ASTM D6374-12(2017)e1

Standard Test Method for Volatile Matter in Green Petroleum Coke Quartz Crucible Procedure

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.
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 and health 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.

General Information

• Status: Historical
• Publication Date: 30-Apr-2017
• ICS: 73.040 - Coals
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.05 - Properties of Fuels, Petroleum Coke and Carbon Material

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
´1
Designation: D6374 − 12 (Reapproved 2017)
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 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method covers the determination of the volatile
E11 Specification for Woven Wire Test Sieve Cloth and Test
matter produced by pyrolysis or evolved when petroleum coke
Sieves
is subjected to the specific conditions of the test method.
E220 Test Method for Calibration of Thermocouples By
1.2 The interlaboratory study for precision covered materi-
Comparison Techniques
alswithavolatilematterconcentrationrangingfromabout8 %
3. Terminology
to 16 %.
3.1 Definitions of Terms Specific to This Standard:
1.3 Samples having a thermal history above 600 °C are
3.1.1 analysis sample, n—the reduced and divided represen-
excluded.
tative portion of the bulk sample, prepared for use in the
1.4 This test method is empirical and requires the entire test laboratory.
procedure to be closely followed to ensure that results from
3.1.2 analysis time, n—period test samples are placed in the
different laboratories will be comparable.
furnace, as determined in Section 9 (5 min to 10 min).
3.1.3 bulk sample, n—the reduced and divided representa-
1.5 This test method is not satisfactory for determining
tiveportionofthegrosssampleaspreparedforshipmenttoand
de-dusting material content.
received by a laboratory, to be prepared for analysis.
1.6 The values stated in SI units are to be regarded as
3.1.4 green petroleum coke, n—same as raw petroleum coke
standard.
3.1.5 gross sample, n—the original, uncrushed, representa-
1.6.1 Exception—Non-SI units are shown in parentheses for
tive portion taken from a shipment or lot of coke.
information only.
3.1.6 petroleum coke, n—a solid, carbonaceous residue
1.7 This standard does not purport to address all of the
produced by thermal decomposition of heavy petroleum frac-
safety concerns, if any, associated with its use. It is the
tions or cracked stocks, or both.
responsibility of the user to establish appropriate safety and
3.1.7 raw petroleum coke, n—petroleum coke that has not
health practices and to determine the applicability of regula-
been calcined.
tory limitations prior to use.
3.1.8 test sample, n—the weighed portion of the analysis
1.8 This international standard was developed in accor-
sample actually used in a test.
dance with internationally recognized principles on standard-
3.1.9 volatile matter, n—the mass loss on heating expressed
ization established in the Decision on Principles for the
as a percent of the moisture free sample used.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
4. Summary of Test Method
Barriers to Trade (TBT) Committee.
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.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
SubcommitteeD02.05onPropertiesofFuels,PetroleumCokeandCarbonMaterial. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
CurrenteditionapprovedMay1,2017.PublishedJuly2017.Originallyapproved contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
in 1999. Last previous edition approved in 2012 as D6374 – 12. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D6374-12R17E01. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D6374 − 12 (2017)
5. Significance and Use 9. Furnace Calibration
5.1 The volatile matter of petroleum coke affects the density 9.1 Avoidingsegregationofparticles,transfer1 g(60.05 g)
of coke particles and can affect artifacts produced from further of an analysis sample (see Annex A1) to each crucible in the
processing of the coke. rack, weigh each crucible with its contents, and cover to the
nearest 0.1 mg. Place the cover on the crucible, and place in
5.2 The volatile matter can be used in estimating the
sample rack.
calorific value of coke.
9.2 Record the furnace temperature at equilibrium (950 °C
6. Interferences 6 20 °C).
9.3 Place the full rack of samples in the furnace, and start
6.1 Moisture has a double effect. The mass loss is increased
and the moisture free sample weight is decreased by the the timer.
amount of moisture actually present in the test sample.
9.4 Monitor the furnace temperature. Record the elapsed
6.2 Particle Size Effect: time required to return to the equilibrium temperature recorded
in 9.2. If the time exceeds 10 min, repeat the procedure,
6.2.1 The particle size range of the analysis sample affects
reducing the number of crucibles in the rack until temperature
the volatile matter. The coarser the analysis sample, the lower
recovery is completed within 10 min of the introduction of the
the reported volatile matter will be. Crush analysis sample (see
sample rack.
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
9.5 When temperature recovery is achieved within the
