ASTM D4292-23

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Designation: D4292 − 17 D4292 − 23
Standard Test Method for
Determination of Vibrated Bulk Density of Calcined
Petroleum Coke
This standard is issued under the fixed designation D4292; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
1.1 This test method covers the determination of bulk density of a representative 2 kg sample of calcined petroleum coke, after
vibration to increase compaction.
1.2 The procedure is limited to particles passing through a 6.68 mm opening sieve (equivalent to a 0.265 in. USA Series) and
retained on a 0.21 mm opening sieve (equivalent to a 70 mesh USA Series). Further, the procedure is limited to a specific test
sample having particles retained between screens having openings that differ by a factor of less than 2=2 and preferably less than
2.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis
D2013 Practice for Preparing Coal Samples for Analysis
D2234/D2234M Practice for Collection of a Gross Sample of Coal
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D5709 Test Method for Sieve Analysis of Petroleum Coke
D6969 Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
D6970 Practice for Collection of Calcined Petroleum Coke Samples for Analysis
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved Dec. 1, 2017Nov. 1, 2023. Published January 2018November 2023. Originally approved in 1992. Last previous edition approved in 20102017
as D4292 – 10.D4292 – 17. DOI: 10.1520/D4292-17.10.1520/D4292-23.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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
D4292 − 23
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, refer to Terminology D4175.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 as-calcined particles, n—of coke, those particles that have not been subject to laboratory crushing.
3.2.2 bulk density, n—of coke, the ratio of the mass of a collection of particles of a specified particle size range to the volume
occupied.
3.2.3 gross sample, n—the original, uncrushed, representative portion taken from a shipment or lot of coke.
3.2.4 laboratory crushed particles, n—of coke, those particles of petroleum coke that have been crushed in the laboratory.
4. Summary of Test Method
4.1 After appropriate crushing of the calcined coke, using both the jaw crusher and roll crusher, the test volume of 100 g is
measured after vibration and the bulk density is calculated.
5. Significance and Use
5.1 Vibrated bulk density, VBD, is an indicator of calcined petroleum coke porosity, which affects its suitability for use in
pitch-bonded carbon applications. (Warning—Vibrated bulk density for a sample of calcined petroleum coke is strongly dependent
upon average particle size and particle size range. Bulk density tends to increase with decreasing coke size. A narrow particle size
range for this test minimizes the possibility for variation due to skewing of the test sample toward either screen defining the sample.
Particle size range tested should be agreed upon by the purchaser and supplier.)
NOTE 1—An example of the use of VBD to characterize coke for prebaked anodes for aluminum smelting is reported by Belitskus who found particles
passing through a 0.59 mm opening, No. 30, sieve and 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, sieve and retained on a 1.17 mm opening, No. 16, sieve for the continuous Soderberg anode process and
particles passing through a 6.68 mm opening sieve (equivalent to a 0.265 in. USA Series) and retained on a 3.33 mm opening, No. 6, sieve for graphite
electrode manufacture.
6. Apparatus
6.1 Jaw Crusher, laboratory type; jaw opening, approximately 50 mm by 200 mm; jaws can be set to gaps of approximately
3.2 mm to 12.7 mm; manganese steel jaw plates.
6.2 Roll Crusher, laboratory type; glass hardened rolls; roll diameter, approximately 200 mm; roll width, approximately 150 mm;
gap range from 0 mm to 12.7 mm, both rolls shall rotate to crush the material. Do not use a disc mill, disc type grinder, or disc
pulverizer, since these contain one stationary roll. Prior to use, check and adjust the springs on the roll crusher according to the
manufacturer’s recommendation.
6.3 Sieve Shaker, electrical drive with an automatic timer; should have a rotating and tapping action.
6.4 Sieves—meeting Specification E11.
6.5 Pan Balance, accurate to 0.1 g, capacity 2.0 kg.
6.6 Vibrator ,with approximately 175 mm by 250 mm deck, must be capable of vibrating at a frequency of 60 Hz and an amplitude
of 0.20 mm to 0.22 mm (peak) when loaded with a 50 g cork ring, 215 g graduated cylinder, and a 100 g coke sample.
Belitskus, D. L., “Evaluating Calcined Coke for Aluminum Smelting by Bulk Density,” Aluminium, Vol 51, No. 2, 1975.
The calibration procedure described later is specific to a Syntron Model J-1A or J-1B Jogger (from FMC Corp., Material Handling Equipment Div., Homer City, PA).
