1、Designation: D7633 10bStandard 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
2、indicates 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 m
3、ethod is applicable to tread, carcass and specialtytype carbon blacks obtained from partial combustion or ther-mal decomposition processes, which typically contain 95-100 % 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 ass
4、tandard. 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 a
5、pplica-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-ments3. Summary of Test Method3.1 In this test method, a sample is weighed in a combustionboat an
6、d 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 carbon dioxide. Moisture and particulates areremoved from the gas stream by traps filled with anhydrousmagnesium perchl
7、orate. 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 spectrum.3.2 This test method is for use with commercially availablecarbon analyzers equipped to carry out the combustion andme
8、asurement 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 content of a carbon black is a require-ment for the calculation and reporting of carbon dioxideemissions. It can also be used
9、 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 Convection Drying Oven, capable of maintain-ing 125 6 5C.5.3 Measurement Apparatus, equipped to automaticallycombust the sampl
10、e 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 shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specification
11、s 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 determination.6.2 Magne
12、sium Perchlorate.6.3 Oxygen, high purity, 99.9 %.1This 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 Dec. 1, 2010. Published January 2011. Originallyapprove
13、d in 2010. Last previous edition approved in 2010 as D7633 10a. DOI:10.1520/D7633-10B.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
14、 page onthe ASTM website.3“Reagent 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 th
15、e United States Pharmacopeia andNational 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.6.4 Calibration standard.47. Sampling7.1 Samples of candidate carbon blacks
16、 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 temperature at 1350 6 15C.8.3 Make a minimum of two determinations to condition theequipment or follow manufacturers re
17、commendation to con-dition equipment prior to calibrating the instrument.9. Calibration9.1 Calibrate the instrument per manufacturers recommen-dation using a carbon calibration standard.9.2 Adjustment of Response of Measurement SystemWeigh approximately 0.1 g of calibration standard or userecommende
18、d 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 Calibration ProcedureFollow the calibration proce-dure recommended by the manufacturer. Confirm the calibra-tion by analy
19、zing a reference material of known carbonconcentration.4Reference standards should be similar to car-bon black with carbon content of approximately 95-100 %. Themeasured value should be within allowable limits of the knownvalue. If not, repeat the procedure. If acceptable results are notobtained ref
20、er to the manufacturers instructions for calibra-tion.10. Procedure10.1 Sample PreparationDry an adequate sample of thecarbon black for at least1hinagravity-convection oven set at125 6 5C, in an open container of suitable dimensions, so thatthe depth of black is no more than 10 mm. Cool to roomtempe
21、rature 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 approximately 0.1 g of the sample or userecommended mass per manufacturer.10.5 Spread the sample in the combustion boat and recor
22、dthe 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 instrument shouldindicate the carbon value. Refer to the manufacturers recom-mended procedure.11. Report11.1 The percent carbo
23、n 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 acarbon black sample is an average value from multiple individualdeterminations. A good practice is to report a minimum
24、 of two individualdeterminations for a given sample.12. Precision and Bias12.1 A precision and bias statement has not been developedas of this time.13. Keywords13.1 carbon black; carbon content; combustion; carbondioxide emissionsASTM International takes no position respecting the validity of any pa
25、tent 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 revisio
26、n at any time by the responsible technical committee and must be reviewed every five years 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 com
27、ments will receive careful consideration at a meeting of theresponsible technical committee, 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 copyright
28、ed by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,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 standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).4Purified carbon standards are typically available from the instrument manufac-turer.D7633 10b2
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