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ASTM D6969-16

(Practice)

Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis

Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis

SIGNIFICANCE AND USE
4.1 This practice provides field personnel and laboratories with standard procedures for dividing, reducing, and mixing gross samples and intermediate samples, such that the resulting prepared analysis samples are more uniform from laboratory to laboratory. Adherence to these guidelines is expected to provide significant reduction in interlaboratory variability.
SCOPE
1.1 This practice covers the preparation procedures necessary for the reduction and division of calcined petroleum coke samples in order to generate appropriate analytical samples upon which physical and chemical analytical tests will be performed.  
1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard.  
1.3 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.

General Information

Status
Historical
Publication Date
31-May-2016
ICS
75.160.10 - Solid fuels
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.05 - Properties of Fuels, Petroleum Coke and Carbon Material
Current Stage
Ref Project

Relations

Replaces
ASTM D6969-15 - Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
Effective Date
01-Jun-2016
Referred By
ASTM D6791-22 - Standard Test Method for Determination of Grain Stability of Calcined Petroleum Coke
Effective Date
01-Jun-2016
Referred By
ASTM D4292-17 - Standard Test Method for Determination of Vibrated Bulk Density of Calcined Petroleum Coke
Effective Date
01-Jun-2016
Referred By
ASTM D5187-21 - Standard Test Method for Determination of Crystallite Size (L<inf>c</inf>) of Calcined Petroleum Coke by X-Ray Diffraction
Effective Date
01-Jun-2016
Referred By
ASTM D5004-11(2017) - Standard Test Method for Real Density of Calcined Petroleum Coke by Xylene Displacement
Effective Date
01-Jun-2016
Referred By
ASTM D6376-10(2017)e1 - Standard Test Method for Determination of Trace Metals in Petroleum Coke by Wavelength Dispersive X-ray Fluorescence Spectroscopy
Effective Date
01-Jun-2016
Referred By
ASTM D2638-21 - Standard Test Method for Real Density of Calcined Petroleum Coke by Helium Pycnometer
Effective Date
01-Jun-2016
Referred By
ASTM D6970-03(2019) - Standard Practice for Collection of Calcined Petroleum Coke Samples for Analysis
Effective Date
01-Jun-2016
Referred By
ASTM D8097-17e1 - Standard Test Method for Determination of Bulk Density for Specific Size Fractions of Calcined Petroleum Coke Using a Transaxial Pressure Pycnometer
Effective Date
01-Jun-2016
Referred By
ASTM D5709-22 - Standard Test Method for Sieve Analysis of Petroleum Coke
Effective Date
01-Jun-2016

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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
Designation: D6969 − 16
Standard Practice for
Preparation of Calcined Petroleum Coke Samples for
1
Analysis
This standard is issued under the fixed designation D6969; 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* Coke by Xylene Displacement
D5056 Test Method for Trace Metals in Petroleum Coke by
1.1 This practice covers the preparation procedures neces-
Atomic Absorption
sary for the reduction and division of calcined petroleum coke
D5187 Test Method for Determination of Crystallite Size
samples in order to generate appropriate analytical samples
(L ) of Calcined Petroleum Coke by X-Ray Diffraction
c
upon which physical and chemical analytical tests will be
D5600 Test Method for Trace Metals in Petroleum Coke by
performed.
Inductively Coupled Plasma Atomic Emission Spectrom-
1.2 The values stated in either SI units or inch-pound units
etry (ICP-AES)
are to be regarded separately as standard. The values stated in
D5709 Test Method for Sieve Analysis of Petroleum Coke
each system may not be exact equivalents; therefore, each
D6376 Test Method for Determination of Trace Metals in
system shall be used independently of the other. Combining
Petroleum Coke by Wavelength Dispersive X-ray Fluo-
values from the two systems may result in non-conformance
rescence Spectroscopy
with the standard.
1.3 This standard does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
3.1 Definitions:
responsibility of the user of this standard to establish appro-
3.1.1 analysis sample, n—the reduced and divided represen-
priate safety and health practices and determine the applica-
tative portion of the bulk sample, prepared for use in the
bility of regulatory limitations prior to use.
laboratory.
3.1.2 composite sample, n—a sample, representative of an
2. Referenced Documents
2 entire consignment of calcined petroleum coke, generated by
2.1 ASTM Standards:
mixingportionsofgrosssamplesfromdifferentlotstogetherin
D1552 Test Method for Sulfur in Petroleum Products by
mass fractions proportioned to the consignment.
High Temperature Combustion and IR Detection
D2638 Test Method for Real Density of Calcined Petroleum 3.1.3 gross sample, n—the original, uncrushed representa-
tive portion taken from a shipment or lot of coke.
Coke by Helium Pycnometer
D4292 Test Method for Determination of Vibrated Bulk
3.1.4 intermediate sample, n—a sample, representative of a
Density of Calcined Petroleum Coke
gross sample, upon which no analysis is to be performed, yet
D4422 Test Method for Ash in Analysis of Petroleum Coke
required for generation of analysis samples after undergoing
D4930 Test Method for Dust Control Material on Calcined
further division and reduction.
Petroleum Coke
3.1.5 lot, n—a quantity of calcined petroleum coke to be
D4931 Test Method for Gross Moisture in Green Petroleum
represented by a gross sample.
Coke
3.1.6 riffle, n—a manual sample divider which splits the
D5004 Test Method for Real Density of Calcined Petroleum
sample stream into a number of alternate elements.
3.1.7 sample division, n—the process whereby a sample is
1
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum
reduced in mass without change in particle size.
Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-
mittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material
3.1.8 sample preparation, n—the process that may include
CurrenteditionapprovedJune1,2016.PublishedJuly2016.Originallyapproved
drying,crushing,division,andmixingofagrosssampleforthe
in 2003. Last previous edition approved in 2015 as D6969 – 15. DOI: 10.1520/
purpose of obtaining an unbiased analysis sample.
D6969-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3.1.9 sample reduction, n—the process whereby a sample is
contactASTM Customer Service at service@astm.org. ForAnnual Book ofASTM
reduced in particle size by crushing or grinding without
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. significant change in chemical properties.
*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

