1、Designation:D637499 (Reapproved 2009) Designation: D6374 12Standard 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, i
2、n the case of revision, 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.1. Scope*1.1 This test method covers the determination of the volatile matter produced by pyro
3、lysis or evolved when petroleum coke issubjected to the specific conditions of the test method.1.2 The interlaboratory study for precision covered materials with a volatile matter concentration ranging from about 8 to 16 %.1.3 Samples having a thermal history above 600C are excluded.1.4 This test me
4、thod is empirical and requires the entire test procedure to be closely followed to ensure that results from differentlaboratories will be comparable.1.5 This test method is not satisfactory for determining de-dusting material content.1.6 The values stated in SI units are to be regarded as standard.
5、No other units of measurement are included in this standard.1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user to establish appropriate safety and health practices and to determine the applicability of regula
6、tory limitations priorto use.2. Referenced Documents2.1 ASTM Standards:2E11 Specification for Woven Wire Test Sieve Cloth and Test SievesE220 Test Method for Calibration of Thermocouples By Comparison Techniques3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 analysis sampleana
7、lysis sample, nthe reduced and divided representative portion of the bulk sample, prepared for usein the laboratory.3.1.2 analysis timeanalysis time, nperiod test samples are placed in the furnace, as determined in Section 9 (5 to 10 min).3.1.3 bulk sample, nthe reduced and divided representative po
8、rtion of athe gross sample as prepared for shipment to andreceived by a laboratory, to be prepared for analysis.3.1.4 green petroleum cokegreen petroleum coke, nsame as raw petroleum coke3.1.5 gross samplegross sample, nthe original, uncrushed, representative portion taken from a shipment or lot of
9、coke.3.1.6 petroleum cokepetroleum coke, na solid, carbonaceous residue produced by thermal decomposition of heavy petroleumfractions or cracked stocks, or both.3.1.7 raw petroleum cokeraw petroleum coke, npetroleum coke that has not been calcined.3.1.8 test sampletest sample, nthe weighed portion o
10、f the analysis sample actually used in a test.3.1.9 volatile mattervolatile matter, nthe mass loss on heating expressed as a percent of the moisture free sample used.4. Summary of Test Method4.1 Volatile matter of a moisture free petroleum coke is determined by measuring the mass loss of the coke wh
11、en heated underthe exact conditions of this test method.1This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.05 onProperties of Fuels, Petroleum Coke and Carbon Material.Current edition approved Ap
12、ril 15, 2009.2012. Published July 2009.May 2012. Originally approved in 1999. Last previous edition approved in 20042009asD637499(20049). DOI: 10.1520/D6374-99R09.10.1520/D6374-12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.or
13、g. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.1This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit
14、 may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at
15、 the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 The volatile matter of petroleum coke affects the density of coke particles and can affect artifacts produced from furtherprocessing
16、of the coke.5.2 The volatile matter can be used in estimating the calorific value of coke.6. Interferences6.1 Moisture has a double effect. The mass loss is increased and the moisture free sample weight is decreased by the amountof moisture actually present in the test sample.6.2 Particle Size Effec
17、t:6.2.1 The particle size range of the analysis sample affects the volatile matter. The coarser the analysis sample, the lower thereported volatile matter will be. Crush analysis sample (see Annex A1) to pass a 0.250-mm opening (No. 60) sieve but do notovercrush. A 0.125-mm opening (No. 120) sieve s
18、hould retain 40 to 55 % of the sample. Do not obtain the analysis sample is byscalping and discarding a portion of the sample.6.2.2 Any segregation of particle sizes within the analysis sample shall be corrected by reblending the sample just prior toweighing the test sample.6.3 The furnace shall rec
19、over to 950 6 20C before the time limit is reached. If the furnace does not recover to the startingtemperature within a maximum of 10 min, reduce the number of samples being analyzed until recovery is achieved within 10 min(see Section 9).7. Apparatus7.1 Electric Muffle FurnaceCalibrated (Test Metho
