1、Designation: D8097 17Standard Test Method forDetermination of Bulk Density for Specific Size Fractions ofCalcined Petroleum Coke Using a Transaxial PressurePycnometer1This standard is issued under the fixed designation D8097; the number immediately following the designation indicates the year oforig
2、inal adoption or, 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 The test method covers the determination of bulkdensity for a s
3、pecific size fraction of calcined petroleum cokeusing an automated pycnometer that compacts coke by apply-ing transaxial pressure under a controlled force.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 standard doe
4、s 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 ASTM Stan
5、dards:2D6969 Practice for Preparation of Calcined Petroleum CokeSamples for AnalysisD6970 Practice for Collection of Calcined Petroleum CokeSamples for AnalysisE11 Specification for Woven Wire Test Sieve Cloth and TestSievesE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE69
6、1 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 Definitions:3.1.1 bulk density, nof coke, the ratio of the mass of acollection of particles of a specified size range to the volumeoccupied.3.1.2 transaxial pressure, npressure applied acro
7、ss a hori-zontal axis.4. Summary of Test Method4.1 A representative sample of calcined petroleum coke iscollected and then screened using Specification E11 sieves(8 mm, 4 mm, 2 mm, 1 mm, 0.5 mm, 0.25 mm) into fractions.Each specific size fraction is then weighed and the bulk volumeis measured using
8、the pycnometer. This test method measuresthe bulk volume by controlling the consolidation force andmeasuring the displacement of a plunger used to compact thebed of coke.5. Significance and Use5.1 The bulk density is an indicator of calcined petroleumcoke porosity and packing capability which is an
9、importantcoke property for anode production in aluminum industry. Thisprocedure will allow an automated measurement of specificsized fractions ranging from 8 mm to 0.25 mm coke particles.5.2 Results from this test method are used in determiningcoke specifications, classification purposes, and for qu
10、alitycontrol.6. Apparatus6.1 Balance, capable of measuring 100 g 6 0.0001 g.6.2 Table Top Riffler:6.2.1 Pycnometer, equipped with a force transducer andsuitable 50.8 mm (2 in.) or larger glass chamber and plungerassembly.NOTE 1GeoPyc 13603has been successfully used for this analysis.6.3 Wire Mesh Si
11、eves, 8 in. diameter, round, 8.00 mm(516 in.), 4.00 mm (No. 5), 2.00 mm (No. 10), 1.00 mm (No.18), 0.50 mm (No. 35), 0.25 mm (No. 60), pan, and cover.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility
12、ofSubcommittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved Jan. 1, 2017. Published March 2017. DOI: 10.1520/D8097-17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Boo
13、k of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The sole source of supply of the apparatus known to the committee at this timeis Micromeritics Instrument Corporation, 4356 Communications Dr., Norcross, GA30093, USA. If you are aware of alternat
14、ive suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-295
15、9. United StatesThis 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 B
16、arriers to Trade (TBT) Committee.16.4 Ro-tap Sieve Shaker, for 8 in. diameter sieves.7. Sampling, Test Specimens, and Test Units7.1 Grab a representative sample according to PracticeD6970 and reduce the sample to 900 g 6 100 g followingPractice D6969.7.2 Sieve the representative sample using the fol
17、lowingscreens: 8.00 mm (516 in.), 4.00 mm (No. 5), 2.00 mm (No.10), 1.00 mm (No. 18), 0.50 mm (No. 35), and 0.25 mm (No.60).7.3 Using a sieve shaker, shake the sieves for 10 min.7.4 Discard of the top sieve material (516 in. (8.00 mm) andtransfer each sized fraction of calcined petroleum coke intoap
18、propriate containers.8. Preparation of Apparatus8.1 Follow manufacturers instructions for initial assembly,conditioning, and preparation of pycnometer.9. Calibration and Standardization9.1 Follow the instructions for the equipment used.9.2 A blank data set can be performed by following theprocedure
19、based upon the equipment used. If the GeoPyc (seeNote 1) is used, follow detail in Annex A1 and Table 1.9.3 A blank data set shall be performed each time a newcylinder is used or when the apparatus is moved.10. Procedure10.1 Split the sieved sample fraction to a test specimen of52 g 6 2g.10.2 Weigh
