1、Designation: D4292 10Standard 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 3-mesh Tyler StandardSeries) and retained on a 0.21-mm opening sieve (equivalent toa 65-mesh Tyler Standard Series). Further, the procedure islimited to a specific te
4、st 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 SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to addr
5、ess 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:2D346 Practice
6、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 Analysis of Petrole
7、um 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 Standard:3.1.1 as-ca
8、lcined 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, representa-tive portion
9、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, the test volume of 1
10、00 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 a sample of calcine
11、d 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 eitherscreen defining the sampl
12、e. Particle size range tested should beagreed upon by 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 ope
13、ning, No. 50, sieve to be preferred. Otherpopular 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-mm1This test method is under the jurisdiction of ASTM
14、Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved July 1, 2010. Published July 2010. Originally approvedin 1992. Last previous edition approved in 2007 as D42929
15、2(2007). DOI:10.1520/D4292-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Belitskus, D. L., “Evaluating
16、Calcined Coke for Aluminum Smelting by BulkDensity,” Aluminium , Vol 51, No. 2, 1975.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.opening sieve (equivalent to a 3-m
17、esh Tyler Standard Series) and retainedon a 3.33-mm opening, No. 6, sieve for graphite electrode manufacture.6. Apparatus6.1 Jaw Crusher, laboratory 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, la
18、boratory type; glass hardened rolls; rolldiameter, approximately 200 mm; roll width, approximately150 mm; gap range from 0 to 12.7 mm, both rolls shall rotateto crush the material. Do not use a disc mill, disc type grinder,or disc pulverizer, since these contain one stationary roll. Priorto use, che
19、ck and adjust the springs on the roll crusheraccording to the manufacturers 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
20、approximately 175- by 250-mm deck,must be capable of vibrating at a frequency of 60 Hz and anamplitude 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, approx
21、imately 100-mm inside diameter by25 mm high by 12 mm thick, weight 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 diame
22、ter of 25 to 30 mm (powder funnel).6.11 Automatic Timer, Clock, or Watch, with a secondindicator.6.12 Riffle Sampler, enclosed drawer, approximately 380 by290 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 operat
23、ion 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 source when equipment isopened for cleaning after the grinding operation.8. Sample Preparation8.1 Use the crushing procedure
24、in 8.2 and subsequentparagraphs so that contributions to 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 bas
25、ed 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 caking.NOTE 3On agreement by purchaser and supplier
26、, 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 and procedures for dividing are described in Te
27、st Methods D346,D2013, D2234/D2234M, and D4057 and Practices 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
28、the jawcrusher motor, slowly feed the sample through the 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 rol
29、l crusher must be limitedto a maximum ratio of 4 to 1. 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 intermedia
30、te settings as possible(but not exceeding the 4 to 1 reduction 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 i
31、nsertedbetween the rolls with the motor deactivated is 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 f
32、ractionrequired (expressed as the opening, in millimetres, 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 38.3.4 For each cru
33、shing step required, 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
34、 to one having 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 =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 mm4The calibration procedure described lat
35、er 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 1023rd setting: 0.661 mm 4 3.179 = 0.208 mm8.3.6 After the roll gap is adjusted, remove the feeler gage(if used), turn
36、 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 sample. Do not sieve the sample between crushingsteps.
37、 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, at least 30 % of the coke generally will be in thede
38、sired 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 screen occurs when too much material is on a screen
39、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 weights ofcoke coarser and finer than the desired fraction
40、, 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 as manyintermediate settings as required. The entire
41、 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-than-desired cokeis greater than 2.0, decrease the roll
42、 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 roll crusher with the original gapsetting.)8.3.9 If the
43、 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. If the starting material is not coarse enough to ob
44、tainthis 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 passes, or both, with trial-and-erroradjustments until a
45、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 acceptable; that is, once a 0.3-kg sample of jawcrus
46、her 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 Apparatus9.1 Graduated CylinderSince vibrator amplitude is af
47、-fected by weight on the table, cut off the graduate below 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 co
48、rk 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 ring isintentionally larger than the base width of the graduatedcylinder. It is designed o
49、nly to keep the graduated cylinderfrom vibrating off the vibrator table. Do not attach thegraduated cylinder to the vibrator by a clamp or other device.The graduated cylinder shall vibrate freely.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 the190-mL mark at the bottom of the tape. Make eight marks onthe bottom of the tape equidis
