1、Designation: D 5709 95 (Reapproved 2005)An American National StandardStandard Test Method forSieve Analysis of Petroleum Coke1This standard is issued under the fixed designation D 5709; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisio
2、n, 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 details a procedure for performingparticle size distribution analysis by dry sieve te
3、sting on greenpetroleum coke with a topsize of no more than 75 mm andcalcined petroleum coke with a topsize of no more than 25 mm.Size fractions go down to and include 4.75 mm for greenpetroleum coke and 75 m for calcined petroleum coke.NOTE 1To convert units, see Table 1 on nominal dimensions inSpe
4、cification E11. For example, 75 mm is approximately equivalent to anominal sieve opening of 3 in. and 25 mm to a nominal sieve opening of1 in. Likewise, 4.75 mm can be converted to approximately 0.187 in. and75 microns to 0.0029 in.1.2 The values stated in SI units are to be regarded as thestandard.
5、 The values given in parentheses are for informationonly. The sieve size is reported as U.S.A. standard test series inany units listed in Table 1 on nominal dimensions of Specifi-cation E11, or their commercial size equivalents.1.3 This standard does not purport to address all of thesafety concerns,
6、 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 Documents2.1 ASTM Standards:2D 346 Practice for Collection and Preparatio
7、n of CokeSamples for Laboratory AnalysisD 2013 Practice of Preparing Coal Samples for AnalysisD 2234 Test Methods for Collection of a Gross Sample ofCoalD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4749 Test Method for Performing the Sieve Analysis ofCoal and Designating C
8、oal SizeE11 Specification for Wire Cloth and Sieves for TestingPurposes3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 bulk samplethe reduced and divided representativeportion of the gross sample as prepared for shipment to andreceived by a laboratory, to be prepared for analy
9、sis.3.1.2 gross samplethe original, uncrushed, representativeportion taken from a shipment or lot of coke.3.1.3 lota quantity of coke to be represented by a grosssample.3.1.4 representative samplea sample collected in such amanner that every particle in the lot to be sampled is equallyrepresented in
10、 the gross sample.3.1.5 topsizethe size of the opening of that sieve of aseries with the smallest opening upon which is cumulativelyretained a total of less than 5 % of the sample. This definedtopsize is not to be confused with the size of the largest particlein a lot.4. Summary of Test Method4.1 A
11、representative coke sample is divided into ranges ofparticle size by the use of a series of square-holed sieves.5. Significance and Use5.1 The test method concerns the sieving of coke intodesignated size fractions for the purpose of characterizing thematerial as to its particle size distribution. It
12、 requires the use ofstandard sieves, standard sampling methods, standard samplepreparation methods, and a minimum initial sample mass basedon lot topsize. Suggestions are given for industry typical sievestacks for both green and calcined petroleum coke.5.2 Particle size distribution is significant i
13、n that manyphysical characteristics of a coke are related to such adistribution including bulk density and surface area. Nuisancecharacteristics, such as excessive fines in a lot, can also becontrolled.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubrica
14、nts and is the direct responsibility of SubcommitteeD02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved May 1, 2005. Published June 2005. Originallyapproved in 1995. Last previous edition approved in 2000 as D 570995(2000)e1.2For referenced ASTM standards, visi
15、t the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.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 19428-29
16、59, United States.5.3 Results from this test method are useful in determiningwhether a coke lot meets purchase specifications, for classifi-cation purposes, and for quality control. The results of this testmethod can also be used to predict the performance of aparticular lot of coke in a process.6.
