ASTM D6374-12(2017)e1 Standard Test Method for Volatile Matter in Green Petroleum Coke Quartz Crucible Procedure.pdf

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1、Designation: D6374 12 (Reapproved 2017)1Standard Test Method forVolatile Matter in Green Petroleum Coke Quartz CrucibleProcedure1This standard is issued under the fixed designation D6374; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revis

2、ion, 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.1NOTESI units formatting was corrected editorially in July 2017.1. Scope1.1 This test method covers the determina

3、tion of the volatilematter produced by pyrolysis or evolved when petroleum cokeis subjected to the specific conditions of the test method.1.2 The interlaboratory study for precision covered materi-als with a volatile matter concentration ranging from about 8 %to 16 %.1.3 Samples having a thermal his

4、tory above 600 C areexcluded.1.4 This test method is empirical and requires the entire testprocedure to be closely followed to ensure that results fromdifferent laboratories will be comparable.1.5 This test method is not satisfactory for determiningde-dusting material content.1.6 The values stated i

5、n SI units are to be regarded asstandard.1.6.1 ExceptionNon-SI units are shown in parentheses forinformation only.1.7 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user to establish appropriate safety andhealth pr

6、actices and to determine the applicability of regula-tory limitations prior to use.1.8 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guid

7、es and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2E11 Specification for Woven Wire Test Sieve Cloth and TestSievesE220 Test Method for Calibration of Thermocouples ByComparison Techniques3. Terminology

8、3.1 Definitions of Terms Specific to This Standard:3.1.1 analysis sample, nthe reduced and divided represen-tative portion of the bulk sample, prepared for use in thelaboratory.3.1.2 analysis time, nperiod test samples are placed in thefurnace, as determined in Section 9 (5 min to 10 min).3.1.3 bulk

9、 sample, nthe reduced and divided representa-tive portion of the gross sample as prepared for shipment to andreceived by a laboratory, to be prepared for analysis.3.1.4 green petroleum coke, nsame as raw petroleum coke3.1.5 gross sample, nthe original, uncrushed, representa-tive portion taken from a

10、 shipment or lot of coke.3.1.6 petroleum coke, na solid, carbonaceous residueproduced by thermal decomposition of heavy petroleum frac-tions or cracked stocks, or both.3.1.7 raw petroleum coke, npetroleum coke that has notbeen calcined.3.1.8 test sample, nthe weighed portion of the analysissample ac

11、tually used in a test.3.1.9 volatile matter, nthe mass loss on heating expressedas a percent of the moisture free sample used.4. Summary of Test Method4.1 Volatile matter of a moisture free petroleum coke isdetermined by measuring the mass loss of the coke whenheated under the exact conditions of th

12、is test method.1This 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 May 1, 2017. Published July 2

13、017. Originally approvedin 1999. Last previous edition approved in 2012 as D6374 12. DOI: 10.1520/D6374-12R17E01.2For 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

14、 standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in th

15、e Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.15. Significance and Use5.1 The volatile matter of petroleum coke affects the densityof coke particles and can affect

16、artifacts produced from furtherprocessing of the coke.5.2 The volatile matter can be used in estimating thecalorific value of coke.6. Interferences6.1 Moisture has a double effect. The mass loss is increasedand the moisture free sample weight is decreased by theamount of moisture actually present in

17、 the test sample.6.2 Particle Size Effect:6.2.1 The particle size range of the analysis sample affectsthe volatile matter. The coarser the analysis sample, the lowerthe reported volatile matter will be. Crush analysis sample (seeAnnex A1) to pass a 0.250 mm opening (No. 60) sieve but donot overcrush

18、. A 0.125 mm opening (No. 120) sieve shouldretain 40 % to 55 % of the sample. Do not obtain the analysissample by scalping and discarding a portion of the sample.6.2.2 Any segregation of particle sizes within the analysissample shall be corrected by reblending the sample just prior toweighing the te

19、st sample.6.3 The furnace shall recover to 950 C 6 20 C before thetime limit is reached. If the furnace does not recover to thestarting temperature within a maximum of 10 min, reduce thenumber of samples being analyzed until recovery is achievedwithin 10 min (see Section 9).7. Apparatus7.1 Electric

20、Muffle FurnaceCalibrated (Test MethodE220) and regulated to maintain a temperature of 950 C 620 C (1742 F), as measured by a thermocouple mountedinside the furnace. Its heat capacity shall be such that the initialtemperature is regained after the introduction of a cold rack ofsamples within 10 min.7