retain 40 % to 55 % of the sample. Do not obtain the analysis
10 min period, record the number of crucibles in the rack. This
sample by scalping and discarding a portion of the sample.
number of crucibles shall be in the rack for all future runs (fill
6.2.2 Any segregation of particle sizes within the analysis
empty spaces in the stand with empty crucibles when neces-
sampleshallbecorrectedbyreblendingthesamplejustpriorto
sary).
weighing the test sample.
9.6 Round the recorded elapsed time to the next higher
6.3 The furnace shall recover to 950 °C 6 20 °C before the
minute. This rounded time will be the analysis time for future
time limit is reached. If the furnace does not recover to the
runs (5 min minimum).
starting temperature within a maximum of 10 min, reduce the
number of samples being analyzed until recovery is achieved 10. Procedure
within 10 min (see Section 9).
10.1 Ignite the quartz crucible and cover at 950 °C 6 20 °C
for5 minperiodstoconstantmass(60.5 mg).Donotcoverthe
7. Apparatus
crucible at this time to allow the carbon to burn off. Cool to
ambient temperature in a desiccator before weighing the
7.1 Electric Muffle Furnace—Calibrated (Test Method
crucible and cover.
E220) and regulated to maintain a temperature of 950 °C 6
20 °C (1742 °F), as measured by a thermocouple mounted
NOTE 1—Placing the empty crucibles in the inverted cover when
inside the furnace. Its heat capacity shall be such that the initial
igniting will reduce breakage and chipping.
temperature is regained after the introduction of a cold rack of
10.2 Avoiding segregation of particles, transfer 1 g 610 mg
samples within 10 min.
of the analysis sample (see Annex A1) to the crucible, weigh
7.2 Quartz Crucibles, self-sealing, 10 mL capacity with the crucible with its contents, and cover to the nearest 0.1 mg.
covers.
Place the cover on the crucible, and place in sample rack.
7.3 Rack,stainlesssteel,designedtoholdupto20crucibles. 10.3 Set the timer for the analysis time (5 min to 10 min).
Place the rack in the furnace. Start the timer.
7.4 Rifflers, with hoppers and closures.
NOTE 2—Place the rack in the center of the furnace. Do not allow the
7.5 Jaw Crusher and Roll Crusher—Other style crushers
rack to touch the walls of the furnace.
that allow control over particle size without contamination are
10.4 After the analysis time (65 s), remove the rack from
acceptable (see Annex A1).
the furnace and immediately place on a heat sink.
7.6 Balance, cap
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D6374 − 12 D6374 − 12 (Reapproved 2017)
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 88 % to
16 %.
1.3 Samples having a thermal history above 600°C600 °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. No other units of measurement are included in this 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 and health 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
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(5 min to 10 min).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.
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 April 15, 2012May 1, 2017. Published May 2012July 2017. Originally approved in 1999. Last previous edition approved in 20092012 as
D6374–99(2009).D6374 – 12. DOI: 10.1520/D6374-12.10.1520/D6374-12R17E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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
´1
D6374 − 12 (2017)
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-mm0.250 mm opening (No. 60) sieve but
do not overcrush. A 0.125-mm0.125 mm opening (No. 120) sieve should retain 4040 % to 55 % of the sample. Do not obtain the
analysis sample is 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 950950 °C 6 20°C20 °C before the time limit is reached. If the furnace does not recover to
the starting temperature within a maximum of 10 min, 10 min, reduce the number of samples being analyzed until recovery is
achieved within 10 min 10 min (see Section 9).
7. Apparatus
7.1 Electric Muffle Furnace—Calibrated (Test Method E220) and regulated to maintain a temperature of 950950 °C 6 20°C
(1742°F),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.10 min.
7.2 Quartz Crucibles, self-sealing, 10 mL 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.0.1 mg.
7.7 Dessicator.
7.8 Sieves, meeting Specification E11.
7.9 Timers, stopwatch or second timer.
7.10 Heat Sink, 1/2 in. 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 (6 0.05 g) 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. 0.1 mg. Place the cover on the crucible,
and place in sample rack.
9.2 Record the furnace temperature at equilibrium (9506 20°C).(950 °C 6 20 °C).
´1
D6374 − 12 (2017)
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, 10 min, repeat the procedure, reducing the number of crucibles in the rack until temperature recovery
is completed within 10 min 10 min of the introduction of the sample rack.
9.5 When temperature recovery is achieved within the 10 min 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 (5 min minimum).
10. Procedure
10.1 Ignite the quartz crucible and cover at 950950 °C 6 20°C20 °C for 5 min 5 min periods to constant mass (60.5 mg).
(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.
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 1 g 610 mg of the analysis
...