1、Designation: D 1619 03Standard Test Methods forCarbon BlackSulfur Content1This standard is issued under the fixed designation D 1619; 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 parenthese
2、s 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 sulfurcontent of carbon
3、 black. The following test methods areincluded:SectionsTest Method A High-Temperature Combustion With In-frared Absorption Detection Procedures6to13Test Method B X-Ray Fluorescence 141.2 The values stated in SI units are to be regarded asstandard.1.3 This standard does not purport to address all of
4、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 applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:D 240 Test Method for Heat
5、 of Combustion of LiquidHydrocarbon Fuels by Bomb Calorimeter2D 1193 Specification for Reagent Water3D 1509 Test Methods for Carbon BlackHeating Loss4D 1799 Practice for Carbon BlackSampling PackagedShipments4D 1900 Practice for Carbon BlackSampling Bulk Ship-ments4D 4483 Practice for Determining Pr
6、ecision for Test MethodStandards in the Rubber and Carbon Black Industries4E 1 Specification for ASTM Thermometers53. Significance and Use3.1 The total sulfur content of a carbon black is useful incalculations for reconstructing a rubber composition fromanalytical data.4. Reagents4.1 Purity of Reage
7、ntsReagent grade chemicals shall 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.6Other grades may beused, provided i
8、t is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.4.2 Purity of Water Unless otherwise indicated, refer-ences to water shall be understood to mean reagent waterconforming to Specification D 1193.5. Sampling5.1 S
9、amples shall be taken in accordance with PracticeD 1799 or Practice D 1900.TEST METHOD A HIGH-TEMPERATURECOMBUSTION WITH INFRARED ABSORPTIONDETECTION PROCEDURES6. Summary of Test Method6.1 The specimen is burned in a tube furnace at a minimumoperating temperature of 1350C in a stream of oxygen tooxi
10、dize the sulfur. Moisture and particulates are removed fromthe gas by traps filled with anhydrous magnesium perchlorate.The gas stream is passed through a cell in which sulfur dioxideis measured by an infrared (IR) absorption detector. Sulfurdioxide absorbs IR energy at a precise wavelength within t
11、heIR spectrum. Energy is absorbed as the gas passes through thecell body in which the IR energy is being transmitted. Thus, atthe detector, less energy is received. All other IR energy iseliminated from reaching the detector by a precise wavelengthfilter. Thus, the absorption of IR energy can be att
12、ributed onlyto sulfur dioxide whose concentration is proportional to thechange in energy at the detector. One cell is used as both areference and a measurement chamber. Total sulfur as sulfur1These test methods are under the jurisdiction of ASTM Committee D24 onCarbon Black and are the direct respon
13、sibility of Subcommittee D24.31 onNon-Carbon-Black Components of Carbon Black.Current edition approved July 10, 2003. Published August 2003. Originallyapproved in 1958. Last previous edition approved in 1999 as D 161999.2Annual Book of ASTM Standards, Vol 05.01.3Annual Book of ASTM Standards, Vol 11
14、.01.4Annual Book of ASTM Standards, Vol 09.01.5Annual Book of ASTM Standards, Vol 14.03.6Reagent 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
15、for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.dioxide is de
16、tected on a continuous basis. This test method isempirical. Therefore, the apparatus must be calibrated by theuse of standard reference materials (SRM).6.2 This test method is for use with commercially availablesulfur analyzers equipped to carry out the preceding operationsautomatically and must be
17、calibrated using standard referencematerial (carbon black) of known sulfur content based on therange of sulfur in each carbon black specimen analyzed.7. Apparatus7.1 Measurement Apparatusequipped to automaticallycombust the specimen.7.2 Combustion Tube, made of mullite, porcelain, or zircon,approxim
18、ately 40- to 45-mm inside diameter with a 3-mmthick wall, at least 450-mm long with provisions for routing thegasses produced by combustion through the infrared cell.7.3 Boat Pullerrod of a heat-resistant material with a bentor disk end to insert and remove boats from the combustiontube.8. Reagents8
19、.1 Purity of Reagentssee 4.1.8.2 Magnesium Perchlorate.9. Preparation of Apparatus9.1 Assemble the apparatus according to the manufacturersinstructions. Make a minimum of two determinations (see10.3) to condition the equipment prior to calibrating thesystem.10. Calibration10.1 Select standards havin
20、g sulfur values of approximately0.5, 1.0, and 1.5 % sulfur7.10.2 Adjustment of Response of Measurement SystemWeigh out approximately 0.5 g of the 1.0 % sulfur standard.Analyze the specimen (see Section 11). Repeat this procedure.Adjust instrument as recommended by the manufacturer untilthe absence o
21、f drift is indicated.10.3 Calibration ProcedureWeigh out four specimens ofthe 1.0 % sulfur standard. Follow the calibration procedurerecommended by the manufacturer. Confirm the calibration byanalyzing the 1.0 % sulfur standard. The value should bewithin the allowable limits of the known value. If n
