An American National Standard

Designation: D 4292 – 92 (Reapproved 2002)e1

Standard Test Method for

Determination of Vibrated Bulk Density of Calcined
Petroleum Coke1
This standard is issued under the fixed designation D 4292; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

e1 NOTE—Warning notes were editorially moved into the standard text in March 2003.

1. Scope 3.1.1 as-calcined particles, n—of coke, those that have not
1.1 This test method covers the determination of bulk been subject to laboratory crushing.
density of a representative 2-kg sample of calcined petroleum 3.1.2 bulk density, n—of coke, the ratio of the mass of a
coke, after vibration to increase compaction. collection of particles of a specified size range to the volume
1.2 The procedure is limited to particles passing through a occupied.
6.68-mm opening sieve (equivalent to a 3-mesh Tyler Standard 3.1.3 laboratory crushed particles, n—of coke, those that
Series) and retained on a 0.21-mm opening sieve (equivalent to have been crushed in the laboratory.
a 65-mesh Tyler Standard Series). Further, the procedure is
4. Summary of Test Method
limited to a specific test sample having particles retained
between screens having openings that differ by a factor of less 4.1 After appropriate crushing of the calcined coke, using
than 2 =2 and preferably less than 2. both the jaw crusher and roll crusher, the test volume of 100 g
1.3 The values stated in acceptable SI units are to be is measured after vibration and the bulk density is calculated.
regarded as the standard. 5. Significance and Use
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5.1 Vibrated bulk density, VBD, is an indicator of calcined
responsibility of the user of this standard to establish appro- petroleum coke porosity, which affects its suitability for use in
priate safety and health practices and determine the applica- pitch-bonded carbon applications. (Warning—Vibrated bulk
bility of regulatory limitations prior to use. density for a sample of calcined petroleum coke is strongly
dependent upon average particle size and particle size range.
2. Referenced Documents Bulk density tends to increase with decreasing coke size. A
2.1 ASTM Standards: narrow particle size range for this test minimizes the possibility
D 346 Practice for Collection and Preparation of Coke for variation due to skewing of the test sample toward either
Samples for Laboratory Analysis2 screen defining the sample. Particle size range tested should be
D 2013 Practice of Preparing Coal Samples for Analysis2 agreed upon by the purchaser and supplier.)
D 2234 Practice for Collection of a Gross Sample of Coal2 NOTE 1—An example of the use of VBD to characterize coke for
D 4057 Practice for Manual Sampling of Petroleum and prebaked anodes for aluminum smelting is reported by Belitskus5 who
Petroleum Products3 found particles passing through a 0.59-mm opening, No. 30, sieve and
E 11 Specification for Wire Cloth and Sieves for Testing retained on a 0.30-mm opening, No. 50, sieve to be preferred. Other
popular ranges are particles passing through a 2.36-mm opening, No. 8,
Purposes4
sieve and retained on a 1.17-mm opening, No. 16, sieve for the continuous
3. Terminology Soderberg anode process and particles passing through a 6.68-mm
opening sieve (equivalent to a 3-mesh Tyler Standard Series) and retained
3.1 Definitions of Terms Specific to This Standard: on a 3.33-mm opening, No. 6, sieve for graphite electrode manufacture.

