1、Designation: D7662 10Standard 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 CON-TENT3. Summary of Test Method3.1 In this test method, a sample of feedstock oil is weighedin a combustion boat containing a tungsten oxide base
7、daccelerator 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 fi
8、lledwith 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 equippe
9、d 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
10、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 calculations for carbon dioxideemissions, estimating yield of a process, or assessing productquality.4.2 The carbon black i
11、ndustry 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.
13、1 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 sam
14、ple combustion rate.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 Oct. 1, 2010. Published October 2010. DOI: 10.1520/D7662-10.2For referenced ASTM sta
15、ndards, 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 page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken,
16、 PA 19428-2959, United States.5.2.4 The sample is combusted at a temperature of 1350Cin an air- or oxygen-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 a
17、bsorption 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 tests. Unless otherwise indicated, it is intended thatall reagents shall confor
18、m 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 ofsufficiently high purity to permit its use without lessening theaccuracy of the de
19、termination.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 specified in Practices D4057or D4177.7.2 SampleThis is the portion or aliquot of the
20、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 described inSection 10.8. Preparation of Apparatus8.1 Assemble the apparatus accor
21、ding to the manufacturersinstructions.8.2 Stabilize the furnace temperature at 1350C.8.3 Make a minimum of two determinations to condition theequipment or follow the manufacturers recommendation tocondition equipment before calibrating the instrument.9. Calibration9.1 Calibrate the instrument per th
22、e 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 manufacturer. Analyze the sample (seeSection 10). Repeat this procedure. Adjust the instrume
23、nt 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-dure recommended by the manufacturer. Confirm the calibra-tion by analyzing a referen
24、ce 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 the known value. If not, repeat the procedure. If acceptableresults are not obtained,
25、 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 1350C.10.3 Weigh approximately 0.5-1 g of tungsten oxide basedaccelerator into the combustion boat (or use a mas
26、s 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 approximately 0.5-1 g oftungsten oxide based accelerator.10.7 Initiate the analysis and pl
27、ace 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 procedure.11. Report11.1 The percent carbon value is obtained directly from theapparatus.12. Pr
28、ecision 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 five years.13. Keywords13.1 carbon black; carbon content; combustion; feedstock;hydrocarbon
29、 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 Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharma
30、copeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD4Carbon calibration and reference standards are typically available from theinstrument manufacturer, and are also available from Alpha Resources, 3090Johnson Road, Stevensville, MI 49127, .D7662 102ASTM Internation
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