1、Designation: D2638 10Standard 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, the year of last re
2、vision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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. Real density, bydefinition is
3、obtained when the particle size of the specimen issmaller than 75 microns (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 standard does not purport to address all of thesafety concerns, if any, assoc
4、iated 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:2D346 Practice for Collection and Preparation of CokeSample
5、s 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 Method for Determination of Vibrated BulkDensity of Calcined Petroleum CokeD4930
6、 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 Method3. Terminology3.1 Definitions:3.1.1 calcined petroleum coke, npetroleum coke
7、 that hasbeen thermally treated to drive off the volatile matter and todevelop crystalline structure.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 bu
8、lk densitythe mass of the particles divided by thevolume they occupy which includes the space between theparticles. Refer to Test Method D4292 for bulk densityprocedures.3.2.2 dedusting materialSee Test Method D4930.3.2.3 real density(RD) (also be referred to as true specificgravity). The mass divid
9、ed by the volume occupied by thematerial 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 requirementis met for the purposes of this test method by reducing the cokeparticles to a size
10、 smaller than 75 microns.3.2.3.1 DiscussionThe density of particles larger than 75microns up to 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 Te
11、st Method4.1 A representative sample of calcined petroleum coke isdried and ground to pass a 75-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
12、ofthe sample to the volume is reported as the real density.5. Significance 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 spe
13、cification of calcinedpetroleum coke and is used as a control in coke calcination.1This test method is under the jurisdiction 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.Cu
14、rrent edition approved May 1, 2010. Published July 2010. Originally approvedin 1991. Last previous edition approved in 2006 as D263806. DOI: 10.1520/D2638-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of A
15、STMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Interferences6.1 Oi
16、l 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 D4930 for dedustoil removal.7. Apparatus7.1 Analytical Balance, accurate to 6 0
17、.1 mg.7.2 Desiccator.7.3 Drying Oven, preferably a vacuum oven, for tempera-ture to 120C.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 closures.7.7 Wire Sieve, 75 mic
18、rons (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 andprocedures for crushing
19、 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 operatinginstructions supplied
20、 by the helium pycnometer manufacturer. However,to assure that the test sample is representative of the 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 D4930 for dedust oilremoval.9.5 Cru
21、sh 100 g of the test sample so that the entire samplewill pass through a 75-micron (No. 200) sieve. Dry 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 hol
22、der being used) of the prepared crushed,sized and dried test sample into the specimen holder providedwith 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
23、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 in each chamber prior t
24、o 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 specific details, the ma
25、nufac-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 density ascalculated i
26、n 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 interlaboratory test r
27、esults 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 the following values only
28、 in one case intwenty:Repeatability 5 0.005 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, exceed the followingvalues only in
29、 one case in twenty:Reproducibility 5 0.013 g/cm3(3)13.1.3 BiasSince there is no 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 made.NOTE 3The reproducibility va
30、lue reflects the overall reproducibilitycovering all makes of pycnometers used in this work.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,”
31、March 1987; Model SPY-2, “Quantachrome Stereopycnometer InstructionManual,” March 1982.Beckman, Model 930, “Beckman Instructions,” 1971.Frank Jones, Model 204, “Coberly-Stevens Porosimeter Instructions,” 1986.Micromeritics: Model 1320, “Instruction Manual Autopycnometer 1320,” March1984, May 1984, F
32、ebruary 1985; Model 1305, “Instruction Manual MultivolumePycnometer 1305,” May 1985.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1687.D2638 10214. Keywords14.1 calcined petroleum coke; helium pycnometer; realdensitySUMMAR
33、Y OF CHANGESSubcommittee D02.05 has identified the location of selected changes to this standard since the last issue(D263806) that may impact the use of this standard.(1) Revised Section 13.(2) Added Research Report and Footnote 4.ASTM International takes no position respecting the validity of any
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35、ion 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. Your c
36、omments 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 copyrig
37、hted 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D2638 103
