1、Designation: D 2638 06An American National StandardStandard Test Method forReal Density of Calcined Petroleum Coke by HeliumPycnometer1This standard is issued under the fixed designation D 2638; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the determination of the realdensity (RD) of calcined petroleum coke
3、. Real density, bydefinition is obtained when the particle size of the specimen issmaller than 75 microns (No. 200 Sieve).1.2 The values stated in acceptable metric units are to beregarded as the standard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated wit
4、h 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:2D 346 Practice for Collection and Preparation of CokeSamples for La
5、boratory AnalysisD 2013 Practice for Preparing Coal Samples for AnalysisD 2234/D 2234M Practice for Collection of a Gross Sampleof CoalD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4292 Test Method for Determination of Vibrated BulkDensity of Calcined Petroleum CokeD 4930 T
6、est Method for Dust Control Material on CalcinedPetroleum CokeE11 Specification for Wire Cloth and Sieves for TestingPurposes3. Terminology3.1 Definitions:3.1.1 calcined petroleum coke, npetroleum coke that hasbeen thermally treated to drive off the volatile matter and todevelop crystalline structur
7、e.3.1.2 petroleum cokea solid, carbonaceous residue pro-duced by thermal decomposition of heavy petroleum fractionsor cracked stocks, or both.3.2 Definitions of Terms Specific to This Standard:3.2.1 bulk densitythe mass of the particles divided by thevolume they occupy which includes the space betwe
8、en theparticles. Refer to Test Method D 4292 for bulk densityprocedures.3.2.2 dedusting materialSee Test Method D 4930.3.2.3 real density (RD) (also be referred to as true specificgravity). The mass divided by the volume occupied by thematerial excluding pores and voids. It is required, therefore,th
9、at voids in the coke be eliminated and that pores in thematerial be filled by the fluid being displaced. This requirementis met for the purposes of this test method by reducing the cokeparticles to a size smaller than 75 microns.3.2.3.1 DiscussionThe density of particles larger than 75microns up to
10、the largest that can be put into the heliumpycnometer can also be determined, but must be designated asparticle density (PD). The precision data obtained for RD maynot be applicable to PD.4. Summary of Test Method4.1 A representative sample of calcined petroleum coke isdried and ground to pass a 75-
11、micron (200-mesh) screen. Themass of the sample is determined directly and the volumederived by the volume of helium displaced when the sample isintroduced into a helium pycnometer. The ratio of the mass ofthe sample to the volume is reported as the real density.5. Significance and Use5.1 The real d
12、ensity of calcined petroleum coke directlyinfluences the physical and chemical properties of the manu-factured carbon and graphite artifacts for which it is used.Density, therefore, is a major quality specification of calcinedpetroleum coke and is used as a control in coke calcination.6. Interferenc
13、es6.1 Oil or other dedust material sprayed on calcined petro-leum coke to control dust will interfere with the determinationof real density so the oil must be removed before reducing thesample to 75 microns. Refer to Test Method D 4930 for dedustoil removal.1This test method is under the jurisdictio
14、n of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved July 1, 2006. Published July 2006. Originally approvedin 1991. Last previous edition approved in 2002
15、 as D 263891(2002).2For referenced ASTM standards, 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.1*A Summary of Changes section appears at
16、the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7. Apparatus7.1 Analytical Balance, accurate to 6 0.1 mg.7.2 Desiccator.7.3 Drying Oven, preferably a vacuum oven, for tempera-ture to 120C.7.4 Helium Pycnometer
17、:7.5 Jaw Crusher and Roll CrusherOther style crusherswhich allow control over particle size without contaminationare acceptable.7.6 Rifflers, with hoppers and closures.7.7 Wire Sieve, 75 microns (No. 200 mesh), meeting Speci-fication E11.8. Reagents and Materials8.1 Helium, 99.9 %.9. Sample Preparat
18、ion9.1 For recommended practice for obtaining, handling, andpreparing coke samples, refer to Test Methods D 346, D 2013,D 2234/D 2234M, D 4057, and D 4930. The equipment andprocedures for crushing and dividing are also described inthese test methods.9.2 Reduce and divide the gross sample to obtain a
19、 labora-tory analysis sample.9.3 Divide, by riffling, a minimum of 100 g from thelaboratory analysis sample.NOTE 1The amount of coke required will be dictated by the operatinginstructions supplied by the helium pycnometer manufacturer. However,to assure that the test sample is representative of the
20、entire sample, aminimum sample size of 100 grams is required.9.4 When a dedusting oil is present it must be removed priorto further sizing. Refer to Test Method D 4930 for dedust oilremoval.9.5 Crush 100 g of the test sample so that the entire samplewill pass through a 75-micron (No. 200) sieve. Dry
21、 the crushedsample in a drying oven at 115 6 5C to constant mass(approximately 8 h). Cool in a desiccator.10. Procedure10.1 Place 5 to 150 g (80 to 90 % of the maximum capacityof the particular holder being used) of the prepared crushed,sized and dried test sample into the specimen holder providedwi
22、th the instrument. Weigh to the nearest milligram.10.2 Place the pre-weighed test sample and specimen holderinto the sample chamber and evacuate.10.3 Connect, either manually or automatically, the controlchamber, containing helium at a higher pressure than thesample chamber, with the sample chamber.
