1、Designation: D7633 13Standard Test Method forCarbon BlackCarbon Content1This standard is issued under the fixed designation D7633; 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 i
2、ndicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the instrumental determinationof carbon content in a carbon black sample. Values obtainedrepresent the total carbon content.1.2 The me
3、thod is applicable to tread, carcass and specialtytype carbon blacks obtained from partial combustion or ther-mal decomposition processes, which typically contain 95 to100 % carbon.1.3 The results of these tests can be expressed as mass %carbon.1.4 The values stated in SI units are to be regarded as
4、standard. No other units of measurement are included in thisstandard.1.5 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 appro-priate safety and health practices and determine the
5、applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon B
6、lack ManufacturingIndustries3. Summary of Test Method3.1 In this test method, a sample is weighed in a combustionboat and the carbon content is determined by placing the boatin a tube furnace operating at 1350C in a stream of oxygenresulting in complete combustion. Carbon in the sample isoxidized to
7、 carbon dioxide. Moisture and particulates areremoved from the gas stream by traps filled with anhydrousmagnesium perchlorate. The gas stream is then passed througha cell in which carbon dioxide concentration is measured by aninfrared (IR) absorption detector at a precise wavelength in theIR spectru
8、m.3.2 This test method is for use with commercially availablecarbon analyzers equipped to carry out the combustion andmeasurement operations automatically.3.3 The carbon analyzer must be calibrated using an appro-priate calibration standard (see 6.4).4. Significance and Use4.1 The total carbon conte
9、nt of a carbon black is a require-ment for the calculation and reporting of carbon dioxideemissions. It can also be used in calculations to estimate yieldof the process.5. Apparatus5.1 Analytical Balance, or equivalent, capable of a weighingsensitivity of 1 mg or better resolution.5.2 Gravity Convec
10、tion Drying Oven, capable of maintain-ing 125 6 5C.5.3 Measurement Apparatus, equipped to automaticallycombust the sample and measure carbon content.5.4 Combustion tube and boat made of a suitable materialsuch as mullite, porcelain or zircon.6. Reagents6.1 Purity of ReagentsReagent grade chemicals s
11、hall 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 available.3Other grades may beused, provided it is first ascertained that
12、the reagent is of1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.66 on Environment,Health, and Safety.Current edition approved Nov. 1, 2013. Published December 2013. Originallyapproved in 2010. Last previous editio
13、n approved in 2010 as D7633 10b. DOI:10.1520/D7633-13.2For 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 Document Summary page onthe ASTM website.3“Reage
14、nt 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.K. and the United States Pharmacopeia and
15、National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1sufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Magnesium
16、Perchlorate.6.3 Oxygen, high purity, 99.9 %.6.4 Calibration standard.47. Sampling7.1 Samples of candidate carbon blacks shall be taken inaccordance with Practice D1799 or D1900.8. Preparation of Apparatus8.1 Assemble the apparatus according to the manufacturersinstructions.8.2 Stabilize the furnace
17、temperature at 1350 6 15C.8.3 Make a minimum of two determinations to condition theequipment or follow manufacturers recommendation to con-dition equipment prior to calibrating the instrument.9. Calibration9.1 Calibrate the instrument per manufacturers recommen-dation using a carbon calibration stan
18、dard.9.2 Adjustment of Response of Measurement SystemWeigh approximately 0.1 g of calibration standard or userecommended mass per manufacturer. Analyze the sample (seeSection 10). Repeat this procedure. Adjust instrument asrecommended by the manufacturer until the absence of drift isindicated.9.3 Ca
19、libration ProcedureFollow the calibration proce-dure recommended by the manufacturer. Confirm the calibra-tion by analyzing a reference material of known carbonconcentration.4Reference standards should be similar to car-bon black with carbon content of approximately 95-100 %. Themeasured value shoul
20、d be within allowable limits of the knownvalue. If not, repeat the procedure. If acceptable results are notobtained refer to the manufacturers instructions for calibra-tion.10. Procedure10.1 Sample PreparationDry an adequate sample of thecarbon black for at least1hinagravity-convection oven set at12
21、5 6 5C, in an open container of suitable dimensions, so thatthe depth of black is no more than 10 mm. Cool to roomtemperature in a desiccator before use.10.2 Stabilize and verify calibration of the analyzer (see 8.1through 9.3).10.3 Confirm the furnace temperature is 1350 6 15C.10.4 Weigh approximat
