Standard Test Methods for Determination of Nickel, Vanadium, and Iron in Crude Oils and Residual Fuels by Inductively Coupled Plasma (ICP) Atomic Emission Spectrometry

SIGNIFICANCE AND USE
These test methods cover, in single procedures, the determination of Ni, V, and Fe in crude oils and residual oils. These test methods complement Test Method D 1548, which covers only the determination of vanadium.
When fuels are combusted, vanadium present in the fuel can form corrosive compounds. The value of crude oils can be determined, in part, by the concentrations of nickel, vanadium, and iron. Nickel and vanadium, present at trace levels in petroleum fractions, can deactivate catalysts during processing. These test methods provide a means of determining the concentrations of nickel, vanadium, and iron.
SCOPE
1.1 These test methods cover the determination of nickel, vanadium, and iron in crude oils and residual fuels by inductively coupled plasma (ICP) atomic emission spectrometry. Two different test methods are presented.
1.2 Test Method A (Sections 7-11 and 18-22)—ICP is used to analyze a sample dissolved in an organic solvent. This test method uses oil-soluble metals for calibration and does not purport to quantitatively determine or detect insoluble particulates.
1.3 Test Method B (Sections 12-22)—ICP is used to analyze a sample that is decomposed with acid.
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 15.2. Typically, the low concentration limits are a few tenths of a mg/kg. Precision data are provided for the concentration ranges specified in Section 21.
1.5 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.6 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.

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ASTM D5708-11 - Standard Test Methods for Determination of Nickel, Vanadium, and Iron in Crude Oils and Residual Fuels by Inductively Coupled Plasma (ICP) Atomic Emission Spectrometry
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REDLINE ASTM D5708-11 - Standard Test Methods for Determination of Nickel, Vanadium, and Iron in Crude Oils and Residual Fuels by Inductively Coupled Plasma (ICP) Atomic Emission Spectrometry
English language
8 pages
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5708 − 11
StandardTest Methods for
Determination of Nickel, Vanadium, and Iron in Crude Oils
and Residual Fuels by Inductively Coupled Plasma (ICP)
1
Atomic Emission Spectrometry
This standard is issued under the fixed designation D5708; 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
1. Scope* D1548 Test Method for Vanadium in Heavy Fuel Oil
3
(Withdrawn 1997)
1.1 These test methods cover the determination of nickel,
D4057 Practice for Manual Sampling of Petroleum and
vanadium, and iron in crude oils and residual fuels by
Petroleum Products
inductively coupled plasma (ICP) atomic emission spectrom-
D4177 Practice for Automatic Sampling of Petroleum and
etry. Two different test methods are presented.
Petroleum Products
1.2 Test Method A (Sections 7-11 and 18-22)—ICPisusedto
D5185 TestMethodforDeterminationofAdditiveElements,
analyze a sample dissolved in an organic solvent. This test
Wear Metals, and Contaminants in Used Lubricating Oils
method uses oil-soluble metals for calibration and does not
and Determination of Selected Elements in Base Oils by
purport to quantitatively determine or detect insoluble particu-
Inductively Coupled Plasma Atomic Emission Spectrom-
lates.
etry (ICP-AES)
1.3 Test Method B (Sections 12-22)—ICPis used to analyze
D6299 Practice for Applying Statistical Quality Assurance
a sample that is decomposed with acid.
and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
1.4 The concentration ranges covered by these test methods
D7260 Practice for Optimization, Calibration, and Valida-
are determined by the sensitivity of the instruments, the
tion of Inductively Coupled Plasma-Atomic Emission
amount of sample taken for analysis, and the dilution volume.
Spectrometry (ICP-AES) for ElementalAnalysis of Petro-
A specific statement is given in 15.2. Typically, the low
leum Products and Lubricants
concentration limits are a few tenths of a mg/kg. Precision data
are provided for the concentration ranges specified in Section
3. Summary of Test Method
21.
3.1 Test Method A—Approximately 10 g of the sample are
1.5 The values stated in SI units are to be regarded as
dissolved in an organic solvent (Warning—Combustible. Va-
standard. The values given in parentheses are for information
por is harmful.) to give a specimen solution containing 10 %
only.
(m/m) of sample. The solution is nebulized into the plasma,
1.6 This standard does not purport to address all of the
and the intensities of the emitted light at wavelengths charac-
safety concerns, if any, associated with its use. It is the
teristic of the analytes are measured sequentially or simultane-
responsibility of the user of this standard to establish appro-
ously. The intensities are related to concentrations by the
priate safety and health practices and determine the applica-
appropriate use of calibration data.
bility of regulatory limitations prior to use.
3.2 Test Method B—One to 20 g of sample are weighed into
2. Referenced Documents
a beaker and decomposed with concentrated sulfuric acid
2
(Warning—Poison. Causes severe burns. Harmful or fatal if
2.1 ASTM Standards:
swallowed or inhaled.) by heating to dryness. Great care must
D1193 Specification for Reagent Water
be used in this decomposition because the acid fumes are
1
corrosive and the mixture is potentially flammable. The re-
These test methods are under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
sidual carbon is burned off by heating at 525°C in a muffle
D02.03 on Elemental Analysis.
furnace. The inorganic residue is digested with nitric
CurrenteditionapprovedJune1,2011.PublishedJuly2011.Originallyapproved
acid(Warning—Poison. Causes severe burns. Harmful or fatal
in 1995. Last previous edition approved in 2005 as D5708–05. DOI: 10.1520/
D5708-11. if swallowed or inhaled.), evaporated to incipient dryness,
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
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
*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 ----------------------
D5708 − 11
dissolved in dilute nitric acid, and made up to volume. The eter, e
...