23、 Determine the finalequilibrated pressure.10.4 The volume of the calcined petroleum coke sample iscalculated from the known volume of the two chambers, theabsolute pressures in each chamber prior to connection and thefinal pressure after the chambers have been connected.10.5 Record the final sample
24、volume or density when thepycnometer has reached equilibrium.NOTE 2This is a generic procedure which describes the basic stepsinvolved to obtain a final result. For further specific details, the manufac-turers operating instructions3are to be reviewed.11. Calculation11.1 Determine the real density o
25、f the sample in g/cm3fromEq 2.Density 5 M/V (1)where:M = mass of sample in g, andV = volume of helium displaced, cm3.12. Report12.1 Report to the third decimal place the real density ascalculated in 11.1.13. Precision and Bias13.1 The precision of this test method as determined by thestatistical exa
26、mination of interlaboratory test results is asfollows:13.1.1 RepeatabilityThe difference between successiveresults by the same operator using the same apparatus underconstant operating conditions on the identical test materials,will in the long run, in normal and correct operation of the testmethod,
27、 exceed the following values only in one case intwenty:Repeatability 5 0.018 g/cm3(2)13.1.2 ReproducibilityThe difference between two singleand independent results obtained by different laboratories onidentical test materials will in the long run, in normal andcorrect operation of the test method, e
28、xceed the followingvalues only in one case in twenty:Reproducibility 5 0.025 g/cm3(3)13.1.3 BiasSince there is not accepted reference materialsuitable for determining the bias for the procedure in this testmethod for measuring the real density of calcined petroleumcoke, no statement on bias is being
29、 made.NOTE 3The reproducibility value reflects the overall reproducibilitycovering all makes of pycnometers used in this work.14. Keywords14.1 calcined petroleum coke; helium pycnometer; realdensity3Specific manufacturers instruction manuals and year of issue used in devel-oping this test method are
30、 given in the following list.Quantachrome: Model MVP-1, “Quantachrome Multipycnometer InstructionManual,” March 1987; Model SPY-2, “Quantachrome Stereopycnometer InstructionManual,” March 1982.Beckman, Model 930, “Beckman Instructions,” 1971.Frank Jones, Model 204, “Coberly-Stevens Porosimeter Instr
31、uctions,” 1986.Micromeritics: Model 1320, “Instruction Manual Autopycnometer 1320,” March1984, May 1984, February 1985; Model 1305, “Instruction Manual MultivolumePycnometer 1305,” May 1985.D2638062SUMMARY OF CHANGESSubcommittee D02.05 has identified the location of selected changes to this standard
32、 since the last issue(D 263891(2002) that may impact the use of this standard.(1) Revised definition of calcined petroleum coke (3.1.1).ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this stan
33、dard 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 revision at any time by the responsible technical committee and must be reviewed every five years and
34、if 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. Your comments will receive careful consideration at a meeting of theresponsible technical committee, w
35、hich 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 copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. 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).D2638063
