1、Designation: D1619 16aStandard Test Methods forCarbon BlackSulfur Content1This standard is issued under the fixed designation D1619; 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.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 sulfurcontent of car
3、bon black. The following test methods areincluded:SectionsTest Method A High-Temperature Combustion With In-frared Absorption Detection Procedures6 to 13Test Method B X-Ray Fluorescence 14 to 191.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are include
4、d 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 appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to u
5、se.2. Referenced Documents2.1 ASTM Standards:2D1509 Test Methods for Carbon BlackHeating LossD1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black
6、 ManufacturingIndustries3. Significance and Use3.1 The total sulfur content of a carbon black is useful indetermining whether a material meets a customersspecifications, providing data for performing a sulfur materialbalance around a process for environmental monitoring andreporting, and in calculat
7、ions for reconstructing a rubbercomposition from analytical data.4. Reagents4.1 Purity of ReagentsReagent 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 America
8、n 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.5. Sampling5.1 Samples of packaged materials shall be taken in acc
9、or-dance with Practice D1799 or Practice D1900.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 tooxidize the sulfur. Moisture an
10、d 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 theIR spectrum. Energy is abs
11、orbed 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 attributed onlyto sulfur dioxid
12、e whose concentration is proportional to thechange in energy at the detector. One cell is used as both a1These test methods are under the jurisdiction of ASTM Committee D24 onCarbon Black and are the direct responsibility of Subcommittee D24.66 onEnvironment, Health, and Safety.Current edition appro
13、ved Sept. 1, 2016. Published October 2016. Originallyapproved in 1958. Last previous edition approved in 2016 as D1619 16. DOI:10.1520/D1619-16A.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards
14、volume information, refer to the standards Document Summary page onthe ASTM website.3Reagent 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
15、LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1reference and a me
16、asurement chamber. Total sulfur as sulfurdioxide is detected 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
17、out the preceding operationsautomatically and must be 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 Apparatus, equipped to automaticallycombust the specimen.7.2 Combust
18、ion Tube, made of mullite, porcelain, or zircon,approximately 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 abent or disk end to inse
19、rt and remove boats from the combus-tion tube.7.4 Gravity Convection Drying Oven, capable of maintain-ing 125 6 5C.8. Reagents8.1 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 tw
20、o determinations (see10.3) to condition the equipment prior to calibrating thesystem.10. Calibration10.1 Select standards having sulfur values of approximately0.5, 1.0, and 1.5 % sulfur4.10.2 Adjustment of Response of Measurement SystemWeigh out approximately 0.5 g of the 1.0 % sulfur standard.Analy
21、ze the specimen (see Section 11). Repeat this procedure.Adjust instrument as recommended by the manufacturer untilthe absence of drift is indicated.10.3 Calibration ProcedureWeigh out four specimens ofthe 1.0 % sulfur standard. Follow the calibration procedurerecommended by the manufacturer. Confirm
22、 the calibration byanalyzing the 1.0 % sulfur standard. The value should bewithin the allowable limits of the known value. If not, repeatthe procedure. Then weigh out and analyze two specimens,each of the other calibration standards. Record the results aftereach analysis. Compare the results obtaine
23、d to the knownsulfur values of the specimens. They should be within theallowable limits of the known value of the respective speci-men. If not, refer to the manufacturers instructions forchecking linearity of the analyzer.11. Procedure11.1 Sample PreparationDry an adequate sample of thecarbon black
24、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 roomtemperature in a desiccator before use.11.2 Stabilize and calibrate the analyzer (see 10.1 through10.3).11.3 Raise the furnace temperatur
25、e as recommended by themanufacturer to at least 1350C. Weigh the specimen not toexceed more than 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 1T
26、he analytical cycle should begin automatically as soon assulfur is detected.11.4 When the analysis 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.12.2 Report
27、 results to the nearest 0.01 %.13. Precision and Bias13.1 These precision statements have been prepared inaccordance with Practice D4483-99. Refer to this practice forterminology and other statistical details.13.2 The precision results in this precision and bias sectiongive an estimate of the precis
28、ion of this test method with thematerials used in the particular interlaboratory program de-scribed in Table 1. The precision parameters should not be usedfor acceptance or rejection testing of any group of materialswithout documentation that they are applicable to those par-ticular materials and th
