1、Designation: D4292 17Standard Test Method forDetermination of Vibrated Bulk Density of CalcinedPetroleum Coke1This standard is issued under the fixed designation D4292; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of la
2、st 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*1.1 This test method covers the determination of bulkdensity of a representative 2 kg sample of calcined petroleumcoke, aft
3、er vibration to increase compaction.1.2 The procedure is limited to particles passing through a6.68 mm opening sieve (equivalent to a 0.265 in. USA Series)and retained on a 0.21 mm opening sieve (equivalent to a70 mesh USA Series). Further, the procedure is limited to aspecific test sample having pa
4、rticles retained between screenshaving openings that differ by a factor of less than 2=2 andpreferably less than 2.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafet
5、y concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance
6、 with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Stand
7、ards:2D346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD2013 Practice for Preparing Coal Samples for AnalysisD2234/D2234M Practice for Collection of a Gross Sampleof CoalD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD5709 Test Method for Sieve
8、 Analysis of Petroleum CokeD6969 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 TestSieves3. Terminology3.1 Definitions of Terms Specific to This
9、Standard:3.1.1 as-calcined particles, nof coke, those particles thathave not been subject to laboratory crushing.3.1.2 bulk density, nof coke, the ratio of the mass of acollection of particles of a specified particle size range to thevolume occupied.3.1.3 gross sample, nthe original, uncrushed, repr
10、esenta-tive portion taken from a shipment or lot of coke.3.1.4 laboratory crushed particles, nof coke, those par-ticles of petroleum coke that have been crushed in thelaboratory.4. Summary of Test Method4.1 After appropriate crushing of the calcined coke, usingboth the jaw crusher and roll crusher,
11、the test volume of 100 gis measured after vibration and the bulk density is calculated.5. Significance and Use5.1 Vibrated bulk density, VBD, is an indicator of calcinedpetroleum coke porosity, which affects its suitability for use inpitch-bonded carbon applications. (WarningVibrated bulkdensity for
12、 a sample of calcined petroleum coke is stronglydependent upon average particle size and particle size range.Bulk density tends to increase with decreasing coke size. Anarrow particle size range for this test minimizes the possibilityfor variation due to skewing of the test sample toward eitherscree
13、n defining the sample. Particle size range tested should beagreed upon by the purchaser and supplier.)1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.05 on Properties of Fuels, Pe
14、troleum Coke and Carbon Material.Current edition approved Dec. 1, 2017. Published January 2018. Originallyapproved in 1992. Last previous edition approved in 2010 as D4292 10. DOI:10.1520/D4292-17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service a
15、t serviceastm.org. For Annual Book 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.
16、 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 Bar
17、riers to Trade (TBT) Committee.1NOTE 1An example of the use of VBD to characterize coke forprebaked anodes for aluminum smelting is reported by Belitskus3whofound particles passing through a 0.59 mm opening, No. 30, sieve andretained on a 0.30 mm opening, No. 50, sieve to be preferred. Otherpopular
18、ranges are particles passing through a 2.36 mm opening, No. 8,sieve and retained on a 1.17 mm opening, No. 16, sieve for the continuousSoderberg anode process and particles passing through a 6.68 mm openingsieve (equivalent to a 0.265 in. USA Series) and retained on a 3.33 mmopening, No. 6, sieve fo
19、r graphite electrode manufacture.6. Apparatus6.1 Jaw Crusher, laboratory type; jaw opening, approxi-mately 50 mm by 200 mm; jaws can be set to gaps ofapproximately 3.2 mm to 12.7 mm; manganese steel jawplates.6.2 Roll Crusher, laboratory type; glass hardened rolls; rolldiameter, approximately 200 mm
20、; roll width, approximately150 mm; gap range from 0 mm to 12.7 mm, both rolls shallrotate to crush the material. Do not use a disc mill, disc typegrinder, or disc pulverizer, since these contain one stationaryroll. Prior to use, check and adjust the springs on the rollcrusher according to the manufa
