1、Designation: D 4292 92 (Reapproved 2007)An American National StandardStandard Test Method forDetermination of Vibrated Bulk Density of CalcinedPetroleum Coke1This standard is issued under the fixed designation D 4292; the number immediately following the designation indicates the year oforiginal ado
2、ption or, in the case of revision, 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 test method covers the determination of bulkdensity of a represen
3、tative 2-kg sample of calcined petroleumcoke, after vibration to increase compaction.1.2 The procedure is limited to particles passing through a6.68-mm opening sieve (equivalent to a 3-mesh Tyler StandardSeries) and retained on a 0.21-mm opening sieve (equivalent toa 65-mesh Tyler Standard Series).
4、Further, the procedure islimited to a specific test sample having particles retainedbetween screens having openings that differ by a factor of lessthan 2=2 and preferably less than 2.1.3 The values stated in acceptable SI units are to beregarded as the standard.1.4 This standard does not purport to
5、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 Standards:2D 346 Prac
6、tice for Collection and Preparation of CokeSamples for Laboratory AnalysisD 2013 Practice for Preparing Coal Samples for AnalysisD 2234/D 2234M Practice for Collection of a Gross Sampleof CoalD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsE11 Specification for Wire Cloth and S
7、ieves for TestingPurposes3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 as-calcined particles, nof coke, those that have notbeen subject to laboratory crushing.3.1.2 bulk density, nof coke, the ratio of the mass of acollection of particles of a specified size range to the vol
8、umeoccupied.3.1.3 laboratory crushed particles, nof coke, those thathave been crushed in the laboratory.4. Summary of Test Method4.1 After appropriate crushing of the calcined coke, usingboth the jaw crusher and roll crusher, the test volume of 100 gis measured after vibration and the bulk density i
9、s 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 a sample of calcined petroleum coke is stronglydependent upon average par
10、ticle 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 eitherscreen defining the sample. Particle size range tested should beagreed upon by
11、the purchaser and supplier.)NOTE 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 rang
12、es 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 continuous1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.05 on Propertie
13、s of Fuels, Petroleum Coke and Carbon Material.Current edition approved May 1, 2007. Published June 2007. Originallyapproved in 1992. Last previous edition approved in 2002 as D 429292 (2002)e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at s
14、erviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Belitskus, D. L., “Evaluating Calcined Coke for Aluminum Smelting by BulkDensity,” Aluminium, Vol 51, No. 2, 1975.1Copyright ASTM International, 100 Barr Harbor Drive
15、, PO Box C700, West Conshohocken, PA 19428-2959, United States.Soderberg anode process and particles passing through a 6.68-mmopening sieve (equivalent to a 3-mesh Tyler Standard Series) and retainedon a 3.33-mm opening, No. 6, sieve for graphite electrode manufacture.6. Apparatus6.1 Jaw Crusher, la
16、boratory type; jaw opening, approxi-mately 50 by 200 mm; jaws can be set to gaps of approximately3.2 to 12.7 mm; manganese steel jaw plates.6.2 Roll Crusher, laboratory type; glass hardened rolls; rolldiameter, approximately 200 mm; roll width, approximately150 mm; gap range from 0 to 12.7 mm.6.3 Si
17、eve 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- by 250-mm deck,must be capable of vibrating at a frequency of 60 Hz and anampl
18、itude of 0.20 to 0.22 mm (peak) when loaded with a 50-gcork ring, 215-g graduated cylinder, and a 100-g coke sample.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, weight approximately 50 g(round-botto
19、m 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 to 30 mm (powder funnel).6.11 Automatic Timer, Clock, or Watch, with a secondindicator.
20、6.12 Riffle Sampler, enclosed drawer, approximately 380 by290 by 360 mm, 24-slot.7. Precautions7.1 Exercise care in the operation of the jaw crusher and rollcrusher. Turn power off at the source when setting the gap.Wear safety glasses and keep hands clear when feedingmaterial. Turn power off at the
21、 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 to VBD from both as-calcinedand laboratory-crushed particles (which differ significantly indensity) are included.NOTE 2B
22、ecause the vibrated bulk density method is based on thepacking of sized particles, the method of sample 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 cakin
23、g.NOTE 3On agreement by purchaser and supplier, density of onlyas-calcined particles in the selected 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 a
24、nd procedures for dividing are described in Test Methods D 346,D 2013, D 2234, and D 4057.8.2 Jaw Crusher OperationUse the procedure appropriateto the 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.
