1、Designation: D6969 17Standard Practice forPreparation of Calcined Petroleum Coke Samples forAnalysis1This standard is issued under the fixed designation D6969; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisi
2、on. 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 practice covers the preparation procedures neces-sary for the reduction and division of calcined petroleum cokesamples in o
3、rder to generate appropriate analytical samplesupon which physical and chemical analytical tests will beperformed.1.2 The values stated in either SI units or inch-pound unitsare to be regarded separately as standard. The values stated ineach system may not be exact equivalents; therefore, eachsystem
4、 shall be used independently of the other. Combiningvalues from the two systems may result in non-conformancewith the standard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish a
5、ppro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1552 Test Method for Sulfur in Petroleum Products byHigh Temperature Combustion and Infrared (IR) Detec-tion or Thermal Conducitivity Detection
6、(TCD)D2638 Test Method for Real Density of Calcined PetroleumCoke by Helium PycnometerD4292 Test Method for Determination of Vibrated BulkDensity of Calcined Petroleum CokeD4422 Test Method for Ash in Analysis of Petroleum CokeD4930 Test Method for Dust Control Material on CalcinedPetroleum CokeD493
7、1 Test Method for Gross Moisture in Green PetroleumCokeD5004 Test Method for Real Density of Calcined PetroleumCoke by Xylene DisplacementD5056 Test Method for Trace Metals in Petroleum Coke byAtomic AbsorptionD5187 Test Method for Determination of Crystallite Size(Lc) of Calcined Petroleum Coke by
8、X-Ray DiffractionD5600 Test Method for Trace Metals in Petroleum Coke byInductively Coupled Plasma Atomic Emission Spectrom-etry (ICP-AES)D5709 Test Method for Sieve Analysis of Petroleum CokeD6376 Test Method for Determination of Trace Metals inPetroleum Coke by Wavelength Dispersive X-ray Fluo-res
9、cence SpectroscopyD7454 Test Method for Determination of Vibrated BulkDensity of Calcined Petroleum Coke using a Semi-Automated Apparatus3. Terminology3.1 Definitions:3.1.1 analysis sample, nthe reduced and divided represen-tative portion of the bulk sample, prepared for use in thelaboratory.3.1.2 c
10、omposite sample, na sample, representative of anentire consignment of calcined petroleum coke, generated bymixing portions of gross samples from different lots together inmass fractions proportioned to the consignment.3.1.3 gross sample, nthe original, uncrushed representa-tive portion taken from a
11、shipment or lot of coke.3.1.4 intermediate sample, na sample, representative of agross sample, upon which no analysis is to be performed, yetrequired for generation of analysis samples after undergoingfurther division and reduction.3.1.5 lot, na quantity of calcined petroleum coke to berepresented b
12、y a gross sample.3.1.6 riffle, na manual sample divider which splits thesample stream into a number of alternate elements.3.1.7 sample division, nthe process whereby a sample isreduced in mass without change in particle size.3.1.8 sample preparation, nthe process that may includedrying, crushing, di
13、vision, and mixing of a gross sample for thepurpose of obtaining an unbiased analysis sample.1This practice is under the jurisdiction of ASTM Committee D02 on PetroleumProducts, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-mittee D02.05 on Properties of Fuels, Petroleum Co
14、ke and Carbon MaterialCurrent edition approved Jan. 1, 2017. Published January 2017. Originallyapproved in 2003. Last previous edition approved in 2016 as D6969 16. DOI:10.1520/D6969-17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceas
15、tm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United Sta
16、tesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Tr
17、ade (TBT) Committee.13.1.9 sample reduction, nthe process whereby a sample isreduced in particle size by crushing or grinding withoutsignificant change in chemical properties.3.1.10 top size, nthe size of the smallest opening of onesieve of a series upon which is cumulatively retained a total ofless
18、 than 5 % of the sample. This defined top size is not to beconfused with the size of the largest particle in a lot.4. Significance and Use4.1 This practice provides field personnel and laboratorieswith standard procedures for dividing, reducing, and mixinggross samples and intermediate samples, such
19、 that the resultingprepared analysis samples are more uniform from laboratory tolaboratory. Adherence to these guidelines is expected to pro-vide significant reduction in interlaboratory variability.5. Organization of Sample Preparation5.1 Initial Division of Gross Sample:5.1.1 Determine the require
20、d analyses for the lot and man-age the division steps accordingly to achieve enough analyticalsample to perform all required analyses in duplicate (seeflowchart in Fig. 1 as an example). Divide the gross sample byuse of a riffle or rotary sample divider to an intermediatesample of sufficient mass.5.