22、ot, repeatthe procedure. Then weigh out and analyze two specimens,each of the other calibration standards. Record the results aftereach analysis. Compare the results obtained to the knownsulfur values of the specimens. They should be within theallowable limits of the known value of the respective sp
23、eci-men. If not, refer to the manufacturers instructions forchecking linearity of the analyzer.11. Procedure11.1 Stabilize and calibrate the analyzer (see 10.1 through10.3).11.2 Raise the furnace temperature as recommended by themanufacturer to at least 1350C. Weigh the specimen not toexceed more th
24、an 0.5 g of carbon black. Spread the specimenevenly in a combustion boat and use a boat puller to positionthe specimen in the hot zone of the furnace for at least 2 min,or until completely combusted.NOTE 1The analytical cycle should begin automatically as soon assulfur is detected.11.3 When the anal
25、ysis is complete, the instrument shouldindicate the sulfur value. Refer to the manufacturers recom-mended procedure.12. Report12.1 The percent sulfur value is obtained directly from theapparatus.13. Precision and Bias13.1 These precision statements have been prepared inaccordance with Practice D 448
26、3. Refer to this practice forterminology and other statistical details.13.2 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
27、 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 of the testmethod. Any appropriate value may be used from Table 113.3 A type 1 inter-laboratory precision program
28、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 laboratoryperforming the test once on each of two days (total of fourtests). A test result is the value obtained from a
29、 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.13.4 The results of the precision calculations for this test aregiven in Table 1. The materials are arranged in ascending“mean level” o
30、rder.13.5 RepeatabilityThe pooled relative repeatability, (r), ofthis test has been established as 5.5 %. Any other value in Table1 may be used as an estimate of repeatability, as appropriate.The difference between two single test results (or determina-tions) found on identical test material under t
31、he repeatabilityconditions prescribed for this test will exceed the repeatability7Coal standards have been found to be suitable standards and are usuallyavailable from the instrument manufacturer or may be obtained from Alpha Productsfor Analysis, 3090 Johnson Road, Stevensville, MI 49127, www.alpha
32、-.TABLE 1 Precision Parameters for D 1619 Sulfur Content,Method B, (Type 1 Precision)Units Percent SulfurMaterial Mean Level Sr (r) SR (R)IRB#6 (N330) 1.11395 0.01979 5.0 0.05440 13.8SRB A5 (N135) 1.22003 0.02582 6.0 0.14246 33.0SRB N762 1.39269 0.02105 4.3 0.07174 14.6N550 1.70521 0.04220 7.0 0.121
33、84 20.2N650 1.92001 0.02888 4.3 0.13966 20.6Average 1.47038Pooled Values 0.02869 5.5 0.11203 21.6D1619032on an average of not more than once in 20 cases in the normaland correct operation of the method. Two single test results thatdiffer by more than the appropriate value from Table 1 must besuspect
34、ed of being from different populations and some appro-priate action taken.NOTE 2Appropriate 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 resu
35、lts.13.6 ReproducibilityThe pooled relative reproducibility,(R), of this test has been established as 21.6 %. 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 t
36、heprescribed 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 method. Two single test resultsproduced in different laboratories that differ by more t
37、han theappropriate value from Table 1 must be suspected of beingfrom different populations and some appropriate investigativeor technical/commercial action taken.13.7 BiasIn test method terminology, bias is the differ-ence between an average test value and the reference (true) testproperty value. Re
38、ference 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.TEST METHOD B X-RAY FLUORESCENCE14. Summary of Test Method14.1 X-ray fluorescence may be used to determine sulfur incarbon blac
39、k. Since there are different types of instruments, nodetail of testing can be given here. Follow manufacturersinstructions for operation of test.14.2 X-ray fluorescence is not a primary test, but work byD24 has shown that only carbon black with suitable levels ofsulfur naturally occuring can be used
40、 to properly calibrate thetechnique. Four carbon black standards have been identified8and their respective sulfur level determined by combustionmethods following D 1619 calibration procedures. They are:% sulfur std deviationStandard A 0.00 0.00Standard B 1.54 0.05Standard C 1.93 0.06Standard D 0.82
41、0.0315. Keywords15.1 carbon black; high temperature combustion; infraredtitration; oxygen bomb calorimeter; sulfur content; sulfurdioxideASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this sta
42、ndard 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 an
43、dif 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 committee,
44、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 19428-295
45、9,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).8Sulfur-in-carbon black standards A-D are available from Titan Industries, P.O.Box 2316, Pampa, TX 79065.TABLE 2 Interlaboratory Precision ProgramNominal Test Period Material Number of LaboratoriesMarch 1996 N650 27October 1996 IRB#6 (N330) 22March 1997 SRB N762 27September 1997 SRB A5 (N135) 25March 1998 N550 29D1619033
