ASTM D4951-09
(Test Method)Standard Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
Standard Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
SIGNIFICANCE AND USE
This test method usually requires several minutes per sample. This test method covers eight elements and thus provides more elemental composition data than Test Method D 4628 or Test Methods D 4927. In addition, this test method provides more accurate results than Test Method D 5185, which is intended for used lubricating oils and base oils.
Additive packages are blends of individual additives, which can act as detergents, antioxidants, antiwear agents, and so forth. Many additives contain one or more elements covered by this test method. Additive package specifications are based, in part, on elemental composition. Lubricating oils are typically blends of additive packages, and their specifications are also determined, in part, by elemental composition. This test method can be used to determine if additive packages and unused lubricating oils meet specifications with respect to elemental composition.
SCOPE
1.1 This test method covers the quantitative determination of barium, boron, calcium, copper, magnesium, molybdenum, phosphorus, sulfur, and zinc in unused lubricating oils and additive packages.
1.2 The precision statements are valid for dilutions in which the mass % sample in solvent is held constant in the range of 1 to 5 mass % oil.
1.3 The precision tables define the concentration ranges covered in the interlaboratory study. However, both lower and higher concentrations can be determined by this test method. The low concentration limits are dependent on the sensitivity of the ICP instrument and the dilution factor. The high concentration limits are determined by the product of the maximum concentration defined by the linear calibration curve and the sample dilution factor.
1.4 Sulfur can be determined if the instrument can operate at a wavelength of 180 nm.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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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Designation: D4951 − 09
StandardTest Method for
Determination of Additive Elements in Lubricating Oils by
1
Inductively Coupled Plasma Atomic Emission Spectrometry
This standard is issued under the fixed designation D4951; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope* D1552 Test Method for Sulfur in Petroleum Products (High-
Temperature Method)
1.1 This test method covers the quantitative determination
D4057 Practice for Manual Sampling of Petroleum and
of barium, boron, calcium, copper, magnesium, molybdenum,
Petroleum Products
phosphorus, sulfur, and zinc in unused lubricating oils and
D4307 Practice for Preparation of Liquid Blends for Use as
additive packages.
Analytical Standards
1.2 Theprecisionstatementsarevalidfordilutionsinwhich
D4628 Test Method for Analysis of Barium, Calcium,
the mass % sample in solvent is held constant in the range of
Magnesium, and Zinc in Unused Lubricating Oils by
1 to 5 mass % oil.
Atomic Absorption Spectrometry
D4927 Test Methods for Elemental Analysis of Lubricant
1.3 The precision tables define the concentration ranges
covered in the interlaboratory study. However, both lower and and Additive Components—Barium, Calcium,
Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive
higher concentrations can be determined by this test method.
The low concentration limits are dependent on the sensitivity X-Ray Fluorescence Spectroscopy
D5185 Test Method for Multielement Determination of
of the ICP instrument and the dilution factor. The high
concentration limits are determined by the product of the Used and Unused Lubricating Oils and Base Oils by
Inductively Coupled Plasma Atomic Emission Spectrom-
maximum concentration defined by the linear calibration curve
and the sample dilution factor. etry (ICP-AES)
D6299 Practice for Applying Statistical Quality Assurance
1.4 Sulfurcanbedeterminediftheinstrumentcanoperateat
and Control Charting Techniques to Evaluate Analytical
a wavelength of 180 nm.
Measurement System Performance
1.5 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
3. Summary of Test Method
standard.
3.1 A sample portion is weighed and diluted by mass with
1.6 This standard does not purport to address all of the
mixed xylenes or other solvent.An internal standard, which is
safety concerns, if any, associated with its use. It is the
required,iseitherweighedseparatelyintothetestsolutionoris
responsibility of the user of this standard to establish appro-
previously combined with the dilution solvent. Calibration
priate safety and health practices and determine the applica-
standards are prepared similarly. The solutions are introduced
bility of regulatory limitations prior to use.
to the ICP instrument by free aspiration or an optional
peristaltic pump. By comparing emission intensities of ele-
2. Referenced Documents
ments in the test specimen with emission intensities measured
2
2.1 ASTM Standards: with the calibration standards and by applying the appropriate
internal standard correction, the concentrations of elements in
the sample are calculable.
1
This test method is under the jurisdiction of ASTM Committee D02 on
4. Significance and Use
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
4.1 This test method usually requires several minutes per
Current edition approved April 15, 2009. Published May 2009. Originally
sample. This test method covers eight elements and thus
approved in 1989. Last previous edition approved in 2006 as D4951–06. DOI:
10.1520/D4951-09.
provides more elemental composition data than Test Method
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
D4628 or Test Methods D4927. In addition, this test method
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
providesmoreaccurateresultsthanTestMethodD5185,which
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. is intended for used lubricating oils and base oils.
*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
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D4951 − 09
A
TABLE 1 Elements Determined and Suggested Wavelengths
Element Wavelength, nm
Barium 233.53, 455.40, 493.41
B
Boron 182.59, 249.68
Calcium 315.88, 317.93, 364.
...
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.
An American National Standard
Designation:D4951–06 Designation:D4951–09
Standard Test Method for
Determination of Additive Elements in Lubricating Oils by
1
Inductively Coupled Plasma Atomic Emission Spectrometry
This standard is issued under the fixed designation D 4951; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope*
1.1This1.1 Thistestmethodcoversthequantitativedeterminationofbarium,boron,calcium,copper,magnesium,molybdenum,
phosphorus, sulfur, and zinc in unused lubricating oils and additive packages.
1.2 The precision statements are valid for dilutions in which the mass % sample in solvent is held constant in the range of 1
to 5 mass % oil.
1.3 The precision tables define the concentration ranges covered in the interlaboratory study. However, both lower and higher
concentrations can be determined by this test method. The low concentration limits are dependent on the sensitivity of the ICP
instrument and the dilution factor. The high concentration limits are determined by the product of the maximum concentration
defined by the linear calibration curve and the sample dilution factor.
1.4 Sulfur can be determined if the instrument can operate at a wavelength of 180 nm.
1.5The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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:
D 1552 Test Method for Sulfur in Petroleum Products (High-Temperature Method)
D 4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D 4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards
D 4628 TestMethodforAnalysisofBarium,Calcium,Magnesium,andZincinUnusedLubricatingOilsbyAtomicAbsorption
Spectrometry
D 4927 Test Methods for ElementalAnalysis of Lubricant andAdditive ComponentsBarium, Calcium, Phosphorus, Sulfur, and
Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
D 5185 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)
D 6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
3. Summary of Test Method
3.1 A sample portion is weighed and diluted by mass with mixed xylenes or other solvent. An internal standard, which is
required, is either weighed separately into the test solution or is previously combined with the dilution solvent. Calibration
standards are prepared similarly. The solutions are introduced to the ICP instrument by free aspiration or an optional peristaltic
pump. By comparing emission intensities of elements in the test specimen with emission intensities measured with the calibration
standards and by applying the appropriate internal standard correction, the concentrations of elements in the sample are calculable.
1
This test method is 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 May 1, 2006.April 15, 2009. Published May 2006.2009. Originally approved in 1989. Last previous edition approved in 20022006 as
D 4951–026.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. ForAnnualBookofASTMStandards
volume information, refer to the standard’s Document Summary page on 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
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D4951–09
4. Significance and Use
4.1 Th
...
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