1、Designation: D7454 141Standard Test Method forDetermination of Vibrated Bulk Density of CalcinedPetroleum Coke using a Semi-Automated Apparatus1This standard is issued under the fixed designation D7454; the number immediately following the designation indicates the year oforiginal adoption or, in th
2、e 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.1NOTEResearch Report information was added editorially to the Precision and Bias section in Septem
3、ber 2014.1. Scope*1.1 This test method covers the determination of bulkdensity of a representative 2-kg sample of calcined petroleumcoke, after vibration to increase compaction, using a semi-automatic apparatus.1.2 The procedure is applied, but not limited, to particlespassing through a 4.75-mm open
4、ing sieve and retained on a1.18-mm opening sieve. Further, the procedure is applied, butnot limited, to a specific test sample having particles passingthrough a 0.85-mm opening sieve and retained on a 0.425-mmopening sieve. This procedure could also be applied to othersieve fractions being agreed on
5、 in the aluminum industry asspecified in Annex A1.1.3 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 thesafety concerns, if any, associated with its use. It is theresponsibil
6、ity 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:2E11 Specification for Woven Wire Test Sieve Cloth and TestSievesE691 Practice for Conducting an In
7、terlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 Definitions: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
8、size range to thevolume occupied.3.1.3 laboratory crushed particles, n of coke, those par-ticles of petroleum coke that have been crushed in thelaboratory.4. Summary of Test Method4.1 The natural 4.75 by 1.18-mm fraction of the originalcoke is separated from the sample by manual screening, groundto
9、0.85 by 0.425 mm, and fed at a controlled rate into agraduated cylinder on a vibrating table until the coke reachesthe 50-mL mark. The collected coke is weighed and the bulkdensity is calculated and reported in g/mL.4.2 The procedure is empirical; close adherence to thetechnique and apparatus is nec
10、essary to ensure reproducibleresults. To provide comparable results in different locations,exact adjustments of operating parameters are required usingreference samples.5. Significance and Use5.1 Vibrated bulk density (VBD) is an indicator of calcinedpetroleum coke porosity, which affects its suitab
11、ility for use inpitch-bonded carbon applications. (WarningVibrated bulkdensity for 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
12、 the possibilityfor variation due to skewing of the test sample toward eitherscreen defining the sample.)6. Apparatus6.1 Pan BalanceAccurate to 0.1 g, with a capacity of2.0 kg.6.2 Riffle SamplerEnclosed drawer, approximately 380 by290 by 360 mm, 24-slot.6.3 SievesMeeting Specification E11.1This test
13、 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, Petroleum Coke and Carbon Material.Current edition approved May 1, 2014. Published May 2014. Originallyapproved in
14、 2008. Last previous edition approved in 2008 as D7454 08. DOI:10.1520/D7454-14E01.2For 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 pa
15、ge 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. United States16.4 Sieve ShakerElectrical drive with an automatic timer;should have a rotating and tapping action.
16、6.5 Roller CrusherLaboratory type; glass hardened rolls;roll diameter of approximately 150 mm; roll width of approxi-mately 150 mm; gap range from 0 to 12.7 mm.6.6 Thickness Gauges (leaf-type)0.4, 1.0, 1.5, and4.0 mm.6.7 Semi-Automated VBD Apparatus, As shown in Fig. 1.See also comments about instal
17、lation in Annex A1.6.7.1 Borosilicate Glass Powder Funnels8-cm diameterfunnels with 1-cm internal diameter and stems about 3.5 cmlong. Tips of funnels should be cut at a right (not oblique)angles (see Fig. 1). The distance between the tip of the upperfunnel and the bottom of the vibrating bowl shoul
18、d be around6 mm.6.7.2 Electromagnetic JoggerWith approximately 175- by250-mm deck, and shall be capable of vibrating at a frequencyof 60 Hz.6.7.3 Acrylic ClampTo hold cylinder.6.7.4 Vibrating BowlHaving a diameter of approximately7.5 cm and a height of 4.0 mm, such as that being used withrotary micr
19、o riffler.6.7.5 Displacement Probe and Reading DevicePermittingcontinuous monitoring of amplitude vibration.6.7.6 Graduated Cylinder50 mL, with inside diameterapproximately 23 mm and height approximately 19 cm.6.7.7 Photoelectric Sensor Switch.6.7.8 Control DevicePermitting real-time adjustment ofth
