ASTM D6374-99
(Test Method)Standard Test Method for Volatile Matter in Green Petroleum Coke Quartz Crucible Procedure
Standard Test Method for Volatile Matter in Green Petroleum Coke Quartz Crucible Procedure
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 dedusting material content.
1.6 The values stated in SI units are to be regarded as the standard.
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 of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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An American National Standard
Designation:D6374–99
Standard Test Method for
Volatile Matter in Green Petroleum Coke Quartz Crucible
Procedure
This standard is issued under the fixed designation D 6374; 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.
1. Scope 3.1.2 analysis time—period test samples are placed in the
furnace, as determined in Section 9 (5 to 10 min).
1.1 This test method covers the determination of the volatile
3.1.3 bulk sample—the reduced and divided representative
matter produced by pyrolysis or evolved when petroleum coke
portion of a gross sample as prepared for shipment to and
is subjected to the specific conditions of the test method.
received by a laboratory, to be prepared for analysis.
1.2 The interlaboratory study for precision covered materi-
3.1.4 green petroleum coke—same as raw petroleum coke
als with a volatile matter concentration ranging from about 8 to
3.1.5 gross sample—the original, uncrushed, representative
16 %.
sample taken from a shipment or lot of coke.
1.3 Samples having a thermal history above 600°C are
3.1.6 petroleum coke—a solid, carbonaceous residue pro-
excluded.
duced by thermal decomposition of heavy petroleum fractions
1.4 This test method is empirical and requires the entire test
or cracked stocks, or both.
procedure to be closely followed to ensure that results from
3.1.7 raw petroleum coke—petroleum coke that has not
different laboratories will be comparable.
been calcined.
1.5 This test method is not satisfactory for determining
3.1.8 test sample—the weighed portion of the analysis
dedusting material content.
sample actually used in a test.
1.6 The values stated in SI units are to be regarded as the
3.1.9 volatile matter—themasslossonheatingexpressedas
standard.
a percent of the moisture free sample used.
1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user to establish appropriate safety and
4.1 Volatile matter of a moisture free petroleum coke is
health practices and to determine the applicability of regula-
determined by measuring the mass loss of the coke when
tory limitations prior to use.
heated under the exact conditions of this test method.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:
5.1 The volatile matter of petroleum coke affects the density
E 11 Specification for Wire Cloth and Sieves for Testing
of coke particles and can affect artifacts produced from further
Purposes
processing of the coke.
E 220 Test Method for Calibration of Thermocouples by
5.2 The volatile matter can be used in estimating the
Comparison Techniques
calorific value of coke.
3. Terminology
6. Interferences
3.1 Definitions of Terms Specific to This Standard:
6.1 Moisture has a double effect. The mass loss is increased
3.1.1 analysis sample—the reduced and divided representa-
and the moisture free sample weight is decreased by the
tive portion of a bulk sample, prepared for use in the labora-
amount of moisture actually present in the test sample.
tory.
6.2 Particle Size Effect:
6.2.1 The particle size range of the analysis sample affects
This test method is under the jurisdiction of ASTM Committee D-2 on
the volatile matter. The coarser the analysis sample, the lower
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
the reported volatile matter will be. Crush analysis sample (see
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Materials.
Annex A1) to pass a 0.250-mm opening (No. 60) sieve but do
Current edition approved Feb. 10, 1999. Published April 1999.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
not overcrush. A 0.125-mm opening (No. 120) sieve should
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
retain 40 to 55 % of the sample. Do not obtain the analysis
Standards volume information, refer to the standard’s Document Summary page on
sample is by scalping and discarding a portion of the sample.
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6374–99
6.2.2 Any segregation of particle sizes within the analysis 10. Procedure
sampleshallbecorrectedbyreblendingthesamplejustpriorto
10.1 Ignite the quartz crucible and cover at 950 6 20°C for
weighing the test sample.
5 min periods to constant mass (60.5 mg). Do not cover the
6.3 Thefurnaceshallrecoverto950 620°Cbeforethetime
crucible at this time to allow the carbon to burn off. Cool to
limit is reached. If the furnace does not recover to the starting
ambient temperature in a desiccator before weighing the
temperature within a maximum of 10 min, reduce the number
crucible and cover.
of samples being analyzed until recovery is achieved within 10
NOTE 1—Placing the empty crucibles in the inverted cover when
min (see Section 9).
igniting will reduce breakage and chipping.
7. Apparatus
10.2 Avoiding segregation of particles, transfer 1 g6 10 mg
of the analysis sample (see Annex A1) to the crucible, weigh
7.1 Electric Muffle Furnace—Calibrated (Test Method
E 220) and regulated to maintain a temperature of 950 6 20°C the crucible with its contents, and cover to the nearest 0.1 mg.
Place the cover on the crucible, and place in sample rack.
(1742°F), as measured by a thermocouple mounted inside the
furnace. Its heat capacity shall be such that the initial tempera- 10.3 Set the timer for the analysis time (5 to 10 min). Place
ture is regained after the introduction of a cold rack of samples the rack in the furnace. Start the timer.
within 10 min.
NOTE 2—Place the rack in the center of the furnace. Do not allow the
7.2 Quartz Crucibles, self-sealing, 10 mL capacity with
rack to touch the walls of the furnace.
covers.
10.4 After the analysis time (65 s), remove the rack from
7.3 Rack,stainlesssteel,designedtoholdupto20crucibles.
the furnace and immediately place on a heat sink.
7.4 Rifflers, with hoppers and closures.
10.5 Weigh the crucible after it has cooled to room tem-
7.5 Jaw Crusher and Roll Crusher—Other style crushers
perature and before it has been at room temperature for longer
that allow control over particle size without contamination are
than 20 min.
acceptable (see Annex A1).
7.6 Balance, capable of weighing to 0.1 mg.
NOTE 3—If cool down is not in a humidity controlled area, desiccation
7.7 Dessicator. is required.
7.8 Sieves, meeting Specification E 11.
11. Calculation
7.9 Timers, stopwatch or second timer.
11.1 Calculate the volatile matter of the moisture free
7.10 Heat Sink, 1/2 in. plate steel or other heat resistant
prepared coke as follows:
material large enough to hold the crucible rack.
Volatile matter, mass % 5 ~~A2B!!/C! 3 100 (1)
8. Precautions
where:
8.1 Effusionofgaseousproducts,includingsootandvarious
A = weight of crucible and prepared sample prior to analy-
hydrocarbons, and the increase of heat associated with the test
sis, g,
can make the use of a hood desirable.
B = weight of crucible and prepared sample after analysis,
9. Furnace Calibration
g, and
C = weight of prepared sample, g.
9.1 Avoiding segregation of particles, transfer1g(6 0.05
g) of an analysis sample (seeAnnexA1) to each crucible in the
12. Report
rack, weigh each crucible with its contents, and cover to the
nearest 0.1 mg. Place the cover on the crucible, and place in
12.1 Report to one decimal the average of duplicate deter-
sample rack.
minations that agree within 0.5 %. Wh
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