---------------------- Page: 1 ----------------------
D6969 − 16
NOTE 1—The tasks outlined in this figure are not necessarily required for analysis.
NOTE 2—Fig. 1 is based on kilogram (kg) and gram (g). To convert from kilogram (kg) to pound (lb ), multiply by 2.205. To
...

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.
Designation: D6969 − 15 D6969 − 16
Standard Practice for
Preparation of Calcined Petroleum Coke Samples for
1
Analysis
This standard is issued under the fixed designation D6969; 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 practice covers the preparation procedures necessary for the reduction and division of calcined petroleum coke samples
in order to generate appropriate analytical samples upon which physical and chemical analytical tests will be performed.
1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each
system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the
two systems may result in non-conformance with the standard.
1.3 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1552 Test Method for Sulfur in Petroleum Products by High Temperature Combustion and IR Detection
D2638 Test Method for Real Density of Calcined Petroleum Coke by Helium Pycnometer
D4292 Test Method for Determination of Vibrated Bulk Density of Calcined Petroleum Coke
D4422 Test Method for Ash in Analysis of Petroleum Coke
D4930 Test Method for Dust Control Material on Calcined Petroleum Coke
D4931 Test Method for Gross Moisture in Green Petroleum Coke
D5004 Test Method for Real Density of Calcined Petroleum Coke by Xylene Displacement
D5056 Test Method for Trace Metals in Petroleum Coke by Atomic Absorption
D5187 Test Method for Determination of Crystallite Size (L ) of Calcined Petroleum Coke by X-Ray Diffraction
c
D5600 Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry
(ICP-AES)
D5709 Test Method for Sieve Analysis of Petroleum Coke
D6376 Test Method for Determination of Trace Metals in Petroleum Coke by Wavelength Dispersive X-ray Fluorescence
Spectroscopy
3. Terminology
3.1 Definitions:
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 composite sample, n—a sample, representative of an entire consignment of calcined petroleum coke, generated by mixing
portions of gross samples from different lots together in mass fractions proportioned to the consignment.
3.1.3 gross sample, n—the original, uncrushed representative portion taken from a shipment or lot of coke.
3.1.4 intermediate sample, n—a sample, representative of a gross sample, upon which no analysis is to be performed, yet
required for generation of analysis samples after undergoing further division and reduction.
1
This practice 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 June 1, 2015June 1, 2016. Published September 2015July 2016. Originally approved in 2003. Last previous edition approved in 20082015 as
D6969 – 03 (2008).D6969 – 15. DOI: 10.1520/D6969-15.10.1520/D6969-16.
2
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
1

---------------------- Page: 1 ----------------------
D6969 − 16
3.1.5 lot, n—a quantity of calcined petroleum coke to be represented by a gross sample.
3.1.6 riffle, n—a manual sample divider which splits the sample stream into a number of alternate elements.
3.1.7 sample division, n—the process whereby a sample is reduced in mass without change in particle size.
3.1.8 sample preparation, n—the process that may include drying, crushing, division, and mixing of a gross sample for the
purpose of obtaining an unbiased analysis
...

