ASTM D4421-94(1999)
(Test Method)Standard Test Method for Volatile Matter in Petroleum Coke (Withdrawn 2004)
Standard Test Method for Volatile Matter in Petroleum Coke (Withdrawn 2004)
SCOPE
1.1 This test method determines the volatile matter produced by pyrolysis or evolved when petroleum coke, or both, is subjected to the specific conditions of the test. Samples having a thermal history above 600°C are excluded.
1.2 This test method is empirical and requires the entire test procedure to be closely followed to ensure results from different laboratories to be comparable.
1.3 This test method is not satisfactory for dedusting material content.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.5 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. Specific precautionary statements are given in Section 8.
General Information
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation:D4421–94 (Reapproved 1999)
Standard Test Method for
Volatile Matter in Petroleum Coke
This standard is issued under the fixed designation D4421; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3.1.3 gross sample—the original, uncrushed, representative
portion taken from a shipment or lot of coke.
1.1 This test method determines the volatile matter pro-
3.1.4 petroleum coke—a solid, carbonaceous residue pro-
duced by pyrolysis or evolved when petroleum coke, or both,
duced by thermal decomposition of heavy petroleum fractions
is subjected to the specific conditions of the test. Samples
and cracked stocks.
having a thermal history above 600°C are excluded.
3.1.5 test sample—the weighed portion of the analysis
1.2 This test method is empirical and requires the entire test
sample actually used in a test.
procedure to be closely followed to ensure results from
3.1.6 volatile matter—an empirical value equal to the mass
different laboratories to be comparable.
loss on heating expressed as a percent of the moisture free
1.3 This test method is not satisfactory for dedusting mate-
sample used. It is determined only by thisASTM standard for
rial content.
petroleum coke.
1.4 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
4. Summary of Test Method
only.
4.1 Volatile matter of a moisture free petroleum coke is
1.5 This standard does not purport to address all of the
determined by measuring the mass loss of the coke when
safety concerns, if any, associated with its use. It is the
heated under the exact conditions of this procedure.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Significance and Use
bility of regulatory limitations prior to use. Specific precau-
5.1 Thevolatilematterofpetroleumcokeaffectsthedensity
tionary statements are given in Section 8.
of coke particles and can affect artifacts produced from further
2. Referenced Documents processing of the coke.
5.2 The volatile matter can be used in estimating the
2.1 ASTM Standards:
calorific value of coke.
E11 Specification for Wire-Cloth Sieves for Testing Pur-
poses
6. Interferences
E220 Test Method for Calibration of Thermocouples by
6.1 Moisture has a double effect.The mass loss is increased
Comparison Techniques
and the moisture free sample weight is decreased by the
amount of moisture actually present in the test sample.
3. Terminology
6.2 Particle Size Effect:
3.1 Descriptions of Terms Specific to This Standard:
6.2.1 The particle size range of the analysis sample affects
3.1.1 analysis sample—the reduced and divided representa-
the volatile matter. The coarser the analysis sample, the lower
tive portion of a bulk sample, prepared for use in the labora-
thevolatilematterwillbe.Theanalysissample(seeAnnexA1)
tory.
iscrushedtopassaNo.60sieve(0.250-mmopening)butisnot
3.1.2 bulk sample—the reduced and divided representative
overcrushed. A No. 120 sieve (0.125-mm opening) should
portion of a gross sample as prepared for shipment to and
retain 40 to 55% of the sample. The analysis sample is not to
received by a laboratory, to be prepared for analysis.
beobtainedbyscalpinganddiscardingaportionofthesample.
6.2.2 Any segregation of particle sizes within the analysis
sampleshallbecorrectedbyreblendingthesamplejustpriorto
This test method is under the jurisdiction of ASTM Committee D-2 on
weighing the test sample.
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
D02.05 on Properties of Fuels, Petroleum Coke, and Oil Shale.
6.3 Downward drift of furnace temperature caused by an
Current edition approved Sept. 15, 1994. Published November 1994. Originally
increase in the millivolts per degrees Celsius generated by an
published as D4421–84. Last previous edition D4421–89.
aging type K thermocouple produces a lower volatile matter
Annual Book of ASTM Standards, Vol 14.02.
Annual Book of ASTM Standards, Vol 14.03. value (Test Method E220).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4421
6.4 Diffusion of air into the crucible caused by a poor fit weighing the crucible and cover. Do not keep the crucible at
between the crucible and its cover or by any other source of room temperature more than 20 min before it is weighed.
availableoxygencauseshighanderraticvolatilemattervalues. Record all masses to 0.1 mg.