20、d E220) and regulated to maintain a temperature of 950 6 20C (1742F),as measured by a thermocouple mounted inside the furnace. Its heat capacity shall be such that the initial temperature is regainedafter the introduction of a cold rack of samples within 10 min.7.2 Quartz Crucibles, self-sealing, 10
21、 mL capacity with covers.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 crushers that allow control over particle size without contamination areacceptable (see Annex A1).7.6 Balance, capable of weighi
22、ng 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 resistant material large enough to hold the crucible rack.8. Precautions8.1 Effusion of gaseous products, including soot and various hydrocarbons,
23、 and the increase of heat associated with the test canmake the use of a hood desirable.9. Furnace Calibration9.1 Avoiding segregation of particles, transfer1g(6 0.05 g) of an analysis sample (see Annex A1) to each crucible in the rack,weigh each crucible with its contents, and cover to the nearest 0
24、.1 mg. Place the cover on the crucible, and place in sample rack.9.2 Record the furnace temperature at equilibrium (9506 20C).9.3 Place the full rack of samples in the furnace, and start the timer.9.4 Monitor the furnace temperature. Record the elapsed time required to return to the equilibrium temp
25、erature recorded in 9.2.If the time exceeds 10 min, repeat the procedure, reducing the number of crucibles in the rack until temperature recovery iscompleted within 10 min of the introduction of the sample rack.9.5 When temperature recovery is achieved within the 10 min period, record the number of
26、crucibles in the rack. This numberof crucibles shall be in the rack for all future runs (fill empty spaces in the stand with empty crucibles when necessary).9.6 Round the recorded elapsed time to the next higher minute. This rounded time will be the analysis time for future runs (5min minimum).10. P
27、rocedure10.1 Ignite the quartz crucible and cover at 950 6 20C for 5 min periods to constant mass (60.5 mg). Do not cover the crucibleat this time to allow the carbon to burn off. Cool to ambient temperature in a desiccator before weighing the crucible and cover.NOTE 1Placing the empty crucibles in
28、the inverted cover when igniting will reduce breakage and chipping.10.2 Avoiding segregation of particles, transfer 1 g 610 mg of the analysis sample (see Annex A1) to the crucible, weigh thecrucible with its contents, and cover to the nearest 0.1 mg. Place the cover on the crucible, and place in sa
29、mple rack.10.3 Set the timer for the analysis time (5 to 10 min). Place the rack in the furnace. Start the timer.D6374 122NOTE 2Place the rack in the center of the furnace. Do not allow the rack to touch the walls of the furnace.10.4 After the analysis time (65 s), remove the rack from the furnace a
30、nd immediately place on a heat sink.10.5 Weigh the crucible after it has cooled to room temperature and before it has been at room temperature for longer than 20min.NOTE 3If cool down is not in a humidity controlled area, desiccation is required.11. Calculation11.1 Calculate the volatile matter of t
31、he moisture free prepared coke as follows:Volatile matter, mass % 5 A2B!/C! 3 100 (1)D6374-12_1where:A = weight of crucible and prepared sample prior to analysis, g,B = weight of crucible and prepared sample after analysis, g, andC = weight of prepared sample, g.12. Report12.1 Report to one decimal
32、the average of duplicate determinations that agree within 0.5 %. When this agreement is not met,the values are considered suspect and another duplicate set shall be run. Report the average of all results agreeing within 0.5 %.If the second set also fails to agree within 0.5 %, report the average of
33、all four values.13. Precision and Bias13.1 PrecisionThe precision of this test method as determined by the statistical examination of the interlaboratory test resultsis as follows:13.2 RepeatabilityThe difference between successive results obtained by the same operator with the same apparatus underc
34、onstant operating conditions on identical test materials would, in the long run, in the normal and correct operation of the testmethod, exceed the following values only one case in twenty.D6374-12_2where: X is the average of two results in weight percent.13.3 ReproducibilityThe difference between tw
35、o single and independent results obtained by different operators working indifferent laboratories on identical material will, in the long run, in normal and correct operation of the test method, exceed thefollowing values only in one case in twenty.D6374-12_3where: X is the average of two results in
