ASTM D5004-23

Standard Test Method for Real Density of Calcined Petroleum Coke by Xylene Displacement

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.
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 test specimen is smaller than 75 μm (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. For specific warning statements, see Sections 10 and 11.1.  
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.

General Information

• Status: Published
• Publication Date: 31-Oct-2023
• 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

Relations

• Replaces: ASTM D5004-11(2017) - Standard Test Method for Real Density of Calcined Petroleum Coke by Xylene Displacement
• Effective Date: 01-Nov-2023
• Refers: ASTM D4175-23a - Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 15-Dec-2023
• Refers: ASTM D4175-23e1 - Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 01-Jul-2023
• Referred By: ASTM D6969-23 - Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
• Effective Date: 01-Nov-2023

Overview

ASTM D5004-23: Standard Test Method for Real Density of Calcined Petroleum Coke by Xylene Displacement provides a validated method to determine the real density of calcined petroleum coke. This standard is crucial for quality control in industries that use calcined petroleum coke as a precursor for manufacturing carbon and graphite artifacts. Real density is a primary property that influences the structural and chemical characteristics of final products. The test method involves measuring the mass of a finely powdered coke sample and determining its volume based on xylene displacement in a pycnometer, ensuring an accurate representation of true material density excluding pores and voids.

Key Topics

• Real Density Determination: Focuses on the determination of real density for coke particles smaller than 75 µm, ensuring exclusion of internal voids and a true representation of material density.
• Quality Control: Real density is a standard specification used to monitor and control coke calcination, directly impacting the performance of downstream carbon and graphite products.
• Standard Test Conditions: All measurements are performed using SI units, with procedures standardized around a controlled temperature (25°C ± 0.1°C) for consistency.
• Sample Preparation: Emphasizes the importance of proper sample collection, reduction to the specified particle size, and removal of surface contaminants such as dedusting oils.
• Safety and Environmental Considerations: Users must adopt appropriate health, safety, and environmental practices, as outlined in the standard and corresponding safety data sheets.
• Precision and Repeatability: The document defines the expected repeatability and reproducibility for robust interlaboratory reliability.

Applications

ASTM D5004-23 is vital for industries that rely on calcined petroleum coke, particularly:

• Aluminum Production: Ensures consistent anode quality by providing a reliable metric for coke density.
• Metallurgical Operations: Used where precise carbon content and structure are required for reduction processes.
• Carbon and Graphite Manufacturing: Supports the production of electrodes, specialty graphite, and other high-performance carbon materials, where density influences strength, porosity, and overall performance.
• Quality Assurances in Procurement: Used by suppliers and purchasers to assess and verify the conformity of raw calcined petroleum coke to contractual and regulatory requirements.
• Research and Development: Laboratories adopt this test method when developing new materials or processes involving calcined petroleum coke.

Related Standards

To comprehensively assess coke and related materials, ASTM D5004-23 references several supporting and complementary standards:

• ASTM D346: Practice for Collection and Preparation of Coke Samples for Laboratory Analysis
• ASTM D4292: Test Method for Determination of Vibrated Bulk Density of Calcined Petroleum Coke
• ASTM D4930: Test Method for Dust Control Material on Calcined Petroleum Coke
• ASTM D7454: Test Method for Determination of Vibrated Bulk Density of Calcined Petroleum Coke Using a Semi-Automated Apparatus
• ASTM D6969/D6970: Practices for Preparation and Collection of Calcined Petroleum Coke Samples for Analysis
• ASTM E11: Specification for Woven Wire Test Sieve Cloth and Test Sieves

Practical Value

Complying with ASTM D5004-23 ensures accurate, repeatable, and dependable real density data for calcined petroleum coke. This enables manufacturers to:

• Optimize process parameters for calcination
• Improve quality and consistency in downstream products (anodes, electrodes, specialty carbons)
• Meet rigorous customer and regulatory requirements
• Benchmark material performance and investigate process deviations

By adhering to this standard, industries strengthen their quality assurance frameworks and maintain competitiveness in demanding global markets involving carbon-based materials.