21、cturers recommendation.6.3 Sieve Shaker, electrical drive with an automatic timer;should have a rotating and tapping action.6.4 Sievesmeeting Specification E11.6.5 Pan Balance, accurate to 0.1 g, capacity 2.0 kg.6.6 Vibrator4, with approximately 175 mm by 250 mmdeck, must be capable of vibrating at
22、a frequency of 60 Hz andan amplitude of 0.20 mm to 0.22 mm (peak) when loaded witha 50 g cork ring, 215 g graduated cylinder, and a 100 g cokesample.6.7 Ohmmeter, adequate to test continuity of an electricalcircuit.6.8 Cork Ring, approximately 100 mm inside diameter by25 mm high by 12 mm thick, weig
23、ht approximately 50 g(round-bottom flask support).6.9 Graduated Cylinder, glass, 250 mL, inside diameterapproximately 37 mm, base diameter approximately 95 mm.6.10 Plastic Funnel, must have a stem with straight sidesand an outside diameter of 25 mm to 30 mm (powder funnel).6.11 Automatic Timer, Cloc
24、k, or Watch, with a secondindicator.6.12 Riffle Sampler, enclosed drawer, approximately380 mm by 290 mm by 360 mm, 24 slot.6.13 Feeler Gauges, mm size for checking the gap settingson the roll crusher.7. Precautions7.1 Exercise care in the operation of the jaw crusher and rollcrusher. Turn power off
25、at the source when setting the gap.Wear safety glasses and keep hands clear when feedingmaterial. Turn power off at the source when equipment isopened for cleaning after the grinding operation.8. Sample Preparation8.1 Use the crushing procedure in 8.2 and subsequentparagraphs so that contributions t
26、o VBD from both as-calcinedand laboratory-crushed particles (which differ significantly indensity) are included. Do not remove dedust oil from thesample prior to sample preparation or testing.NOTE 2Because the vibrated bulk density method is based on thepacking of sized particles, the method of samp
27、le preparation can affectresults due to differences in particle shapes affecting packing characteris-tics.8.1.1 Air-dry the laboratory sample, if it appears to be wet,prior to crushing to avoid caking.NOTE 3On agreement by purchaser and supplier, density of onlyas-calcined particles in the selected
28、size range are determined. If so,proceed to Section 11 and report as part of the result that only as-calcinedparticles were used.NOTE 4Recommended practice for collecting samples and the equip-ment and procedures for dividing are described in Test Methods D346,D2013, D2234/D2234M, and D4057 and Prac
29、tices D6969 and D6970.8.2 Jaw Crusher OperationUse the procedure appropriateto the jaw crusher being used, adjust the jaws so that the gapbetween them (at their closest position to each other in thecrushing cycle) is approximately 5 mm. Turn on the jawcrusher motor, slowly feed the sample through th
30、e jaw crusher,and collect the product for further reduction through a rollcrusher. In this step, the entire gross sample shall pass throughthe jaw crusher.8.3 Roll Crusher Operation(WarningTo avoid damageto the rolls, size reduction with the roll crusher must be limitedto a maximum ratio of 4 to 1.
31、Depending on the fractiondesired, a one-step reduction is often not possible from themaximum particle size in the jaw crusher product and inter-mediate roll settings are used. The sample is reduced to thedesired mesh size using as few intermediate settings as possible(but not exceeding the 4 to 1 re
32、duction ratio).8.3.1 With the motor deactivated, and using a methodappropriate to the roll crusher being used, adjust the roll gapaccording to the following procedure. If the rolls are readilyaccessible, adjustment with a leaf-type feeler gage insertedbetween the rolls with the motor deactivated is
33、useful.8.3.2 Calculate the ratio of the maximum particle size of theroll crusher feed (expressed as the opening, in millimetres, ofthe finest screen through which the largest particles will pass)to the maximum particle size of the bulk density fractionrequired (expressed as the opening, in millimetr
34、es, of thecoarser of the two screens used to define the bulk densityfraction).8.3.3 Select the number of crushing steps required from thefollowing table:RatioNumber of CrushingSteps Required1.1to4.0 14.1 to 16.0 216.1 to 64.0 33Belitskus, D. L., “Evaluating Calcined Coke for Aluminum Smelting by Bul
35、kDensity,” Aluminium, Vol 51, No. 2, 1975.4The calibration procedure described later is specific to a Syntron Model J-1Aor J-1B Jogger (from FMC Corp., Material Handling Equipment Div., Homer City,PA). Statistical data were obtained using Model J-1A Joggers.D4292 1728.3.4 For each crushing step requ