20、the prepared test specimen to 0.0001 g andrecord the weight.10.3 Pour the entire test specimen into the glass chamberand insert PTFE plunger.10.4 Fit the chamber and plunger assembly onto the pyc-nometer.10.5 Start the analysis following the procedure in theinstruction manual.10.6 Enter the necessar
21、y or required information such assample identification, sample mass, or other user-selectedinformation.10.7 Choose the stored blank data set for the analysis.10.8 Press “Enter.” The analysis will begin and will beperformed automatically.10.9 Record the final volume or density when pycnometerhas fini
22、shed analyzing the test specimen. You may also print acopy of the report if a printer is attached.11. Calculation or Interpretation of Results11.1 The pycnometer measures the volume of each consoli-dation cycle and then averages the results of all the runs. Theaverage volume and specimen weight are
23、used to calculate thespecimen bulk density. The final results are reported in cm3andg/cm3, with three decimals.12. Report12.1 The specific size fraction must be reported as part ofthe test results.13. Precision and Bias13.1 The precision of this test method is based on aninterlaboratory study of D80
24、97, conducted in 2016. Fivelaboratories tested five unique petroleum coke specimen types/sizes. Every test result represents an individual determination,and all participants reported duplicate test results for eachmaterial tested. Practice E691 was followed for the design andanalysis of the data; th
25、e details are given in ASTM ResearchReport No. RR:D02-1848.413.1.1 Repeatability (r)The difference between repetitiveresults obtained by the same operator in a given laboratoryapplying the same test method with the same apparatus underconstant operating conditions on identical test material withinsh
26、ort intervals of time would in the long run, in the normal andcorrect operation of the test method, exceed the followingvalues only in one case in 20.13.1.1.1 Repeatability can be interpreted as maximum dif-ference between two results, obtained under repeatability4Supporting data have been filed at
27、ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1848. ContactASTM CustomerService at serviceastm.org.TABLE 2 Bulk Density (g/cm3), 0.50 mm by 0.25 mmMaterialAverageAxRepeatability StandardDeviationSrReproducibility StandardDeviationSRRepeatability LimitrReprod
28、ucibility LimitRCoke A 0.8849 0.0037 0.0065 0.0102 0.0181Coke B 0.8178 0.0026 0.0103 0.0073 0.0288Coke C 0.9773 0.0032 0.0136 0.0090 0.0381Coke D 0.9010 0.0019 0.0064 0.0052 0.0180Coke E 0.8358 0.0091 0.0107 0.0254 0.0299AThe average of the laboratories calculated averages.TABLE 1 Recommended Equipm
29、ent SettingNumber of Cycles: 10Consolidation Force: 30 NPreparation Cycles: 5Agitation: HighSpeed: 150 steps/sD8097 172conditions, that is accepted as plausible due to random causesunder normal and correct operation of the test method.13.1.1.2 Repeatability limits are listed in Tables 2-6.Repeatabil
30、ity = 0.016g/cm3(1)13.1.2 Reproducibility (R)The difference between twosingle and independent results obtained by different operatorsapplying the same test method in different laboratories usingdifferent apparatus on identical test material would, in the longrun, in the normal and correct operation
31、of the test method,exceed the following values only in one case in 20.13.1.2.1 Reproducibility can be interpreted as maximumdifference between two results, obtained under reproducibilityconditions, that is accepted as plausible due to random causesunder normal and correct operation of the test metho
32、d.13.1.2.2 Reproducibility limits are listed in Tables 2-6.Reproducibility = 0.031 g/cm3(2)13.1.3 The above terms (repeatability limit and reproduc-ibility limit) are used as specified in Practice E177.13.1.4 Any judgment in accordance with statements 13.1.1and 13.1.2 would have an approximate 95 %
33、probability ofbeing correct.13.2 BiasAt the time of the study, no accepted referencematerial suitable for determining the bias for this test methodwas incorporated, therefore no statement on bias is being made.13.3 The precision statement was determined through sta-tistical examination of 250 test r
