ASTM D4951-02

Standard Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry

SCOPE
1.1 This test method covers the quantitative determination of barium, boron, calcium, copper, magnesium, 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 the 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.

General Information

• Status: Historical
• Publication Date: 09-Jan-2002
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Replaces: ASTM D4951-00 - Standard Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
• Effective Date: 10-Jan-2002
• Replaced By: ASTM D4951-06 - Standard Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
• Effective Date: 01-May-2006
• Referred By: ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 10-Jan-2002
• Referred By: ASTM D8110-17 - Standard Test Method for Elemental Analysis of Distillate Products by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
• Effective Date: 10-Jan-2002
• Referred By: ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
• Effective Date: 10-Jan-2002
• Referred By: ASTM D6074-15(2022) - Standard Guide for Characterizing Hydrocarbon Lubricant Base Oils
• Effective Date: 10-Jan-2002
• Referred By: ASTM D7303-23 - Standard Test Method for Determination of Metals in Lubricating Greases by Inductively Coupled Plasma Atomic Emission Spectrometry
• Effective Date: 10-Jan-2002
• Referred By: ASTM D7876-13(2018) - Standard Practice for Practice for Sample Decomposition Using Microwave Heating (With or Without Prior Ashing) for Atomic Spectroscopic Elemental Determination in Petroleum Products and Lubricants
• Effective Date: 10-Jan-2002
• Referred By: ASTM D5185-18 - Standard Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 10-Jan-2002
• Referred By: ASTM D6443-14(2019)e1 - Standard Test Method for Determination of Calcium, Chlorine, Copper, Magnesium, Phosphorus, Sulfur, and Zinc in Unused Lubricating Oils and Additives by Wavelength Dispersive X-ray Fluorescence Spectrometry (Mathematical Correction Procedure)
• Effective Date: 10-Jan-2002
• Referred By: ASTM D6751-23a - Standard Specification for Biodiesel Fuel Blendstock (B100) for Middle Distillate Fuels
• Effective Date: 10-Jan-2002
• Referred By: ASTM D7260-20 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 10-Jan-2002
• Referred By: ASTM D4485-22e1 - Standard Specification for Performance of Active API Service Category Engine Oils
• Effective Date: 10-Jan-2002
• Referred By: ASTM D7040-04(2020) - Standard Test Method for Determination of Low Levels of Phosphorus in ILSAC GF 4 and Similar Grade Engine Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
• Effective Date: 10-Jan-2002

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
An American National Standard
Designation:D4951–02
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 (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
3
1. Scope* Analytical Standards
D 4628 Test Method for Analysis of Barium, Calcium,
1.1 This test method covers the quantitative determination
Magnesium, and Zinc in Unused Lubricating Oils by
of barium, boron, calcium, copper, magnesium, phosphorus,
3
Atomic Absorption Spectrometry
sulfur, and zinc in unused lubricating oils and additive pack-
D 4927 Test Methods for Elemental Analysis of Lubricant
ages.
and Additive Components—Barium, Calcium, Phospho-
1.2 The precision statements are valid for dilutions in which
rus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray
the mass % sample in solvent is held constant in the range of
3
Fluorescence Spectroscopy
1 to 5 mass % oil.
D 5185 Test Method for Determination of Additive Ele-
1.3 The precision tables define the concentration ranges
ments, Wear Metals, and Contaminants in Used Lubricat-
covered in the interlaboratory study. However, both lower and
ing Oils and Determination of Selected Elements in Base
higher concentrations can be determined by this test method.
Oils by Inductively Coupled Plasma Atomic Emission
The low concentration limits are dependent on the sensitivity
3
Spectrometry (ICP-AES)
of the ICP instrument and the dilution factor. The high
D 6299 Practice for Applying Statistical Quality Assurance
concentration limits are determined by the product of the
Techniques to Evaluate Analytical Measurement System
maximum concentration defined by the linear calibration curve
4
Performance
and the sample dilution factor.
1.4 Sulfurcanbedeterminediftheinstrumentcanoperateat
3. Summary of Test Method
a wavelength of 180 nm.
3.1 A sample portion is weighed and diluted by mass with
1.5 The values stated in SI units are to be regarded as the
mixed xylenes or other solvent.An internal standard, which is
standard. The values given in parentheses are for information
required,iseitherweighedseparatelyintothetestsolutionoris
only.
previously combined with the dilution solvent. Calibration
1.6 This standard does not purport to address all of the
standards are prepared similarly. The solutions are introduced
safety concerns, if any, associated with its use. It is the
to the ICP instrument by free aspiration or an optional
responsibility of the user of this standard to establish appro-
peristaltic pump. By comparing emission intensities of ele-
priate safety and health practices and determine the applica-
ments in the test specimen with emission intensities measured
bility of regulatory limitations prior to use.
with the calibration standards and by applying the appropriate
2. Referenced Documents internal standard correction, the concentrations of elements in
the sample are calculable.
2.1 ASTM Standards:
D 1552 Test Method for Sulfur in Petroleum Products
4. Significance and Use
2
(High-Temperature Method)
4.1 This test method usually requires several minutes per
D 4057 Practice for Manual Sampling of Petroleum and
3 sample. This test method covers eight elements and thus
Petroleum Products
provides more elemental composition data than Test Method
D 4307 PracticeforPreparationofLiquidBlendsforUseas
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.
1
This test method is under the jurisdiction of ASTM Committee D02 on
4.2 Additive packages are blends of individual additives,
PetroleumProductsandLubricants andisthedirectresponsibilityofSubcommittee
which can act as detergents, antioxidants, antiwear agents, and
D02.03 on Elemental Analysis.
Current edition approved Jan. 10, 2002. Published March 2002. Originally
published as D 4951 – 89. Last previous edition D 4951 – 00.
2
Annual Book of ASTM Standards, Vol 05.01.
3 4
Annual Book of ASTM Standards, Vol 05.02. Annual Book of ASTM Standards, Vol 05.03.
*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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D4951–02
A
TABLE 1 Elements Determined and Suggested Wavelengths
Element Wavelength, nm
Barium 233.53, 455.40, 493.41
B
Bor
...