ASTM D5863-00a(2016)
(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
SIGNIFICANCE AND USE
4.1 When fuels are combusted, metals present in the fuels can form low melting compounds that are corrosive to metal parts. Metals present at trace levels in petroleum can deactivate catalysts during processing. These test methods provide a means of quantitatively determining the concentrations of vanadium, nickel, iron, and sodium. Thus, these test methods can be used to aid in determining the quality and value of the crude oil and residual oil.
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 7–13—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 14–19—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. Hence, this test method may underestimate the metal content, especially sodium, present as inorganic sodium salts.
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 standard. No other units of measurement are included in this standard.
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.
General Information
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Designation: D5863 − 00a (Reapproved 2016)
Standard Test Methods for
Determination of Nickel, Vanadium, Iron, and Sodium in
Crude Oils and Residual Fuels by Flame Atomic Absorption
1
Spectrometry
This standard is issued under the fixed designation D5863; 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 2. Referenced Documents
2
1.1 These test methods cover the determination of nickel,
2.1 ASTM Standards:
vanadium, iron, and sodium in crude oils and residual fuels by
D1193 Specification for Reagent Water
flame atomic absorption spectrometry (AAS). Two different
D4057 Practice for Manual Sampling of Petroleum and
test methods are presented.
Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and
1.2 Test Method A, Sections 7–13—Flame AAS is used to
Petroleum Products
analyze a sample that is decomposed with acid for the
D6299 Practice for Applying Statistical Quality Assurance
determination of total Ni, V, and Fe.
and Control Charting Techniques to Evaluate Analytical
1.3 Test Method B, Sections 14–19—Flame AAS is used to
Measurement System Performance
analyze a sample diluted with an organic solvent for the
determination of Ni, V, and Na. This test method uses oil-
3. Summary of Test Method
soluble metals for calibration to determine dissolved metals
and does not purport to quantitatively determine nor detect
3.1 Test Method A—One to twenty grams of sample are
insoluble particulates. Hence, this test method may underesti-
weighed into a beaker and decomposed with concentrated
mate the metal content, especially sodium, present as inorganic
sulfuric acid by heating to dryness. The residual carbon is
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
incipient dryness, dissolved in dilute nitric and made up to
are determined by the sensitivity of the instruments, the
volume with dilute nitric acid. Interference suppressant is
amount of sample taken for analysis, and the dilution volume.
added to the dilute nitric acid solution. The solution is
A specific statement is given in Note 1.
nebulized into the flame of an atomic absorption spectrometer.
1.5 For each element, each test method has its own unique
A nitrous oxide/acetylene flame is used for vanadium and an
precision.Theusercanselecttheappropriatetestmethodbased
air/acetylene flame is used for nickel and iron. The instrument
on the precision required for the specific analysis.
is calibrated with matrix-matched standard solutions. The
1.6 The values stated in SI units are to be regarded as
measuredabsorptionintensitiesarerelatedtoconcentrationsby
standard. No other units of measurement are included in this
the appropriate use of calibration data.
standard.
3.2 Test Method B—Sample is diluted with an organic
1.7 This standard does not purport to address all of the
solvent to give a test solution containing either 5 % (m/m) or
safety concerns, if any, associated with its use. It is the
20 % (m/m) sample. The recommended sample concentration
responsibility of the user of this standard to establish appro-
is dependent on the concentrations of the analytes in the
priate safety and health practices and determine the applica-
sample. For the determination of vanadium, interference sup-
bility of regulatory limitations prior to use. Specific warning
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
1
These test methods are under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricantsand are the direct responsibility of
2
Subcommittee D02.03 on Elemental Analysis. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved April 1, 2016. Published May 2016. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1995. Last previous edition approved in 2011 as D5863 – 00a (2011). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D5863-00AR16. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5863 − 00a (2016)
air/acetylene flame is used for nickel and sodium. The mea-
sured absorption intensities are related to con
...
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: D5863 − 00a (Reapproved 2011) D5863 − 00a (Reapproved 2016)
Standard Test Methods for
Determination of Nickel, Vanadium, Iron, and Sodium in
Crude Oils and Residual Fuels by Flame Atomic Absorption
1
Spectrometry
This standard is issued under the fixed designation D5863; 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 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 7–13—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 14–19—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. Hence, this test method may underestimate the metal
content, especially sodium, present as inorganic sodium salts.
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 standard. No other units of measurement are included in this standard.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
3. Summary of Test Method
3.1 Test Method A—One to twenty grams of sample are weighed into a beaker and decomposed with concentrated sulfuric acid
by heating to dryness. The residual carbon is burned off by heating at 525°C525 °C in a muffle furnace. The inorganic residue is
digested in dilute nitric acid, evaporated to incipient dryness, dissolved in dilute nitric and made up to volume with dilute nitric
acid. Interference suppressant is added to the dilute nitric acid solution. The solution is nebulized into the flame of an atomic
absorption spectrometer. A nitrous oxide/acetylene flame is used for vanadium and an air/acetylene flame is used for nickel and
1
These test methods are under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricantsand are the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
Current edition approved May 1, 2011April 1, 2016. Published May 2011May 2016. Originally approved in 1995. Last previous edition approved in 20052011 as
D5863–00a(2005).D5863 – 00a (2011). DOI: 10.1520/D5863-00AR11.10.1520/D5863-00AR16.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5863 − 00a (2016)
iron. The instrument is calibrated with matrix-matched standard solutions. The measured absorption intensities are related to
concentrations by the appropriate use of calibration data.
3.2 Test Method B—Sample is diluted with an organic solvent to give a test solution containing either 5 % (m/m) or 20 % (m/m)
sample. The recommended sample concentration is dependent on the co
...
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