ASTM D4530-07
(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 &si-value;
1.7 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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Designation:D4530–07
Standard Test Method for
1
Determination of Carbon Residue (Micro Method)
This standard is issued under the fixed designation D4530; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope* responsibility of the user of this standard to establish appro-
priate safety practices and to determine the applicability of
1.1 Thistestmethodcoversthedeterminationoftheamount
regulatory limitations prior to use. For specific warning
of carbon residue (see Note 1) formed after evaporation and
statements, see 8.2.3 and 8.4.
pyrolysis of petroleum materials under certain conditions and
is intended to provide some indication of the relative coke
2. Referenced Documents
forming tendency of such materials.
3
2.1 ASTM Standards:
1.2 The test results are equivalent to the Conradson Carbon
D189 Test Method for Conradson Carbon Residue of Pe-
Residue test (see Test Method D189).
troleum Products
NOTE 1—This procedure is a modification of the original method and
D482 Test Method for Ash from Petroleum Products
apparatus for carbon residue of petroleum materials, where it has been
D4046 Test Method for Alkyl Nitrate in Diesel Fuels by
2
demonstrated that thermogravimetry is another applicable technique.
Spectrophotometry
However, it is the responsibility of the operator to establish operating
D4057 Practice for Manual Sampling of Petroleum and
conditions to obtain equivalent results when using thermogravimetry.
Petroleum Products
1.3 Thistestmethodisapplicabletopetroleumproductsthat
D4177 Practice for Automatic 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).
E1 Specification for ASTM Liquid-in-Glass Thermometers
Samples expected to be below 0.10 weight % (m/m) residue
E133 Specification for Distillation Equipment
should be distilled to remove 90 % (V/V) of the flask charge
2.2 Energy Institute Standard:
(see Section 9). The 10 % bottoms remaining is then tested for
4
Specification for IP Standard Thermometers
carbon residue by this test method.
1.4 Ash-forming constituents, as defined by Test Method
3. Terminology
D482, or non-volatile additives present in the sample will add
3.1 Definitions:
to the carbon residue value and be included as part of the total
3.1.1 carbon residue, n—in petroleum products, the part
carbon residue value reported.
remaining after a sample has been subjected to thermal
1.5 Alsoindieselfuel,thepresenceofalkylnitrates,suchas
decomposition.
amyl nitrate, hexyl nitrate, or octyl nitrate, causes a higher
3.1.1.1 Discussion—The amount of residue is dependent on
carbon residue value than observed in untreated fuel, which
the test conditions of evaporation and pyrolysis. The term may
may lead to erroneous conclusions as to the coke-forming
be misleading here in that the residue may contain other than
propensity of the fuel. The presence of alkyl nitrate in the fuel
carbon decomposition products. However, the term is retained
may be detected by Test Method D4046.
due to its wide common usage.
1.6 The values stated in SI units are to be regarded as
standard. The values given in parentheses are for information
4. Summary of Test Method
only.
4.1 A weighed quantity of sample is placed in a glass vial
1.7 This standard does not purport to address all of the
and heated to 500°C under an inert (nitrogen) atmosphere in a
safety concerns, if any, associated with its use. It is the
controlled manner for a specific time. The sample undergoes
1 3
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
D02.06 on Analysis of Lubricants. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Nov. 1, 2007. Published December 2007. Originally the ASTM website.
´1 4
approved in 1985. Last previous edition approved in 2006 as D4530–06 . DOI: “Methods for Analysis and Testing,” Institute of Petroleum Standard Methods
10.1520/D4530-07. 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
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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.
An American National Standard
e1
Designation:D4530–06 Designation:D4530–07
Standard Test Method for
1
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.
1
e NOTE—Deleted original footnote 5 editorially in July 2006.
1. 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).
NOTE 1—This procedure is a modification of the original method and apparatus for carbon residue of petroleum materials, where it has been
2
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
bedistilledtoremove90 %(V/V)oftheflaskcharge(seeSection9).The10 %bottomsremainingisthentestedforcarbonresidue
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.
1.7 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.
2. Referenced Documents
3
2.1 ASTM Standards:
D 189 Test Method for Conradson Carbon Residue of Petroleum Products
D 482 Test Method for Ash from Petroleum Products
D 4046 Test Method for Alkyl Nitrate in Diesel Fuels by Spectrophotometry
D 4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D 4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
E 1 Specification for ASTM Liquid-in-Glass Thermometers
E 133 Specification for Distillation Equipment
2.2 IP Standard: Energy Institute Standard:
4
Specification for IP Standard Thermometers
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.06 on
Analysis of Lubricants.
Current edition approved Jan. 1, 2006. Published February 2006. Originally approved in 1985. Last previous edition approved in 2003 as D4530–03.
e1
Current edition approved Nov. 1, 2007. Published December 2007. Originally approved in 1985. Last previous edition approved in 2006 as D 4530–06 .
2
See Fuel, Vol 63, July 1984, pp. 931–934.
3
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
4
“Methods for Analysis and Testing,” Institute of Petroleum Standard Methods for Petroleum and Its Products, Part I, Vol 2. Available from Energy Institute, 61 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.
1
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