6. Apparatus
1
This test method is under the jurisdiction of ASTM Committee D02 on 6.1 Jaw Crusher, laboratory type; jaw opening, approxi-
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
mately 50 by 200 mm; jaws can be set to gaps of approximately
Current edition approved Dec. 10, 2002. Published April 2003. Originally 3.2 to 12.7 mm; manganese steel jaw plates.
approved in 1992. Last previous edition approved in 1997 as D 4292 – 92 (1997).
2
Annual Book of ASTM Standards, Vol 05.06.
3 5
Annual Book of ASTM Standards, Vol 05.02. Belitskus, D. L., “Evaluating Calcined Coke for Aluminum Smelting by Bulk
4
Annual Book of ASTM Standards, Vol 14.02. Density,” Aluminium, Vol 51, No. 2, 1975.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 D 4292 – 92 (2002)e1
6.2 Roll Crusher, laboratory type; glass hardened rolls; roll crusher motor, slowly feed the sample through the crusher, and
diameter, approximately 200 mm; roll width, approximately collect the product for further reduction through a roll crusher.
150 mm; gap range from 0 to 12.7 mm. 8.3 Roll Crusher Operation—(Warning—To avoid damage
6.3 Sieve Shaker, electrical drive with an automatic timer; to the rolls, size reduction with the roll crusher must be limited
should have a rotating and tapping action. to a maximum ratio of 4 to 1. Depending on the fraction
6.4 Sieves—meeting Specification E 11. desired, a one-step reduction is often not possible from the
6.5 Pan Balance, accurate to 0.1 g, capacity 2.0 kg. maximum particle size in the jaw crusher product and inter-
6.6 Vibrator6, with approximately 175- by 250-mm deck, mediate roll settings are used. The sample is reduced to the
must be capable of vibrating at a frequency of 60 Hz and an desired mesh size using as few intermediate settings as possible
amplitude of 0.20 to 0.22 mm (peak) when loaded with a 50-g (but not exceeding the 4 to 1 reduction ratio).
cork ring, 215-g graduated cylinder, and a 100-g coke sample. 8.3.1 With the motor deactivated, and using a method
6.7 Ohmmeter, adequate to test continuity of an electrical appropriate to the roll crusher being used, adjust the roll gap
circuit. according to the following procedure. If the rolls are readily
6.8 Cork Ring, approximately 100-mm inside diameter by accessible, adjustment with a leaf-type feeler gage inserted
25 mm high by 12 mm thick, weight approximately 50 g between the rolls with the motor deactivated is useful.
(round-bottom flask support). 8.3.2 Calculate the ratio of the maximum particle size of the
6.9 Graduated Cylinder, glass, 250 mL, inside diameter roll crusher feed (expressed as the opening, in millimetres, of
approximately 37 mm, base diameter approximately 95 mm. the finest screen through which the largest particles will pass)
6.10 Plastic Funnel, must have a stem with straight sides to the maximum particle size of the bulk density fraction
and an outside diameter of 25 to 30 mm (powder funnel). required (expressed as the opening, in millimetres, of the
6.11 Automatic Timer, Clock, or Watch, with a second coarser of the two screens used to define the bulk density
indicator. fraction).
6.12 Riffle Sampler, enclosed drawer, approximately 380 by 8.3.3 Select the number of crushing steps required from the
290 by 360 mm, 24-slot. following table:
Number of Crushing
7. Precautions Ratio Steps Required
1.1 to 4.0 1
7.1 Exercise care in the operation of the jaw crusher and roll 4.1 to 16.0 2
crusher. Turn power off at the source when setting the gap. 16.1 to 64.0 3
Wear safety glasses and keep hands clear when feeding
8.3.4 For each crushing step required, the roll gap is
material. Turn power off at the source when equipment is
decreased (from a value equivalent to the maximum particle
opened for cleaning after the grinding operation.
size of the feed) by a factor of:
8. Sample Preparation n
=Ratio ~as defined in 8.3.2! (1)
8.1 Use the crushing procedure in 8.2 and subsequent
where:
paragraphs so that contributions to VBD from both as-calcined
n = number of crushing steps required (8.3.3)
and laboratory-crushed particles (which differ significantly in
8.3.5 For example, it is desired to reduce a coke having a
density) are included.
maximum particle size of 6.68 mm to one having a maximum
NOTE 2—Because the vibrated bulk density method is based on the particle size of 0.208 mm. The calculation is as follows:
packing of sized particles, the method of sample preparation can affect Ratio = 32.115 (see 8.3.2)
results due to differences in particle shapes affecting packing characteris-
Crushing steps required = 3 (see 8.3.3)
tics. 3
Factor = =32.115 = 3.179 (see 8.3.4)
8.1.1 Air-dry the laboratory sample, if it appears to be wet, 1st setting: 6.68 mm 4 3.179 = 2.101 mm
prior to crushing to avoid caking. 2nd setting: 2.101 mm 4 3.179 = 0.661 mm
NOTE 3—On agreement by purchaser and supplier, density of only 3rd setting: 0.661 mm 4 3.179 = 0.208 mm
as-calcined particles in the selected size range are determined. If so, 8.3.6 After the roll gap is adjusted, remove the feeler gage
proceed to Section 11 and report as part of the result that only as-calcined (if used), turn on the roll crusher motor, slowly feed 0.3 kg of
particles were used.
the jaw crusher product through the roll crusher, and collect the
NOTE 4—Recommended practice for collecting samples and the equip-
ment and procedures for dividing are described in Test Methods D 346, sample. When more than one roll crushing step is required,
D 2013, D 2234, and D 4057. regrind through smaller openings and collect the sample. Then,
using the appropriate screens (those defining the bulk density
8.2 Jaw Crusher Operation—Use the procedure appropriate
fraction), sample receiver, and cover, sieve the roll-crushed
to the crusher being used, adjust the jaws so that the gap
sample in the sieve shaker. With this final roll crusher setting,
between them (at their closest position to each other in the
at least 30 % of the coke generally will be in the desired
crushing cycle) is approximately 5 mm. Turn on the jaw
particle size range.
8.3.7 This setting will produce roughly equal weights of
6
The calibration procedure described later is specific to a Syntron Model J-1A
coke coarser and finer than the desired fraction, provided that
or J-1B Jogger (from FMC Corp., Material Handling Equipment Div., Homer City, the starting material is sufficiently coarse. If yield is at least
PA). Statistical data were obtained using Model J-1A Joggers. 30 % and the ratio of coarser to finer product is between 0.8

