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ASTM D6969-03(2008)

(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
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 SI units are to be regarded as standard. No other units of measurement are included in this 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
14-Oct-2008
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 D6969-03 - Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
Effective Date
15-Oct-2008
Replaced By
ASTM D6969-15 - Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
Effective Date
01-Jun-2015
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
15-Oct-2008
Referred By
ASTM D6791-22 - Standard Test Method for Determination of Grain Stability of Calcined Petroleum Coke
Effective Date
15-Oct-2008
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
15-Oct-2008
Referred By
ASTM D6970-03(2019) - Standard Practice for Collection of Calcined Petroleum Coke Samples for Analysis
Effective Date
15-Oct-2008
Referred By
ASTM D5004-11(2017) - Standard Test Method for Real Density of Calcined Petroleum Coke by Xylene Displacement
Effective Date
15-Oct-2008
Referred By
ASTM D5709-22 - Standard Test Method for Sieve Analysis of Petroleum Coke
Effective Date
15-Oct-2008
Referred By
ASTM D4292-17 - Standard Test Method for Determination of Vibrated Bulk Density of Calcined Petroleum Coke
Effective Date
15-Oct-2008
Referred By
ASTM D2638-21 - Standard Test Method for Real Density of Calcined Petroleum Coke by Helium Pycnometer
Effective Date
15-Oct-2008
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
15-Oct-2008

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ASTM D6969-03(2008) - Standard Practice for Preparation of Calcined Petroleum Coke Samples for AnalysisASTM D6969-03(2008) - Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
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ASTM D6969-03(2008) - Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
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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 − 03(Reapproved 2008)
Standard Practice for
Preparation of Calcined Petroleum Coke Samples for
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 D5187 TestMethodforDeterminationofCrystalliteSize(L
c
of Calcined Petroleum Coke by X-Ray Diffraction
1.1 This practice covers the preparation procedures neces-
D5600 Test Method for Trace Metals in Petroleum Coke by
sary for the reduction and division of calcined petroleum coke
Inductively Coupled Plasma Atomic Emission Spectrom-
samples in order to generate appropriate analytical samples
etry (ICP-AES)
upon which physical and chemical analytical tests will be
D5709 Test Method for Sieve Analysis of Petroleum Coke
performed.
D6376 Test Method for Determination of Trace Metals in
1.2 The values stated in SI units are to be regarded as
Petroleum Coke by Wavelength Dispersive X-ray Fluo-
standard. No other units of measurement are included in this
rescence Spectroscopy
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—the reduced and divided representa-
priate safety and health practices and determine the applica-
tive portion of the bulk sample, prepared for use in the
bility of regulatory limitations prior to use.
laboratory.
2. Referenced Documents
3.1.2 composite sample—a sample, representative of an
entire consignment of calcined petroleum coke, generated by
2.1 ASTM Standards:
mixingportionsofgrosssamplesfromdifferentlotstogetherin
D1552 Test Method for Sulfur in Petroleum Products (High-
mass fractions proportioned to the consignment.
Temperature Method)
D2638 Test Method for Real Density of Calcined Petroleum
3.1.3 gross sample—the original, uncrushed representative
Coke by Helium Pycnometer
portion taken from a shipment or lot of coke.
D4292 Test Method for Determination of Vibrated Bulk
3.1.4 intermediate sample—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—a quantity of calcined petroleum coke to be
D4931 Test Method for Gross Moisture in Green Petroleum
represented by a gross sample.
Coke
D5004 Test Method for Real Density of Calcined Petroleum
3.1.6 riffle—a manual sample divider which splits the
Coke by Xylene Displacement
sample stream into a number of alternate elements.
D5056 Test Method for Trace Metals in Petroleum Coke by
3.1.7 sample division—the process whereby a sample is
Atomic Absorption
reduced in mass without change in particle size.
3.1.8 sample preparation—the process that may include
This practice is under the jurisdiction ofASTM Committee D02 on Petroleum
drying,crushing,division,andmixingofagrosssampleforthe
Products and Lubricants and is the direct responsibility of Subcommittee D02.05 on
purpose of obtaining an unbiased analysis sample.
Properties of Fuels, Petroleum Coke and Carbon Material
Current edition approved Oct. 15, 2008. Published December 2008. Originally
3.1.9 sample reduction—the process whereby a sample is
approved in 2003. Last previous edition approved in 2003 as D6969–03. DOI:
reduced in particle size by crushing or grinding without
10.1520/D6969-03R08.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or significant change in chemical properties.
contactASTM Customer Service at service@astm.org. ForAnnual Book ofASTM
3.1.10 top size—the size of the smallest opening of one
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. sieve of a series upon which is cumulatively retained a total of
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6969 − 03 (2008)
NOTE 1—The tasks outlined in this figure are not necessarily required for analysis.
FIG. 1 Preparation of Calcined Petroleum Coke
less than 5 % of the sample. This defined top size is not to be 5.1.2 Exercise care in the division operation to preserve the
confused with the size of the largest particle in a lot.
particle size distribution of the gross sample. Riffle openings
must be at least three times the top size of the calcined
4. Significance and Use
petr
...

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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 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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1.1 This test method covers the determination of the real density (RD) of calcined petroleum coke. Real density, by definition, is obtained when the particle size of the test specimen is smaller than 75 μm (No. 200 sieve).  
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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.)  
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1.1 This test method covers the determination of bulk density of a representative 2 kg sample of calcined petroleum coke, after vibration to increase compaction.  
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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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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.  
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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.
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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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1.1 This test method covers the analysis for the commonly determined trace metals (aluminum, calcium, iron, nickel, silicon, sodium, and vanadium) in laboratory analysis samples of raw and calcined petroleum coke by atomic absorption spectroscopy.  
1.2 The elemental concentration ranges for which this test method is applicable and the limits of detection of this test method are listed in Table 1.  
1.3 The values stated in SI units are to be regarded as the standard.  
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. For warning statements, see Sections 9 – 11.  
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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.  
5.2 The test method provides a standard procedure for use by buyer and seller in the commercial transfer of petroleum coke to determine whether the petroleum coke meets the specifications of the purchasing party.
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1.1 This test method covers the analysis for commonly determined trace metals in test specimens of raw and calcined petroleum coke by inductively coupled plasma atomic emission spectroscopy.  
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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.  
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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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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.  
5.3 Results from this test method are useful in determining whether a coke lot meets purchase specifications, for classification purposes, and for quality control. The results of this test method can also be used to predict the performance of a particular lot of coke in a process.
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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.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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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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
1.1 This test method covers the determination of the real density (RD) of calcined petroleum coke. Real density, by definition is obtained when the particle size of the specimen is smaller than 75 µm (U.S. No. 200 Sieve).  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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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