ASTM D7679-2013 5252 Standard Test Method for Sulfur Content in Carbon Black Feedstock Oils《炭黑原料油中硫含量的标准试验方法》.pdf
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1、Designation: D7679 13Standard 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. Two analysismethods are available for use:Test Method A: High-Temperature CombustionWithInfrared Absorption Detection ProceduresSections 410Test Method B: X-Ray Fluorescence Sections 13171.2 This test method is applicable to carbon black feedstockoils derived from petroleu
4、m, 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 products typically containing 0 to 5mass % sulfur.1.3 The results of these tests can be expressed as mass %sulfur.1.
5、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 concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-
6、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 BlackSulfur ContentD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sam
7、pling of Petroleum andPetroleum ProductsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3. Significance and Use3.1 Measuring the total sulfur content of feedstock oil isoften a necessary component in calculations for sulfur dioxi
8、deemissions.3.2 The carbon black industry measures sulfur content offeedstock oils along with sulfur content of carbon blackproducts per Test Method D1619 in calculations to determinesulfur dioxide emissions for compliance with governmentalreporting requirements.TEST METHOD A: HIGH-TEMPERATURECOMBUS
9、TION WITH INFRARED ABSORPTIONDETECTION PROCEDURES4. Summary of Test Method4.1 In this test method, a sample of feedstock oil is weighedin a combustion boat containing either a tungsten oxide basedaccelerator, sand or aluminum oxide absorbent, and the sulfurcontent is determined by placing the boat i
10、n 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 from the gas stream by traps filled with anhydrousmagnesium perchlorate. The gas stream is then passed
11、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-out the entire combustion process. The integral of the detectorsignal is the basis for the total sulfur c
12、ontent of a sample.4.2 This test method is for use with commercially availablesulfur analyzers equipped to carry out the combustion andmeasurement operations automatically.4.3 The sulfur analyzer shall be calibrated using appropriatecalibration standards (see 6.7).4.4 The instrument may be configure
13、d 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.1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.66
14、on Environment,Health, and Safety.Current edition approved Nov. 1, 2013. Published December 2013. Originallyapproved in 2010. Last previous edition approved in 2011 as D7679 11. DOI:10.1520/D7679-13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service
15、 at serviceastm.org. For Annual Book of ASTMStandards 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. Apparatus5.1 There are a number of commercial
16、ly available instru-ments designed to measure sulfur content in organic materialsincluding sulfur and carbon-sulfur combustion analyzers. Thistest method makes no specifications regarding system designs.5.2 Functionally, however, the following are specified for allinstruments:5.2.1 An analytical bal
17、ance, 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 a solid which mayinclude the following materials: (1) tungsten oxide
18、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 air or oxygen-enriched atmosphere.5.2.5 The combustion gas is passed through an absorbent(anhydrous magnesium perchlorate) to rem
19、ove 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 concentration over the full rangeof possible concentrations.6. Reagents6.1 Purity of ReagentsReagent-grade chemicals shall beused in all
20、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
21、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 (optional).6.5 Sea Sand, purified by acid and calcinated (optional).6.6 A
22、luminum 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 the feedstockoil for use in obtaining a result.7.3 PreparationWarm viscous samples until they are fluidand shake for 5 s.7.4 Tra
23、nsferUse 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 minimum of two determin
24、ations 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 sulfur calibration standards.9.2 Adjustment of Response of Measuremen
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