20、e vibration amplitude and automatic stopping of the feedingdevice when the coke level reaches the 50-mL mark.6.7.9 Automatic Timer, Clock, or WatchWith a secondindicator.6.7.10 Line Stabilizer (Optional)Use if the noise on thepower line is significant and affects the apparatus performance.6.7.11 Rou
21、nd Level.6.7.12 Balance0 to 300 g and sensitive to 0.01 g.7. Hazards7.1 Exercise care in the operation of the roll crusher.7.1.1 Wear safety glasses and keep hands clear when feed-ing material.7.1.2 Turn power off at the source when equipment isopened for cleaning after the grinding operation.8. Sam
22、ple Preparation8.1 Reduce the original sample volume to about 1 kg.8.2 Manually screen out the natural to 4.75 by 1.18 mm and0.85-mm fraction.8.8 Adjust the roller spacing to 0.5 mm and grind the 0.85-mm fraction. Manually screen out the 0.85 byFIG. 1 Example of Semi-Automated Apparatus Set-UpD7454
23、14120.425-mm fraction and add this fraction into the same plasticbag referred to in 8.7. Discard the 0.85-mm fraction, if present.8.9 Repeat, if necessary, the grinding procedure in 8.8 of the 0.85-mm fraction, until all particles pass through the0.85-mm sieve. It is possible that at this step, abou
24、t 1 to3gofparticles larger than 0.85 mm cannot be ground to finerparticles. Do not attempt to grind them using roller spacingsmaller than 0.5 mm. Simply discard them (these particles arein general, plate-like shape particles and should not be used forbulk density measurement).8.10 Manually mix the c
25、ontents of the plastic bag.8.11 Divide the 0.85 by 0.425-mm material between twosets of sieves with openings of 0.85 mm and 0.425 mm andtheir pan. Using a sieving shaker screen out the 0.85 by0.425-mm fraction for 7 min. Discard the 0.425 mm material.8.12 Transfer the 0.85 by 0.425-mm material into
26、an appro-priate plastic container and manually mix the contents (about100 mL of material is needed for analysis).9. Preparation of Apparatus9.1 Install the apparatus as shown Fig. 1.10. Calibration and Standardization10.1 Calibration of Graduated CylinderAdjust the heightof the photodetector, and de
27、termine the true volume at the50-mL mark of the graduated cylinder, following the detailedprocedure given in Annex A2. Calibration shall be made eachtime a new cylinder is used or when the apparatus is moved.10.2 Determination of the Displacement Speed Target of theJoggerDetermine the displacement t
28、arget, in accordancewith Annex A3, using standard reference materials. Onceestablished, this target shall be kept indefinitely unless theprobe, the controller or the jogger have to be changed.10.3 Feeding RateCheck/adjust the feeding rate for eachsample.11. Procedure11.1 Make sure that the vibrating
29、 table is levelled.11.2 Turn on the apparatus at least 10 min before initiatingmeasurements. The power should not be turned off betweenreadings.11.3 Weigh the graduated cylinder to the nearest 0.01 g,insert it into the clamping device on the vibrating table whileensuring it does not touch the photoe
30、lectric sensor, and let thetable vibration stabilize to the set points (it takes a fewseconds).11.4 Fill the upper funnel with the coke sample.11.5 Fill the cylinder to about half, using maximum feedingrate, to make a constant bed in the vibrator bowl. Stop thefeeding, empty the cylinder in the uppe
31、r funnel, and reinsert itin the clamping device.11.6 Using the automatic mode, reset the chronometer,initiate the feeding and adjust if necessary, the bowl vibrationintensity to obtain the feeding time of 30 6 3 s/10 mL. Thefeeding will automatically stop when the 50-mL mark isreached. If no feeding
32、 time adjustment was necessary and if thedischarge time falls within 135 and 165 s, proceed to 11.7.Otherwise, repeat 11.6 until the time target is met.11.7 Empty the cylinder in the upper funnel, reinsert it intothe clamping device, and let the table vibration stabilize to theset points (it takes f
33、ew seconds). Then, using the automaticmode, reset the chronometer and initiate feeding. The feedingwill stop automatically.11.8 Check that the discharge time falls within 135 and165 s (150 6 15 s). If not, return the coke to the upper funneland repeat from 11.6 to readjust the feeding time.11.9 Remo
34、ve the cylinder containing the coke and weigh tothe nearest 0.01 g. Take two additional readings according to11.7, readjusting, if necessary, the feeding time to meet thetarget (between 135 and 165 s).11.10 If the difference between the lowest and highestweight readings exceeds 0.40 g, check if the