36、 weight percent.13.4 BiasSince there is no accepted reference material for determining the bias for this test method for measuring the volatilematter in green petroleum coke, no statement on bias is being made.14. Keywords14.1 analysis time; green petroleum coke; volatile matterANNEX(Mandatory Infor
37、mation)A1. PREPARATION OF SAMPLESA1.1 Preparation of Bulk SampleA1.1.1 The bulk sample is prepared by reducing the gross sample in such a manner as to obtain a representative bulk sample.A1.1.2 The bulk sample can vary in weight from 22.7 to 90.6 kg (50 to 200 lb) and will vary in top particle size
38、from 6 to 75mm (14 to 3 in.), depending upon the particle size of the gross sample.A1.1.3 Air dry the bulk sample, if needed, so that it can be properly ground and fed through riffles. Air dry using drying pans38-mm (112-in.) deep made of noncorroding metal and of sufficient size that the sample may
39、 be spread to a depth of approximately25 mm (1.0 in.). The maximum depth of the sample shall be no more than twice the diameter of the largest particles. The roomshall be free of dust and excessive air currents. Avoid excessive drying time.A1.1.4 An air drying oven can be used to pass slightly heate
40、d air over the sample. The oven is to be capable of maintaininga temperature of 30 to 40C. Air changes should be at a rate of 1 to 4 min. Avoid over-heating and excessive drying.A1.1.5 A drying floor can be used to dry bulk samples. This is a smooth clean floor in a room free from dust and excessive
41、 aircurrent.D6374 123A1.1.6 Any modification of the above that will not overheat or contaminate the bulk sample is permitted.A1.1.7 After the bulk samples have been air dried, grind the entire sample to pass a 6.7 mm sieve, using a jaw crusher. Do notovergrind. Keep a maximum amount of sample as coa
42、rse as possible.A1.2 Preparation of Analysis SampleA1.2.1 Using a riffle, split the bulk sample to obtain a 700-g portion.A1.2.2 Pass the coke through the riffle from a feed scoop, feed bucket, or riffle pan length or opening equal to the full lengthof the riffle. When using any of the above contain
43、ers to feed the riffle, spread the coke evenly in the container, raise the container,and hold it with its front edge resting on the top of the feed trough; then slowly tilt it so that the coke flows in uniform streamsthrough the hopper straight down the chutes into the pans. Under no circumstances s
44、hovel the coke into the riffle or dribble thecoke into the riffle from a small mouth container. Make sure the riffle has a chute opening of at least 2 to 212 times greater thanthe top size particle of the coke being riffled.A1.2.3 Grind the sample to pass a 3.35-mm (No. 6) sieve using a roll crusher
45、 or other suitable crushing device that yields theresult 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 coarse particles to be crushed. This is called scalping.A1.2.5 Set the rolls gaps of the crusher far enough apart to crush only the largest p
46、articles of the sample. Turn the roll crusheron, and pour the coarse portion of the sample very slowly through the rolls. Once more scalp off the coarse particles that are tobe ground through the roll crusher again. Close the rollscrusher not more than 1.5 mm (116 in.) for each pass of the scalped s
47、ample.Repeat the crushing and scalping of the sample until all of the sample has passed through the 3.35-mm sieve. Make sure allparticles are well blended and none of the sample has been discarded.A1.2.6 Riffle the sample to obtain two 350-g portions. Do not discard any of the sample.A1.2.7 Using a
48、procedure analogous to A1.2.3, grind one of the 350-g samples in the roll crusherscrusher to pass a 0.250-mmsieve (No. 60). Do not overgrind.A1.2.8 About one half of the sample at this point shall be retained on a 0.125-mm sieve (No. 120). If this condition is not met,go back to A1.2.5, and grind th
49、e second 350-g portion. Adjust the roll crusher in smaller increments to increase the amount ofsample retained on the 0.125-mm sieve. Likewise, use large increments to decrease the amount of sample on the 0.125-mm sieve.A1.2.9 Recombine the 350-g sample, and dry it to constant weight at 95 to 105C. This dried sample is now ready for analysisand can be stored in a closed container within a dessicator. Samples shall be redried on the fourth day. Excessive heating can resultin higher volatile matter values because of oxidation of some cokes.SUMMARY OF
