ASTM D5863-00a
(Test Method)Standard Test Methods for Determination of Nickel, Vanadium, Iron, and Sodium in Crude Oils and Residual Fuels by Flame Atomic Absorption Spectrometry
Standard Test Methods for Determination of Nickel, Vanadium, Iron, and Sodium in Crude Oils and Residual Fuels by Flame Atomic Absorption Spectrometry
SCOPE
1.1 These test methods cover the determination of nickel, vanadium, iron, and sodium in crude oils and residual fuels by flame atomic absorption spectrometry (AAS). Two different test methods are presented.
1.2 Test Method A, Sections 7-12—Flame AAS is used to analyze a sample that is decomposed with acid for the determination of total Ni, V, and Fe.
1.3 Test Method B, Sections 13-17—Flame AAS is used to analyze a sample diluted with an organic solvent for the determination of Ni, V, and Na. This test method uses oil-soluble metals for calibration to determine dissolved metals and does not purport to quantitatively determine nor detect insoluble particulates.
1.4 The concentration ranges covered by these test methods are determined by the sensitivity of the instruments, the amount of sample taken for analysis, and the dilution volume. A specific statement is given in Note 1.
1.5 For each element, each test method has its own unique precision. The user can select the appropriate test method based on the precision required for the specific analysis.
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 and health practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in 7.1, 8.2, 8.5, 10.2, 10.4, and 15.1
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An American National Standard
Designation:D5863–00a
Standard Test Methods for
Determination of Nickel, Vanadium, Iron, and Sodium in
Crude Oils and Residual Fuels by Flame Atomic Absorption
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Spectrometry
This standard is issued under the fixed designation D 5863; 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.
1. Scope 2. Referenced Documents
1.1 These test methods cover the determination of nickel, 2.1 ASTM Standards:
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vanadium, iron, and sodium in crude oils and residual fuels by D 1193 Specification for Reagent Water
flame atomic absorption spectrometry (AAS). Two different D 4057 Practice for Manual Sampling of Petroleum and
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test methods are presented. Petroleum Products
1.2 Test Method A, Sections 7–12—Flame AAS is used to D 4177 Practice for Automatic Sampling of Petroleum and
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analyze a sample that is decomposed with acid for the Petroleum Products
determination of total Ni, V, and Fe. D 6299 Practice for Applying Statistical Quality Assurance
1.3 Test Method B, Sections 13–17—Flame AAS is used to Techniques to Evaluate Analytical Measurement System
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analyze a sample diluted with an organic solvent for the Performance
determination of Ni, V, and Na. This test method uses oil-
3. Summary of Test Methods
soluble metals for calibration to determine dissolved metals
3.1 Test Method A—One to twenty grams of sample are
and does not purport to quantitatively determine nor detect
insoluble particulates. Hence, this test method may underesti- weighed into a beaker and decomposed with concentrated
sulfuric acid by heating to dryness. The residual carbon is
mate the metal content, especially sodium, present as inorganic
sodium salts. burned off by heating at 525°C in a muffle furnace. The
inorganic residue is digested in dilute nitric acid, evaporated to
1.4 The concentration ranges covered by these test methods
are determined by the sensitivity of the instruments, the incipient dryness, dissolved in dilute nitric and made up to
amount of sample taken for analysis, and the dilution volume. volume with dilute nitric acid. Interference suppressant is
added to the dilute nitric acid solution. The solution is
A specific statement is given in Note 1.
1.5 For each element, each test method has its own unique nebulized into the flame of an atomic absorption spectrometer.
A nitrous oxide/acetylene flame is used for vanadium and an
precision.Theusercanselecttheappropriatetestmethodbased
on the precision required for the specific analysis. air/acetylene flame is used for nickel and iron. The instrument
is calibrated with matrix-matched standard solutions. The
1.6 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information measuredabsorptionintensitiesarerelatedtoconcentrationsby
the appropriate use of calibration data.
only.
1.7 This standard does not purport to address all of the 3.2 Test Method B—Sample is diluted with an organic
solvent to give a test solution containing either 5 % (m/m) or
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 20 % (m/m) sample. The recommended sample concentration
is dependent on the concentrations of the analytes in the
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific warning sample. For the determination of vanadium, interference sup-
pressant is added to the test solution. The test solution is
statements are given in 7.1, 8.2, 8.5, 10.2, 10.4, and 15.1.
nebulized into the flame of an atomic absorption spectrometer.
A nitrous oxide/acetylene flame is used for vanadium and an
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These test methods are under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
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tee D02.03 on Elemental Analysis. Annual Book of ASTM Standards, Vol 11.01.
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Current edition approved Nov. 10, 2000. Published November 2000. Originally Annual Book of ASTM Standards, Vol 05.02.
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published as D 5863 – 95. Last previous edition D 5863 – 00. Annual Book of ASTM Standards, Vol 05.03.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D5863–00a
air/acetylene flame is used for nickel and sodium. The mea-
sured absorption intensities are related to concentrations by the
appropriate use of calibration data.
4. Significance and Use
4.1 When fuels are combusted, metals present in the fuels
can form low melting compounds that ar
...
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