21、1.2 Exercise care in the division operation to preserve theparticle size distribution of the gross sample. Riffle openingsmust be at least three times the top size of the calcinedpetroleum coke being divided. A feed hopper or vibratoryfeeder, or both, are recommended to feed the coke into theriffle.
22、 Enclosed riffles are recommended to minimize dustingand loss of sample.5.2 Subsequent Reduction and Division:5.2.1 Crushing processes are to be carried out such that theapparatus does not contribute significant impurities into theanalysis sample. For example, if trace metal analyses are to beperfor
23、med on a number 60 mesh analysis sample, a ring andNOTE 1The tasks outlined in this figure are not necessarily required for analysis.NOTE 2Fig. 1 is based on kilogram (kg) and gram (g). To convert from kilogram (kg) to pound (lbm), multiply by 2.205. To convert from gram topound (lbm), multiply by 0
24、.002205. To convert from millimeters to inches, divide by 25.4.FIG. 1 Preparation of Calcined Petroleum CokeD6969 172puck mill with tungsten carbide grinding components isrecommended to minimize the metallic impurities of analyticalinterest that may be added to sample.5.2.2 If trace metals are not r
25、equired for testing on a number60 mesh analysis sample, a bench-top hammer mill or ball millare adequate for performing the grinding operation.5.3 Refer to actual test methods for size and mass ofsamples required for analysis.5.4 Removal of dedusting oil may be required for analyticalpurposes and fo
26、r subsequent analyses such as real density orporosity. Oil may be extracted and quantified by Test MethodD4930 or thermally removed.5.5 Mixing of gross samples to generate a composite samplerepresenting more than one lot is frequently required. Mixingmust be planned such that the final composite sam
27、ple has amass of no less than 10 kg so that all the required analyses maybe performed.5.5.1 Divide each gross sample down into an intermediatesample weighing no less than 1.5 kg such that each interme-diate sample is still representative for sizing determination byTest Method D5709.5.5.2 Each lot sa
28、mple will be proportionately represented inthe composite, as the lot tonnage was representative of the totalcargo. An example of a large seven-hold vessel cargo repre-sented by a 10 kg vessel composite sample is illustrated inTable 1. To calculate the individual target sample mass, use thefollowing
29、formula:target sample mass 5AB3 C (1)where:A = mass of individual lot in tons,B = mass of total vessel in tons, andC = mass of composite sample in grams.5.5.3 Adjust the mass of the intermediate sample to within2 % of the target mass contribution to the composite sample byremoving material from the
30、intermediate sample. Use appro-priate means to preserve the particle size distribution of theoriginal gross sample.6. Keywords6.1 calcined petroleum coke; sample division; samplepreparation; sample reductionSUMMARY OF CHANGESSubcommittee D02.05 has identified the location of selected changes to this
31、 standard since the last issue(D6969 16) that may impact the use of this standard. (Approved Jan. 1, 2017.)(1) Added Test Method D7454 to Referenced Documents andto Fig. 1.Subcommittee D02.05 has identified the location of selected changes to this standard since the last issue(D6969 15) that may imp
32、act the use of this standard. (Approved June 1, 2016.)(1) Note about kilogram/gram to pound conversion added toFig. 1.TABLE 1 Example of Mixing Gross Samples to Generate a Weighted Average Vessel Composite SampleNOTE 1Table 1 is based on the Lot Tonnage in short ton (2000 lb). To convert from short
33、ton (2000 lb) to metric ton, multiply by 0.9072. A metricton is equal to 1000 kilogram (kg). To convert from short ton (2000 lb) to long ton (2240 lb), multiply by 0.8929.Lot 1Hold 1Lot 2Hold 2Lot 3Hold 3Lot 4Hold 4Lot 5Hold 5Lot 6Hold 6Lot 7Hold 7TotalLot tonnage (short tons) 7800 7500 8200 7500 80
34、00 7800 7900 54 700Target sample mass mixed intocomposite (grams)1426 29 1371 27 1499 30 1371 27 1463 29 1426 29 1444 29 10 000 200D6969 173ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this
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