34、esults, from five laboratories,on five materials. The materials tested were described as:13.3.1 Coke ACalcined petroleum cokerotary kiln, an-ode.13.3.2 Coke BCalcined petroleum cokerotary kiln, an-ode.13.3.3 Coke CCalcined petroleum cokevertical shaft,anode.13.3.4 Coke DCalcined petroleum cokerotary
35、 kiln, an-ode.13.3.5 Coke ECalcined petroleum cokerotary kiln, an-ode.13.4 To judge the equivalency of two test results, it isrecommended to choose the average for the specified sizefraction being analyzed as listed in Table 7.14. Keywords14.1 bulk density; calcined petroleum coke; natural fraction;
36、pycnometers; tapped bulk density (TBD); transaxial pressure;vibrated bulk density (VBD)TABLE 3 Bulk Density (g/cm3), 1 mm by 0.50 mmMaterialAverageAxRepeatability StandardDeviationSrReproducibility StandardDeviationSRRepeatability LimitrReproducibility LimitRCoke A 0.8244 0.0058 0.0096 0.0162 0.0268
37、Coke B 0.7631 0.0019 0.0094 0.0052 0.0263Coke C 0.9205 0.0054 0.0118 0.0152 0.0331Coke D 0.8796 0.0084 0.0090 0.0234 0.0251Coke E 0.7764 0.0031 0.0087 0.0086 0.0243AThe average of the laboratories calculated averages.D8097 173ANNEX(Mandatory Information)A1. BLANK DATA SETA1.1 Mount the empty glass c
38、hamber/plunger assembly intoinstrument securely.A1.2 Select the “Store Blank Data” setup.A1.3 Name the blank data set (1 to 10) by pressing thesecond key, then “Analyze.” Use the arrow keys to choose“Store Blank Data,” and then choose a blank data set number(1 to 10).A1.4 Select (10) for the number
39、of cycles.A1.5 Enter the diameter of the chamber being used. Thisdiameter will be used for all subsequent runs in this storedblank data set.NOTE A1.1If you wish to store data for a different size chamber, youmust start another blank data set.A1.6 Enter the consolidation force being used.TABLE 4 Bulk
40、 Density (g/cm3),2mmby1mmMaterialAverageAxRepeatability StandardDeviationSrReproducibility StandardDeviationSRRepeatability LimitrReproducibility LimitRCoke A 0.7548 0.0034 0.0075 0.0094 0.0209Coke B 0.7213 0.0120 0.0192 0.0336 0.0538Coke C 0.8453 0.0052 0.0148 0.0145 0.0414Coke D 0.8449 0.0056 0.00
41、94 0.0158 0.0263Coke E 0.7294 0.0048 0.0099 0.0134 0.0278AThe average of the laboratories calculated averages.TABLE 5 Bulk Density (g/cm3),4mmby2mmMaterialAverageAxRepeatability StandardDeviationSrReproducibility StandardDeviationSRRepeatability LimitrReproducibility LimitRCoke A 0.6864 0.0079 0.011
42、4 0.0222 0.0319Coke B 0.7104 0.0109 0.0143 0.0305 0.0400Coke C 0.7635 0.0016 0.0114 0.0045 0.0320Coke D 0.7816 0.0106 0.0108 0.0296 0.0304Coke E 0.6695 0.0103 0.0154 0.0290 0.0431AThe average of the laboratories calculated averages.TABLE 6 Bulk Density (g/cm3),8mmby4mmMaterialAverageAxRepeatability
43、StandardDeviationSrReproducibility StandardDeviationSRRepeatability LimitrReproducibility LimitRCoke A 0.6559 0.0063 0.0080 0.0177 0.0223Coke B 0.6929 0.0057 0.0149 0.0159 0.0418Coke C 0.7142 0.0039 0.0102 0.0110 0.0286Coke D 0.7202 0.0036 0.0117 0.0102 0.0328Coke E 0.6513 0.0090 0.0124 0.0252 0.034
44、7AThe average of the laboratories calculated averages.TABLE 7 Average Repeatability and Reproducibility Limit for Each Specified Size FractionSpecific SizeAverageAxRepeatabilityStandard DeviationSrReproducibilityStandard DeviationSRRepeatability LimitrReproducibility LimitR0.50 mm by 0.25 mm 0.8834
45、0.0041 0.0095 0.0114 0.02661.00 mm by 0.50 mm 0.8328 0.0049 0.0097 0.0137 0.02712.00 mm by 1.00 mm 0.7791 0.0062 0.0122 0.0173 0.03404.00 mm by 2.00 mm 0.7223 0.0083 0.0127 0.0232 0.03558.00 mm by 4.00 mm 0.6869 0.0057 0.0114 0.0160 0.0320AThe average of the laboratories calculated averages.D8097 17
46、4NOTE A1.2The software prevents you from storing duplicate forces/pressures within a single blank data set.A1.7 Start analysis by selecting “Enter.” The GeoPyc 1360automatically collects blank data for the selected chamberusing the designated force. The following message is dis-played: “Press Enter
47、for another blank run, or Esc to end.”A1.8 To continue storing the blank data in this set, repeatthis process beginning with the force. To end, press “Escape.”ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this stand
48、ard. 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 any time by the responsible technical committee and must be review
49、ed 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 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 ASTM Internation