36、ired, the roll gap isdecreased (from a value equivalent to the maximum particlesize of the feed) by a factor of:n=Ratio as defined in 8.3.2! (1)where:n = number of crushing steps required (8.3.3)8.3.5 For example, it is desired to reduce a coke having amaximum particle size of 6.68 mm to one having
37、a maximumparticle size of 0.208 mm. The calculation is as follows:Ratio = 32.115 (see 8.3.2)Crushing steps required = 3 (see 8.3.3)Factor 5=332.11553.179 (see 8.3.4)1st setting: 6.68 mm 3.179 = 2.101 mm2nd setting: 2.101 mm 3.179 = 0.661 mm3rd setting: 0.661 mm 3.179 = 0.208 mm8.3.6 After the roll g
38、ap is adjusted, remove the feeler gage(if used), turn on the roll crusher motor, slowly feed 0.3 kg ofthe jaw crusher product through the roll crusher, and collect thesample. When more than one roll crushing step is required,regrind through smaller openings the entire 0.3 kg sample, andcollect the s
39、ample. Do not sieve the sample between crushingsteps. Then, using the appropriate screens (those defining thebulk density fraction), sample receiver, and cover, sieve theroll-crushed sample in the sieve shaker for 15 min, as requiredby Test Method D5709, Table 3. With this final roll crushersetting,
40、 at least 30 % of the coke generally will be in thedesired particle size range. A sieve shaker shall be used for thefinal sieving step to remove the undersize. Do not use othermeans of removing the undersize. Do not overload the screenas described in Test Method D5709, subsection 9.5. Overload-ing a
41、 screen occurs when too much material is on a screen andprevents a particle from touching the screen and having theopportunity to pass through the screen. For a 200 mm diameterscreen and calcined petroleum coke, the quantity is approxi-mately 200 g.8.3.7 This setting will produce roughly equal weigh
42、ts ofcoke coarser and finer than the desired fraction, provided thatthe starting material is sufficiently coarse. If yield is at least30 % and the ratio of coarser to finer product is between 0.8and 2.0, crushing is satisfactory and the remainder of thematerial is fed through the roll crusher, using
43、 as manyintermediate settings as required. The entire roll crusherproduct is consolidated and the desired fraction separated.8.3.8 At the roll gap setting intended to maximize the finalproduct, proceed as follows if the criteria in 8.3.7 are not met.If after one pass the ratio of coarser to finer-th
44、an-desired cokeis greater than 2.0, decrease the roll gap to 80 % of its originalvalue and test another 0.3 kg sample of jaw crusher product orintermediate roll crusher product, if required. (If the product isjust slightly too coarse, an alternative procedure is to makemultiple passes through the ro
45、ll crusher with the original gapsetting.)8.3.9 If the ratio is less than 0.8 and the starting material iscoarse enough to permit this ratio to be attained, increase theroll gap by 20 % of its original value and retest with 0.3 kg ofjaw crusher product or intermediate roll crusher product, ifrequired
46、. If the starting material is not coarse enough to obtainthis ratio for the particle size range selected for the test,disregard this restriction.8.3.10 These procedures will result in a satisfactory sampleas defined in 8.3.7 in the majority of cases. If not, adjust rollsettings or make multiple pass
47、es, or both, with trial-and-erroradjustments until a satisfactory composite sample is obtainedfrom the 2 kg starting sample. Observe that 0.3 kg fractions ofthe jaw crusher product can be discarded in their entirety if toofine after roll crushing. Partial consolidation of roll crusherproducts is not
48、 acceptable; that is, once a 0.3 kg sample of jawcrusher product has been passed through the roll crusher, itmust either be consolidated in its entirety with other rollcrusher products or discarded.Aminimum of 210 g of properlysized vibrated bulk density sample is required.9. Preparation of Apparatu
49、s9.1 Graduated CylinderSince vibrator amplitude is af-fected by weight on the table, cut off the graduate below thepouring lip so that the weight is 215 g 6 10 g. Sand sharpedges. With one common brand of graduated cylinder, thiscorresponds to an overall length of about 305 mm. Fit thegraduate with a No. 8 stopper (tight fit).9.2 VibratorFasten the cork ring securely with screws tothe table top of the vibrator as a retainer ring for the graduatedcylinder during the test. (Drill and tap holes in the vibratortable as required.) The inner diameter of the cork rin
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