21、.2 Quartz Crucibles, self-sealing, 10 mL capacity withcovers.7.3 Rack, stainless steel, designed to hold up to 20 crucibles.7.4 Rifflers, with hoppers and closures.7.5 Jaw Crusher and Roll CrusherOther style crushersthat allow control over particle size without contamination areacceptable (see Annex

22、 A1).7.6 Balance, capable of weighing to 0.1 mg.7.7 Dessicator.7.8 Sieves, meeting Specification E11.7.9 Timers, stopwatch or second timer.7.10 Heat Sink, 12.7 mm plate steel or other heat resistantmaterial large enough to hold the crucible rack.8. Precautions8.1 Effusion of gaseous products, includ

23、ing soot and varioushydrocarbons, and the increase of heat associated with the testcan make the use of a hood desirable.9. Furnace Calibration9.1 Avoiding segregation of particles, transfer 1 g (60.05 g)of an analysis sample (see Annex A1) to each crucible in therack, weigh each crucible with its co

24、ntents, and cover to thenearest 0.1 mg. Place the cover on the crucible, and place insample rack.9.2 Record the furnace temperature at equilibrium (950 C6 20 C).9.3 Place the full rack of samples in the furnace, and startthe timer.9.4 Monitor the furnace temperature. Record the elapsedtime required

25、to return to the equilibrium temperature recordedin 9.2. If the time exceeds 10 min, repeat the procedure,reducing the number of crucibles in the rack until temperaturerecovery is completed within 10 min of the introduction of thesample rack.9.5 When temperature recovery is achieved within the10 min

26、 period, record the number of crucibles in the rack. Thisnumber of crucibles shall be in the rack for all future runs (fillempty spaces in the stand with empty crucibles when neces-sary).9.6 Round the recorded elapsed time to the next higherminute. This rounded time will be the analysis time for fut

27、ureruns (5 min minimum).10. Procedure10.1 Ignite the quartz crucible and cover at 950 C 6 20 Cfor 5 min periods to constant mass (60.5 mg). Do not cover thecrucible at this time to allow the carbon to burn off. Cool toambient temperature in a desiccator before weighing thecrucible and cover.NOTE 1Pl

28、acing the empty crucibles in the inverted cover whenigniting will reduce breakage and chipping.10.2 Avoiding segregation of particles, transfer 1 g 610 mgof the analysis sample (see Annex A1) to the crucible, weighthe crucible with its contents, and cover to the nearest 0.1 mg.Place the cover on the

29、 crucible, and place in sample rack.10.3 Set the timer for the analysis time (5 min to 10 min).Place the rack in the furnace. Start the timer.NOTE 2Place the rack in the center of the furnace. Do not allow therack to touch the walls of the furnace.10.4 After the analysis time (65 s), remove the rack

30、 fromthe furnace and immediately place on a heat sink.10.5 Weigh the crucible after it has cooled to room tem-perature and before it has been at room temperature for longerthan 20 min.NOTE 3If cool down is not in a humidity controlled area, desiccationis required.11. Calculation11.1 Calculate the vo

31、latile matter of the moisture freeprepared coke as follows:Volatile matter, mass percent 5 A 2 B!/C) 3100 (1)D6374 12 (2017)12where:A = weight of crucible and prepared sample prior toanalysis, g,B = weight of crucible and prepared sample after analysis, g,andC = weight of prepared sample, g.12. Repo

32、rt12.1 Report to one decimal the average of duplicate deter-minations that agree within 0.5 %. When this agreement is notmet, the values are considered suspect and another duplicateset shall be run. Report the average of all results agreeingwithin 0.5 %. If the second set also fails to agree within

33、0.5 %,report the average of all four values.13. Precision and Bias13.1 PrecisionThe precision of this test method as deter-mined by the statistical examination of the interlaboratory testresults is as follows:13.2 RepeatabilityThe difference between successive re-sults obtained by the same operator

34、with the same apparatusunder constant operating conditions on identical test materialswould, in the long run, in the normal and correct operation ofthe test method, exceed the following values only one case intwenty.Repeatability 5 0.01905 3 X12.826! (2)where: X is the average of two results in weig

35、ht percent.13.3 ReproducibilityThe difference between two singleand independent results obtained by different operators work-ing in different laboratories on identical material will, in thelong run, in normal and correct operation of the test method,exceed the following values only in one case in tw

