ASTM D4951-14
(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
4.1 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 D4628 or Test Methods D4927. In addition, this test method provides more accurate results than Test Method D5185, which is intended for used lubricating oils and base oils.
4.2 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.
4.3 Several additive elements and their compounds are added to the lubricating oils to give beneficial performance (Table 1).
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.
General Information
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Designation: D4951 − 14
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 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 The precision statements are valid for dilutions in which
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 Oct. 1, 2014. Published October 2014. Originally
sample. This test method covers eight elements and thus
approved in 1989. Last previous edition approved in 2009 as D4951 – 09. DOI:
10.1520/D4951-14.
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
1
---------------------- Page: 1 ----------------------
D4951 − 14
TABLE 1 Lubricants and Additive Materials
Element Compound Performance
Barium Sulfonates, phenates Detergent inhibitors, corrosion inhibitors, dete
...
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: D4951 − 09 D4951 − 14
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 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*
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1552 Test Method for Sulfur in Petroleum Products (High-Temperature Method)
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards
D4628 Test Method for Analysis of Barium, Calcium, Magnesium, and Zinc in Unused Lubricating Oils by Atomic Absorption
Spectrometry
D4927 Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur,
and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
D5185 Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils by Inductively
Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
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 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
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved April 15, 2009Oct. 1, 2014. Published May 2009October 2014. Originally approved in 1989. Last previous edition approved in 20062009 as
D4951D4951 – 09.–06. DOI: 10.1520/D4951-09.10.1520/D4951-14.
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.
*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 ----------------------
D4951 − 14
TABLE 1 Lubricants and Additive Materials
Element Compound Performance
Barium Sulfonates, phenates Detergent inhibitors, corrosion inhibitors, detergents, rust inhibitors, and
ATF
Boron Inorganic borates and borate esters, borated Anti-wear agents, anti-oxidant, deodorant, cutting oils, and brake fluids
dispersants and detergents
Calcium Sulfonates, phenates Detergent inhibitors and dispersants
Copper Copper dit
...
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