29、e specific testing protocols of the testmethod. Any appropriate value may be used from Table 1.13.3 A type 1 inter-laboratory precision program was con-ducted as detailed in Table 1. Both repeatability and reproduc-ibility represent short term (daily) testing conditions. Thetesting was performed usi
30、ng 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 singledetermination. Acceptable difference values were not mea-sured. The between operator component of variation is in-cluded in the calculated values for
31、 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” order. The absolute reproducibility is moreindependent of the mean level so the absolute repeatability, r,and reproducibility, R, are the preferred parameter
32、s.13.5 RepeatabilityThe pooled absolute repeatability, r, ofthis test has been established as 0.0456 %. Any other value in4Coal standards have been found to be suitable standards and are usuallyavailable from the instrument manufacturer or may be obtained fromAlpha Productsfor Analysis, 3090 Johnson
33、 Road, Stevensville, MI 49127, www.alpha-.D1619 16a2Table 1 may be used as an estimate of repeatability, asappropriate. The difference between two single test results (ordeterminations) found on identical test material under therepeatability conditions prescribed for this test will exceed therepeata
34、bility 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 populationsand some appropriate action taken.NOTE 2Appropriate action m
35、ay 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.13.6 ReproducibilityThe pooled absolute reproducibility,R, of this test has been established as
36、0.1931 %. Any othervalue in Table 1 may be used as an estimate of reproducibility,as appropriate. The difference between two single and inde-pendent test results found by two operators working under theprescribed reproducibility conditions in different laboratorieson identical test material will exc
37、eed 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 populations and some
38、appropriate investigativeor technical/commercial action taken.13.7 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 isexclus
39、ively 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 black. Each element has an unique energy response(fluorescence) when exposed to x-ray energy that can be u
40、sedto identify the element. An x-ray source excites the sulfuratoms in the sample material. The instrument detects theexcited sulfur atoms and produces a numeric value.15. Apparatus15.1 X-ray Fluorescence Instrument, designed specificallyfor the test of trace amounts of sulfur, with x-ray source(rad
41、ioisotope or x-ray tube), detection, and numeric display.X-ray fluorescence instruments are either wavelength disper-sive or energy dispersive. Energy dispersive instruments havea lower detectable limit of 15 ppm while wavelength dispersiveinstruments have a lower detectable limit of less than 1 ppm
42、.Since the sulfur in oil furnace type carbon blacks is usuallypresent in percent levels, either instrument type is suitable.15.2 Gravity Convection Drying Oven, capable of maintain-ing 125 6 5C.15.3 Desiccator.16. Calibration16.1 The ability of the instrument to detect an elementsenergy signature is
43、 strongly influenced by the sample matrix.Therefore, the materials used to calibrate the instrument needto be as similar as possible to the unknown sample to be tested.If the unknown sample is a liquid, slurry, powder, or solid, thecalibration materials need to be a similar liquid, slurry, powder,or
44、 solid. The preferred calibration materials will be made by (orcome from) the same process as the unknown sample.16.2 X-ray fluorescence is not a primary test, but work byASTM International Committee D24 on Carbon Black hasshown that only carbon black with suitable levels of sulfurnaturally occurrin
45、g (that is, coming from the carbon blackmanufacturing process.) can be used to properly calibrate thetechnique. It has been determined that a standard materialcannot be made by adding elemental sulfur to carbon black.16.3 Calibrate the instrument according to the manufactur-ers instructions.16.4 Fou
46、r carbon black standards have been identified5andtheir respective sulfur level determined by combustion meth-ods following Test Methods D1619 Method A calibrationprocedures. They are:5Sulfur-in-carbon black standards A-D are available from Laboratory Standardsand Technologies, Inc., 227 Somerset Str
47、eet, Borger, TX, 79007, www.carbonstan-.TABLE 1 Precision Parameters for Test Methods D1619, Method A, (Type 1 Precision)Units PercentMaterial PeriodNumber ofLaboratoriesMean Level Sr r (r) SR R (R)SRB C6 (N326) March 2003 4 0.8056 0.0150 0.0426 5.28 0.0966 0.2734 33.94HS Tread September 2003 7 1.07
48、79 0.0123 0.0349 3.24 0.0174 0.0494 4.58SRB8E (N660) September 2008 9 1.1085 0.0067 0.0188 1.70 0.1182 0.3344 30.17SRB8B (N134) June 2009 13 1.1738 0.0117 0.0330 2.81 0.0600 0.1698 14.46SRB8A (N326) March 2008 12 1.1945 0.0179 0.0507 4.25 0.0409 0.1157 9.69SRB A6 (N134) September 2004 9 1.2556 0.010
49、3 0.0291 2.32 0.0400 0.1133 9.03N234 September 2007 10 1.3094 0.0210 0.0595 4.54 0.0616 0.1743 13.31N299 March 2006 10 1.5716 0.0113 0.0320 2.04 0.0414 0.1173 7.46N772 March 2005 9 1.8256 0.0176 0.0499 2.74 0.1026 0.2903 15.90LS Carcass March 2004 6 1.8565 0.0202 0.0573 3.09 0.0265 0.0751 4.04SRB8D (LS Carcass) March 2009 12 1.8988 0.0254 0.0718 3.78 0.0862 0.2439 12.84SRB D7 (LS Carcass) September 2006 12 1.9172 0.0142 0.0401 2.09 0.0348 0.0986 5.14Average 1.4163Pooled Values 0.0161 0.0456 3.22 0.0682 0.1931 13.63D1619 16a3Material %
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