ASTM D4422-19
(Test Method)Standard Test Method for Ash in Analysis of Petroleum Coke
Standard Test Method for Ash in Analysis of Petroleum Coke
SIGNIFICANCE AND USE
4.1 The ash content is one of the properties used to evaluate petroleum coke and indicates the amount of undesirable residue present. Acceptable ash content varies with the intended use.
SCOPE
1.1 This test method covers the determination of the ash content of petroleum coke.
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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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: D4422 − 19
Standard Test Method for
1
Ash in Analysis of Petroleum Coke
This standard is issued under the fixed designation D4422; 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* 5. Interferences
1.1 This test method covers the determination of the ash
5.1 High sulfur content of the furnace gases, regardless of
content of petroleum coke.
the source of the sulfur, can react with an alkaline ash to
produce erratic results. The furnace must be swept with air to
1.2 The values stated in SI units are to be regarded as
achieve oxidation and to decrease the sulfur content of the
standard. No other units of measurement are included in this
gases.
standard.
5.2 Preparation and testing of the analysis sample must
1.3 This standard does not purport to address all of the
neither remove nor add ash. Improper dividing, sieving, and
safety concerns, if any, associated with its use. It is the
crushing equipment, and some muffle furnace lining material
responsibility of the user of this standard to establish appro-
can contaminate the sample.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
6. Apparatus
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
6.1 Crucibles, low wide form glazed porcelain or platinum,
ization established in the Decision on Principles for the 30 mL capacity.
Development of International Standards, Guides and Recom-
6.2 Muffle Furnace, with temperature control between
mendations issued by the World Trade Organization Technical
700 °C and 750 °C and equipped with a means to regulate air
Barriers to Trade (TBT) Committee.
circulation.
2. Referenced Documents
6.3 Analytical Balance capable of weighing to 0.1 mg.
2
2.1 ASTM Standards:
6.4 Drying Oven controlled at 110 °C 6 5 °C.
D346 Practice for Collection and Preparation of Coke
6.5 Desiccator.
Samples for Laboratory Analysis
D2013 Practice for Preparing Coal Samples for Analysis
7. Sample Preparation
3. Summary of Test Method
7.1 Crush the laboratory sample to pass a 6.3 mm sieve. If
3.1 A representative sample of petroleum coke is dried, the quantity exceeds 2.3 kg, divide the sample to obtain about
ground, and ashed in a muffle furnace at 700 °C to 750 °C.The 2.3 kg and crush this fraction to pass a 850 µm (No. 20) sieve.
residueorashisexpressedasapercentageofthedrypetroleum Further divide the sample to obtain a portion of approximately
coke. 200 g and crush to pass a 250 µm (No. 60) sieve. Divide again
toobtainapproximately50 g.Thisistheanalysissamplewhich
4. Significance and Use
is dried to constant weight at 110 °C 6 5 °C.
4.1 The ash content is one of the properties used to evaluate
NOTE 1—If the laboratory sample appears to be wet it must be air-dried
petroleum coke and indicates the amount of undesirable
prior to crushing to avoid caking.
residue present. Acceptable ash content varies with the in-
NOTE 2—Recommended practice for collecting samples and the equip-
tended use.
ment and procedures for crushing and dividing are described in Practices
D346 and D2013.
1
This test method is under the jurisdiction of ASTM Committee D02 on
8. Preparation of Apparatus
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
SubcommitteeD02.05onPropertiesofFuels,PetroleumCokeandCarbonMaterial.
8.1 The muffle furnace, when initially set up, must be tested
Current edition approved Jan. 1, 2019. Published February 2019. Originally
foradequateaircirculation.Theairflowisadequateifreplicate
approved in 1984. Last previous edition approved in 2013 as D4422 – 13. DOI:
10.1520/D4422-18.
samplesdonotproducealowerashathigherairflowrateswith
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
the same furnace loading. Maintain air flow at the same level
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
for subsequent analyses to ensure consistency in analytical
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. technique.
*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 ----------------------
D4422 − 19
3
9. Procedure 12. Precision and Bias
9.1 Ignite a coded
...
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: D4422 − 13 D4422 − 19
Standard Test Method for
1
Ash in Analysis of Petroleum Coke
This standard is issued under the fixed designation D4422; 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 test method covers the determination of the ash content of petroleum coke.
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.
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
2.1 ASTM Standards:
D346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis
D2013 Practice for Preparing Coal Samples for Analysis
3. Summary of Test Method
3.1 A representative sample of petroleum coke is dried, ground, and ashed in a muffle furnace at 700700 °C to 750°C.750 °C.
The residue or ash is expressed as a percentage of the dry petroleum coke.
4. Significance and Use
4.1 The ash content is one of the properties used to evaluate petroleum coke and indicates the amount of undesirable residue
present. Acceptable ash content varies with the intended use.
5. Interferences
5.1 High sulfur content of the furnace gases, regardless of the source of the sulfur, can react with an alkaline ash to produce
erratic results. The furnace must be swept with air to achieve oxidation and to decrease the sulfur content of the gases.
5.2 Preparation and testing of the analysis sample must neither remove nor add ash. Improper dividing, sieving, and crushing
equipment, and some muffle furnace lining material can contaminate the sample.
6. Apparatus
6.1 Crucibles, low wide form glazed porcelain or platinum, 30-mL30 mL capacity.
6.2 Muffle Furnace, with temperature control between 700700 °C and 750°C750 °C and equipped with a means to regulate air
circulation.
6.3 Analytical Balance capable of weighing to 0.1 mg.0.1 mg.
6.4 Drying Oven controlled at 110110 °C 6 5°C.5 °C.
6.5 Desiccator.
1
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 Dec. 1, 2013Jan. 1, 2019. Published December 2013February 2019. Originally approved in 1984. Last previous edition approved in 20082013
as D4422 – 03 (2008). – 13. DOI: 10.1520/D4422-13.10.1520/D4422-18.
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 ----------------------
D4422 − 19
7. Sample Preparation
7.1 Crush the laboratory sample to pass a 6.3-mm sieve. If the quantity exceeds 2.3 kg, divide the sample to obtain about 2.3
kg and crush this fraction to pass a 850-μm (No. 20) sieve. Further divide the sample to obtain a portion of approximately 200
g and crush to pass a 250-μm (No. 60) sieve. Divide again to obtain approximately 50 g and pulverize this fraction such that 95 %
or more passes a 75-μm (No. 200) sieve. This is the analysis sample which is dried to constant weight at 110 6 5°C.Crush the
laboratory sample to pass a 6.3 mm sieve. If the quantity exceeds 2.3 kg, divide the sample to obtain about 2.3 kg and crush this
fraction to pass a 850 μm (No. 20) sieve. Further divide the sample to obtain a portion of approximately 200 g and crush to pass
a 250 μm (No. 60) sieve. Divide again to o
...
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