25、 Turn on the jawcrusher motor, slowly feed the sample through the crusher, andcollect the product for further reduction through a roll 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. Depending on
26、 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 reduction rati
27、o).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 useful.8.3.2
28、 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 millimetres, of theco
29、arser 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 38.3.4 For each crushing step required, the roll gap isdecreased (from a value equival
30、ent 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 a maximumparticle size of 0.208 mm. The calculation
31、is as follows:Ratio = 32.115 (see 8.3.2)Crushing steps required = 3 (see 8.3.3)Factor =332.115 = 3.179 (see 8.3.4)1st setting: 6.68 mm 4 3.179 = 2.101 mm2nd setting: 2.101 mm 4 3.179 = 0.661 mm3rd setting: 0.661 mm 4 3.179 = 0.208 mm8.3.6 After the roll gap is adjusted, remove the feeler gage(if use
32、d), 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 and collect the sample. Then,4The calibration procedure described later is specific to
33、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.D 4292 92 (2007)2using the appropriate screens (those defining the bulk densityfraction), sample receiver, and cover, sieve the roll-crushedsa
34、mple in the sieve shaker. With this final roll crusher setting,at least 30 % of the coke generally will be in the desiredparticle size range.8.3.7 This setting will produce roughly equal weights ofcoke coarser and finer than the desired fraction, provided thatthe starting material is sufficiently co
35、arse. 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 as manyintermediate settings as required. The entire roll crusherproduct is consolidated and the desired fr
36、action 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-than-desired cokeis greater than 2.0, decrease the roll gap to 80 % of its originalvalue and test another 0.3
37、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 roll crusher with the original gapsetting.)8.3.9 If the ratio is less than 0.8 and the starting material iscoa
38、rse 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. If the starting material is not coarse enough to obtainthis ratio for the particle size range selected for
39、 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 passes, or both, with trial-and-erroradjustments until a satisfactory composite sample is obtainedfrom the 2-kg
40、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 acceptable; that is, once a 0.3-kg sample of jawcrusher product has been passed through the roll crusher, i
41、tmust 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 Apparatus9.1 Graduated CylinderSince vibrator amplitude is af-fected by weight on the table, cut off the graduate be
42、low thepouring lip so that the weight is 215 6 10 g. Sand sharp edges.With one common brand of graduated cylinder, this corre-sponds to an overall length of about 305 mm. Fit the graduatewith a No. 8 stopper (tight fit).9.2 VibratorFasten the cork ring securely with screws tothe table top of the vib
43、rator 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 ring isintentionally larger than the base width of the graduatedcylinder. It is designed only to keep the graduated cylinderfrom vibrating off th
44、e vibrator table.10. Calibration of Apparatus10.1 Graduated Cylinder Calibration FactorMeasure thedistance, in millimetres, between the 90-mLand 170-mLmarkson the graduated cylinder.B 5 170290/distance in mm (2)where:B = calibration factor, mL/mm.Wrap a piece of masking tape around the graduate with
45、 the190-mL mark at the bottom of the tape. Make eight marks onthe bottom of the tape equidistantly around the cylinder. Theseare used only for equally spacing height measurements (not asa volume measurement base line).10.2 Determination of Accuracy of Graduated CylinderUsing distilled water at 25 6
46、5C, fill the graduate to the90-mL mark and determine the weight of water at that volume.Using a density of 0.997 g/cm3for water, determine the truevolume. Do the same at 20-mL increments up to the 170-mLmark. If the deviation at any indicated volume is greater than60.5 mL, a table of indicated volum
47、es versus true volumesshould be made for use in computing bulk density.10.3 Vibrator5Using a hex wrench, remove the fourscrews that hold the vibrator table and remove the table.Loosen the core locking screw. If the aluminum table isgrounded, remove the ground wire. Turn the vibrator on its sideand a
48、ttach the ohmmeter to the table support and ground. Turnthe core into the case (clockwise) until the ohmmeter registerszero (core is touching armature). Back off the core (counter-clockwise) until the ohmmeter reads infinite resistance. Markthe zero position with arrows on each side of the screw slo
49、t andturn the core out exactly one and three-eighths turns. Replacethe table and tighten the four screws.11. Procedure11.1 Weigh 100.0 6 0.1 g of the coke fraction to be testedinto a container. Pour the coke slowly through a funnel into thegraduate. Transfer time must be 70 to 100 s. The importance ofthis step on the density value cannot be overemphasized. Arapid pour results in a higher volume than a slow pour and apart of the difference in volume is retained through thevibrating step.11.2 Fit the rubber stopper tightly to the top of the graduate.11.3 Place the gr
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