1、Designation: D6969 16Standard 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 IR DetectionD2638 Test Method for Real Density of Calcined P
6、etroleumCoke 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 CokeD4931 Test Method for Gross Moisture in Green PetroleumCo
7、keD5004 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 X-Ray DiffractionD5600 Test Method for Trace Metals i
8、n 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-rescence Spectroscopy3. Terminology3.1 Definitions:3.1.1
9、 analysis sample, nthe reduced and divided represen-tative portion of the bulk sample, prepared for use in thelaboratory.3.1.2 composite sample, na sample, representative of anentire consignment of calcined petroleum coke, generated bymixing portions of gross samples from different lots together inm
10、ass fractions proportioned to the consignment.3.1.3 gross sample, nthe original, uncrushed representa-tive portion taken from a 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 anal
11、ysis samples after undergoingfurther division and reduction.3.1.5 lot, na quantity of calcined petroleum coke to berepresented by 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 samp
12、le isreduced in mass without change in particle size.3.1.8 sample preparation, nthe process that may includedrying, crushing, division, and mixing of a gross sample for thepurpose of obtaining an unbiased analysis sample.3.1.9 sample reduction, nthe process whereby a sample isreduced in particle siz
13、e by crushing or grinding withoutsignificant change in chemical properties.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 Coke and Carbon Mate
14、rialCurrent edition approved June 1, 2016. Published July 2016. Originally approvedin 2003. Last previous edition approved in 2015 as D6969 15. DOI: 10.1520/D6969-16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual B
15、ook 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 States13.1.10 top size,
16、 nthe size of the smallest opening of onesieve of a series upon which is cumulatively retained a total ofless 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 labora
17、torieswith standard procedures for dividing, reducing, and mixinggross samples and intermediate samples, such that the resultingprepared analysis samples are more uniform from laboratory tolaboratory. Adherence to these guidelines is expected to pro-vide significant reduction in interlaboratory vari
18、ability.5. Organization of Sample Preparation5.1 Initial Division of Gross Sample:5.1.1 Determine the required 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). Divi
19、de the gross sample byuse of a riffle or rotary sample divider to an intermediatesample of sufficient mass.5.1.2 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 co
20、ke being divided. A feed hopper or vibratoryfeeder, or both, are recommended to feed the coke into theriffle. Enclosed riffles are recommended to minimize dustingand loss of sample.5.2 Subsequent Reduction and Division:NOTE 1The tasks outlined in this figure are not necessarily required for analysis
21、.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 0.002205.FIG. 1 Preparation of Calcined Petroleum CokeD6969 1625.2.1 Crushing processes are to be carried out such that theapparatus
22、does not contribute significant impurities into theanalysis sample. For example, if trace metal analyses are to beperformed on a number 60 mesh analysis sample, a ring andpuck mill with tungsten carbide grinding components isrecommended to minimize the metallic impurities of analyticalinterest that
23、may be added to sample.5.2.2 If trace metals are not required 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 dedus
24、ting oil may be required for analyticalpurposes and for 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. M
25、ixingmust be planned such that the final composite sample 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 sizi
26、ng determination byTest Method D5709.5.5.2 Each lot sample 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 calculat
27、e the individual target sample mass, use thefollowing 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
28、 to the composite sample byremoving material from the 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 h
29、as identified the location of selected changes to this standard since the last issue(D6969 15) that may impact the use of this standard. (Approved June 1, 2016.)(1) Note about kilogram/gram to pound conversion added toFig. 1.ASTM International takes no position respecting the validity of any patent
30、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 infringement of such rights, are entirely their own responsibility.This standard is subject to revision at
31、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
32、 will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by
33、 ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail)
34、; or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 1 Example of Mixing Gross Samples to Generate a Weighted Average Vessel Composite Sample
35、NOTE 1Table 1 is based on the Lot Tonnage in short ton (2000 lb). To convert from short 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 8000 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 163