17、Interferences6.1 A sieve analysis is very sensitive to the sieve cloth andsieve cloth-frame integrity. Minor separations of the sieve clothfrom the frame such as one broken sieve wire, and slightdistortions of sieve wires, can cause serious inaccuracies in thefinal results of a sieve analysis.6.2 Bl
18、inding of or a reduction in the number of openings ina sieve due to a collection of particles caught in the mesh canintroduce errors.6.3 Flooding or overloading of any sieve with particlesreduces the probability of any given particle encountering anopening in the sieve.7. Apparatus7.1 Sieves:7.1.1 S
19、ieves will be used in a descending size openingsequence, larger mesh openings above smaller.7.1.1.1 Typical sets of sieves to be used are listed in Table 1.NOTE 2Sets of sieves are often modified. Typically, specifications onsets of sieves are negotiated between the buyer and the seller. The actuals
20、equence used by the operator performing the analysis can vary. Forexample, intermediate sieves can be chosen to avoid sieve flooding and tomake the sieving operation more efficient. Table 1 on nominal dimensionsin Specification E11is to be used as a guide.7.1.2 A topsize sieve shall be used.7.1.3 Wi
21、re sieve cloth and frames used will conform toSpecification E11.7.1.4 Wire composition and types of frames must be sizedproperly for potential sieving operations. Stainless steel sievecloth is very resistant to distortion and preferred over softermetals.7.1.5 Collecting pans and sieve covers designe
22、d to fit thesieves are required.7.1.6 Check Specification E11for more details on standardsieves, service checks, and calibration.7.2 Sieve Shaker:7.2.1 Use a batch type sieve shaker.37.2.2 For sieving small quantities of coke or very fine coke(below 70 mesh), use a laboratory type sieving machine.48
23、. Sample Preparation8.1 A representative gross sample of the coke lot must becollected using appropriate procedures from Practice D 346,Test Methods D 2234, or Practice D 4057.(WarningThegross sample must not be crushed or reduced in topsize duringthe gross sample collection process or during subseq
24、uentdivisions of the sample.)8.2 The gross sample is divided into a smaller bulk samplefollowing guidelines in Test Methods D 2234. The bulk samplemust remain representative including no loss in topsize. Keep-ing in mind the initial sample mass requirements (see Table 2),the bulk sample must be at l
25、east twice the largest minimummass that you estimate will be required for the analysis.8.3 Upon delivery of the bulk sample to the laboratory, thesample shall be stored in a safe, dry location. Prevent any sizedegradation, loss of mass, or contamination of the sample untilneeded for the sieve analys
26、is.8.4 Immediately prior to the sieve analysis, examine thebulk sample determining whether it is dry and free flowing. Ifnot, use the air drying apparatus and drying procedure ofPractice D 2013.8.5 Determine the initial minimum test sample mass re-quired for the analysis from Table 2.8.6 Reduce the
27、bulk sample to the recommended minimumtest sample mass required using the division methods outlinedin Test Methods D 2234 or D 4749.3The sole source of supply of the model number TS-1 Gilson Testing Screenmachine known to the committee at this time is Gilson Company, Inc., P. O. Box677, Worthington,
28、 OH 43085-0677. If you are aware of alternative suppliers, pleaseprovide this information to ASTM International Headquarters. Your comments willreceive careful consideration at a meeting of the responsible technical committee,1which you may attend.4The sole source of supply of the Ro-Tap Testing Sie
29、ve Shaker known to thecommittee at this time is W. S. Tyler, Inc., 3200 Bessemer City Rd., P. O. Box 8900,Gastonia, NC 28053-9065. If you are aware of alternative suppliers, please providethis information to ASTM International Headquarters. Your comments will receivecareful consideration at a meetin
30、g of the responsible technical committee1, whichyou may attend.TABLE 1 Industry Typical SievesCalcined Petroleum Coke Green Petroleum Coke25.0 mm 25.0 mm19.0 mm 12.5 mm12.5mm 4.75mm4.75 mm 4.75 mm3.35 mm2.36 mm1.18 mm600 m300 m212 m150 m75 m75 mTABLE 2 Initial Minimum Test Sample Mass Requirements f
31、orSieve AnalysisTopsize Type of CokeInitial SampleMass Requirement,gExpectedRelativeError, %75 mm Green 50,000 650 mm Green 30,000 625 mm Green/Calcined 1,500 319 mm Green/Calcined 1,300 112.5 mm Green/Calcined 1,000 14.75 mm Green/Calcined 800 12.36 mm Green/Calcined 700 11.18 mm Green/Calcined 500
32、 1600 m Green/Calcined 300 1300 m Green/Calcined 100 1150 mAGreen/Calcined 50 1AFor topsize less than 150 m, use an initial sample mass requirement of 50 g.D 5709 95 (2005)29. Procedure9.1 Accurately weigh the minimum test sample mass (see8.6) before sieving with a precision equal to or better than0
33、.5 % of the fraction being weighed. This mass is Mi(initialtest sample mass).9.2 Start with the sieve having the largest required opening.9.3 All sieving is to be done using a batch type sieve shaker.NOTE 3It is recommended that coke 50 mm in diameter and larger behand sieved by the methods outlined