2
 D 4292 – 92 (2002)e1
and 2.0, crushing is satisfactory and the remainder of the are used only for equally spacing height measurements (not as
material is fed through the roll crusher, using as many a volume measurement base line).
intermediate settings as required. The entire roll crusher 10.2 Determination of Accuracy of Graduated Cylinder—
product is consolidated and the desired fraction separated. Using distilled water at 25 6 5°C, fill the graduate to the
8.3.8 At the roll gap setting intended to maximize the final 90-mL mark and determine the weight of water at that volume.
product, proceed as follows if the criteria in 8.3.7 are not met. Using a density of 0.997 g/cm3 for water, determine the true
If after one pass the ratio of coarser to finer-than-desired coke volume. Do the same at 20-mL increments up to the 170-mL
is greater than 2.0, decrease the roll gap to 80 % of its original mark. If the deviation at any indicated volume is greater than
value and test another 0.3 kg sample of jaw crusher product or 60.5 mL, a table of indicated volumes versus true volumes
intermediate roll crusher product, if required. (If the product is should be made for use in computing bulk density.
just slightly too coarse, an alternative procedure is to make 10.3 Vibrator7—Using a hex wrench, remove the four
multiple passes through the roll crusher with the original gap screws that hold the vibrator table and remove the table.
setting.) Loosen the core locking screw. If the aluminum table is
8.3.9 If the ratio is less than 0.8 and the starting material is grounded, remove the ground wire. Turn the vibrator on its side
coarse enough to permit this ratio to be attained, increase the and attach the ohmmeter to the table support and ground. Turn
roll gap by 20 % of its original value and retest with 0.3 kg of the core into the case (clockwise) until the ohmmeter registers
jaw crusher product or intermediate roll crusher product, if zero (core is touching armature). Back off the core (counter-
required. If the starting material is not coarse enough to obtain clockwise) until the ohmmeter reads infinite resistance. Mark
this ratio for the particle size range selected for the test, the zero position with arrows on each side of the screw slot and
disregard this restriction. turn the core out exactly one and three-eighths turns. Replace
8.3.10 These procedures will result in a satisfactory sample the table and tighten the four screws.
as defined in 8.3.7 in the majority of cases. If not, adjust roll
settings or make multiple passes, or both, with trial-and-error 11. Procedure
adjustments until a satisfactory composite sample is obtained 11.1 Weigh 100.0 6 0.1 g of the coke fraction to be tested
from the 2-kg starting sample. Observe that 0.3-kg fractions of into a container. Pour the coke slowly through a funnel into the
the jaw crusher product can be discarded in their entirety if too graduate. Transfer time must be 70 to 100 s. The importance of
fine after roll crushing. Partial consolidation of roll crusher this step on the density value cannot be overemphasized. A
products is not acceptable; that is, once a 0.3-kg sample of jaw rapid pour results in a higher volume than a slow pour and a
crusher product has been passed through the roll crusher, it part of the difference in volume is retained through the
must either be consolidated in its entirety with other roll vibrating step.
crusher products or discarded. A minimum of 210 g of properly 11.2 Fit the rubber stopper tightly to the top of the graduate.
sized vibrated bulk density sample is required. 11.3 Place the graduate inside the retaining ring on the
vibrator.
9. Preparation of Apparatus 11.4 Vibrate for 5 min at a dial setting giving an amplitude
9.1 Graduated Cylinder—Since vibrator amplitude is af- of 0.20 to 0.22 mm (peak) at 60 Hz.
fected by weight on the table, cut off the graduate below the NOTE 5—Although the statistical data in Section 14 were obtained
pouring lip so that the weight is 215 6 10 g. Sand sharp edges. using a 5-min vibration time, a subsequent test at one laboratory on 8 coke
With one common brand of graduated cylinder, this corre- samples resulted in an average vibrated bulk density only 0.022 g/cm3
sponds to an overall length of about 305 mm. Fit the graduate lower after 1 min of vibration than after 5 min of vibration. For routine use
with a No. 8 stopper (tight fit). of this test method within a laboratory, the shorter time may be preferred.
9.2 Vibrator—Fasten the cork ring securely with screws to 11.5 Measurement of Compacted Volume:
the table top of the vibrator as a retainer ring for the graduated 11.5.1 Choose and record a line on the graduate below the
cylinder during the test. (Drill and tap holes in the vibrator top of the compacted sample column from which to measure
table as required.) The inner diameter of the cork ring is the height of the sample. This will be known as the base line.
intentionally larger than the base width of the graduated For example, if the top of the sample column is near the
cylinder. It is designed only to keep the graduated cylinder 100-mL mark, the 90-mL mark may be chosen for the base
from vibrating off the vibrator table. line.
11.5.2 If deemed necessary (see 10.2), consult the table of
10. Calibration of Apparatus
indicated volume versus true volume and use the true volume
10.1 Graduated Cylinder Calibration Factor—Measure the at the base line.
distance, in millimetres, between the 90-mL and 170-mL marks 11.5.3 Using a small metric rule, measure the distance from
on the graduated cylinder. the base line to the top of the compacted column at eight points
B 5 170290/distance in mm (2)

