1、Designation: D6969 03 (Reapproved 2008)D6969 15Standard 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 revisio
2、n, 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. Scope Scope*1.1 This practice covers the preparation procedures necessary for the reduction and division of calc
3、ined petroleum coke samplesin order to generate appropriate analytical samples upon which physical and chemical analytical tests will be performed.1.2 The values stated in either SI units or inch-pound units are to be regarded as standard. No other units of measurement areincluded in this separately
4、 as standard. The values stated in each system may not be exact equivalents; therefore, each system shallbe used independently of the other. Combining values from the two systems may result in non-conformance with the standard.1.3 This standard does not purport to address all of the safety concerns,
5、 if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1552 Test Method for Sulfur in Petroleum Produ
6、cts by High Temperature Combustion and IR DetectionD2638 Test Method for Real Density of Calcined Petroleum Coke by Helium PycnometerD4292 Test Method for Determination of Vibrated Bulk Density of Calcined Petroleum CokeD4422 Test Method for Ash in Analysis of Petroleum CokeD4930 Test Method for Dus
7、t Control Material on Calcined Petroleum CokeD4931 Test Method for Gross Moisture in Green Petroleum CokeD5004 Test Method for Real Density of Calcined Petroleum Coke by Xylene DisplacementD5056 Test Method for Trace Metals in Petroleum Coke by Atomic AbsorptionD5187 Test Method for Determination of
8、 Crystallite Size (Lc of Calcined Petroleum Coke by X-Ray DiffractionD5600 Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry(ICP-AES)D5709 Test Method for Sieve Analysis of Petroleum CokeD6376 Test Method for Determination of Trace Metals in Pe
9、troleum Coke by Wavelength Dispersive X-ray FluorescenceSpectroscopy3. Terminology3.1 Definitions:3.1.1 analysis samplesample, nthe reduced and divided representative portion of the bulk sample, prepared for use in thelaboratory.3.1.2 composite samplesample, na sample, representative of an entire co
10、nsignment of calcined petroleum coke, generatedby mixing portions of gross samples from different lots together in mass fractions proportioned to the consignment.3.1.3 gross samplesample, nthe original, uncrushed representative portion taken from a shipment or lot of coke.1 This practice is under th
11、e jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon MaterialCurrent edition approved Oct. 15, 2008June 1, 2015. Published December 2008September 2015
12、. Originally approved in 2003. Last previous edition approved in 20032008as D6969D6969 03 (2008).03. DOI: 10.1520/D6969-03R08.10.1520/D6969-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. ForAnnual Book ofASTM Standardsvolum
13、e information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequa
14、tely depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM In
15、ternational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.4 intermediate samplesample, na sample, representative of a gross sample, upon which no analysis is to be performed,yet required for generation of analysis samples after undergoing further division a
16、nd reduction.3.1.5 lotlot, na quantity of calcined petroleum coke to be represented by a gross sample.3.1.6 riffleriffle, na manual sample divider which splits the sample stream into a number of alternate elements.3.1.7 sample divisiondivision, nthe process whereby a sample is reduced in mass withou
17、t change in particle size.3.1.8 sample preparationpreparation, nthe process that may include drying, crushing, division, and mixing of a grosssample for the purpose of obtaining an unbiased analysis sample.3.1.9 sample reductionreduction, nthe process whereby a sample is reduced in particle size by
18、crushing or grinding withoutsignificant change in chemical properties.3.1.10 top sizesize, nthe size of the smallest opening of one sieve of a series upon which is cumulatively retained a totalof less than 5 % of the sample. This defined top size is not to be confused with the size of the largest pa
19、rticle in a lot.4. Significance and Use4.1 This practice provides field personnel and laboratories with standard procedures for dividing, reducing, and mixing grosssamples and intermediate samples, such that the resulting prepared analysis samples are more uniform from laboratory tolaboratory. Adher
20、ence to these guidelines is expected to provide significant reduction in interlaboratory variability.5. Organization of Sample Preparation5.1 Initial Division of Gross Sample : Sample:5.1.1 Determine the required analyses for the lot and manage the division steps accordingly to achieve enough analyt
21、ical sampleto perform all required analyses in duplicate (see flowchart in Fig. 1 as an example). Divide the gross sample by use of a riffle orrotary sample divider to an intermediate sample of sufficient mass.5.1.2 Exercise care in the division operation to preserve the particle size distribution o
22、f the gross sample. Riffle openings mustbe at least three times the top size of the calcined petroleum coke being divided. A feed hopper or vibratory feeder, or both, arerecommended to feed the coke into the riffle. Enclosed riffles are recommended to minimize dusting and loss of sample.5.2 Subseque
23、nt Reduction and Division : Division:5.2.1 Crushing processes are to be carried out such that the apparatus does not contribute significant impurities into the analysissample. For example, if trace metal analyses are to be performed on a number 60 mesh analysis sample, a ring and puck mill withtungs
24、ten carbide grinding components is recommended to minimize the metallic impurities of analytical interest that may be addedto sample.5.2.2 If trace metals are not required for testing on a number 60 mesh analysis sample, a bench-top hammer mill or ball millare adequate for performing the grinding op
25、eration.5.3 Refer to actual test methods for size and mass of samples required for analysis.5.4 Removal of dedusting oil may be required for analytical purposes and for subsequent analyses such as real density orporosity. Oil may be extracted and quantified by Test Method D4931D4930 or thermally rem
26、oved.5.5 Mixing of gross samples to generate a composite sample representing more than one lot is frequently required. Mixing mustbe planned such that the final composite sample has a mass of no less than 10 kg so that all the required analyses may be performed.5.5.1 Divide each gross sample down in
27、to an intermediate sample weighing no less than 1.5 kg such that each intermediatesample is still representative for sizing determination by Test Method D5709.5.5.2 Each lot sample will be proportionately represented in the composite, as the lot tonnage was representative of the totalcargo. An examp
28、le of a large seven-hold vessel cargo represented by a 10 kg vessel composite sample is illustrated in Table 1. Tocalculate the individual target sample mass, use the following formula:target sample mass5AB 3C (1)where:A = mass of individual lot in tons,B = mass of total vessel in tons, andC = mass
29、of composite sample in grams.5.5.3 Adjust the mass of the intermediate sample to within 2 % of the target mass contribution to the composite sample byremoving material from the intermediate sample. Use appropriate means to preserve the particle size distribution of the originalgross sample.6. Keywor
30、ds6.1 calcined petroleum coke; sample division; sample preparation; sample reductionD6969 152NOTE 1The tasks outlined in this figure are not necessarily required for analysis.FIG. 1 Preparation of Calcined Petroleum CokeTABLE 1 Example of Mixing Gross Samples to Generate a Weighted Average Vessel Co
31、mposite SampleNOTE 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 3
32、Hold 3Lot 4Hold 4Lot 5Hold 5Lot 6Hold 6Lot 7Hold 7 TotalLot 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 153SUMMARY OF CHANGESSubcommittee D02.05 has identified the
33、location of selected changes to this standard since the last issue(D6969 03 (2008) that may impact the use of this standard. (Approved June 1, 2015.)(1) Added Note 1 to Table 1.(2) Revised reference in 5.4.(3) Units information in 1.2 was revised.ASTM International takes no position respecting the v
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36、arters. Your comments 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 stand
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