ASTM D4530-06e1
(Test Method)Standard Test Method for Determination of Carbon Residue (Micro Method)
Standard Test Method for Determination of Carbon Residue (Micro Method)
SIGNIFICANCE AND USE
The carbon residue value of the various petroleum materials serves as an approximation of the tendency of the material to form carbonaceous type deposits under degradation conditions similar to those used in the test method, and can be useful as a guide in manufacture of certain stocks. However, care needs to be exercised in interpreting the results.
This test method offers advantages of better control of test conditions, smaller samples, and less operator attention compared to Test Method D 189, to which it is equivalent.
Up to twelve samples may be run simultaneously, including a control sample when the vial holder shown in Fig. 1 is used exclusively for sample analysis.
SCOPE
1.1 This test method covers the determination of the amount of carbon residue (see Note 1) formed after evaporation and pyrolysis of petroleum materials under certain conditions and is intended to provide some indication of the relative coke forming tendency of such materials.
1.2 The test results are equivalent to the Conradson Carbon Residue test (see Test Method D 189). This procedure is a modification of the original method and apparatus for carbon residue of petroleum materials, where it has been demonstrated that thermogravimetry is another applicable technique. However, it is the responsibility of the operator to establish operating conditions to obtain equivalent results when using thermogravimetry.
1.3 This test method is applicable to petroleum products that partially decompose on distillation at atmospheric pressure and was tested for carbon residue values of 0.10 to 30 % (m/m). Samples expected to be below 0.10 weight % (m/m) residue should be distilled to remove 90 % (V/V) of the flask charge (see Section ). The 10 % bottoms remaining is then tested for carbon residue by this test method.
1.4 Ash-forming constituents, as defined by Test Method D 482, or non-volatile additives present in the sample will add to the carbon residue value and be included as part of the total carbon residue value reported.
1.5 Also in diesel fuel, the presence of alkyl nitrates, such as amyl nitrate, hexyl nitrate, or octyl nitrate, causes a higher carbon residue value than observed in untreated fuel, which may lead to erroneous conclusions as to the coke-forming propensity of the fuel. The presence of alkyl nitrate in the fuel may be detected by Test Method D 4046.
1.6 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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 practices and to determine the applicability of regulatory limitations prior to use. For specific warning statements, see 8.2.3 and 8.4.
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An American National Standard
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Designation:D4530–06
Standard Test Method for
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Determination of Carbon Residue (Micro Method)
This standard is issued under the fixed designation D 4530; 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 (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
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e NOTE—Deleted original footnote 5 editorially in July 2006.
1. Scope* 1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 Thistestmethodcoversthedeterminationoftheamount
responsibility of the user of this standard to establish appro-
of carbon residue (see Note 1) formed after evaporation and
priate safety practices and to determine the applicability of
pyrolysis of petroleum materials under certain conditions and
regulatory limitations prior to use. For specific warning
is intended to provide some indication of the relative coke
statements, see 8.2.3 and 8.4.
forming tendency of such materials.
1.2 The test results are equivalent to the Conradson Carbon
2. Referenced Documents
Residue test (see Test Method D 189).
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2.1 ASTM Standards:
NOTE 1—This procedure is a modification of the original method and
D 189 Test Method for Conradson Carbon Residue of
apparatus for carbon residue of petroleum materials, where it has been
Petroleum Products
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demonstrated that thermogravimetry is another applicable technique.
D 482 Test Method for Ash from Petroleum Products
However, it is the responsibility of the operator to establish operating
D 4046 Test Method for Alkyl Nitrate in Diesel Fuels by
conditions to obtain equivalent results when using thermogravimetry.
Spectrophotometry
1.3 Thistestmethodisapplicabletopetroleumproductsthat
D 4057 Practice for Manual Sampling of Petroleum and
partially decompose on distillation at atmospheric pressure and
Petroleum Products
was tested for carbon residue values of 0.10 to 30 % (m/m).
D 4177 Practice for Automatic Sampling of Petroleum and
Samples expected to be below 0.10 weight % (m/m) residue
Petroleum Products
should be distilled to remove 90 % (V/V) of the flask charge
E1 Specification forASTM Liquid-in-Glass Thermometers
(see Section 9). The 10 % bottoms remaining is then tested for
E 133 Specification for Distillation Equipment
carbon residue by this test method.
2.2 IP Standard:
1.4 Ash-forming constituents, as defined by Test Method
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Specification for IP Standard Thermometers
D 482, or non-volatile additives present in the sample will add
to the carbon residue value and be included as part of the total
3. Terminology
carbon residue value reported.
3.1 Definitions:
1.5 Alsoindieselfuel,thepresenceofalkylnitrates,suchas
3.1.1 carbon residue, n—in petroleum products, the part
amyl nitrate, hexyl nitrate, or octyl nitrate, causes a higher
remaining after a sample has been subjected to thermal
carbon residue value than observed in untreated fuel, which
decomposition.
may lead to erroneous conclusions as to the coke-forming
3.1.1.1 Discussion—The amount of residue is dependent on
propensity of the fuel. The presence of alkyl nitrate in the fuel
the test conditions of evaporation and pyrolysis. The term may
may be detected by Test Method D 4046.
be misleading here in that the residue may contain other than
1.6 The values stated in SI units are to be regarded as the
carbon decomposition products. However, the term is retained
standard. The values given in parentheses are for information
due to its wide common usage.
only.
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
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This test method is under the jurisdiction of ASTM Committee D02 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Standards volume information, refer to the standard’s Document Summary page on
D02.06 on Analysis of Lubricants. the ASTM website.
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Current edition approved Jan. 1, 2006. Published February 2006. Originally “Methods for Analysis and Testing,” Institute of Petroleum Standard Methods
approved in 1985. Last previous edition approved in 2003 as D 4530–03. for Petroleum and Its Products, Part I, Vol 2. Available from Energy Institute, 61
2
See Fuel, Vol 63, July 1984, pp. 931–934. New Cavendish St., London, WIM 8AR, UK.
*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.
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D4530–06
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