1、Designation: D7662 13Standard Test Method forCarbon Content in Carbon Black Feedstock Oils1This standard is issued under the fixed designation D7662; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A numb
2、er in parentheses 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 samples of carbon black feedstock oils.Values obtained represent
3、 the total carbon content.1.2 This test method is applicable to carbon black feedstockoils derived from petroleum, coal, and other sources whichinclude fuel oils, residues, tars, pitches, reclaimed oils, andsimilar materials that are normally handled as liquids. This testmethod is applicable to prod
4、ucts that typically contain 75 to 94mass % carbon.1.3 The results of these tests can be expressed as mass %carbon.1.4 UnitsThe values stated in SI units are to be regardedas standard. No other units of measurement are included in thisstandard.1.5 This standard does not purport to address all of thes
5、afety 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:2D4057 Practice for Manual Sam
6、pling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD7633 Test Method for Carbon BlackCarbon Content3. Summary of Test Me
7、thod3.1 In this test method, a sample of feedstock oil is weighedin a combustion boat containing a tungsten oxide basedaccelerator and the carbon content is determined by placing theboat in a tube furnace at 1350C in an air- or oxygen-enrichedatmosphere resulting in complete combustion. Carbon in th
8、esample is completely oxidized to carbon dioxide. Moisture andparticulates are removed from the gas stream by traps filledwith anhydrous magnesium perchlorate. The gas stream is thenpassed through a cell in which carbon dioxide concentration ismeasured by an infrared (IR) absorption detector at a pr
9、ecisewavelength in the IR spectrum.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 shall be calibrated using an appro-priate calibration standard (see 6.5).3.4 The instrum
10、ent may be configured to analyze more thanone element such as a carbon-sulfur analyzer. In this case, theanalyzer has individual detectors for each element that arearranged in series.4. Significance and Use4.1 Measuring the total carbon content of feedstock oil isoften a necessary component in calcu
11、lations for carbon dioxideemissions, estimating yield of a process, or assessing productquality.4.2 The carbon black industry measures carbon content offeedstock oils along with carbon content of carbon blackproducts per Test Method D7633 for Carbon Black-CarbonContent in calculations to determine c
12、arbon dioxide emissionsfor compliance with governmental greenhouse-gas-reportingrequirements.5. Apparatus5.1 There are a number of commercial instruments availablethat are designed to measure carbon content in organic mate-rials including carbon and carbon-sulfur analyzers. This testmethod makes no
13、specifications regarding system designs.5.2 Functionally, however, the following are specified for allinstruments: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
14、 approved Nov. 1, 2013. Published December 2013. Originallyapproved in 2010. Last previous edition approved in 2011 as D7662 11. DOI:10.1520/D7662-13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStand
15、ards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.2.1 An analytical balance, or equivalent, that is capable ofa weighing sensitivity of 0.1 mg or
16、 better resolution.5.2.2 The combustion tube and boat are made of a suitablematerial such as mullite, porcelain, or zircon.5.2.3 The sample is absorbed onto tungsten oxide basedaccelerator to control the sample combustion rate.5.2.4 The sample is combusted at a temperature of 1350Cin an air- or oxyg
17、en-enriched atmosphere.5.2.5 The combustion gas is passed through an absorbent(anhydrous magnesium perchlorate) to remove water vapor.5.2.6 The detection system measures carbon dioxide usingan IR absorption detector at a wavelength suitable for linearresponses with respect to the concentration over
18、the full rangeof possible concentrations.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 specifications of the Commit-tee on Analytical Reagents of the American Chemical Societywhere
19、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 Magnesium Perchlorate.6.3 Oxygen, high purity, 99.9 %.6.4 Tungsten (VI) Oxide Accelerat
20、or containing potassiumdihydrogen-phosphate.6.5 Calibration Standard.47. Sampling7.1 Collect a feedstock oil as specified in Practices D4057or D4177.7.2 SampleThis is the portion or aliquot of the feedstockoil for use in obtaining a result.7.3 PreparationWarm viscous samples until they are fluidand
21、shake for 5 s.7.4 TransferUse any convenient, clean syringe or pipet totransfer a sample to the combustion boat as described inSection 10.8. 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 mi
22、nimum of two determinations to condition theequipment or follow the manufacturers recommendation tocondition equipment before calibrating the instrument.9. Calibration9.1 Calibrate the instrument per the manufacturers recom-mendation using appropriate carbon calibration standards.9.2 Adjustment of R