Statistical data were obtained using Model J-1A Joggers.
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6.7 Ohmmeter, adequate to test continuity of an electrical circuit.
6.8 Cork Ring, approximately 100 mm inside diameter by 25 mm high by 12 mm thick, weight approximately 50 g
(round-bottom flask support).
6.9 Graduated Cylinder, glass, 250 mL, inside diameter approximately 37 mm, base diameter approximately 95 mm.
6.10 Plastic Funnel, must have a stem with straight sides and an outside diameter of 25 mm to 30 mm (powder funnel).
6.11 Automatic Timer, Clock, or Watch, with a second indicator.
6.12 Riffle Sampler, enclosed drawer, approximately 380 mm by 290 mm by 360 mm, 24 slot.
6.13 Feeler Gauges, mm size for checking the gap settings on the roll crusher.
7. Precautions
7.1 Exercise care in the operation of the jaw crusher and roll crusher. Turn power off at the source when setting the gap. Wear
safety glasses and keep hands clear when feeding material. Turn power off at the source when equipment is opened for cleaning
after the grinding operation.
8. Sample Preparation
8.1 Use the crushing procedure in 8.2 and subsequent paragraphs so that contributions to VBD from both as-calcined and
laboratory-crushed particles (which differ significantly in density) are included. Do not remove dedust oil from the sample prior
to sample preparation or testing.
NOTE 2—Because the vibrated bulk density method is based on the packing of sized particles, the method of sample preparation can affect results due
to differences in particle shapes affecting packing characteristics.
8.1.1 Air-dry the laboratory sample, if it appears to be wet, prior to crushing to avoid caking.
NOTE 3—On agreement by purchaser and supplier, density of only as-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-calcined particles were used.
NOTE 4—Recommended practice for collecting samples and the equipment and procedures for dividing are described in Test Methods D346, D2013,
D2234/D2234M, and D4057 and Practices D6969 and D6970.
8.2 Jaw Crusher Operation—Use the procedure appropriate to the jaw crusher being used, adjust the jaws so that the gap between
them (at their closest position to each other in the crushing cycle) is approximately 5 mm. Turn on the jaw crusher motor, slowly
feed the sample through the jaw crusher, and collect the product for further reduction through a roll crusher. In this step, the entire
gross sample shall pass through the jaw crusher.
8.3 Roll Crusher Operation—(Warning—To avoid damage to the rolls, size reduction with the roll crusher must be limited to a
maximum ratio of 4 to 1. Depending on the fraction desired, a one-step reduction is often not possible from the maximum particle
size in the jaw crusher product and intermediate roll settings are used. The sample is reduced to the desired mesh size using as
few intermediate settings as possible (but not exceeding the 4 to 1 reduction ratio).
8.3.1 With the motor deactivated, and using a method appropriate to the roll crusher being used, adjust the roll gap according to
the following procedure. If the rolls are readily accessible, adjustment with a leaf-type feeler gage inserted between the rolls with
the motor deactivated is useful.
8.3.2 Calculate the ratio of the maximum particle size of the roll crusher feed (expressed as the opening, in millimetres, of the
finest screen through which the largest particles will pass) to the maximum particle size of the bulk density fraction required
(expressed as the opening, in millimetres, of the coarser of the two screens used to define the bulk density fraction).
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8.3.3 Select the number of crushing steps required from the following table:
Number of Crushing
Ratio Steps Required
1.1 to 4.0 1
4.1 to 16.0 2
16.1 to 64.0 3
8.3.4 For each crushing step required, the roll gap is decreased (from a value equivalent to the maximum particle size 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 a maximum particle size of 6.68 mm to one having a maximum particle
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=32.11553.179 (see 8.3.4)
1st setting: 6.68 mm ÷ 3.179 = 2.101 mm
2nd setting: 2.101 mm ÷ 3.179 = 0.661 mm
3rd setting: 0.661 mm ÷ 3.179 = 0.208 mm
8.3.6 After the roll gap is adjusted, remove the feeler gage (if used), turn on the roll crusher motor, slowly feed 0.3 kg of the jaw
crusher product through the roll crusher, and collect the sample. When more than one roll crushing step is required, regrind through
smaller openings the entire 0.3 kg sample, and collect the sample. Do not sieve the sample between crushing steps. Then, using
the appropriate screens (those defining the bulk density fraction), sample receiver, and cover, sieve the roll-crushed sample in the
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