationsand some appropriate actio
26、n taken.NOTE 3Appropriate 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.11.6 ReproducibilityThe pooled relative reproducibility,(R), o
27、f this test has been established as 29.7 %.Any other valuein Table 1 may be used as an estimate of reproducibility, asappropriate. The difference between two single and indepen-dent test results found by two operators working under theprescribed reproducibility conditions in different laboratorieson
28、 identical test material will exceed the reproducibility on anaverage of not more than once in 20 cases in the normal andcorrect operation of the method. Two single test resultsproduced in different laboratories that differ by more than theappropriate value from Table 1 must be suspected of beingfro
29、m different populations and some appropriate investigativeor technical/commercial action taken.11.7 BiasIn test method terminology, bias is the differ-ence between an average test value and the reference (true) testproperty value. Reference values do not exist for this testTABLE 1 Precision Paramete
30、rs for D 1506 Ash Content, (Type 1Precision)Units Percent AshMaterial Mean Level Sr (r) SR (R)IRB#6 (N330) 0.233 0.018 21.4 0.027 32.4SRB D5 (N762) 0.258 0.015 16.0 0.030 32.6N650 0.289 0.019 18.7 0.031 30.4N550 0.436 0.025 16.1 0.037 23.7SRB A5 (N135) 0.565 0.023 11.5 0.056 27.9Average 0.356Pooled
31、Values 0.020 16.0 0.037 29.7TABLE 2 Interlaboratory Precision ProgramNominal Test Period Material Number of LaboratoriesMarch 1996 N650 45October 1996 IRB#6 (N330) 37March 1997 SRB N762 48September 1997 SRB A5 (N135) 43March 1998 N550 46D 1506 99 (2007)2method since the value or level of the test pr
32、operty isexclusively defined by the test method. Bias, therefore, cannotbe determined.Method BMicrowave Furnace Method12. Apparatus12.1 Microwave Ashing Furnace, capable of temperatureregulation of 625C at 550C.12.2 Porcelain Crucible, high-form, size 0, rim 35 mm,height 29 mm, capacity 15 cm3, with
33、 cover size E or quartzfiber ashing dish.12.3 Analytical Balance, having a sensitivity of 0.1 mg.12.4 Desiccator.12.5 Oven, gravity-convection type, capable of temperatureregulation within 61C at 125C and temperature uniformitywithin 65C.13. Hazards13.1 Precautions:13.1.1 Always keep the sample cove
34、red when transferring itto and from the desiccator to prevent the loss of ash due to aircurrents.13.1.2 After the test portion has cooled in the desiccator,admit air slowly to avoid loss of ash from the crucible.14. Procedure14.1 Pre-heat the furnace containing crucibles and covers toa set point of
35、550C 6 25C for 1 h. Place the crucible andcover in the desiccator and cool to room temperature.14.2 Place an adequate sample of carbon black in an opencontainer so that the depth of the black is no more than 10 mm.Dry the sample for1hinthegravity convection oven set at125C, cool and store the sample
36、 in a desiccator.14.3 Determine and record the mass of the empty crucible.After the crucible has been conditioned, it is important not totouch or contaminate the cleaned crucibles.14.4 Add approximately2gofcarbon black to the crucibleand determine its mass to 0.1 mg.14.5 Place samples in the ashing
37、chamber of the microwavefurnace. Prop open the door of the ashing chamber approxi-mately 6 mm to allow a flow of air. This is necessary to ensurethat enough air flows into the ashing chamber to support thecombustion of organic material.14.6 In general, test portions should take2htoashforquartz cruci
38、bles and 6 h for porcelain crucibles.14.7 After the allotted time, remove the crucibles from themicrowave furnace. Take care not to lose any ash whilehandling the crucibles. Place the crucible and test portion intoa desiccator for cooling. Store in a desiccator until ready todetermine the mass of th
39、e ashed test portion.14.8 Determine the mass of the crucible and ash to thenearest 0.1 mg. If trying to determine the proper ashing time,place the crucible back into the microwave furnace and heat foran additional hour. If there is less than 0.5 mg loss in mass, theblack has been adequately heated.
40、If the change is greater than0.5 mg, continue this procedure until the mass change is lessthan 0.5 mg.14.9 Repeat the procedure on subsequent test portions.NOTE 4For carbon blacks with very low ash content (such as highpurity blacks) larger sample mass and longer ashing time may be required.15. Calc
41、ulation15.1 Calculate the percentage of ash to the nearest 0.01 % asfollows:A 5 D 2 B!/C 2 B!# 3 100 (2)where:A = ash, %,B = mass of crucible, g,C = mass of crucible plus the test portion, g, andD = mass of crucible plus the ash, g.16. Report16.1 Report the following information:16.1.1 Proper identi
42、fication of the sample, and16.1.2 Results obtained from a single determination re-ported to the nearest 0.01%.17. Precision and Bias17.1 This precision and bias has been prepared in accor-dance with Practice D 4483. Refer to this practice for termi-nology and other statistical details.17.2 The preci
43、sion results in this precision and bias give anestimate of the precision as described below. The precisionparameters should not be used for acceptance/rejection testingof any group of materials without documentation that they areapplicable to those particular materials and the specific testingprotoc
44、ols that include this test method.17.3 A Type 1 inter-laboratory precision program was con-ducted in 1990. Both repeatability and reproducibility repre-sent short term testing conditions. Three laboratories tested fivecarbon blacks (A, B, C, D, and E) twice on two different days.Therefore, p =3,q =
45、5, and n = 4.Acceptable difference valueswere not measured.17.4 The result of the precision calculations are given inTable 3 with the material arranged in ascending mean levelorder.17.5 The precision for the pooled values for ash contentmay be expressed as follows:17.6 RepeatabilityThe repeatability
46、, r, of the ash contentresult has been established as 0.08 % ash. Two single testresults (or determinations) that differ by more than 0.08 % ashmust be considered suspect and dictates that some appropriateinvestigative action be taken.17.7 ReproducibilityThe reproducibility, R, of the ashcontent res
47、ult has been established as 0.08 % ash. Two singletest results (or determinations) produced in separate laborato-ries that differ by more than 0.08 % ash must be consideredsuspect and dictates that some appropriate investigative ortechnical/commercial action be taken.17.8 BiasIn test method terminol
48、ogy, 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.D 1506 99 (2007)318.
49、Keywords18.1 ash; carbon black; microwave furnaceASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved
