ASTM D4422-13
(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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D4422 − 13
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* produce erratic results. The furnace must be swept with air to
achieve oxidation and to decrease the sulfur content of the
1.1 This test method covers the determination of the ash
gases.
content of petroleum coke.
5.2 Preparation and testing of the analysis sample must
1.2 The values stated in SI units are to be regarded as
neither remove nor add ash. Improper dividing, sieving, and
standard. No other units of measurement are included in this
crushing equipment, and some muffle furnace lining material
standard.
can contaminate the sample.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
6. Apparatus
responsibility of the user of this standard to establish appro-
6.1 Crucibles, low wide form glazed porcelain or platinum,
priate safety and health practices and determine the applica-
30-mL capacity.
bility of regulatory limitations prior to use.
6.2 Muffle Furnace, with temperature control between 700
2. Referenced Documents
and 750°C and equipped with a means to regulate air circula-
2
2.1 ASTM Standards:
tion.
D346 Practice for Collection and Preparation of Coke
6.3 Analytical Balance capable of weighing to 0.1 mg.
Samples for Laboratory Analysis
D2013 Practice for Preparing Coal Samples for Analysis
6.4 Drying Oven controlled at 110 6 5°C.
6.5 Desiccator.
3. Summary of Test Method
3.1 A representative sample of petroleum coke is dried,
7. Sample Preparation
ground, and ashed in a muffle furnace at 700 to 750°C. The
7.1 Crush the laboratory sample to pass a 6.3-mm sieve. If
residueorashisexpressedasapercentageofthedrypetroleum
the quantity exceeds 2.3 kg, divide the sample to obtain about
coke.
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
4. Significance and Use
200 g and crush to pass a 250-µm (No. 60) sieve. Divide again
4.1 The ash content is one of the properties used to evaluate
to obtain approximately 50 g and pulverize this fraction such
petroleum coke and indicates the amount of undesirable
that 95 % or more passes a 75-µm (No. 200) sieve. This is the
residue present. Acceptable ash content varies with the in-
analysis sample which is dried to constant weight at 110 6
tended use.
5°C.
5. Interferences
NOTE 1—If the laboratory sample appears to be wet it must be air-dried
prior to crushing to avoid caking.
5.1 High sulfur content of the furnace gases, regardless of
NOTE 2—Recommended practice for collecting samples and the equip-
the source of the sulfur, can react with an alkaline ash to
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 Dec. 1, 2013. Published December 2013. Originally
foradequateaircirculation.Theairflowisadequateifreplicate
approved in 1984. Last previous edition approved in 2008 as D4422 – 03 (2008).
DOI: 10.1520/D4422-13.
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 − 13
9. Procedure 11.2 Report the ash content mass percent to the second
decimal (hundredth of a percent) when only single values are
9.1 Ignite a coded crucible to constant weight at 750°C.
determined.
Record the mass to 0.1 mg.
3
12. Precision and Bias
9.2 Weigh a 10 g portion of the dried analysis sample into
the coded crucible. Record the mass to 0.1 mg. 12.1 Precision—The precision of this test method as deter-
mined by the statistical examination of the interlaborator
...
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 − 03 (Reapproved 2008) D4422 − 13
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 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 and health practices and determine the applicability of regulatory
limitations prior to use.
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 700 to 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-mL capacity.
6.2 Muffle Furnace, with temperature control between 700 and 750°C and equipped with a means to regulate air circulation.
6.3 Analytical Balance capable of weighing to 0.1 mg.
6.4 Drying Oven controlled at 110 6 5°C.
6.5 Desiccator.
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
1
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 Oct. 15, 2008Dec. 1, 2013. Published November 2008 December 2013. Originally approved in 1984. Last previous edition approved in 20032008
as D4422–03. DOI: 10.1520/D4422-03R08. – 03 (2008). DOI: 10.1520/D4422-13.
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 − 13
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.
NOTE 1—If the laboratory sample appears to be wet it must be air-dried prior to crushing to avoid caking.
NOTE 2—Recommended practice for collecting samples and the equipment and procedures for crushing and dividing are described in Practices D346
and D2013.
8. Preparation of Apparatus
8.1 The muffle furnace, when initially set up, must be tested for adequate air circulation. The air flow is adequate if replicate
samples do not produce a lower ash at higher air flow rates with the same furnace loading. Maintain air flow at the same level for
subsequent analyses to ensure consistency in analytical technique.
9. Procedure
9.1 Ignite a coded crucible to constant wei
...
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