ASTM D5004-11(2017)
(Test Method)Standard Test Method for Real Density of Calcined Petroleum Coke by Xylene Displacement
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
Relations
Buy Standard
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 − 11 (Reapproved 2017)
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 Density of Calcined Petroleum Coke
D4930 Test Method for Dust Control Material on Calcined
1.1 This test method covers the determination of the real
Petroleum Coke
density (RD) of calcined petroleum coke. Real density, by
D6969 Practice for Preparation of Calcined Petroleum Coke
definition, is obtained when the particle size of the test
Samples for Analysis
specimen is smaller than 75 µm (No. 200 sieve).
D6970 Practice for Collection 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
D7454 Test Method for Determination of Vibrated Bulk
standard.
Density of Calcined Petroleum Coke using a Semi-
1.3 This standard does not purport to address all of the
Automated Apparatus
safety concerns, if any, associated with its use. It is the
E11 Specification for Woven Wire Test Sieve Cloth and Test
responsibility of the user of this standard to establish appro-
Sieves
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
3. Terminology
For specific warning statements, see Sections 10 and 11.1.
3.1 Definitions:
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
3.1.1 calcined petroleum coke, n—petroleum coke that has
ization established in the Decision on Principles for the
been thermally treated to drive off the volatile matter and to
Development of International Standards, Guides and Recom-
develop crystalline structure.
mendations issued by the World Trade Organization Technical
3.1.2 petroleum coke, n—solid, carbonaceous residue pro-
Barriers to Trade (TBT) Committee.
duced by thermal decomposition of heavy petroleum fractions
2. Referenced Documents or cracked stocks, or both.
2.1 ASTM Standards: 3.2 Definitions of Terms Specific to This Standard:
D346 Practice for Collection and Preparation of Coke
3.2.1 bulk density, n—mass of the particles divided by the
Samples for Laboratory Analysis
volume they occupy that includes the space between the
D1193 Specification for Reagent Water
particles. Refer to Test Methods D4292 and D7454 for bulk
D2013 Practice for Preparing Coal Samples for Analysis
density procedures.
D2234/D2234M Practice for Collection of a Gross Sample
3.2.2 dedusting material, n—see Test Method D4930.
of Coal
D4057 Practice for Manual Sampling of Petroleum and
3.2.3 real density, n—(also referred to as true specific
Petroleum Products
gravity), the mass divided by the volume occupied by the
D4292 Test Method for Determination of Vibrated Bulk
material excluding pores and voids. It is required, therefore,
that voids in the coke be eliminated and that pores in the
materialbefilledbythefluidbeingdisplaced.Thisrequirement
This test method is under the jurisdiction of ASTM Committee D02 on
ismetforthepurposesofthistestmethodbyreducingthecoke
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
SubcommitteeD02.05onPropertiesofFuels,PetroleumCokeandCarbonMaterial.
particles to a size smaller than 75 µm.
Current edition approved Oct. 1, 2017. Published November 2017. Originally
3.2.3.1 Discussion—The density of particles larger than
approved in 1989. Last previous edition approved in 2011 as D5004 – 11. DOI:
10.1520/D5004-11R17.
75 µm up to the largest that can be put into the helium
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
pycnometer can also be determined, but must be designated as
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
particle density (PD). The precision data obtained for RD may
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. not be applicable to PD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5004 − 11 (2017)
4. Summary of Test Method 7.6 Drying Oven, preferably a vacuum oven, for tempera-
ture to 120 °C.
4.1 The mass of the sample is determined directly and the
volume derived by determining the mass of liquid displaced 7.7 Lead Weights, for the pycnometers, to prevent tipping
when the sample is introduced into a pycnometer. over in the water bath.These can be made by coiling solid wire
solder.
RD 5 M 3D/L (1)
7.8 Wire Sieve, 75 µm (No. 200 mesh), meeting Specifica-
where:
tion E11.
M = mass of sample,
D = density of displaced liquid, and
8. Reagents
L = mass of displaced liquid.
8.1 Purity of Water—References to distilled water shall be
understood to mean reagent water as defined by Type III of
5. Significance and Use
Specification D1193.
