ASTM D5708-02

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An American National Standard
Designation:D5708–02
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 D 5708; 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* D 4057 Practice for Manual Sampling of Petroleum and
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Petroleum Products
1.1 These test methods cover the determination of nickel,
D 4177 Practice for Automatic Sampling of Petroleum and
vanadium, and iron in crude oils and residual fuels by
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Petroleum Products
inductively coupled plasma (ICP) atomic emission spectrom-
D 5185 Test Method for Determination of Additive Ele-
etry. Two different test methods are presented.
ments, Wear Metals, and Contaminants in Used Lubricat-
1.2 Test Method A (Sections 7-11 and 18-22)—ICP is used
ing Oils and Determination of Selected Elements in Base
to analyze a sample dissolved in an organic solvent. This test
Oils by Inductively Coupled Plasma Atomic Emission
method uses oil-soluble metals for calibration and does not
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Spectrometry (ICP-AES)
purport to quantitatively determine or detect insoluble particu-
D 6299 Practice for Applying Statistical Quality Assurance
lates.
Techniques to Evaluate Analytical Measurement System
1.3 Test Method B (Sections 12-22)—ICPis used to analyze
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Performance
a sample that is decomposed with acid.
1.4 The concentration ranges covered by these test methods
3. Summary of Test Method
are determined by the sensitivity of the instruments, the
3.1 Test Method A—Approximately 10 g of the sample are
amount of sample taken for analysis, and the dilution volume.
dissolved in an organic solvent (Warning—Combustible. Va-
A specific statement is given in 15.2. Typically, the low
por is harmful.) to give a specimen solution containing 10 %
concentration limits are a few tenths of a mg/kg. Precision data
(m/m) of sample. The solution is nebulized into the plasma,
are provided for the concentration ranges specified in Section
and the intensities of the emitted light at wavelengths charac-
21.
teristic of the analytes are measured sequentially or simulta-
1.5 The values stated in SI units are to be regarded as the
neously. The intensities are related to concentrations by the
standard. The values given in parentheses are provided for
appropriate use of calibration data.
information only.
3.2 Test Method B—One to 20 g of sample are weighed into
1.6 This standard does not purport to address all of the
a beaker and decomposed with concentrated sulfuric acid
safety concerns, if any, associated with its use. It is the
(Warning—Poison. Causes severe burns. Harmful or fatal if
responsibility of the user of this standard to establish appro-
swallowed or inhaled.) by heating to dryness. Great care must
priate safety and health practices and determine the applica-
be used in this decomposition because the acid fumes are
bility of regulatory limitations prior to use.
corrosive and the mixture is potentially flammable. The re-
2. Referenced Documents sidual carbon is burned off by heating at 525°C in a muffle
furnace. The inorganic residue is digested with nitric acid
2.1 ASTM Standards:
2
(Warning—Poison. Causes severe burns. Harmful or fatal if
D 1193 Specification for Reagent Water
swallowed or inhaled.), evaporated to incipient dryness, dis-
D 1548 Test Method for Vanadium in Navy Special Fuel
3
solved in dilute nitric acid, and made up to volume. The
Oil
solution is nebulized into the plasma of an atomic emission
spectrometer. The intensities of light emitted at characteristic
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved Feb. 10, 2002. Published April 2002. Originally
published as D 5708 – 95. Last previous edition D 5708 – 00.
2 4
Annual Book of ASTM Standards, Vol 11.01. Annual Book of ASTM Standards, Vol 05.02.
3 5
Discontinued; see 1997 Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 05.03.
*A Summary of Changes section appears at the end of this standard.
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D5708–02
wavelengths of the metals are measured sequentially or simul- 7.2 Nebulizer—The use of a high-solids nebulizer is op-
taneously.These intensities are related to concentrations by the tional but st
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