1、Designation: D 6969 03 (Reapproved 2008)An 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,
2、 in 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. Scope1.1 This practice covers the preparation procedures neces-sary for the reduction and
3、 division of calcined petroleum cokesamples in order to generate appropriate analytical samplesupon which physical and chemical analytical tests will beperformed.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This stand
4、ard 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 appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 AS
5、TM Standards:2D 1552 Test Method for Sulfur in Petroleum Products(High-Temperature Method)D 2638 Test Method for Real Density of Calcined Petro-leum Coke by Helium PycnometerD 4292 Test Method for Determination of Vibrated BulkDensity of Calcined Petroleum CokeD 4422 Test Method forAsh inAnalysis of
6、 Petroleum CokeD 4930 Test Method for Dust Control Material on CalcinedPetroleum CokeD 4931 Test Method for Gross Moisture in Green Petro-leum CokeD 5004 Test Method for Real Density of Calcined Petro-leum Coke by Xylene DisplacementD 5056 Test Method for Trace Metals in Petroleum Coke byAtomic Abso
7、rptionD 5187 Test Method for Determination of Crystallite Size(Lcof Calcined Petroleum Coke by X-Ray DiffractionD 5600 Test Method for Trace 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
8、 Method for Determination of Trace Metals inPetroleum Coke by Wavelength Dispersive X-ray Fluores-cence Spectroscopy3. Terminology3.1 Definitions: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,
9、 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 samplethe original, uncrushed representativeportion taken from a shipment or lot of coke.3.1.4 in
10、termediate samplea 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 lota quantity of calcined petroleum coke to berepresented by a gross sample.3.1.6 rifflea manual
11、sample divider which splits thesample stream into a number of alternate elements.3.1.7 sample divisionthe process whereby a sample isreduced in mass without change in particle size.3.1.8 sample preparationthe process that may includedrying, crushing, division, and mixing of a gross sample for thepur
12、pose of obtaining an unbiased analysis sample.3.1.9 sample reductionthe process whereby a sample isreduced in particle 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 reta
13、ined 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.1This practice is under the jurisdiction of ASTM Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.05 onPropertie
14、s of Fuels, Petroleum Coke and Carbon MaterialCurrent edition approved Oct. 15, 2008. Published December 2008. Originallyapproved in 2003. Last previous edition approved in 2003 as D 696903.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at servi
15、ceastm.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 19428-2959, United States.4. Significance and Use4.1 This practice provides field
16、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. Adherence to these guidelines is expected to pro-vide significant reduction in
17、interlaboratory 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 analyticalsample to perform all required analyses in duplicate (seeflowchart in Fig. 1
18、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 the gross sample. Riffle openingsmust be at least three times the top size of the
19、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 Reduction and Division:5.2.1 Crushing processes are to be carried out such that thea
20、pparatus 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 analyticalinter
21、est 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 actual test methods for size and mass ofsamples required for analysis.NOTEThe tas
22、ks outlined in this figure are not necessarily required for analysis.FIG. 1 Preparation of Calcined Petroleum CokeD 6969 03 (2008)25.4 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 T
23、est MethodD 4931 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 sample has amass of no less than 10 kg so that all the required analyses maybe performed.5.5.1 Di
24、vide 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 D 5709.5.5.2 Each lot sample will be proportionately represented inthe composite, as the lot tonnage was representati
25、ve 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 formula:target sample mass 5AB3 C (1)where:A = mass of individual lot in tons,B = mass of tot
26、al 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 intermediate sample. Use appro-priate means to preserve the particle size distribution of the
27、original gross sample.6. Keywords6.1 calcined petroleum coke; sample division; samplepreparation; sample reductionASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly adv
28、ised 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 revised, either
29、 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 you may attend. I
30、f 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,United States. Indivi
31、dual 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).TABLE 1 Example of Mixing Gross Samples to Generate a Weighted Aver
32、age 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 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 200D 6969 03 (2008)3
