1、Designation: D7662 11Standard 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 ProductsD7633 Test Method for Carbon BlackCarbon Content3. Summary of Test Method3.1 In this test method, a sample of feedstock oil is weighedin a combustion boat containing a tungsten oxide based
7、accelerator 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 thesample is completely oxidized to carbon dioxide. Moisture andparticulates are removed from the gas stream by traps fil
8、ledwith 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 precisewavelength in the IR spectrum.3.2 This test method is for use with commercially availablecarbon analyzers equipped
9、 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 instrument may be configured to analyze more thanone element such as a carbon-sulfur analyzer. In this case, theanalyzer has i
10、ndividual 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 calculations for carbon dioxideemissions, estimating yield of a process, or assessing productquality.4.2 The carbon black in
11、dustry measures carbon content offeedstock oils along with carbon content of carbon blackproducts per Test Method D7633 for Carbon Black-CarbonContent in calculations to determine carbon dioxide emissionsfor compliance with governmental greenhouse-gas-reportingrequirements.5. Apparatus5.1 There are
12、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 specifications regarding system designs.5.2 Functionally, however, the following are specified for allinstruments:5.2.1
13、 An analytical balance, or equivalent, that is capable ofa weighing sensitivity of 0.1 mg or 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 samp
14、le combustion rate.5.2.4 The sample is combusted at a temperature of 1350Cin an air- or oxygen-enriched atmosphere.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 editio
15、n approved Jan. 1, 2011. Published February 2011. Originallyapproved in 2010. Last previous edition approved in 2010 as D7662 10. DOI:10.1520/D7662-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStan
16、dards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.2.5 The combustion gas is passed through an absorbent(anhydrous magnesium perchlorate) to rem
17、ove 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 the full rangeof possible concentrations.6. Reagents6.1 Purity of ReagentsReagent-grade chemicals shall beused in all
18、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 such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsuf
19、ficiently 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 Accelerator containing potassiumdihydrogen-phosphate.6.5 Calibration Standard.47. Sampling7.1 Collect a feedstock oil as specif
20、ied 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 shake for 5 s.7.4 TransferUse any convenient, clean syringe or pipet totransfer a sample to the combustion boat as des
21、cribed 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 minimum of two determinations to condition theequipment or follow the manufacturers recommendation tocondition equipment
22、 before calibrating the instrument.9. Calibration9.1 Calibrate the instrument per the manufacturers recom-mendation using appropriate carbon calibration standards.9.2 Adjustment of Response of Measurement SystemWeigh approximately 0.1 g of calibration standard or use therecommended mass per manufact
23、urer. Analyze the sample (seeSection 10). Repeat this procedure. Adjust the instrument asrecommended by the manufacturer until the absence of drift isindicated. Insure the minimum analysis time is sufficient forcomplete combustion of the sample.9.3 Calibration ProcedureFollow the calibration proce-d
24、ure 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 with carbon content in the range of approximately 75to 94 %. The measured value should be within allowable limitsof t
25、he known value. If not, repeat the procedure. If acceptableresults are not obtained, refer to the manufacturers instructionsfor calibration.10. Procedure10.1 Stabilize and verify calibration of the analyzer (see8.1-8.3 and 9.1-9.3).10.2 Confirm the furnace temperature is 1350 6 15C.10.3 Weigh approx
26、imately 0.5-1 g of tungsten oxide basedaccelerator into the combustion boat (or use a mass recom-mended by the manufacturer), spreading evenly.10.4 Weigh approximately 0.1-0.15 g of the sample into thecombustion boat (on top the accelerator).10.5 Record the sample weight.10.6 Cover the sample with a
27、pproximately 0.5-1 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 When the analysis is complete, the instrument shouldindicate the carbon value. Refer to the manufacturers recom-mended proced
28、ure.11. Report11.1 The percent carbon value is obtained directly from theapparatus.12. Precision and Bias12.1 PrecisionThe repeatability and reproducibility ofthis test method are being determined and will be availablewithin five years.12.2 BiasThe bias of this test method will be availablewithin fi
29、ve years.13. Keywords13.1 carbon black; carbon content; combustion; feedstock;hydrocarbon oil3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Stand
30、ards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD4Carbon calibration and reference standards are typically available from theinstrument manufacturer, and are also available f
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34、ceived 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 States. Individual reprints (single or multiple copies)
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