6.5 Free or tramp iron or mill scale in the coke coats the
10.2 Avoidingsegregationofparticles,transfer1g(61mg)
surface of the platinum crucible and decreases its life. The
of the analysis sample (Annex A1) to the crucible and weigh
coating tends to form an oxide film during the preburning step
thecruciblewithitscontentandcovertothenearest0.1mg.Fit
(10.1). The oxide film provides a source of excess weight loss
the cover on the crucible and press it gently into position.
equal to almost twice the oxygen weight gained. Clean the
Avoid physical distortion of the crucible and cover.
crucible and buff with sand. Buffing will restore luster to the
10.3 Manual Method:
surface of the crucible.
10.3.1 Set the crucible vertically in the holder and center it
overthefurnaceopeningwiththebottomofthecrucibleinline
7. Apparatus
with the top surface of the transite furnace cover (Note 1). Be
7.1 Furnace, Fieldner, electric, ASTM, calibrated (Test
sure neither the crucible nor the holder touch the wall of the
Method E220) and regulated to maintain a temperature of
furnace. Start the timer.
950°C (1742°F) 6 15°C as measured by a thermocouple
NOTE 1—There are some coke-VM relationships which require the
mounted inside the furnace.
crucible bottom to be 6 mm ( ⁄4 in.) above the top surface of the
7.2 Nickel Chromium Crucible Support for the platinum
transite-coverintheinitialposition.Theserelationshipspreventcontrolof
crucible.
sparks or flames, or both.
7.3 Platinum 90%−Rhodium 10% Crucible, volatile mat-
terform,reinforcedtopandbottom,capacity15mL;height33 10.3.2 After60s(65s),lowertheholderapproximately8.5
mm; top diameter 29 mm; fitted with a capsule-type cover 10 mm( ⁄3in.)intothefurnace.Theholderisloweredanother8.5
mm high. The cover is to have a 0.5-mm diameter hole drilled mm ( ⁄3in.) after each total elapsed time of 120, 180, 240, 300,
through the center. The total weight, crucible and cover, and 360 s (each6 5 s).After the move at 360 s, the top of the
approximately 20 g. crucible should be 19 mm ( ⁄4 in.) below the top surface of the
7.4 Reshapers for the platinum crucible and cover. transite cover. DO NOT position the bottom of the crucible
morethan57mm(2 ⁄4in.)belowthetopsurfaceofthetransite
7.5 Rifflers, with hoppers and closures.
7.6 Jaw Crusher and Roll Crusher—Other style crushers cover at this time (Note 2).
which allow control over particle size without contamination
NOTE 2—The heating rate is extremely important since the test is
are acceptable. (See Annex A1.)
empirical and equilibrium is not achieved. The heating rate is controlled
7.7 Sieves, as required (Specification E11).
by the rate of lowering the crucible into the furnace. Once the holder is
7.8 Timers, stopwatch or second-timer accurate to 61s.
positioned immediately over the furnace the time schedule must be
observed. The crucible shall not be removed, or raised and relowered,
8. Precautions
without verifying the test.
8.1 Effusionofgaseousproducts,includingsootandvarious
10.3.3 If at any time during the test, sparking occurs such
hydrocarbons and the increase of heat associated with the test
that the sparks are seen to be above the height of the crucible
can make use of a hood desirable.
cover or if a flame or flames occur such that the sum of all
visible simultaneous flames extend above the height of the
9. Preparation of Furnace
crucible cover, the test must be repeated with slight variations
9.1 If desired, the radiant heat loss to the room from the
during the first 600 s. These variations are to be made with
outsidemetalcylindercanbereducedbyinsulatingthefurnace
respecttothepositionwhenthesparksorflamesoccur.Amore
with a thick layer of insulation and glass wool.
severe heatup rate (more rapidly lowering) will result in less
9.2 Fit a thermocouple into the bottom of the furnace. Use
sparking or flaming subsequently but can result in sparking or
borosilicate glass wool to close the opening around the
flaming earlier in the test. Discretion is necessary.Amaximum
thermocouple. Adjust the thermocoupled position so it rests 2
furnacedepthforthebottomofthecrucibleof57mm(2 ⁄4in.)
to 3 mm below the bottom of the platinum crucible with the
is to be maintained during the first 600 s.
platinum crucible positioned in the crucible support and the
10.3.4 After 600 s (65 s) total elapsed time, lower the
support resting on the top of the furnace.
holder so the brass ring of the holder rests directly upon the
9.3 Hang a 100 to 150-mm (4 to 6-in.) mirror above the
transite furnace cover (maximum depth in furnace).
furnace, positioned to allow the operator to observe the
10.3.5 After960s(65s)totalelapsedtime,raisetheholder
platinum crucible during the time it is positioned in the
and crucible out of the furnace and immediately place the
furnace.
crucible in a desiccator.
10. Procedure
10.3.6 Weigh the crucible after it has cooled to room
temperature and before it has been at room temperature for
10.1 Ignite a platinum crucible and cover at 950°C for
longer than 20 min.
5-min periods to constant mass (60.5 mg). A burner or any
10.4 Automatic Method (See Annex A2):
furnace is to be used but the crucible can be set in a nic
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