1、Designation: D1506 15Standard Test Methods forCarbon BlackAsh Content1This standard is issued under the fixed designation D1506; 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 ind
2、icates 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 cover the determination of the ashcontent of carbon bla
3、ck.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 standard to establish a
4、ppro-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:2D1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon Bl
5、ackSampling Bulk Ship-mentsD4483 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 isweighed and calcu
6、lated 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 Furnace Method5. Apparat
7、us5.1 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, 20, 50, and 100 mLwith optional disk inserts and lids.35.3 Analytical Balan
8、ce, 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
9、material.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 o
10、f ash from the crucible.7. Sampling7.1 Samples shall be taken in accordance with PracticesD1799 or D1900.1These 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 June 1, 2015. Published July 2015. Originally approvedin 1957. Last previous edition approved in 2013 as D1506 99 (2013). DOI:10.1520/D1506-15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of
12、 ASTMStandards volume information, 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 altern
13、ative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2
14、959. United States18. Procedure8.1 Porous quartz fiber crucibles and optional disks shouldbe ignited in the furnace at 550 6 25C for at least 15 min.Porcelain crucibles should be ignited with cover in the mufflefurnace at 550 6 25C for 1 h. Place the crucible and cover inthe desiccator. Cool to room
15、 temperature and weigh to nearest0.1 mg.8.2 Dry an adequate sample of carbon black for1hinthegravity-convection oven set at 125C in an open container ofsuitable 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 6 0.1 g of the dried
16、 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 (porcelain crucible) or 1.5 h (porous quartzfiber cruciblesee 6.1.1). Cover the crucible containing theash, remove from the furnace to the desicc
17、ator, and allow tocool to room temperature. Weigh the covered crucible to thenearest 0.1 mg. Put the covered crucible back into the furnacefor additional 0.5 h. Reweigh to the nearest 0.1 mg. Repeat thisweighing process until constant mass is obtained.NOTE 1For carbon blacks with very low ash conten
18、t (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 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!# 31
19、00 (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 following information:10.1.1 Proper identification of the sample, and10.1.2 A result obtained from an individual determinationreported to the near
20、est 0.01 %.11. Precision and Bias11.1 These precision statements have been prepared inaccordance with Practice D4483. Refer to this practice forterminology and other statistical details.11.2 The precision results in this precision and bias sectiongive an estimate of the precision of this test method
21、 with thematerials used in the particular interlaboratory program de-scribed below. The precision parameters should not be used foracceptance or rejection testing of any group of materialswithout documentation that they are applicable to those par-ticular materials and the specific testing protocols
22、 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. Both repeatability and reproduc-ibility represent short term (daily) testing conditions. Thetesting was performed using two operators in each lab
23、oratoryperforming the test once on each of two days (total of fourtests). A test result is the value obtained from a singledetermination. Acceptable difference 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
24、 the precision calculations for this test aregiven in Table 1. The materials are arranged in ascending“mean level” order.11.5 RepeatabilityThe pooled relative repeatability, (r), ofthis test has been established as 16.0 %. Any other value inTable 1 may be used as an estimate of repeatability, asappr
25、opriate. 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 si
26、ngletest results that differ by more than the appropriate value fromTable 1 must be suspected of being from different populationsand some appropriate action taken.NOTE 3Appropriate action may be an investigation of the test methodprocedure or apparatus for faulty operation or the declaration of asig
27、nificant difference in the two materials, samples, etc., which generatedthe two test results.11.6 ReproducibilityThe pooled relative reproducibility,(R), of this test has been established as 29.7 %.Any other valuein Table 1 may be used as an estimate of reproducibility, asappropriate. The difference
28、 between two single and indepen-dent test results found by two operators working under theprescribed reproducibility conditions in different laboratorieson identical test material will exceed the reproducibility on anaverage of not more than once in 20 cases in the normal andcorrect operation of the
29、 method. Two single test resultsproduced in different laboratories that differ by more than theappropriate value from Table 1 must be suspected of beingfrom different populations and some appropriate investigativeor technical/commercial action taken.TABLE 1 Precision Parameters for D1506 Ash Content
30、, (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 Values 0.020 16.0 0.037 2
31、9.7TABLE 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 46D1506 15211.7 BiasIn test method terminology, bias is the differencebetween an average t
32、est 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.Method BMicrowave Furnace Method12. Apparatus12.1 Microwave Ashing Fur
33、nace, 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 cover size E or PorousQuartz Fiber Crucible, 20, 50 and 100 mL with optional diskinserts and lids.312.3 Analytical Balance, having a sensitivity of 0.1 mg.
34、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 covered when transferring itto and from the desiccator to prevent the loss of ash due to aircurrents.
35、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 550C 6 25C for 1 h. Place the crucible andcover in the desiccator and cool to room temperature.14
36、.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 in a desiccator.14.3 Determine and record the mass of the empty crucible.After the crucible has
37、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 chamber of the microwavefurnace. Prop open the door of the ashing chamber approxi-mately 6 mm to
38、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 crucibles and 6 h for porcelain crucibles.14.7 After the allotted time, remove the crucibles from them
39、icrowave 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 the ashed test portion.14.8 Determine the mass of the crucible and ash to thenearest 0.1 mg. If try
40、ing 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. If the change is greater than0.5 mg, continue this procedure until the mass change is lessthan 0.
41、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. Calculation15.1 Calculate the percentage of ash to the nearest 0.01 % asfollows:A 5 D 2 B!/C 2 B!# 31
42、00 (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 identification of the sample, and16.1.2 Results obtained from a single determination re-ported to the ne
43、arest 0.01%.17. Precision and Bias17.1 This precision and bias has been prepared in accor-dance with Practice D4483. Refer to this practice for terminol-ogy and other statistical details.17.2 The precision results in this precision and bias give anestimate of the precision as described below. The pr
44、ecisionparameters should not be used for acceptance/rejection testingof any group of materials without documentation that they areapplicable to those particular materials and the specific testingprotocols that include this test method.17.3 A Type 1 inter-laboratory precision program was con-ducted i
45、n 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 = 5, and n = 4.Acceptable difference valueswere not measured.17.4 The result of the precision calcula
46、tions 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, r, of the ash contentresult has been established as 0.08 % ash. Two single testresults (or determ
47、inations) 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 result has been established as 0.08 % ash. Two singleD1506 153test results (or determinations) produce
48、d 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 terminology, bias is the differencebetween an average test value and the reference (true) testprop
49、erty 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.18. 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 enti