where: 7
This calibration procedure is for a Syntron Model J-1A or J-1B Jogger only.
B = calibration factor, mL/mm. With a weight equivalent to the total weight of the cork ring, graduate, and test
sample attached to the vibrator table, the procedure results in a vibration amplitude
Wrap a piece of masking tape around the graduate with the
of 0.20–0.22 mm (peak) at a fixed 60 Hz at a dial setting of 5 for Model J-1A or 35
190-mL mark at the bottom of the tape. Make eight marks on for Model J-1B. To be satisfactory, other vibrator models must be able to be
the bottom of the tape equidistantly around the cylinder. These calibrated to produce these vibration parameters.

3
 D 4292 – 92 (2002)e1
around the graduate. These distances are measured to the participants to pass through a 0.83-mm opening, (No. 20 sieve)
nearest 0.5 mm. Record and average the measurements. and be retained on a 0.30-mm opening, (No. 50 sieve).
11.6 Repeat the procedure, beginning at 11.1, with a second Statistical information was calculated in accordance with
100.0-g sample. methods outlined in RR:D02-1007.
12. Calculations NOTE 6—Precision for vibrated bulk density on other ranges has not
been determined.
12.1 Calculate the volume as follows:
14.2 Precision—The precision of this test method as deter-
Volume, mL 5 ~A 3 B! 1 C (3)
mined by the statistical examination of interlaboratory test
where: results is as follows.
A = average sample height from base line, mm, 14.2.1 Repeatability—The difference between successive
B = calibration factor, mL/mm, and results obtained by the same operator with the same apparatus
C = base line, mL, corrected for graduated cylinder error, if under constant operating conditions on identical test material
necessary (see 10.2). would, in the long run, in the normal and correct operation of
weight in grams the test method, exceed the following values only in one case
VBD, g/cm3 5 (4) in twenty.
volume in millilitres
Average the values for the two determinations. Repeatability 5 0.014 g/cm3 (5)

13. Report 14.2.2 Reproducibility—The difference between two single

and independent results obtained by different operators work-
13.1 Report the average of the two determinations to the ing in different laboratories on identical test material would, in
nearest 0.001 g/cm3. The particle size range must be reported the long run, exceed the following values only in one case in
as part of the test results. For example, VBD (−30 + 50 sieve twenty.
size) = 0.890 g/cm3.
Reproducibility 5 0.046g/cm3 (6)
14. Precision and Bias 8
14.3 Bias—This test method is empirical and no statement
14.1 Precision was determined by interlaboratory testing of as to bias is made.
calcined petroleum coke samples crushed and sized by the
15. Keywords
8
Supporting data have been filed at ASTM International Headquarters and may 15.1 calcined petroleum coke; porosity; vibrated bulk
be obtained by requesting Research Report RR: D02–1166. density

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