1、Designation: D2638 10 (Reapproved 2015)1Standard Test Method forReal Density of Calcined Petroleum Coke by HeliumPycnometer1This standard is issued under the fixed designation D2638; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEEditorial changes were made throughout in December 2015.1. Scope1.1 This test method covers the determination of
3、the realdensity (RD) of calcined petroleum coke. Real density, bydefinition is obtained when the particle size of the specimen issmaller than 75 m (U.S. No. 200 Sieve).1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This
4、 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-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents
5、2.1 ASTM Standards:2D346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD2013 Practice for Preparing Coal Samples for AnalysisD2234/D2234M Practice for Collection of a Gross Sampleof CoalD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4292 Test Me
6、thod for Determination of Vibrated BulkDensity of Calcined Petroleum CokeD4930 Test Method for Dust Control Material on CalcinedPetroleum CokeE11 Specification for Woven Wire Test Sieve Cloth and TestSievesE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Meth
7、od3. Terminology3.1 Definitions:3.1.1 calcined petroleum coke, npetroleum coke that hasbeen thermally treated to drive off the volatile matter and todevelop crystalline structure.3.1.2 petroleum coke, na solid, carbonaceous residueproduced by thermal decomposition of heavy petroleum frac-tions or cr
8、acked stocks, or both.3.2 Definitions of Terms Specific to This Standard:3.2.1 bulk density, nthe mass of the particles divided bythe volume they occupy which includes the space between theparticles. Refer to Test Method D4292 for bulk densityprocedures.3.2.2 dedusting material, nSee Test Method D49
9、30.3.2.3 real density, n(RD) (also be referred to as truespecific gravity). The mass divided by the volume occupied bythe material excluding pores and voids. It is required, therefore,that voids in the coke be eliminated and that pores in thematerial be filled by the fluid being displaced. This requ
10、irementis met for the purposes of this test method by reducing the cokeparticles to a size smaller than 75 m.3.2.3.1 DiscussionThe density of particles larger than75 m up to the largest that can be put into the heliumpycnometer can also be determined, but must be designated asparticle density (PD).
11、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 m (200-mesh) screen. The massof the sample is determined directly and the volume derived bythe volume of helium displaced when
12、 the sample is introduced1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved Oct. 1, 2015. Publi
13、shed December 2015. Originallyapproved in 1991. Last previous edition approved in 2010 as D2638 10. DOI:10.1520/D2638-10R15E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information
14、, 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 States1into a helium pycnometer. The ratio of the mass of the sampleto the volume is reported as the real density.5. Significan
15、ce and Use5.1 The real density 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 ca
16、lcination.6. Interferences6.1 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 m. Refer to Test Method D4930 for dedust oilremoval.7. Apparatus7.1 Analytica
17、l Balance, accurate to 60.1 mg.7.2 Desiccator.7.3 Drying Oven, preferably a vacuum oven, for tempera-ture to 120 C.7.4 Helium Pycnometer:7.5 Jaw Crusher and Roll CrusherOther style crusherswhich allow control over particle size without contaminationare acceptable.7.6 Rifflers, with hoppers and closu
18、res.7.7 Wire Sieve, 75 m (U.S. No. 200 mesh), meeting Speci-fication E11.8. Reagents and Materials8.1 Helium, 99.9 %.9. Sample Preparation9.1 For recommended practice for obtaining, handling, andpreparing coke samples, refer to Test Methods D346, D2013,D2234/D2234M, D4057, and D4930. The equipment a
19、ndprocedures for crushing and dividing are also described inthese test methods.9.2 Reduce and divide the gross sample to obtain a 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 opera
20、tinginstructions supplied by the helium pycnometer manufacturer. However,to assure that the test sample is representative of the entire sample, aminimum sample size of 100 g is required.9.4 When a dedusting oil is present it must be removed priorto further sizing. Refer to Test Method D4930 for dedu
21、st oilremoval.9.5 Crush 100 g of the test sample so that the entire samplewill pass through a 75 m (No. 200) sieve. Dry the crushedsample in a drying oven at 115 C 6 5 C to constant mass(approximately 8 h). Cool in a desiccator.10. Procedure10.1 Place 5 g to 150 g (80 % to 90 % of the maximumcapacit
22、y of the particular holder being used) of the preparedcrushed, sized and dried test sample into the specimen holderprovided with 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
23、 or automatically, the controlchamber, containing helium at a higher pressure than thesample chamber, with the sample chamber. 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
24、in each chamber prior to connection and thefinal pressure after the chambers have been connected.10.5 Record the final sample 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 s
25、pecific details, the manufac-turers operating instructions3are to be reviewed.11. Calculation11.1 Determine the real density of the sample in g/cm3fromEq 1.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
26、 density ascalculated in 11.1.13. Precision and Bias413.1 The values in the statements were determined in acooperative program following Practice E691. In this 2008study, there were twelve laboratories and eight samples. Theprecision of this test method as determined by the statisticalexamination of
27、 interlaboratory test results is as follows: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, exceed th
28、e following values only in one case intwenty:3Specific manufacturers instruction manuals and year of issue used in devel-oping this test method are given in the following list.Quantachrome: Model MVP-1, “Quantachrome Multipycnometer InstructionManual,” March 1987; Model SPY-2, “Quantachrome Stereopy
29、cnometer InstructionManual,” March 1982.Beckman, Model 930, “Beckman Instructions,” 1971.Frank Jones, Model 204, “Coberly-Stevens Porosimeter Instructions,” 1986.Micromeritics: Model 1320, “Instruction ManualAutopycnometer 1320,” March1984, May 1984, February 1985; Model 1305, “Instruction Manual Mu
30、ltivolumePycnometer 1305,” May 1985.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1687.D2638 10 (2015)12Repeatability 5 0.005 g/cm3(2)13.1.2 ReproducibilityThe difference between two singleand independent results obtained
31、by different laboratories onidentical test materials will in the long run, in normal andcorrect operation of the test method, exceed the followingvalues only in one case in twenty:Reproducibility 5 0.013 g/cm3(3)13.1.3 BiasSince there is no accepted reference materialsuitable for determining the bia
32、s for the procedure in this testmethod for measuring the real density of calcined petroleumcoke, no statement on bias is being made.NOTE 3The reproducibility value reflects the overall reproducibilitycovering all makes of pycnometers used in this work.14. Keywords14.1 calcined petroleum coke; helium
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