Standards Content (Sample)

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.
Designation: D5004 − 23
Standard Test Method for
Real Density of Calcined Petroleum Coke by Xylene
Displacement
This standard is issued under the fixed designation D5004; 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* Fuels, and Lubricants
D4292 Test Method for Determination of Vibrated Bulk
1.1 This test method covers the determination of the real
Density of Calcined Petroleum Coke
density (RD) of calcined petroleum coke. Real density, by
D4930 Test Method for Dust Control Material on Calcined
definition, is obtained when the particle size of the test
Petroleum Coke
specimen is smaller than 75 μm (No. 200 sieve).
D6969 Practice for Preparation of Calcined Petroleum Coke
1.2 The values stated in SI units are to be regarded as
Samples for Analysis
standard. No other units of measurement are included in this
D6970 Practice for Collection of Calcined Petroleum Coke
standard.
Samples for Analysis
1.3 This standard does not purport to address all of the D7454 Test Method for Determination of Vibrated Bulk
safety concerns, if any, associated with its use. It is the
Density of Calcined Petroleum Coke using a Semi-
responsibility of the user of this standard to establish appro- Automated Apparatus
priate safety, health, and environmental practices and deter-
E11 Specification for Woven Wire Test Sieve Cloth and Test
mine the applicability of regulatory limitations prior to use. Sieves
For specific warning statements, see Sections 10 and 11.1.
1.4 This international standard was developed in accor-
3. Terminology
dance with internationally recognized principles on standard-
3.1 Definitions:
ization established in the Decision on Principles for the
3.1.1 For definitions of terms used in this test method, refer
Development of International Standards, Guides and Recom-
to Terminology D4175.
mendations issued by the World Trade Organization Technical
3.1.2 calcined petroleum coke, n—petroleum coke that has
Barriers to Trade (TBT) Committee.
been thermally treated to drive off the volatile matter and to
develop crystalline structure.
2. Referenced Documents
3.1.3 petroleum coke, n—solid, carbonaceous residue pro-
2.1 ASTM Standards:
duced by thermal decomposition of heavy petroleum fractions
D346 Practice for Collection and Preparation of Coke
or cracked stocks, or both.
Samples for Laboratory Analysis
D1193 Specification for Reagent Water 3.2 Definitions of Terms Specific to This Standard:
D2013 Practice for Preparing Coal Samples for Analysis
3.2.1 bulk density, n—mass of the particles divided by the
D2234/D2234M Practice for Collection of a Gross Sample
volume they occupy that includes the space between the
of Coal
particles. Refer to Test Methods D4292 and D7454 for bulk
D4057 Practice for Manual Sampling of Petroleum and
density procedures.
Petroleum Products
3.2.2 dedusting material, n—see Test Method D4930.
D4175 Terminology Relating to Petroleum Products, Liquid
3.2.3 real density, n—(also referred to as true specific
gravity), the mass divided by the volume occupied by the
This test method is under the jurisdiction of ASTM Committee D02 on material excluding pores and voids. It is required, therefore,
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
that voids in the coke be eliminated and that pores in the
Subcommittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
material be filled by the fluid being displaced. This requirement
Current edition approved Nov. 1, 2023. Published November 2023. Originally
is met for the purposes of this test method by reducing the coke
approved in 1989. Last previous edition approved in 2017 as D5004 – 11 (2017).
DOI: 10.1520/D5004-23.
particles to a size smaller than 75 μm.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3.2.3.1 Discussion—The density of particles larger than
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
75 μm up to the largest that can be put into the helium
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. pycnometer can also be determined, but must be designated as
*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
D5004 − 23
particle density (PD). The precision data obtained for RD may 7.4 Vacuum Desiccator, with guard, connected to a vacuum
not be applicable to PD. source capable of lowering pressure to 75 mm of Hg (10 kPa).
7.5 Desiccator, with drying agent. Anhydrous calcium sul-
4. Summary of Test Method
phate is satisfactory.
4.1 The mass of the sample is determined directly and the
7.6 Drying Oven, preferably a vacuum oven, for tempera-