36、enty.Reproducibility 5 0.06662 3 X12.826! (3)where: X is the average of two results in weight percent.13.4 BiasSince there is no accepted reference material fordetermining the bias for this test method for measuring thevolatile matter in green petroleum coke, no statement on bias isbeing made.14. Ke

37、ywords14.1 analysis time; green petroleum coke; volatile matterANNEX(Mandatory Information)A1. PREPARATION OF SAMPLESA1.1 Preparation of Bulk SampleA1.1.1 The bulk sample is prepared by reducing the grosssample in such a manner as to obtain a representative bulksample.A1.1.2 The bulk sample can vary

38、 in weight from 22.7 kg to90.6 kg (50 lb to 200 lb) and will vary in top particle size from6mmto75mm(14 in. to 3 in.), depending upon the particlesize of the gross sample.A1.1.3 Air dry the bulk sample, if needed, so that it can beproperly ground and fed through riffles. Air dry using dryingpans 38

39、mm (112 in.) deep made of noncorroding metal and ofsufficient size that the sample may be spread to a depth ofapproximately 25 mm (1.0 in.). The maximum depth of thesample shall be no more than twice the diameter of the largestparticles. The room shall be free of dust and excessive aircurrents. Avoi

40、d excessive drying time.A1.1.4 An air drying oven can be used to pass slightlyheated air over the sample. The oven is to be capable ofmaintaining a temperature of 30 C to 40 C. Air changesshould be at a rate of 1 min to 4 min. Avoid over-heating andexcessive drying.A1.1.5 A drying floor can be used

41、to dry bulk samples. Thisis a smooth clean floor in a room free from dust and excessiveair current.A1.1.6 Any modification of the above that will not overheator contaminate the bulk sample is permitted.A1.1.7 After the bulk samples have been air dried, grind theentire sample to pass a 6.7 mm sieve,

42、using a jaw crusher. Donot overgrind. Keep a maximum amount of sample as coarse aspossible.A1.2 Preparation of Analysis SampleA1.2.1 Using a riffle, split the bulk sample to obtain a 700 gportion.A1.2.2 Pass the coke through the riffle from a feed scoop,feed bucket, or riffle pan length or opening e

43、qual to the fulllength of the riffle. When using any of the above containers tofeed the riffle, spread the coke evenly in the container, raise thecontainer, and hold it with its front edge resting on the top ofthe feed trough; then slowly tilt it so that the coke flows inuniform streams through the

44、hopper straight down the chutesinto the pans. Under no circumstances shovel the coke into theriffle or dribble the coke into the riffle from a small mouthcontainer. Make sure the riffle has a chute opening of at least 2to 212 times greater than the top size particle of the coke beingriffled.A1.2.3 G

45、rind the sample to pass a 3.35 mm (No. 6) sieveusing a roll crusher or other suitable crushing device that yieldsthe result specified in A1.2.8. Do not overgrind (see A1.2.8).D6374 12 (2017)13A1.2.4 Using a 3.35 mm sieve (No. 6), separate the coarseparticles to be crushed. This is called scalping.A1

46、.2.5 Set the gaps of the crusher far enough apart to crushonly the largest particles of the sample. Turn the roll crusheron, and pour the coarse portion of the sample very slowlythrough the rolls. Once more scalp off the coarse particles thatare to be ground through the roll crusher again. Close the

47、crusher not more than 1.5 mm (116 in.) for each pass of thescalped sample. Repeat the crushing and scalping of the sampleuntil all of the sample has passed through the 3.35-mm sieve.Make sure all particles are well blended and none of the samplehas been discarded.A1.2.6 Riffle the sample to obtain t

48、wo 350 g portions. Donot discard any of the sample.A1.2.7 Using a procedure analogous to A1.2.3, grind one ofthe 350 g samples in the crusher to pass a 0.250 mm sieve (No.60). Do not overgrind.A1.2.8 About one half of the sample at this point shall beretained on a 0.125 mm sieve (No. 120). If this c

49、ondition is notmet, go back to A1.2.5, and grind the second 350 g portion.Adjust the crusher in smaller increments to increase the amountof sample retained on the 0.125 mm sieve. Likewise, use largeincrements to decrease the amount of sample on the 0.125 mmsieve.A1.2.9 Recombine the 350 g sample, and dry it to constantweight at 95 C to 105 C. This dried sample is now ready foranalysis and can be stored in a closed container within adessicator. Samples shall be redried on the fourth day. Exces-sive heating can result in h