1、Designation: D 6374 99 (Reapproved 2004)An American National StandardStandard Test Method forVolatile Matter in Green Petroleum Coke Quartz CrucibleProcedure1This standard is issued under the fixed designation D 6374; the number immediately following the designation indicates the year oforiginal ado
2、ption or, in the case of 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. Scope1.1 This test method covers the determination of the volatilematter produc
3、ed 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 to16 %.1.3 Samples having a thermal history above 600C areexcluded.1.4 Thi
4、s 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 in SI units are to be regarded as the
5、standard.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 practices and to determine the applicability of regula-tory limitations prior to use.2. Referenced Document
6、s2.1 ASTM Standards:2E11 Specification for Wire-Cloth Sieves for Testing Pur-posesE 220 Test Method for Calibration of Thermocouples byComparison Techniques3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 analysis samplethe reduced and divided representa-tive portion of a bulk
7、sample, prepared for use in the labora-tory.3.1.2 analysis timeperiod test samples are placed in thefurnace, as determined in Section 9 (5 to 10 min).3.1.3 bulk samplethe reduced and divided representativeportion of a gross sample as prepared for shipment to andreceived by a laboratory, to be prepar
8、ed for analysis.3.1.4 green petroleum cokesame as raw petroleum coke3.1.5 gross samplethe original, uncrushed, representativesample taken from a shipment or lot of coke.3.1.6 petroleum cokea solid, carbonaceous residue pro-duced by thermal decomposition of heavy petroleum fractionsor cracked stocks,
9、 or both.3.1.7 raw petroleum cokepetroleum coke that has notbeen calcined.3.1.8 test samplethe weighed portion of the analysissample actually used in a test.3.1.9 volatile matterthe mass loss on heating expressed asa percent of the moisture free sample used.4. Summary of Test Method4.1 Volatile matt
10、er of a moisture free petroleum coke isdetermined by measuring the mass loss of the coke whenheated under the exact conditions of this test method.5. Significance and Use5.1 The volatile matter of petroleum coke affects the densityof coke particles and can affect artifacts produced from furtherproce
11、ssing 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 the test sample.6.2 Particle Size E
12、ffect: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. A 0.125-mm opening (No. 120) sieve
13、 shouldretain 40 to 55 % of the sample. Do not obtain the analysissample is by scalping and discarding a portion of the sample.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
14、 Fuels, Petroleum Coke, and Carbon Materials.Current edition approved Nov. 1, 2004. Published November 2004. Originallyapproved in 1999. Last previous edition approved in 1999 as D 6374 99.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at servic
15、eastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2.2 Any segregation of particle sizes within the analys
16、issample shall be corrected by reblending the sample just prior toweighing the test sample.6.3 The furnace shall recover to 950 6 20C before the timelimit is reached. If the furnace does not recover to the startingtemperature within a maximum of 10 min, reduce the numberof samples being analyzed unt
17、il recovery is achieved within 10min (see Section 9).7. Apparatus7.1 Electric Muffle FurnaceCalibrated (Test MethodE 220) and regulated to maintain a temperature of 950 6 20C(1742F), as measured by a thermocouple mounted inside thefurnace. Its heat capacity shall be such that the initial tempera-tur
18、e is regained after the introduction of a cold rack of sampleswithin 10 min.7.2 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 al
19、low control over particle size without contamination areacceptable (see Annex 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, 1/2 in. plate steel or other heat resistantmaterial large enough to
20、hold the crucible rack.8. Precautions8.1 Effusion of gaseous products, including 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, transfer1g(6 0.05g) of an analysis sample
21、(see Annex A1) to each crucible in therack, weigh each crucible with its contents, 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 (950620C).9.3 Place the full rack of samples in the furnace, and startthe time
22、r.9.4 Monitor the furnace temperature. Record the elapsedtime required 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 th
23、esample rack.9.5 When temperature recovery is achieved within the 10min 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
24、 next higherminute. This rounded time will be the analysis time for futureruns (5 min minimum).10. Procedure10.1 Ignite the quartz crucible and cover at 950 6 20C for5 min periods to constant mass (60.5 mg). Do not cover thecrucible at this time to allow the carbon to burn off. Cool toambient temper
25、ature in a desiccator before weighing thecrucible and cover.NOTE 1Placing 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
26、its contents, and cover to the nearest 0.1 mg.Place the cover on the crucible, and place in sample rack.10.3 Set the timer for the analysis time (5 to 10 min). Placethe 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
27、the furnace.10.4 After the analysis time (65 s), remove the rack 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 a
28、rea, desiccationis required.11. Calculation11.1 Calculate the volatile matter of the moisture freeprepared coke as follows:Volatile matter, mass % 5 A2B!/C! 3 100 (1)where:A = weight of crucible and prepared sample prior to analy-sis, g,B = weight of crucible and prepared sample after analysis,g, an
29、dC = weight of prepared sample, g.12. Report12.1 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
30、the second set also fails to agree within 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 successi
31、ve re-sults obtained by the same operator 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 X 1 2.826! (2)wh
32、ere: X is the average of two results in weight percent.D 6374 99 (2004)213.3 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 t
33、est method,exceed the following values only in one case in twenty.Reproducibility 5 0.06662 3 X 1 2.826! (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
34、 green petroleum coke, no statement on bias isbeing made.14. Keywords14.1 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 obt
35、ain a representative bulksample.A1.1.2 The bulk sample can vary in weight from 22.7 to90.6 kg (50 to 200 lb) and will vary in top particle size from 6to 75 mm (14 to 3 in.), depending upon the particle size of thegross sample.A1.1.3 Air dry the bulk sample, if needed, so that it can beproperly groun
36、d and fed through riffles. Air dry using dryingpans 38-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 roo
37、m shall be free of dust and excessive aircurrents. Avoid 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 to 40C. Air changes shouldbe at a rate of 1 to 4 min. Avoid over-heating and ex
38、cessivedrying.A1.1.5 A drying floor can be used 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,
39、 grind theentire sample to pass a 6.7 mm sieve, 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 scoo
40、p,feed bucket, or riffle pan length or opening equal 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 th
41、at the coke flows inuniform streams through the 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
42、 size particle of the coke beingriffled.A1.2.3 Grind 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).A1.2.4 Using a 3.35-mm sieve (No. 6), separate the coarseparticles to be crus
43、hed. This is called scalping.A1.2.5 Set the rolls far enough apart to crush only thelargest particles of the sample. Turn the roll crusher on, andpour the coarse portion of the sample very slowly through therolls. Once more scalp off the coarse particles that are to beground through the roll crusher
44、 again. Close the rolls not morethan 1.5 mm (116 in.) for each pass of the scalped sample.Repeat the crushing and scalping of the sample until all of thesample has passed through the 3.35-mm sieve. Make sure allparticles are well blended and none of the sample has beendiscarded.A1.2.6 Riffle the sam
45、ple to obtain two 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 roll crushers 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
46、 (No. 120). If this condition is notmet, go back to A1.2.5, and grind the second 350-g portion.Adjust the roll crusher in smaller increments to increase theamount of sample retained on the 0.125-mm sieve. Likewise,use large increments to decrease the amount of sample on the0.125-mm sieve.A1.2.9 Reco
47、mbine the 350-g sample, and dry it to constantweight at 95 to 105C. 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 higher volatile matter values becauseof oxidation of
48、 some cokes.D 6374 99 (2004)3ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof inf
49、ringement 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 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 comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not