volume derived by determining the mass of liquid displaced
ture to 120 °C.
when the sample is introduced into a pycnometer.
7.7 Lead Weights, for the pycnometers, to prevent tipping
RD 5 M × D/L (1)
over in the water bath. These can be made by coiling solid wire
solder.
where:
M = mass of sample,
7.8 Wire Sieve, 75 μm (No. 200 mesh), meeting Specifica-
D = density of displaced liquid, and
tion E11.
L = mass of displaced liquid.
8. Reagents
5. Significance and Use
8.1 Purity of Water—References to distilled water shall be
5.1 The density of petroleum coke directly influences the
understood to mean reagent water as defined by Type III of
physical and chemical properties of the manufactured carbon
Specification D1193.
and graphite artifacts for which it is used. Density, therefore, is
8.2 Analytical reagent grade solvents are not required but
a major quality specification of calcined petroleum coke and is
can be used. The technical grade of each of the following is
used as a control in coke calcination.
satisfactory:
8.2.1 Acetone, Xylene, and Ethyl Alcohol. (See 6.1.2.)
6. Interferences
6.1 Oil or other material sprayed on calcined petroleum 9. Sample Preparation
coke to control dust will interfere with the determination of real
9.1 For recommended practice for obtaining, handling, and
density so the oil must be removed before reducing the sample
preparing coke samples, refer to Practices D346, D2013,
to 75 μm.
D2234/D2234M, and D4057, and Test Methods D6969 and
6.1.1 When a petroleum oil was used, it can be removed by
D6970. See Section 6.
flushing with a solvent such as methylene chloride,
9.2 Crush 50 g of coke so that the entire sample will pass
dichloroethane, or toluene. The solvent must be completely
through a 75 μm (No. 200) sieve. Dry the crushed sample in a
removed before proceeding with the RD determination. Heat-
drying oven at 115 °C 6 5 °C to constant mass (approximately
ing to 10 °C above the boiling point of the solvent used or
8 h). Cool in a desiccator.
application of vacuum is satisfactory for the removal of the
dedusting oil.
NOTE 3—Constant mass is considered to be achieved when change in
mass is less than 60.05 g after a 30 min test drying period.
NOTE 1—Consult the Material Safety Data Sheet (MSDS) for the
selected solvent.
10. Pycnometer Calibration (Determination of
6.1.2 An alternative method of oil removal is by heating the
Pycnometer Volume)
calcined petroleum coke sample in an oven at 700 °C for 1 h.
10.1 Clean the pycnometer and its stopper with detergent,
rinse thoroughly with water then with acetone. Place in a
7. Apparatus
desiccator to dry, then weigh the empty pycnometer together
7.1 Pycnometer, or specific gravity bottle, 50 mL, with a
with its stopper to 0.1 mg (mass W ). The temperature of the
o
ground glass stopper with a capillary hole. Bottles with a large
pycnometer is to be close to room temperature when its mass
neck (12 mm to 13 mm outside diameter) are preferred.
is determined. (Warning—Commercial pycnometers (specific
gravity bottles) can either have not been calibrated at 25 °C or
7.2 Water Bath, controlled to a temperature of 25 °C 6
else not calibrated to the accuracy required for this test method,
0.1 °C.
so it is necessary that the pycnometer volume be determined.)
NOTE 2—This test method is written to be performed at 25 °C 6 0.1 °C;
however, some laboratories may not have the provisions to perform the
NOTE 4—Do not handle the pycnometer with bare fingers. Finger cots
test at this temperature. It is permissible to perform the test procedure at
or surgical gloves can be worn, or tongs can be used, when handling the
any temperature between 20 °C and 40 °C providing that the water bath is
pycnometer to prevent moisture from fingers influencing the mass.
controlled at 60.1 °C of the chosen temperature and the pycnometers are
10.2 Fill the pycnometer with freshly boiled (to remove air)
calibrated at the same temperature that is used to determine the real
and cooled distilled water, and replace the stopper. Immerse the
density of the petroleum coke sample. This is possible due to the fact that
the real density of calcined petroleum coke is not affected by temperature
pycnometer up to the neck in the 25 °C 6 0.1 °C water bath for
changes over a limited temperature range.
1 h. Use the lead weights to prevent tipping. Replace water that
7.3 Analytical Balance, accurate to 60.1 mg. leaves the capillary during this period. A syringe is convenient
for this purpose.
10.3 At the end of the temperature stabilization period,
A Gay-
...