5.1 The density of petroleum coke directly influences the
8.2 Analytical reagent grade solvents are not required but
physical and chemical properties of the manufactured carbon
can be used. The technical grade of each of the following is
and graphite artifacts for which it is used. Density, therefore, is
satisfactory:
a major quality specification of calcined petroleum coke and is
8.2.1 Acetone, Xylene, and Ethyl Alcohol. (See 6.1.2.)
used as a control in coke calcination.
9. Sample Preparation
6. Interferences
9.1 For recommended practice for obtaining, handling, and
6.1 Oil or other material sprayed on calcined petroleum
preparing coke samples, refer to Practices D346, D2013,
coketocontroldustwillinterferewiththedeterminationofreal
D2234/D2234M, and D4057, and Test Methods D6969 and
density so the oil must be removed before reducing the sample
D6970. See Section 6.
to 75 µm.
6.1.1 When a petroleum oil was used, it can be removed by
9.2 Crush 50 g of coke so that the entire sample will pass
flushing with a solvent such as methylene chloride,
through a 75 µm (No. 200) sieve. Dry the crushed sample in a
dichloroethane, or toluene. The solvent must be completely
drying oven at 115 °C 6 5 °C to constant mass (approximately
removed before proceeding with the RD determination. Heat-
8 h). Cool in a desiccator.
ing to 10 °C above the boiling point of the solvent used or
NOTE 3—Constant mass is considered to be achieved when change in
application of vacuum is satisfactory for the removal of the
mass is less than 60.05 g after a 30 min test drying period.
dedusting oil.
10. Pycnometer Calibration (Determination of
NOTE 1—Consult the Material Safety Data Sheet (MSDS) for the
Pycnometer Volume)
selected solvent.
10.1 Clean the pycnometer and its stopper with detergent,
6.1.2 An alternative method of oil removal is by heating the
rinse thoroughly with water then with acetone. Place in a
calcined petroleum coke sample in an oven at 700 °C for 1 h.
desiccator to dry, then weigh the empty pycnometer together
7. Apparatus
with its stopper to 0.1 mg (mass W ). The temperature of the
o
pycnometer is to be close to room temperature when its mass
7.1 Pycnometer, or specific gravity bottle, 50 mL, with a
is determined. (Warning—Commercial pycnometers (specific
groundglassstopperwithacapillaryhole. Bottleswithalarge
gravity bottles) can either have not been calibrated at 25 °C or
neck (12 mm to 13 mm outside diameter) are preferred.
elsenotcalibratedtotheaccuracyrequiredforthistestmethod,
7.2 Water Bath, controlled to a temperature of 25 °C 6
so it is necessary that the pycnometer volume be determined.)
0.1 °C.
NOTE 4—Do not handle the pycnometer with bare fingers. Finger cots
NOTE2—Thistestmethodiswrittentobeperformedat25 °C 60.1 °C;
or surgical gloves can be worn, or tongs can be used, when handling the
however, some laboratories may not have the provisions to perform the
pycnometer to prevent moisture from fingers influencing the mass.
test at this temperature. It is permissible to perform the test procedure at
10.2 Fill the pycnometer with freshly boiled (to remove air)
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 andcooleddistilledwater,andreplacethestopper.Immersethe
calibrated at the same temperature that is used to determine the real
pycnometeruptotheneckinthe25 °C 60.1 °Cwaterbathfor
density of the petroleum coke sample. This is possible due to the fact that
1 h.Usetheleadweightstopreventtipping.Replacewaterthat
the real density of calcined petroleum coke is not affected by te
...
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: D5004 − 11 (Reapproved 2017)
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 Density of Calcined Petroleum Coke
D4930 Test Method for Dust Control Material on Calcined
1.1 This test method covers the determination of the real
Petroleum Coke
density (RD) of calcined petroleum coke. Real density, by
D6969 Practice for Preparation of Calcined Petroleum Coke
definition, is obtained when the particle size of the test
Samples for Analysis
specimen is smaller than 75 µm (No. 200 sieve).
D6970 Practice for Collection 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
D7454 Test Method for Determination of Vibrated Bulk
standard.
Density of Calcined Petroleum Coke using a Semi-
1.3 This standard does not purport to address all of the
Automated Apparatus
safety concerns, if any, associated with its use. It is the
E11 Specification for Woven Wire Test Sieve Cloth and Test
responsibility of the user of this standard to establish appro-
Sieves
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
3. Terminology
For specific warning statements, see Sections 10 and 11.1.
