1、Designation: D7679 10Standard Test Method forSulfur Content in Carbon Black Feedstock Oils1This standard is issued under the fixed designation D7679; 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 sulfur content in samples of carbon black feedstock oils.Values obtained represent
3、 the total sulfur 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 typically containing 0 to 5mass % sulfur.1.3 The results of these tests can be expressed as mass %sulfur.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 This standard does not purport to address all of thesafety con
5、cerns, 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:2D1619 Test Methods for Carbon BlackSul
6、fur ContentD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum Products3. Summary of Test Method3.1 In this test method, a sample of feedstock oil is weighedin a combustion boat containing either a tungsten oxide baseda
7、ccelerator, sand or aluminum oxide absorbent, and the sulfurcontent is determined by placing the boat in a tube furnace at1350C in an air or oxygen-enriched atmosphere resulting incomplete combustion. Sulfur in the sample is completelyoxidized to sulfur dioxide. Moisture and particulates areremoved
8、from the gas stream by traps filled with anhydrousmagnesium perchlorate. The gas stream is then passed througha cell in which sulfur dioxide concentration is measured by aninfrared (IR) absorption detector at a precise wavelength in theIR spectrum. The IR absorption detects sulfur dioxide through-ou
9、t the entire combustion process. The integral of the detectorsignal is the basis for the total sulfur content of a sample.3.2 This test method is for use with commercially availablesulfur analyzers equipped to carry out the combustion andmeasurement operations automatically.3.3 The sulfur analyzer s
10、hall be calibrated using appropriatecalibration standards (see 6.7).3.4 The instrument 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 Measuri
11、ng the total sulfur content of feedstock oil isoften a necessary component in calculations for sulfur dioxideemissions.4.2 The carbon black industry measures sulfur content offeedstock oils along with sulfur content of carbon blackproducts per Test Method D1619 in calculations to determinesulfur dio
12、xide emissions for compliance with governmentalreporting requirements.5. Apparatus5.1 There are a number of commercially available instru-ments designed to measure sulfur content in organic materialsincluding sulfur and carbon-sulfur combustion analyzers. Thistest method makes no specifications rega
13、rding system designs.5.2 Functionally, however, the following are specified for allinstruments:5.2.1 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, porcel
14、ain, or zircon.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 Dec. 1, 2010. Published January 2011. DOI: 10.1520/D7679-10.2For referenced ASTM standard
15、s, 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, PA 1
16、9428-2959, United States.5.2.3 The sample is absorbed onto a solid which mayinclude the following materials: (1) tungsten oxide basedaccelerator; (2) Sea sand; (3) Aluminum oxide. Refer to theinstrument manufacturers recommendations.5.2.4 The sample is combusted at a temperature of 1350 615C in an a
17、ir 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 sulfur dioxide using anIR absorption detector at a wavelength suitable for linearresponses with respect to the concentra
18、tion 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 conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Soc
19、ietywhere 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
20、 Accelerator, containing potassiumdihydrogen-phosphate (optional).6.5 Sea Sand, purified by acid and calcinated (optional).6.6 Aluminum Oxide, optional.6.7 Calibration Standards.47. Sampling7.1 Collect feedstock oil as specified in Practices D4057 orD4177.7.2 SampleThis is the portion or aliquot of
21、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 described inSection 10.8. Preparation of Apparatus8.1 Assemble the apparatus a
22、ccording 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 before calibrating the instrument.9. Calibration9.1 Calibrate the instrume
23、nt per the manufacturers recom-mendation using appropriate sulfur calibration standards.9.2 Adjustment of Response of Measurement SystemWeigh approximately 0.1 to 0.2 g of calibration standard or usethe recommended mass per manufacturer. Analyze the sample(see Section 10). Repeat this procedure. Adj
24、ust the instrumentas recommended by the manufacturer until the absence of driftis indicated. 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 ana
25、lyzing a reference material of known sulfur con-centration. Reference standards should be similar to feedstockoils with sulfur content in the range of approximately 0 to 5 %.The measured value should be within allowable limits of theknown value. If not, repeat the procedure. If acceptable resultsare
26、 not obtained, refer to the manufacturers instructions forcalibration.10. Procedure10.1 Stabilize and verify calibration of the analyzer (seeSections 8 and 9).10.2 Confirm the furnace temperature is 1350 6 15C.10.3 Weigh an appropriate mass of accelerator or absorbentinto the combustion boat.NOTE 1U
27、se a material and mass recommended by the instrumentmanufacturer suitable for the combustion boat in use. Calibration stan-dards and feedstock samples should be analyzed using a similar mass ofaccelerator or absorbent.10.4 Weigh approximately 0.1 to 0.2 g of the sample intothe combustion boat on top
28、 of the accelerator or absorbent.10.5 Record the sample weight.10.6 A portion of the accelerator or absorbent within theboat may be used to cover the sample, or alternatively,additional accelerator or absorbent may be weighed and addedto cover the sample.NOTE 2When covering the sample use care to in
29、sure none of thesample is accidentally removed from the combustion boat due to contactwith a spatula or other tool used to transfer or position the accelerator orabsorbent.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
30、analysis is complete, the instrument shouldindicate the sulfur value. Refer to the manufacturers recom-mended procedure.11. Report11.1 The percent sulfur value is obtained directly from theapparatus.12. Precision and Bias12.1 PrecisionThe repeatability standard deviation hasbeen determined to be _.
31、The reproducibility of this testmethod is being determined and will be available within fiveyears.12.2 BiasThe bias of this test method will be availablewithin five years.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the te
32、sting 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,MD.4Sulfur calibration and reference standards ar
33、e typically available from theinstrument manufacturer, and are also available from Alpha Resources, 3090Johnson Road, Stevensville, MI 49127, .D7679 10213. Keywords13.1 carbon black; combustion; feedstock; hydrocarbon oil;sulfur contentASTM International takes no position respecting the validity of
34、any patent rights asserted in connection with any item mentionedin this standard. Users of this standard 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 r
35、evision at any time by the responsible technical committee and must be reviewed every five years andif 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. Yo
36、ur comments will receive careful consideration at a meeting of theresponsible technical committee, 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 cop
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