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ASTM D4951-06

(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 the standard. The values given in parentheses are for information only.
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
30-Apr-2006
ICS
75.100 - Lubricants, industrial oils and related products
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.03 - Elemental Analysis
Current Stage
Ref Project

Relations

Replaces
ASTM D4951-02 - Standard Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
Effective Date
01-May-2006
Replaced By
ASTM D4951-09 - Standard Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
Effective Date
15-Apr-2009
Referred By
ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
Effective Date
01-May-2006
Referred By
ASTM D8110-17 - Standard Test Method for Elemental Analysis of Distillate Products by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
Effective Date
01-May-2006
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
01-May-2006
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
01-May-2006
Referred By
ASTM D6751-23a - Standard Specification for Biodiesel Fuel Blendstock (B100) for Middle Distillate Fuels
Effective Date
01-May-2006
Referred By
ASTM D7303-23 - Standard Test Method for Determination of Metals in Lubricating Greases by Inductively Coupled Plasma Atomic Emission Spectrometry
Effective Date
01-May-2006
Referred By
ASTM D4485-22e1 - Standard Specification for Performance of Active API Service Category Engine Oils
Effective Date
01-May-2006
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
01-May-2006
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
01-May-2006
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
01-May-2006
Referred By
ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
01-May-2006
Referred By
ASTM D6074-15(2022) - Standard Guide for Characterizing Hydrocarbon Lubricant Base Oils
Effective Date
01-May-2006

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ASTM D4951-06 - Standard Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission SpectrometryASTM D4951-06 - Standard Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
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ASTM D4951-06 - Standard Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
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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:D4951–06
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.
1. Scope* D 4307 PracticeforPreparationofLiquidBlendsforUseas
Analytical Standards
1.1 This test method covers the quantitative determination
D 4628 Test Method for Analysis of Barium, Calcium,
of barium, boron, calcium, copper, magnesium, molybdenum,
Magnesium, and Zinc in Unused Lubricating Oils by
phosphorus, sulfur, and zinc in unused lubricating oils and
Atomic Absorption Spectrometry
additive packages.
D 4927 Test Methods for Elemental Analysis of Lubricant
1.2 Theprecisionstatementsarevalidfordilutionsinwhich
and Additive Components—Barium, Calcium, Phospho-
the mass % sample in solvent is held constant in the range of
rus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray
1 to 5 mass % oil.
Fluorescence Spectroscopy
1.3 The precision tables define the concentration ranges
D 5185 Test Method for Determination of Additive Ele-
covered in the interlaboratory study. However, both lower and
ments, Wear Metals, and Contaminants in Used Lubricat-
higher concentrations can be determined by this test method.
ing Oils and Determination of Selected Elements in Base
The low concentration limits are dependent on the sensitivity
Oils by Inductively Coupled Plasma Atomic Emission
of the ICP instrument and the dilution factor. The high
Spectrometry (ICP-AES)
concentration limits are determined by the product of the
D 6299 Practice for Applying Statistical Quality Assurance
maximum concentration defined by the linear calibration curve
Techniques to Evaluate Analytical Measurement System
and the sample dilution factor.
Performance
1.4 Sulfurcanbedeterminediftheinstrumentcanoperateat
a wavelength of 180 nm.
3. Summary of Test Method
1.5 The values stated in SI units are to be regarded as the
3.1 A sample portion is weighed and diluted by mass with
standard. The values given in parentheses are for information
mixed xylenes or other solvent.An internal standard, which is
only.
required,iseitherweighedseparatelyintothetestsolutionoris
1.6 This standard does not purport to address all of the
previously combined with the dilution solvent. Calibration
safety concerns, if any, associated with its use. It is the
standards are prepared similarly. The solutions are introduced
responsibility of the user of this standard to establish appro-
to the ICP instrument by free aspiration or an optional
priate safety and health practices and determine the applica-
peristaltic pump. By comparing emission intensities of ele-
bility of regulatory limitations prior to use.
ments in the test specimen with emission intensities measured
2. Referenced Documents with the calibration standards and by applying the appropriate
2
internal standard correction, the concentrations of elements in
2.1 ASTM Standards:
the sample are calculable.
D 1552 Test Method for Sulfur in Petroleum Products
(High-Temperature Method)
4. Significance and Use
D 4057 Practice for Manual Sampling of Petroleum and
4.1 This test method usually requires several minutes per
Petroleum Products
sample. This test method covers eight elements and thus
provides more elemental composition data than Test Method
1
This test method is under the jurisdiction of ASTM Committee D02 on
D 4628 or Test Methods D 4927. In addition, this test method
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
provides more accurate results than Test Method D 5185,
D02.03 on Elemental Analysis.
which is intended for used lubricating oils and base oils.
Current edition approved May 1, 2006. Published May 2006. Originally
approved in 1989. Last previous edition approved in 2002 as D 4951–02.
4.2 Additive packages are blends of individual additives,
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
which can act as detergents, antioxidants, antiwear agents, and
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
soforth.Manyadditivescontainoneormoreelementscovered
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. by this test method.Additive package specifications are based,
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700
...