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: D5004 − 11 (Reapproved 2017) D5004 − 23
Standard Test Method for
Real Density of Calcined Petroleum Coke by Xylene
Displacement
This standard is issued under the fixed designation D5004; 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 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 test specimen is smaller than 75 μm (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. For specific warning statements, see Sections 10 and 11.1.
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.
2. Referenced Documents
2.1 ASTM Standards:
D346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis
D1193 Specification for Reagent Water
D2013 Practice for Preparing Coal Samples for Analysis
D2234/D2234M Practice for Collection of a Gross Sample of Coal
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D4292 Test Method for Determination of Vibrated Bulk Density of Calcined Petroleum Coke
D4930 Test Method for Dust Control Material on Calcined Petroleum Coke
D6969 Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
D6970 Practice for Collection of Calcined Petroleum Coke Samples for Analysis
D7454 Test Method for Determination of Vibrated Bulk Density of Calcined Petroleum Coke using a Semi-Automated
Apparatus
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
3. Terminology
3.1 Definitions:
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 Oct. 1, 2017Nov. 1, 2023. Published November 2017November 2023. Originally approved in 1989. Last previous edition approved in 20112017
as D5004 – 11.D5004 – 11 (2017). DOI: 10.1520/D5004-11R17.10.1520/D5004-23.
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
D5004 − 23
3.1.1 For definitions of terms used in this test method, refer to Terminology D4175.
3.1.2 calcined petroleum coke, n—petroleum coke that has been thermally treated to drive off the volatile matter and to develop
crystalline structure.
3.1.3 petroleum coke, n—solid, carbonaceous residue produced by thermal decomposition of heavy petroleum fractions or cracked
stocks, or both.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 bulk density, n—mass of the particles divided by the volume they occupy that includes the space between the particles. Refer
to Test Methods D4292 and D7454 for bulk density procedures.
3.2.2 dedusting material, n—see Test Method D4930.
3.2.3 real density, n—(also referred to as true specific gravity), the mass divided by the volume occupied by the material excluding
pores and voids. It is required, therefore, that voids in the coke be eliminated and that pores in the material be filled by the fluid
being displaced. This requirement is met for the purposes of this test method by reducing the coke particles to a size smaller than
75 μm.
3.2.3.1 Discussion—
The density of particles larger than 75 μm up to the largest that can be put into the helium pycnometer can also be determined,
but must be designated as particle density (PD). The precision data obtained for RD may not be applicable to PD.
4. Summary of Test Method
4.1 The mass of the sample is determined directly and the volume derived by determining the mass of liquid displaced when the
sample is introduced into a pycnometer.
RD 5 M ×D/L (1)
where:
M = mass of sample,
D = density of displaced liquid, and
L = mass of displaced liquid.
5. 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.
6. Interferences
6.1 Oil or other material sprayed on calcined petroleum coke to control dust will interfere with the determination of real density
so the oil must be removed before reducing the sample to 75 μm.
6.1.1 When a petroleum oil was used, it can be removed by flushing with a solvent such as methylene chloride, dichloroethane,
or toluene. The solvent must be completely removed before proceeding with the RD determination. Heating to 10 °C above the
