ASTM D5863-22
(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
5.1 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 Procedure A, Sections 8–14—Flame AAS is used to analyze a sample that is decomposed with acid for the determination of total Ni, V, and Fe.
1.3 Procedure B, Sections 15–20—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, unless specifically stated. Other units that appear in this standard are included for information purposes only or because they are in embedded pictures that cannot be edited.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in 8.1, 9.2, 9.5, 11.2, 11.4, and 16.1.
1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
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Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5863 − 22
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* mine the applicability of regulatory limitations prior to use.
Specific warning statements are given in 8.1, 9.2, 9.5, 11.2,
1.1 These test methods cover the determination of nickel,
11.4, and 16.1.
vanadium, iron, and sodium in crude oils and residual fuels by
1.8 This international standard was developed in accor-
flame atomic absorption spectrometry (AAS). Two different
dance with internationally recognized principles on standard-
test methods are presented.
ization established in the Decision on Principles for the
1.2 Procedure A, Sections 8–14—Flame AAS is used to
Development of International Standards, Guides and Recom-
analyze a sample that is decomposed with acid for the
mendations issued by the World Trade Organization Technical
determination of total Ni, V, and Fe.
Barriers to Trade (TBT) Committee.
1.3 Procedure B, Sections 15–20—Flame AAS is used to
2. Referenced Documents
analyze a sample diluted with an organic solvent for the
2
determination of Ni, V, and Na. This test method uses oil-
2.1 ASTM Standards:
soluble metals for calibration to determine dissolved metals
D1193 Specification for Reagent Water
and does not purport to quantitatively determine nor detect
D4057 Practice for Manual Sampling of Petroleum and
insoluble particulates. Hence, this test method may underesti-
Petroleum Products
mate the metal content, especially sodium, present as inorganic
D4175 Terminology Relating to Petroleum Products, Liquid
sodium salts.
Fuels, and Lubricants
D4177 Practice for Automatic Sampling of Petroleum and
1.4 The concentration ranges covered by these test methods
Petroleum Products
are determined by the sensitivity of the instruments, the
D6299 Practice for Applying Statistical Quality Assurance
amount of sample taken for analysis, and the dilution volume.
and Control Charting Techniques to Evaluate Analytical
A specific statement is given in Note 1.
Measurement System Performance
1.5 For each element, each test method has its own unique
precision.Theusercanselecttheappropriatetestmethodbased
3. Terminology
on the precision required for the specific analysis.
3.1 Definitions:
1.6 The values stated in SI units are to be regarded as
3.1.1 For definitions of terms used in these test methods,
standard. No other units of measurement are included in this
refer to Terminology D4175.
standard, unless specifically stated. Other units that appear in
this standard are included for information purposes only or
4. Summary of Test Method
because they are in embedded pictures that cannot be edited.
4.1 Procedure A—One to twenty grams of sample are
1.7 This standard does not purport to address all of the
weighed into a beaker and decomposed with concentrated
safety concerns, if any, associated with its use. It is the
sulfuric acid by heating to dryness. The residual carbon is
responsibility of the user of this standard to establish appro-
burned off by heating at 525 °C in a muffle furnace. The
priate safety, health, and environmental practices and deter-
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
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 Dec. 1, 2022. Published January 2023. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1995. Last previous edition approved in 2016 as D5863 – 00a (2016). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D5863-22. 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 ----------------------
D5863 − 22
added to the dilute nitric acid solution. The solution is
nebulized int
...
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 2016) D5863 − 22
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 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 Procedure A, Sections 78–1314—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 Procedure B, Sections 1415–1920—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.standard, unless specifically stated. Other units that appear in this standard are included for information purposes only or
because they are in embedded pictures that cannot be edited.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Specific warning statements are given in 7.18.1, 8.29.2, 8.59.5, 10.211.2,
10.411.4, and 15.116.1.
1.8 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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 April 1, 2016Dec. 1, 2022. Published May 2016January 2023. Originally approved in 1995. Last previous edition approved in 20112016 as
D5863 – 00a (2011).(2016). DOI: 10.1520/D5863-00AR16. 10.1520/D5863-22.
*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 ----------------------
D5863 − 22
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
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. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in these test methods, refer to Terminology D4175.
4. Summary of Test Method
4.1 Test Method Procedure 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 °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 n
...
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