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.
Designation:D5708–05 Designation:D5708–11
Standard Test Methods for
Determination of Nickel, Vanadium, and Iron in Crude Oils
and Residual Fuels by Inductively Coupled Plasma (ICP)
1
Atomic Emission Spectrometry
This standard is issued under the fixed designation D5708; 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, and iron in crude oils and residual fuels by inductively
coupled plasma (ICP) atomic emission spectrometry. Two different test methods are presented.
1.2 Test MethodA(Sections 7-11 and 18-22)—ICPisusedtoanalyzeasampledissolvedinanorganicsolvent.Thistestmethod
uses oil-soluble metals for calibration and does not purport to quantitatively determine or detect insoluble particulates.
1.3 Test Method B (Sections 12-22) —ICP is used to analyze a sample that is decomposed with acid.
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.Aspecific statement is given in 15.2.Typically, the low concentration limits
are a few tenths of a mg/kg. Precision data are provided for the concentration ranges specified in Section 21.
1.5 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.6 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
3
D1548 Test Method for Vanadium in Navy Special Fuel Oil
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D5185 Test Method for Determination of Additive Elements, Wear Metals, and Contaminants in Used Lubricating Oils and
Determination of Selected Elements in Base Oils by Inductively Coupled PlasmaAtomic Emission Spectrometry (ICP-AES)
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical
Measurement System Performance Practice for Applying Statistical Quality Assurance and Control Charting Techniques to
Evaluate Analytical Measurement System Performance
D7260 Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry
(ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
3. Summary of Test Method
3.1 Test Method A—Approximately 10 g of the sample are dissolved in an organic solvent ( Warning—Combustible. Vapor is
harmful.) to give a specimen solution containing 10 % (m/m) of sample. The solution is nebulized into the plasma, and the
intensities of the emitted light at wavelengths characteristic of the analytes are measured sequentially or simultaneously. The
intensities are related to concentrations by the appropriate use of calibration data.
3.2 Test Method B—One to 20 g of sample are weighed into a beaker and decomposed with concentrated sulfuric acid
(Warning—Poison.Causessevereburns.Harmfulorfatalifswallowedorinhaled.)byheatingtodryness.Greatcaremustbeused
1
These test methods are under the jurisdiction ofASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.03
on Elemental Analysis.
Current edition approved Nov.June 1, 2005.2011. Published November 2005.July 2011. Originally approved in 1995. Last previous edition approved in 20022005 as
D5708–02.D5708–05. DOI: 10.1520/D5708-05.10.1520/D5708-11.
2
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.
3
Withdrawn.
3
Withdrawn. The last approved version of this historical standard is referenced on www.astm.org.
*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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...

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