23、esponse of Measurement SystemWeigh approximately 0.1 g of calibration standard or use therecommended mass per manufacturer. Analyze the sample (seeSection 10). Repeat this procedure. Adjust the instrument asrecommended by the manufacturer until the absence of drift isindicated. Insure the minimum an
24、alysis time is sufficient forcomplete combustion of the sample.9.3 Calibration ProcedureFollow the calibration proce-dure recommended by the manufacturer. Confirm the calibra-tion by analyzing a reference material of known carbonconcentration. Reference standards should be similar to feed-stock oils
25、 with carbon content in the range of approximately 75to 94 %. The measured value should be within allowable limitsof the known value. If not, repeat the procedure. If acceptableresults are not obtained, refer to the manufacturers instructionsfor calibration.10. Procedure10.1 Stabilize and verify cal
26、ibration of the analyzer (see 8.1 8.3 and 9.1 9.3).10.2 Confirm the furnace temperature is 1350 6 15C.10.3 Weigh approximately 0.5 to1goftungsten oxidebased accelerator into the combustion boat (or use a massrecommended by the manufacturer), spreading evenly.10.4 Weigh approximately 0.1 to 0.15 g of
27、 the sample intothe combustion boat (on top the accelerator).10.5 Record the sample weight.10.6 Cover the sample with approximately 0.5 to 1 g oftungsten oxide based accelerator.10.7 Initiate the analysis and place the boat in the instru-ment using a boat puller or an auto-sampler mechanism.10.8 Whe
28、n the analysis is complete, the instrument shouldindicate the carbon value. Refer to the manufacturers recom-mended procedure.11. Report11.1 The percent carbon value is obtained directly from theapparatus.12. Precision and Bias512.1 These precision statements have been prepared inaccordance with Pra
29、ctice D4483. Refer to this practice 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 the3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washingt
30、on, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD4Carbon calibr
31、ation and reference standards are typically available from theinstrument manufacturer, and are also available from Alpha Resources, 3090Johnson Road, Stevensville, MI 49127, .5A research report is pending.D7662 132materials used in the particular inter-laboratory program de-scribed below. The precis
32、ion parameters should 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 1 forthe High Temperature Com
33、bustion Method. A common alter-nate method for carbon content, CHN, was included in theinter-laboratory program used to generate this precision state-ment since a number labs use this instrumental method.Precision data specific to the CHN method is found in Table 2.12.3 A type 1 inter-laboratory pre
34、cision program was con-ducted. Both repeatability and 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. Accep
35、table difference values were notmeasured.12.4 The results 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 1.80 %. Any other value inT
36、able 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 therepeatability on an average of not more than once in 20 case
37、sin 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 1Appropriate action may be an investigation of the test methodprocedure or
38、 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 been established as 3.71 %. Any other valuein Table 1 may be used as an e
39、stimate 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 material will exceed the reproducibility on anaverage of not more than onc
40、e 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 appropriate investigativeaction taken.12.7 BiasIn test me
41、thod 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, cannotbe determined.13. Keywor
42、ds13.1 carbon black; carbon content; combustion; feedstock;hydrocarbon oilTABLE 1 Precision Parameters for Test Method D7662, Type 1 Precision, High Temperature Combustion, Carbon Content of FeedstockUnitsPercentMaterialNumber ofLaboratoriesMean Level Sr r (r) SR R (R)5. NA Tar Oil 5 80.10 0.843 2.3
43、9 2.94 2.240 6.34 7.836. Leco 502-816(85.7 % C)5 86.52 0.502 1.42 1.64 0.925 2.62 3.037. Asian Coal Tar 5 90.70 0.454 1.29 1.42 0.547 1.55 1.718. NA Coal Tar 5 91.75 0.671 1.90 2.07 0.841 2.38 2.59Average 87.49Pooled Values 0.636 1.80 2.06 1.312 3.71 4.24TABLE 2 Precision Parameters for Test Method
44、D7662, Type 1 Precision, CHN, Carbon Content of FeedstockUnitsPercentMaterialNumber ofLaboratoriesMean Level Sr r (r) SR R (R)5. NA Tar Oil 8 82.20 0.509 1.441 1.75 1.269 3.59 4.376. Leco 502-816(85.7 % C)8 85.99 0.346 0.978 1.14 0.426 1.21 1.407. Asian Coal Tar 8 90.92 0.528 1.495 1.64 0.887 2.51 2
45、.768. NA Coal Tar 8 91.85 0.314 0.888 0.97 0.689 1.95 2.12Average 87.74Pooled Values 0.435 1.23 1.40 0.874 2.47 2.82D7662 133ASTM 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 ex
46、pressly 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 revi
47、sed, 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, which you ma
48、y 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 19428-2959,United Sta
49、tes. 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/).D7662 134
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