1.4 This international standard was developed in accor- 3.1 Definitions:
dance with internationally recognized principles on standard-
3.1.1 calcined petroleum coke, n—petroleum coke that has
ization established in the Decision on Principles for the
been thermally treated to drive off the volatile matter and to
Development of International Standards, Guides and Recom-
develop crystalline structure.
mendations issued by the World Trade Organization Technical
3.1.2 petroleum coke, n—solid, carbonaceous residue pro-
Barriers to Trade (TBT) Committee.
duced by thermal decomposition of heavy petroleum fractions
2. Referenced Documents or cracked stocks, or both.
2.1 ASTM Standards: 3.2 Definitions of Terms Specific to This Standard:
D346 Practice for Collection and Preparation of Coke
3.2.1 bulk density, n—mass of the particles divided by the
Samples for Laboratory Analysis
volume they occupy that includes the space between the
D1193 Specification for Reagent Water
particles. Refer to Test Methods D4292 and D7454 for bulk
D2013 Practice for Preparing Coal Samples for Analysis
density procedures.
D2234/D2234M Practice for Collection of a Gross Sample
3.2.2 dedusting material, n—see Test Method D4930.
of Coal
D4057 Practice for Manual Sampling of Petroleum and
3.2.3 real density, n—(also referred to as true specific
Petroleum Products
gravity), the mass divided by the volume occupied by the
D4292 Test Method for Determination of Vibrated Bulk
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
This test method is under the jurisdiction of ASTM Committee D02 on
is met for the purposes of this test method by reducing the coke
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
particles to a size smaller than 75 µm.
Current edition approved Oct. 1, 2017. Published November 2017. Originally
3.2.3.1 Discussion—The density of particles larger than
approved in 1989. Last previous edition approved in 2011 as D5004 – 11. DOI:
10.1520/D5004-11R17. 75 µm up to the largest that can be put into the helium
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
pycnometer can also be determined, but must be designated as
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
particle density (PD). The precision data obtained for RD may
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. not be applicable to PD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5004 − 11 (2017)
4. Summary of Test Method 7.6 Drying Oven, preferably a vacuum oven, for tempera-
ture to 120 °C.
4.1 The mass of the sample is determined directly and the
volume derived by determining the mass of liquid displaced 7.7 Lead Weights, for the pycnometers, to prevent tipping
when the sample is introduced into a pycnometer. over in the water bath. These can be made by coiling solid wire
solder.
RD5 M 3D/L (1)
7.8 Wire Sieve, 75 µm (No. 200 mesh), meeting Specifica-
where:
tion E11.
M = mass of sample,
D = density of displaced liquid, and
8. Reagents
L = mass of displaced liquid.
8.1 Purity of Water—References to distilled water shall be
understood to mean reagent water as defined by Type III of
5. Significance and Use
Specification D1193.
5.1 The density of petroleum coke directly influences the
8.2 Analytical reagent grade solvents are not required but
physical and chemical properties of the manufactured carbon
can be used. The technical grade of each of the following is
and graphite artifacts for which it is used. Density, therefore, is
satisfactory:
a major quality specification of calcined petroleum coke and is
8.2.1 Acetone, Xylene, and Ethyl Alcohol. (See 6.1.2.)
used as a control in coke calcination.
9. Sample Preparation
6. Interferences
9.1 For recommended practice for obtaining, handling, and
6.1 Oil or other material sprayed on calcined petroleum
preparing coke samples, refer to Practices D346, D2013,
coke to control dust will interfere with the determination of real
D2234/D2234M, and D4057, and Test Methods D6969 and
density so the oil must be removed before reducing the sample
D6970. See Section 6.
to 75 µm.
6.1.1 When a petroleum oil was used, it can be removed by
9.2 Crush 50 g of coke so that the entire sample will pass
flushing with a solvent such as methylene chloride,
through a 75 µm (No. 200) sieve. Dry the crushed sample in a
dichloroethane, or toluene. The solvent must be completely
drying oven at 115 °C 6 5 °C to constant mass (approximately
removed before proceeding with the RD determination. Heat-
8 h). Cool in a desiccator.
ing to 10 °C above the boiling point of the solvent used or
NOTE 3—Constant mass is considered to be achieved when change in
application of vacuum is satisfactory for the removal of the
mass is less than 60.05 g after a 30 min test drying period.
dedusting oil.
