ASTM D6374-22

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Designation: D6374 − 12 (Reapproved 2017) D6374 − 22
Standard Test Method for
Volatile Matter in Green Petroleum Coke Quartz Crucible
Procedure
This standard is issued under the fixed designation D6374; 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.
ε NOTE—SI units formatting was corrected editorially in July 2017.
1. Scope Scope*
1.1 This test method covers the determination of the volatile matter produced by pyrolysis or evolved when petroleum coke is
subjected to the specific conditions of the test method.
1.2 The interlaboratory study for precision covered materials with a volatile matter concentration ranging from about 8 % to 16 %.
1.3 Samples having a thermal history above 600 °C are excluded.
1.4 This test method is empirical and requires the entire test procedure to be closely followed to ensure that results from different
laboratories will be comparable.
1.5 This test method is not satisfactory for determining de-dusting material content.
1.6 The values stated in SI units are to be regarded as standard.
1.6.1 Exception—Non-SI units are shown in parentheses for information only.
1.7 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 to establish appropriate safety safety, health, and healthenvironmental practices and to determine the applicability of
regulatory limitations prior to use.
1.8 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:
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
E220 Test Method for Calibration of Thermocouples By Comparison Techniques
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 May 1, 2017May 1, 2022. Published July 2017May 2022. Originally approved in 1999. Last previous edition approved in 20122017 as
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D6374 – 12.D6374 – 12 (2017) . DOI: 10.1520/D6374-12R17E01.10.1520/D6374-22.
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
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3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 analysis sample, n—the reduced and divided representative portion of the bulk sample, prepared for use in the laboratory.
3.1.2 analysis time, n—period test samples are placed in the furnace, as determined in Section 9 (5 min to 10 min).
3.1.3 bulk sample, n—the reduced and divided representative portion of the gross sample as prepared for shipment to and received
by a laboratory, to be prepared for analysis.
3.1.4 green petroleum coke, n—same as raw petroleum coke
3.1.5 gross sample, n—the original, uncrushed, representative portion taken from a shipment or lot of coke.
3.1.6 petroleum coke, n—a solid, carbonaceous residue produced by thermal decomposition of heavy petroleum fractions or
cracked stocks, or both.
3.1.7 raw petroleum coke, n—petroleum coke that has not been calcined.
3.1.8 test sample, n—the weighed portion of the analysis sample actually used in a test.
3.1.9 volatile matter, n—the mass loss on heating expressed as a percent of the moisture free sample used.
4. Summary of Test Method
4.1 Volatile matter of a moisture free petroleum coke is determined by measuring the mass loss of the coke when heated under
the exact conditions of this test method.
5. Significance and Use
5.1 The volatile matter of petroleum coke affects the density of coke particles and can affect artifacts produced from further
processing of the coke.
5.2 The volatile matter can be used in estimating the calorific value of coke.
6. Interferences
6.1 Moisture has a double effect. The mass loss is increased and the moisture free sample weight is decreased by the amount of
moisture actually present in the test sample.
6.2 Particle Size Effect:
6.2.1 The particle size range of the analysis sample affects the volatile matter. The coarser the analysis sample, the lower the
reported volatile matter will be. Crush analysis sample (see Annex A1) to pass a 0.250 mm opening (No. 60) sieve but do not
overcrush. A 0.125 mm opening (No. 120) sieve should retain 40 % to 55 % of the sample. Do not obtain the analysis sample by
scalping and discarding a portion of the sample.
6.2.2 Any segregation of particle sizes within the analysis sample shall be corrected by reblending the sample just prior to
weighing the test sample.
6.3 The furnace shall recover to 950 °C 6 20 °C before the time limit is reached. If the furnace does not recover to the starting
temperature within a maximum of 10 min, reduce the number of samples being analyzed until recovery is achieved within 10 min
(see Section 9).
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7. Apparatus
7.1 Electric Muffle Furnace—Calibrated (Test Method E220) and regulated to maintain a temperature of 950 °C 6 20 °C
(1742 °F), as measured by a thermocouple mounted inside the furnace. Its heat capacity shall be such that the initial temperature
is regained after the introduction of a cold rack of samples within 10 min.
7.2 Quartz Crucibles, self-sealing, 10 mL capacity with covers.
7.3 Rack, stainless steel, designed to hold up to 20 crucibles.
7.4 Rifflers, with hoppers and closures.
7.5 Jaw Crusher and Roll Crusher—Other style crushers that allow control over particle size without contamination are acceptable
(see Annex A1).
7.6 Balance, capable of weighing to 0.1 mg.
7.7 Dessicator.
7.8 Sieves, meeting Specification E11.
7.9 Timers, stopwatch or second timer.
7.10 Heat Sink, 12.7 mm plate steel or other heat resistant material large enough to hold the crucible rack.
8. Precautions
8.1 Effusion of gaseous products, including soot and various hydrocarbons, and the increase of heat associated with the test can
make the use of a hood desirable.
9. Furnace Calibration
9.1 Avoiding segregation of particles, transfer 1 g (60.05 g) of an analysis sample (see Annex A1) to each crucible in the rack,
weigh each crucible with its contents, and cover to the nearest 0.1 mg. Place the cover on the crucible, and place in sample rack.
9.2 Record the furnace temperature at equilibrium (950 °C 6 20 °C).
9.3 Place the full rack of samples in the furnace, and start the timer.
9.4 Monitor the furnace temperature. Record the elapsed time required to return to the equilibrium temperature recorded in 9.2.
If the time exceeds 10 min, repeat the procedure, reducing the number of crucibles in the rack until temperature recovery is
completed within 10 min of the introduction of the sample rack.
9.5 When temperature recovery is achieved within the 10 min period, record the number of crucibles in the rack. This number of
crucibles shall be in the rack for all future runs (fill empty spaces in the stand with empty crucibles when necessary).
9.6 Round the recorded elapsed time to the next higher minute. This rounded time will be the analysis time for future runs (5 min
minimum).
10. Procedure
10.1 Ignite the quartz crucible and cover at 950 °C 6 20 °C for 5 min periods to constant mass (60.5 mg). Do not cover the
crucible at this time to allow the carbon to burn off. Cool to ambient temperature in a desiccator before weighing the crucible and
cover.
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NOTE 1—Placing the empty crucibles in the inverted cover when igniting will reduce breakage and chipping.
10.2 Avoiding segregation of particles, transfer 1 g 610 mg of the analysis sample (see Annex A1) to the crucible, weigh the
crucible with its contents, and cover to the nearest 0.1 mg. Place the cover on the crucible, and place in sample rack.
10.3 Set the timer for the analysis time (5 min to 10 min). Place the rack in the furnace. Start
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