22、ely 0.1 g of the sample or userecommended mass per manufacturer.10.5 Spread the sample in the combustion boat and recordthe sample weight.10.6 Initiate the analysis and place the sample in theinstrument using a boat puller or the auto-sampler mechanism.10.7 When the analysis is complete, the instrum
23、ent shouldindicate the carbon value. Refer to the manufacturers recom-mended procedure.11. Report11.1 The percent carbon value is obtained directly from theapparatus.11.2 Report results from individual determinations to thenearest 0.1 %.NOTE 1The most representative measurement of carbon content in
24、acarbon black sample is an average value from multiple individualdeterminations. A good practice is to report a minimum of two individualdeterminations for a given sample.12. Precision and Bias512.1 These precision statements have been prepared inaccordance with Practice D4483. Refer to this practic
25、e forterminology and other statistical details.12.2 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 foracceptan
26、ce 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 forthe High Temperature Combustion Method. An alternatemethod for carbon
27、 content, CHN, was included in the inter-laboratory program used to generate this precision statementsince a number labs use this instrumental method. Precisiondata specific to the CHN method is found in Table 2.12.3 A type 1 inter-laboratory precision program was con-ducted. Both repeatability and
28、reproducibility represent short-term (daily) testing conditions. The testing was performed ineach laboratory performing the test twice on each of two days(total of four tests). A test result is the value obtained from asingle determination. Acceptable difference values were notmeasured.12.4 The resu
29、lts of the precision calculations for this test aregiven in Table 1. The materials are arranged in ascending“mean level” order.12.5 RepeatabilityThe pooled absolute repeatability, r, ofthis test has been established as 0.74 %. Any other value inTable 1 may be used as an estimate of repeatability, as
30、appropriate. 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. Tw
31、o singletest results that differ by more than the appropriate value fromTable 1 must be suspected of being from different populationsand some appropriate action taken.4Purified carbon standards are typically available from the instrument manufac-turer.5A research report is pending.D7633 132NOTE 2App
32、ropriate 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.12.6 ReproducibilityThe pooled absolute reproducibility,R, of this test has bee
33、n established as 2.68 %. 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 operators working under the pre-scribed reproducibility conditions in different laboratories onidentical test mate
34、rial 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 beingfrom different populati
35、ons and some appropriate investigativeaction taken.12.7 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 defin
36、ed by the test method. Bias, therefore, cannotbe determined.13. Keywords13.1 carbon black; carbon content; combustion; carbondioxide emissionsASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of thi
37、s 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 yea
38、rs andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical commit
39、tee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 1942
40、8-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the sta
41、ndard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 1 Precision Parameters for Test Method D7633, Type 1 Precision, High Temperature Combustion, Carbon Content of CarbonBlackUnitsPercentMaterialNumber ofLaboratoriesMean Level Sr r (r) SR R (R)1. AR-2029A3 100.03 0.115 0.3
42、3 0.33 0.115 0.33 0.332. SRB8G (N990) 4 99.62 0.238 0.67 0.68 0.388 1.10 1.103. SRB8E (N660) 4 98.32 0.393 1.11 1.13 0.932 2.64 2.684. Specialty 4 91.63 0.224 0.64 0.69 1.594 4.51 4.92Average 97.40Pooled Values 0.262 0.74 0.76 0.945 2.68 2.75AAR-2029 is a high purity graphite (99.998 % C) certified
43、reference material (CRM). This CRM was used as a calibration standard for the High Temperature CombustionMethod within the inter-laboratory program.The sole source of supply of the CRM known to the committee at this time is Alpha Resources, Inc. If you are aware of alternative suppliers, please prov
44、idethisinformation to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee,1which you mayattend.TABLE 2 Precision Parameters for Test Method D7633, Type 1 Precision, CHN, Carbon Content of Carbon BlackUnitsPercentMateri
45、alNumber ofLaboratoriesMean Level Sr r (r) SR R (R)1. AR-2029 7 99.59 0.448 1.27 1.27 0.726 2.06 2.062. SRB8G (N990) 7 99.10 0.207 0.59 0.59 0.615 1.74 1.763. SRB8E (N660) 7 97.39 0.254 0.72 0.74 0.434 1.23 1.264. Specialty 7 88.79 0.252 0.71 0.80 2.823 7.99 9.00Average 96.22Pooled Values 0.305 0.86 0.90 1.505 4.26 4.43D7633 133
