1、Designation: D 6969 03An American National StandardStandard Practice forPreparation of Calcined Petroleum Coke Samples forAnalysis1This standard is issued under the fixed designation D 6969; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re
2、vision, 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 practice covers the preparation procedures neces-sary for the reduction and division of calc
3、ined petroleum cokesamples in order to generate appropriate analytical samplesupon which physical and chemical analytical tests will beperformed.1.2 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 stand
4、ard 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 1552 Test Method for Sulfur in Petroleum Products(High-Temperature Method)D 2638 Test Method of Real Density of Calcined Petr
5、oleumCoke by Helium PycnometerD 4292 Test Method of Determination for Vibrated BulkDensity of Calcined Petroleum CokeD 4422 Test Method of Ash in the Analysis of PetroleumCokeD 4930 Test Method for Dust Control Material on CalcinedPetroleum CokeD 4931 Test Method for Gross Moisture in Green Petro-le
6、um CokeD 5004 Test Method of Real Density for Calcined Petro-leum Coke, Xylene DisplacementD 5056 Test Method for Trace Metals in Petroleum Coke byAtomic AbsorptionD 5187 Test Method for Determination of Crystallite Size(Lc) of Calcined Petroleum Coke by X-Ray DiffractionD 5600 Test Method for Trace
7、 Metals in Petroleum Coke byInductively Coupled Plasma Atomic Emission Spectrom-etry (ICP-AES)D 5709 Test Method for Sieve Analysis of Petroleum CokeD 6376 Test Method for Determination of Trace Metals inPetroleum Coke by Wavelength Dispersive X-ray Fluores-cence Spectroscopy3. Terminology3.1 Defini
8、tions:3.1.1 analysis samplethe reduced and divided representa-tive portion of the bulk sample, prepared for use in thelaboratory.3.1.2 composite samplea sample, representative of anentire consignment of calcined petroleum coke, generated bymixing portions of gross samples from different lots togethe
9、r inmass fractions proportioned to the consignment.3.1.3 gross samplethe original, uncrushed representativeportion taken from a shipment or lot of coke.3.1.4 intermediate samplea sample, representative of agross sample, upon which no analysis is to be performed, yetrequired for generation of analysi
10、s samples after undergoingfurther division and reduction.3.1.5 lota quantity of calcined petroleum coke to berepresented by a gross sample.3.1.6 rifflea manual sample divider which splits thesample stream into a number of alternate elements.3.1.7 sample divisionthe process whereby a sample isreduced
11、 in mass without change in particle size.1This practice is under the jurisdiction of ASTM Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.05 onProperties of Fuels, Petroleum Coke and Carbon MaterialCurrent edition approved Nov. 1, 2003. Publishe
12、d December 2003.2For referenced ASTM standards, visit 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 Harbo
13、r Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.8 sample preparationthe process that may includedrying, crushing, division, and mixing of a gross sample for thepurpose of obtaining an unbiased analysis sample.3.1.9 sample reductionthe process whereby a sample isreduced in p
14、article size by crushing or grinding withoutsignificant change in chemical properties.3.1.10 top sizethe 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 lar
15、gest 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 that the resultingprepared analysis samples are more uniform from laboratory tolaboratory.
16、Adherence to these guidelines is expected to pro-vide significant reduction in inter-laboratory variability.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 analyti
17、calsample 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.5.1.2 Exercise care in the division operation to preserve theparticle size distribution of th
18、e 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. Enclosed riffles are recommended to minimize dustingand loss of sample.5.2 Subsequent Redu
19、ction 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 beperformed on a number 60 mesh analysis sample, a ring andpuck mill with tungsten carbide grinding
20、 components isrecommended to minimize the metallic impurities of analyticalinterest that 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 a
21、ctual test methods for size and mass ofsamples required for analysis.5.4 Removal of dedusting oil may be required for analyticalpurposes and for subsequent analyses such as real density orporosity. Oil may be extracted and quantified by Test MethodD 4931 or thermally removed.5.5 Mixing of gross samp
22、les to generate a composite samplerepresenting more than one lot is frequently required. Mixingmust 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 weighin
23、g no less than 1.5 kg such that each interme-diate sample is still representative for sizing determination byTest Method D 5709.5.5.2 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
24、cargo repre-sented by a 10 kg vessel composite sample is illustrated inTable 1. To calculate 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.
25、5.3 Adjust the mass of the intermediate sample to within2 % of the target mass contribution 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;
26、sample division; samplepreparation; sample reductionTABLE 1 Example of Mixing Gross Samples to Generate a Weighted Average Vessel Composite SampleLot 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
27、 sample mass mixed intocomposite (grams)1426 6 29 1371 6 27 1499 6 30 1371 6 27 1463 6 29 1426 6 29 1444 6 29 10 000 6 200D6969032ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard a
28、re 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 any time by the responsible technical committee and must be reviewed every five years andif not
29、 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 y
30、ou 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 ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,Unite
31、d 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); or through the ASTM website(www.astm.org).NOTEThe tasks outlined in this figure are not necessarily required for analysis.FIG. 1 Preparation of Calcined Petroleum CokeD6969033
