ASTM D4951-14(2019)
(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 % by mass of 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.7 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
Relations
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: D4951 − 14 (Reapproved 2019)
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 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This test method covers the quantitative determination
of barium, boron, calcium, copper, magnesium, molybdenum, D1552 Test Method for Sulfur in Petroleum Products by
High Temperature Combustion and Infrared (IR) Detec-
phosphorus, sulfur, and zinc in unused lubricating oils and
additive packages. tion or Thermal Conductivity Detection (TCD)
D4057 Practice for Manual Sampling of Petroleum and
1.2 The precision statements are valid for dilutions in which
Petroleum Products
the mass % sample in solvent is held constant in the range of
D4307 Practice for Preparation of Liquid Blends for Use as
1 % to 5 % by mass of oil.
Analytical Standards
1.3 The precision tables define the concentration ranges
D4628 Test Method for Analysis of Barium, Calcium,
covered in the interlaboratory study. However, both lower and
Magnesium, and Zinc in Unused Lubricating Oils by
higher concentrations can be determined by this test method.
Atomic Absorption Spectrometry
The low concentration limits are dependent on the sensitivity
D4927 Test Methods for Elemental Analysis of Lubricant
of the ICP instrument and the dilution factor. The high
and Additive Components—Barium, Calcium,
concentration limits are determined by the product of the
Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive
maximum concentration defined by the linear calibration curve
X-Ray Fluorescence Spectroscopy
and the sample dilution factor.
D5185 Test Method for Multielement Determination of
Used and Unused Lubricating Oils and Base Oils by
1.4 Sulfurcanbedeterminediftheinstrumentcanoperateat
Inductively Coupled Plasma Atomic Emission Spectrom-
a wavelength of 180 nm.
etry (ICP-AES)
1.5 The values stated in SI units are to be regarded as
D6299 Practice for Applying Statistical Quality Assurance
standard. No other units of measurement are included in this
and Control Charting Techniques to Evaluate Analytical
standard.
Measurement System Performance
1.6 This standard does not purport to address all of the
3. Summary of Test Method
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.1 A sample portion is weighed and diluted by mass with
priate safety, health, and environmental practices and deter-
mixed xylenes or other solvent.An internal standard, which is
mine the applicability of regulatory limitations prior to use.
required,iseitherweighedseparatelyintothetestsolutionoris
1.7 This international standard was developed in accor-
previously combined with the dilution solvent. Calibration
dance with internationally recognized principles on standard-
standards are prepared similarly. The solutions are introduced
ization established in the Decision on Principles for the
to the ICP instrument by free aspiration or an optional
Development of International Standards, Guides and Recom-
peristaltic pump. By comparing emission intensities of ele-
mendations issued by the World Trade Organization Technical
ments in the test specimen with emission intensities measured
Barriers to Trade (TBT) Committee.
with the calibration standards and by applying the appropriate
internal standard correction, the concentrations of elements in
the sample are calculable.
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This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
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Subcommittee D02.03 on Elemental Analysis. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 1, 2019. Published December 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1989. Last previous edition approved in 2014 as D4951 – 14. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D4951-14R19. the ASTM website.
*A Summary of Changes section appears at the end of this standard
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