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SIGNIFICANCE AND USE
5.1 The density of petroleum coke directly influences the physical and chemical properties of the manufactured carbon and graphite artifacts for which it is used. Density, therefore, is a major quality specification of calcined petroleum coke and is used as a control in coke calcination.
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SIGNIFICANCE AND USE
5.1 The bulk density is an indicator of calcined petroleum coke porosity and packing capability which is an important coke property for anode production in aluminum industry. This procedure will allow an automated measurement of specific sized fractions ranging from 8 mm to 0.25 mm coke particles.  
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1.1 The test method covers the determination of bulk density for a specific size fraction of calcined petroleum coke using an automated pycnometer that compacts coke by applying transaxial pressure under a controlled force.  
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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 Belitskus3 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.
SCOPE
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ASTM D4930-23(Test Method)
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SIGNIFICANCE AND USE
5.1 The test is designed to quantify the amount of dust control material added to calcined coke. The dust control material is applied to calcined coke to help maintain a dust-free environment. It generally serves no other useful purpose. It adds mass to the coke and can have a negative effect on the quality of carbon and graphite artifacts made from the treated coke. For these reasons the coke customer wants to know the amount of dust control material on the coke and can specify a maximum level.
SCOPE
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ASTM D6969-23(Practice)
Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis

SIGNIFICANCE AND USE
4.1 This practice provides field personnel and laboratories with standard procedures for dividing, reducing, and mixing gross samples and intermediate samples, such that the resulting prepared analysis samples are more uniform from laboratory to laboratory. Adherence to these guidelines is expected to provide significant reduction in interlaboratory variability.
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5.1 The presence and concentration of various metallic elements in a petroleum coke are major factors in the suitability of the coke for various uses. This test method provides a means of measuring the amounts of those metallic elements in the coke sample.  
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SIGNIFICANCE AND USE
5.1 The presence and concentration of various metallic elements in a petroleum coke are major factors in determining the suitability of the coke for various end uses. This test method provides a means of determining the concentrations of these metallic elements in a coke sample.  
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1.4 Elements present at concentrations above the upper limit of the working ranges can be determined with additional, appropriate dilutions.  
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.6 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.  
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ASTM D5709-22(Test Method)
Standard Test Method for Sieve Analysis of Petroleum Coke

SIGNIFICANCE AND USE
5.1 The test method concerns the sieving of coke into designated size fractions for the purpose of characterizing the material as to its particle size distribution. It requires the use of standard sieves, standard sampling methods, standard sample preparation methods, and a minimum initial sample mass based on lot topsize. Suggestions are given for industry typical sieve stacks for both green and calcined petroleum coke.  
5.2 Particle size distribution is significant in that many physical characteristics of a coke are related to such a distribution including bulk density and surface area. Nuisance characteristics, such as excessive fines in a lot, can also be controlled.  
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SCOPE
1.1 This test method details a procedure for performing particle size distribution analysis by dry sieve testing on green petroleum coke with a topsize of no more than 75 mm and calcined petroleum coke with a topsize of no more than 25 mm. Size fractions go down to and include 4.75 mm for green petroleum coke and 75 μm for calcined petroleum coke.  
Note 1: To convert units, see Table 1 on nominal dimensions in Specification E11. For example, 75 mm is approximately equivalent to a nominal sieve opening of 3 in. and 25 mm to a nominal sieve opening of 1 in. Likewise, 4.75 mm can be converted to approximately 0.187 in. and 75 microns to 0.0029 in.  
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1.2.1 The sieve size is reported as U.S.A. standard test series in any units listed in Table 1 on nominal dimensions of Specification E11, or their commercial size equivalents.  
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ASTM D2638-21(Test Method)
Standard Test Method for Real Density of Calcined Petroleum Coke by Helium Pycnometer

SIGNIFICANCE AND USE
5.1 The real density of calcined petroleum coke directly influences the physical and chemical properties of the manufactured carbon and graphite artifacts for which it is used. Density, therefore, is a major quality specification of calcined petroleum coke and is used as a control in coke calcination.
SCOPE
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ASTM D5187-21(Test Method)
Standard Test Method for Determination of Crystallite Size (Lc) of Calcined Petroleum Coke by X-Ray Diffraction

SIGNIFICANCE AND USE
5.1 The crystallinity of petroleum coke, as reflected by the Lc  value, is a general measure of quality affecting suitability for end use and is a function of the heat treatment.  
5.2 The crystallite thickness is used to determine the extent of such heat treatment, for example, during calcination. The value of the Lc  determined is not affected by coke microporosity or the presence of foreign, non-crystalline materials such as dedust oil.
SCOPE
1.1 This test method covers the determination of the mean crystallite thickness of a representative, pulverized sample of calcined petroleum coke by interpretation of a X-ray diffraction pattern produced through conventional X-ray scanning techniques.  
1.2 Calcined petroleum coke contains crystallites of different thicknesses. This test method covers the determination of the average thickness of all crystallites in the sample by empirical interpretation of the X-ray diffraction pattern. The crystallite diameter (La) is not determined by this test method.  
1.3 The values stated in SI (metric) units are to be regarded as the standard. The inch-pound units given in parentheses are provided for information purposes only.  
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.

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