34、 in Test Method D 4749 rather thanattempting the use of a mechanical sieving device.9.4 Clean sieves prior to each use following the methodrecommended by the sieve manufacturer. If this information isunavailable, thoroughly brush the sieves using an appropriatebristle or soft metal brush. Do not dis
35、tort or damage sievesduring this process.9.5 Limit the portions of coke used for each sieving so thatall coke particles will be in direct contact with the mesh at thecompletion of sieving on each successive sieve.9.5.1 To determine the length of sieving time, refer to Table3 for an estimated startin
36、g point. Use a sample divider asdescribed in Practice D 2013 to form four subsamples from agross sample of a coke similar to that being tested. Sieve oneof these for the time given as an appropriate starting point, asecond for starting point plus 1 min, a third for starting pointplus 2 min, and a fo
37、urth for starting point plus 3 min. Tabulatethe results of these tests by the percentages retained on eachsieve (see Section 10), and the length of sieving time requiredto stabilize the sieving result without particle size degradationshould be readily apparent and can be established. If necessary,ke
38、ep adding additional minutes until the percentages are stable.9.6 Sieve until all portions of the sample are used. Combineall separately sieved material representing a particular sizefraction, but obtained from sieving separate portions of thesame sample.9.7 Continue sieving with successive sieves w
39、hich have thedesired size openings until the sieve having the smallestdesired size opening is used. Combine all the pan contents thathave passed through this smallest size opening and considerthese a particle size fraction.NOTE 4When larger particles are present that can physically affect thedimensi
40、onal stability of sieve openings or possibly damage the sieve cloth,use a cover sieve (protective sieve of a larger mesh) to keep coarseparticles off the surface of the finer sieve.9.8 Sieving can be done by grouping sieves having thedesired size openings, always stacking larger sieve openingsabove
41、smaller, thus accomplishing the sieving in fewer opera-tions. This is known as nesting sieves.9.9 Always use sieve covers and collecting pans to preventloss of fines and larger coke particles.9.10 Weigh each size fraction of sieved coke including thebottom pan size fraction with a precision equal to
42、 or better than0.5 % of the fraction being weighed. These masses are mf(finalsize fraction mass).9.11 Be aware that the objective of mechanically shakingsieves is to place all of the given particles of a given size on theappropriate sieve while avoiding size degradation of any ofthese particles. Lar
43、ger coke particles are especially susceptibleto particle degradation; avoid excessive sieving time (see9.5.1).10. Calculation10.1 Calculate the sum of the size fractions including panfraction (see 9.9) and call the sum Mf(combined final mass).10.1.1 Convert all masses to the same units before calcul
44、a-tion, that is, kilograms or grams.10.1.2 Convert and utilize the masses of the size fractionsby both multiplying and making proper use of significantfigures. For example, if a size fraction weighed 11.25 kganother 204 g, and another 148 g, determine all the masses tothe nearest 0.01 kg (since 11.2
45、5 kg is reported to the nearest0.01 kg) before proceeding with calculations, as follows:(1)11.25 kg0.20 kg0.15 kg11.60 kg10.2 If the percentage mass loss or gain is over 1 %, rejectthe analysis and make another test. The formula for thecalculation of the percentage mass loss or gain is as follows:%
46、M 5Mf2 Mi!100Mi(2)where:Mf= combined final mass (10.1), g or kg,Mi= initial test sample mass (9.1), g or kg, and%M = % mass loss or gain upon sieving, g or kg.A mass gain will result in a positive percent while a massloss will result in a negative percent.10.2.1 If the variation is greater than the
47、above tolerance of1 %, recheck the figures for possible errors in determiningmass, calculating, blinding of the sieve openings, or accidentalspillage. If a calculation, transcription, or other error isdetected and correctable, correct the error. If the resultingvariation from initial sample weight i
48、s within the 1 % toler-ance, accept and report the corrected results. If the source oferror is not detected, or if it is detected but uncorrectable,repeat the test.10.3 Convert the mass mf(see 9.8) of an individual sizefraction to a percentage basis by dividing the mass of thatportion by the combine
49、d final mass Mf, or by the initial testsample mass Mias follows:%m5MfMforMi* 100 (3)where:mf= final size fraction mass (9.9), g or kg,Mf= combined final mass (10.1), g or kg,TABLE 3 Suggested Starting Points for Sieving TimeTime, min Size of Coke, mm5 coarse (greater than 12.5)10 medium (1.18 to 12.5)15 fine (less than 1.18)D 5709 95 (2005)3Mi= initial test sample mass (9.1), g or kg, and% m = % mass of size fraction, g or kg.Calculate each mass % to the nearest 0.01 % and then roundto the nearest 0.1 %.10.3.1 The sum of the fractional masses, rather than the