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1.3 Spectra and distribution profiles presented herein are for illustrative purposes only and are not to be construed as representing or establishing lubricant or machinery guidelines.  
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5.5 The reference elastomers, reference oil, and the physical properties involved in this test method address the specific requirements of engine oils. Although other tests exist for compatibility of elastomers with liquids, these are considered too generalized for engine oils.
SCOPE
1.1 This test method covers quantitative procedures for the evaluation of the compatibility of automotive engine oils with several reference elastomers typical of those used in the sealing materials in contact with these oils. Compatibility is evaluated by determining the changes in volume, Durometer A hardness, and tensile properties when the elastomer specimens are immersed in the oil for a specified time and temperature.  
1.2 Effective sealing action requires that the physical properties of elastomers used for any seal have a high level of resistance to the liquid or oil in which they are immersed. When such a high level of resistance exists, the elastomer is said to be compatible with the liquid or oil.
Note 1: The user of this test method should be proficient in the use of Test Methods D412 (tensile properties), D471 (effect of rubber immersion in liquids), D2240 (Durometer hardness), and D5662 (gear oil compatibility with typical oil seal elastomers), all of which are involved in the execution of the operations of this test method.  
1.3 This test method provides a preliminary or first order evaluation of oil/elastomer compatibility only. Because seals might be subjected to static or dynamic loads, or both, and they can operate over a range of conditions, a complete evaluation of the potential sealing performance of any elastomer-oil combination in any service condition usually requires tests additional to those described in this test method.  
1.4 The several reference elastomer formulations specified in this test method were chosen to be representative of those used in both heavy-duty diesel engines (detailed in Annex A1) and passenger-car spark-ignition engines (the latter are covered in Annex A2). The procedures described in this test method can, however, also be used to evaluate the compatibility of automotive engine oils with different elastomer types/formulations or different test durations and temperatures to those employed in this test method.
Note 2: In such cases, the precision and bias statement in Section 12 does not apply. In addition to agreeing acceptable limits of precision, where relevant, the user and supplier should also agree:  (1) test temperatures and immersion times to be used; (2) the formulations and typical properties of the elastomers; and (3) the sourcing and quality control of the elastomer sheets.
Note 3: The TMC may also issue In...

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ASTM
ASTM D7918-23(Test Method)
Standard Test Method for Measurement of Flow Properties and Evaluation of Wear, Contaminants, and Oxidative Properties of Lubricating Grease by Die Extrusion Method and Preparation

SIGNIFICANCE AND USE
5.1 Trending the wear, contamination, consistency, and oxidative properties of a lubricating grease is a crucial part of condition-monitoring programs. Changes in these properties or deviations from the new grease can be indicative of problems within the lubricated component, such as the mixing of incompatible thickener types, excessive wear or contaminant levels, or significant depletion of antioxidant levels. These test methods also makes it possible to develop trends that can be used to predict failures before they occur and allow for corrective action to be taken.
SCOPE
1.1 This test method covers the determination and evaluation of flow properties, wear levels, contaminants, and oxidative condition of new and in-service lubricating grease.  
1.2 This test method provides guidance on evaluating in-service grease samples, NLGI grades 00 to 3, for wear, consistency, contamination, and oxidation.  
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3.1 Exception—The exception to this will be where units of references were developed by the developers of the test equipment and necessary to report the results of the test.  
1.4 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.  
1.5 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.

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ASTM
ASTM D7922-23(Test Method)
Standard Test Method for Determination of Glycol for In-Service Engine Oils by Gas Chromatography

SIGNIFICANCE AND USE
5.1 Some glycol/antifreeze dilution of in-service engine oil is normal under typical operating conditions. However, excessive glycol dilution can lead to decreased performance, premature wear, or sudden engine failure. This test method provides a means of quantifying the level of glycol based antifreeze dilution, allowing the user to take necessary action.
SCOPE
1.1 This test method covers the determination of glycol based antifreeze for in-service engine oil by derivative headspace/gas chromatography.  
1.2 Sample is derivatized in-situ directly in a headspace sampling vial prior to vapor phase extraction and injection into a gas chromatograph.  
1.3 The chemistry of the derivatization is unique to the detection of the molecules of ethylene glycol and 1,2-propylene glycol. 1,3-propylene glycol could also be detected but is not used in any known anti-freeze at this time. Other coolant analyses are beyond the scope of this test method.  
1.4 The derivatization process does not affect glycol breakdown products such as glycolate and formate and hence the presence of these compounds in the oil will not be quantified.  
1.5 The test method concentration range is from 50 µg/g to 1000 µg/g. Lower levels are possible by method modifications. Higher levels are possible through sample dilution.  
1.6 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 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.  
1.8 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.

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