boiling point of the solvent used or application of vacuum is satisfactory for the removal of the dedusting oil.
NOTE 1—Consult the Material Safety Data Sheet (MSDS) for the selected solvent.
6.1.2 An alternative method of oil removal is by heating the calcined petroleum coke sample in an oven at 700 °C for 1 h.
D5004 − 23
7. Apparatus
7.1 Pycnometer, or specific gravity bottle, 50 mL, with a ground glass stopper with a capillary hole. Bottles with a large neck
(12 mm to 13 mm outside diameter) are preferred.
7.2 Water Bath, controlled to a temperature of 25 °C 6 0.1 °C.
NOTE 2—This test method is written to be performed at 25 °C 6 0.1 °C; however, some laboratories may not have the provisions to perform the test at
this temperature. It is permissible to perform the test procedure at any temperature between 20 °C and 40 °C providing that the water bath is controlled
at 60.1 °C of the chosen temperature and the pycnometers are calibrated at the same temperature that is used to determine the real density of the
petroleum coke sample. This is possible due to the fact that the real density of calcined petroleum coke is not affected by temperature changes over a
limited temperature range.
7.3 Analytical Balance, accurate to 60.1 mg.
7.4 Vacuum Desiccator, with guard, connected to a vacuum source capable of lowering pressure to 75 mm of Hg (10 kPa).
7.5 Desiccator, with drying agent. Anhydrous calcium sulphate is satisfactory.
7.6 Drying Oven, preferably a vacuum oven, for temperature to 120 °C.
7.7 Lead Weights, for the pycnometers, to prevent tipping over in the water bath. These can be made by coiling solid wire solder.
7.8 Wire Sieve, 75 μm (No. 200 mesh), meeting Specification E11.
8. Reagents
8.1 Purity of Water—References to distilled water shall be understood to mean reagent water as defined by Type III of
Specification D1193.
8.2 Analytical reagent grade solvents are not required but can be used. The technical grade of each of the following is satisfactory:
8.2.1 Acetone, Xylene, and Ethyl Alcohol. (See 6.1.2.)
9. Sample Preparation
9.1 For recommended practice for obtaining, handling, and preparing coke samples, refer to Practices D346, D2013,
D2234/D2234M, and D4057, and Test Methods D6969 and D6970. See Section 6.
9.2 Crush 50 g of coke so that the entire sample will pass through a 75 μm (No. 200) sieve. Dry the crushed sample in a drying
oven at 115 °C 6 5 °C to constant mass (approximately 8 h). Cool in a desiccator.
NOTE 3—Constant mass is considered to be achieved when change in mass is less than 60.05 g after a 30 min test drying period.
10. Pycnometer Calibration (Determination of Pycnometer Volume)
10.1 Clean the pycnometer and its stopper with detergent, rinse thoroughly with water then with acetone. Place in a desiccator to
dry, then weigh the empty pycnometer together with its stopper to 0.1 mg (mass W ). The temperature of the pycnometer is to be
o
close to room temperature when its mass is determined. (Warning—Commercial pycnometers (specific gravity bottles) can either
have not been calibrated at 25 °C or else not calibrated to the accuracy required for this test method, so it is necessary that the
pycnometer volume be determined.)
A Gay-Lussac pycnometer has been found suitable for this purpose.
D5004 − 23
NOTE 4—Do not handle the pycnometer with bare fingers. Finger cots or surgical gloves can be worn, or tongs can be used, when handling the pycnometer
to prevent moisture from fingers influencing the mass.
10.2 Fill the pycnometer with freshly boiled (to remove air) and cooled distilled water, and replace the stopper. Immerse the
pycnometer up to the neck in the 25 °C 6 0.1 °C water bath for 1 h. Use the lead weights to prevent tipping. Replace water that
leaves the capillary during this period. A syringe is convenient for this purpose.
10.3 At the end of the temperature stabilization period, check the capillary to be certain it is completely filled. Remove excess
water on th
...