10. Pycnometer Calibration (Determination of
NOTE 1—Consult the Material Safety Data Sheet (MSDS) for the
Pycnometer Volume)
selected solvent.
10.1 Clean the pycnometer and its stopper with detergent,
6.1.2 An alternative method of oil removal is by heating the
rinse thoroughly with water then with acetone. Place in a
calcined petroleum coke sample in an oven at 700 °C for 1 h.
desiccator to dry, then weigh the empty pycnometer together
7. Apparatus
with its stopper to 0.1 mg (mass W ). The temperature of the
o
pycnometer is to be close to room temperature when its mass
7.1 Pycnometer, or specific gravity bottle, 50 mL, with a
is determined. (Warning—Commercial pycnometers (specific
ground glass stopper with a capillary hole. Bottles with a large
gravity bottles) can either have not been calibrated at 25 °C or
neck (12 mm to 13 mm outside diameter) are preferred.
else not calibrated to the accuracy required for this test method,
7.2 Water Bath, controlled to a temperature of 25 °C 6
so it is necessary that the pycnometer volume be determined.)
0.1 °C.
NOTE 4—Do not handle the pycnometer with bare fingers. Finger cots
NOTE 2—This test method is written to be performed at 25 °C 6 0.1 °C;
or surgical gloves can be worn, or tongs can be used, when handling the
however, some laboratories may not have the provisions to perform the
pycnometer to prevent moisture from fingers influencing the mass.
test at this temperature. It is permissible to perform the test procedure at
10.2 Fill the pycnometer with freshly boiled (to remove air)
any temperature between 20 °C and 40 °C providing that the water bath is
and cooled distilled water, and replace the stopper. Immerse the
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
pycnometer up to the neck in the 25 °C 6 0.1 °C water bath for
density of the petroleum coke sample. This is possible due to the fact that
1 h. Use the lead weights to prevent tipping. Replace water that
the real density of calcined petroleum coke is not affected by temperature
leaves the capillary during this period. A syringe is convenient
changes over a li
...
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 D5004 − 11 (Reapproved 2017)
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 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 safety, health, and healthenvironmental 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
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:
3.1.1 calcined petroleum coke, n—petroleum coke that has been thermally treated to drive off the volatile matter and to develop
crystalline structure.
3.1.2 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.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products 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, 2011Oct. 1, 2017. Published July 2011November 2017. Originally approved in 1989. Last previous edition approved in 20092011 as
D5004–89(2009).D5004 – 11. DOI: 10.1520/D5004-11.10.1520/D5004-11R17.
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
D5004 − 11 (2017)
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.75 μm.
3.2.3.1 Discussion—
The density of particles larger than 75 μm 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 3D/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.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°C10 °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°C700 °C for
1 h.
7. Apparatus
7.1 Pycnometer, or specific gravity bottle, 50 mL, 50 mL, with a ground glass stopper with a capillary hole. Bottles with a large
neck (12(12 mm to 13 mm 13 mm outside diameter) are preferred.
7.2 Water Bath, controlled to a temperature of 2525 °C 6 0.1°C.0.1 °C.
NOTE 2—This test method is written to be performed at 2525 °C 6 0.1°C;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 2020 °C and 40°C40 °C providing that the water
bath is controlled at 60.1°C60.1 °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.60.1 mg.
7.4 Vacuum Desiccator, with guard, connected to a vacuum source capable of lowering pressure to 75 mm 75 mm of Hg (10
kPa).(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.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 75 μm (No. 200 mesh), meeting Specification E11.
A Gay-Lussac pycnometer has been found suitable for this purpose.
D5004 − 11 (2017)
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 50 g of coke so that the entire sample will pass through a 75 μm 75 μm (No. 200) sieve. Dry the crushed sample
in a drying oven at 1156 5°C 115 °C 6 5 °C to constant mass (approximately 8 h). 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 60.05 g after a 30 min 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 0.1 mg (mass W ). The temperature of the pycnometer
o
is to be close to room temperature when its weightmass is determined. (Warning—Commercial pycnometers (specific gravity
bottles) can either have not been calibrated at 25°C25 °C or else not calibrated to the accuracy required for this test method, so
it is necessary that the pycnometer volume be determined.)
NOTE 4—Do not handle the pycnometer with bare fingers. Finger cots or surgical gloves can be worn, or tongs
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.