35、apparatus isproperly functioning, and repeat the test until two consecutiveruns agree within the specified 0.40 g. Discard readings only ifa malfunction was identified (for example, the apparatus wasnot on speed displacement target, or the time target was notmet).12. Calculation or Interpretation of
36、 Results12.1 Calculate the average of all acceptable weight readings(at least three).12.2 Calculate VBD using the following equation:Vibrated Bulk Density g/mL! 5Average weight of coke g!Calibrated volume of cylinder mL!(1)13. Report13.1 Report the average of the readings to the nearest0.001 g mL.14
37、. Precision and Bias314.1 PrecisionPrecicion was determined by interlabora-tory testing of calcined petroleum coke samples. Samplescovers the density range included between 0.78 and 0.94 g/mL.Each sample were prepared by participants and statisticaltreatment of data was performed in accordance with
38、PracticeE691.14.2 RepeatabilityWith a confidence limit of 95 %, thedifference between consecutive results obtained with the sameoperator, the same machine within the same day under constantconditions do not exceed the following value.Repeatability r! = 0.02 g/mL14.3 ReproducibilityWith a confidence
39、limit of 95 %, thedifference between two single and independent analysis, per-formed by different operators, with different machines, in3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1782. ContactASTM CustomerService at ser
40、viceastm.org.D7454 1413different laboratories on identical test material would notexceed the following value:Reproducibility R! = 0.02 g/mL14.4 BiasThis test method is empirical; no statement as tobias is made.15. Keywords15.1 calcined petroleum coke; porosity; vibrated bulk den-sityANNEXES(Mandator
41、y Information)A1. OTHER SIEVE FRACTIONS USED IN THE ALUMINUM INDUSTRY TO DETERMINED VIBRATED BULK DENSITYA1.1 Froma2kgas-received sample, split the test samplewith a riffle sampler to a subsample of 350 6 50 g.A1.2 Sieve the subsample to collect the as-received particlefraction to be measured in acc
42、ordance with TableA1.1. Discardthe undersized particle fraction.A1.3 Taking care to avoid overcrushing, crush the over-sized fraction of the subsample in a jaw crusher (of thelaboratory type, having manganese steel jaws capable of beingset to gaps of approximately 3 to 15 mm) or roll crusher, andpla
43、ce the material between the appropriate two sieves with apan on the bottom and a lid on the top. Gently agitate the sievesby hand but vigorously enough to collect the crushed particlefraction to be measured and discard the undersized material.Repeat until at least 90 % (and preferably more) of thesu
44、bsample passes through the upper size sieve for the particlefraction to be measured.A1.4 Mix the as-received and crushed particle fractions. Aminimum of 110 g of sieved, crushed and mixed particles arerequired for the VBD test. The mixed sample is sieved for10 min in a sieve shaker. Discard undersiz
45、ed material.A2. ADJUSTMENT OF THE PHOTOELECTRIC SENSOR HEIGHT AND GRADUATED CYLINDER CALIBRATIONA2.1 Ensure that the table is level, and turn the apparatuson.A2.2 Insert the cylinder into the clamping device of theVBD apparatus while ensuring it does not touch the photoelec-tric sensor.A2.3 Fill the
46、 upper funnel with a typical coke sample.A2.4 Make sure the electromagnetic jogger is turned on, fillthe cylinder approximately up to the 45-mL line using maxi-mum feeding rate, and stop the feeding.A2.5 Using the automatic mode, alternately start and stopthe feeding whenever necessary to bring the
47、coke level to thedesired position (should be the 50-mL line of the cylinder).A2.6 Bring the photoelectric sensor very slightly above thedesired position by sliding the bracket (the knob should beunscrewed) while holding the sensor (do not forget to screw theknob afterward).A2.7 Set the vibrating bow
48、l control to OFF to avoidfeeding. Reset the chronometer, press START to get thechronometer running, and adjust the photoelectric sensorheight very slowly until it stops the chronometer.A2.8 Remove the cylinder, transfer the coke back into theupper funnel and reinsert it into the clamping device. Usi
49、ng theautomatic mode, reset the chronometer and press start thefeeding. The feeding will automatically be stopped by thephotoelectric sensor. If necessary, make a fine readjustment ofthe height of the sensor. Repeat A2.8 until the desired positionis reached (should be the 50-mL line).A2.9 Once the photoelectric sensor is at the desiredposition, empty the vibrating bowl.A2.10 Set the vibrating bowl control to OFF.A2.11 Make sure the electromagnetic jogger is turned OFF.A2.12 Clean the graduated cylinder, and tare it.TABLE A1.1 Sieve Fractions
