1、Designation: D1506 99 (Reapproved 2013)Standard 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
2、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 cover the determination of the ashcon
3、tent 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 stand
4、ard 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:2D1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Prac
5、tice for Carbon BlackSampling 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 i
6、sweighed 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 Furnac
7、e 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 Balance
8、, 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 ma
9、terial.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 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 ed
11、ition approved Nov. 1, 2013. Published January 2014. Originallyapproved in 1957. Last previous edition approved in 2007 as D1506 99 (2007).DOI: 10.1520/D1506-99R13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Boo
12、k of 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 al
13、ternative 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 194
14、28-2959. United States18. Procedure8.1 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
15、 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 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 furnac
16、e (Note 1)at550C for 16 h (porcelain 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 t
17、he desiccator foradditional 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 content (such as highpurity blacks) larger sample mass and longer ashing time may be required.NOTE 2If control testing is done at te
18、mperatures 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!# 3100 (1)where:A = ash, %,B = mass of crucible, g,C = mass of crucible plus the sample, g, andD = mass of crucible plus the ash,
19、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 nearest 0.01 %.11. Precision and Bias11.1 These precision statements have been prepared inaccordance with Practice D4483. Refer to
20、 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 with thematerials used in the particular interlaboratory program de-scribed below. The precision parameters should not be use
21、d foracceptance or rejection 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-du
22、cted as detailed in Table 2. 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 singledet
23、ermination. 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 the precision calculations for this test aregiven in Table 1. The materials are arranged in ascending“mean level” order.11.5
24、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, asappropriate. The difference between two single test results (ordeterminations) found on identical test material under therepeatabi
25、lity 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 1 must be suspected of being from different populati
26、onsand some appropriate action 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 re
27、lative 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 between two single and indepen-dent test results found by two operators working under theprescribed reproducibility condition
28、s 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 method. Two single test resultsproduced in different laboratories that differ by more than theappropriate value from Table 1
29、must be suspected of beingfrom different populations and some appropriate investigativeor technical/commercial action taken.11.7 BiasIn test method terminology, bias is the differencebetween an average test value and the reference (true) testTABLE 1 Precision Parameters for D1506 Ash Content, (Type
30、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 29.7TABLE
31、 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 99 (2013)2property value. Reference values do not exist for this testmethod since the valu
32、e or level of the test property 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
33、mm, capacity 15 cm3, with 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 Al
34、ways keep the sample covered 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
35、 covers toa set point of 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,
36、cool and store the sample 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 Pla
37、ce samples in the ashing 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 t
38、ake2htoashforquartz crucibles 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 t
39、odetermine the mass of the 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
40、 been adequately heated. 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
41、 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!# 3100 (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 informat
42、ion:16.1.1 Proper identification 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 D4483. Refer to this practice for terminol-ogy and other statistical
43、 details.17.2 The precision 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
44、 specific testingprotocols 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 da
45、ys.Therefore, p =3,q = 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 Repeata
46、bilityThe repeatability, 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
47、, of the ashcontent result 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 consideredD1506 99 (2013)3suspect and dictates that some appropriate investigative ortechnical/commercial action be
48、 taken.17.8 BiasIn test method terminology, bias is the differencebetween 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, cann
49、otbe 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 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 revise
