ASTM D7751-16(2021)

Standard Test Method for Determination of Additive Elements in Lubricating Oils by EDXRF Analysis

SIGNIFICANCE AND USE
5.1 Lubricating oils are formulated with organo-metallic additives, which act, for example, as detergents, antioxidants, antifoaming, or antiwear agents, or a combination thereof. Some of these additives contain one or more of the following elements: magnesium, phosphorus, sulfur, chlorine, calcium, zinc, and molybdenum. This test method provides a means of determining the concentrations of these elements, which in turn provides an indication of the additive content of these oils.  
5.2 Several additive elements and their compounds are added to the lubricating oils to give beneficial performance (Table 2).  
5.3 Additive packages are the concentrates that are used to blend lubricating oils.  
5.4 This test method is primarily intended to be used for the monitoring of additive elements in lubricating oils.  
5.5 If this test method is applied to lubricating oils with matrices significantly different from the calibration materials specified in this test method, the cautions and recommendations in Section 6 should be observed when interpreting the results.
SCOPE
1.1 This test method covers the quantitative determination of additive elements in unused lubricating oils and additive packages, as shown in Table 1.    
1.2 Additive packages require dilution with a contamination free diluent (base oil) prior to analysis. The dilution factor has to be calculated from the expected concentrations to bring the concentrations for all elements into the ranges listed in Table 1.  
1.3 Some lubrication oils will contain higher concentrations than the maximum concentrations listed in Table 1. These samples require dilution with a contamination free diluent (base oil) prior to analysis. The dilution factor has to be calculated from the expected concentrations to bring the concentrations for all elements into the ranges listed in Table 1.  
1.4 This test method is limited to the use of energy dispersive X-ray fluorescence (EDXRF) spectrometers employing an X-ray tube for excitation in conjunction with the ability to separate the signals of adjacent elements by using a high resolution semiconductor detector.  
1.5 This test method uses inter-element correction factors calculated from a fundamental parameters (FP) approach or from another matrix correction method.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6.1 The preferred concentration units are mg/kg or mass %.  
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.

General Information

• Status: Published
• Publication Date: 30-Jun-2021
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

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: D7751 − 16 (Reapproved 2021)
Standard Test Method for
Determination of Additive Elements in Lubricating Oils by
1
EDXRF Analysis
This standard is issued under the fixed designation D7751; 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.
1. Scope ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.1 This test method covers the quantitative determination
mendations issued by the World Trade Organization Technical
of additive elements in unused lubricating oils and additive
Barriers to Trade (TBT) Committee.
packages, as shown in Table 1.
1.2 Additivepackagesrequiredilutionwithacontamination
2. Referenced Documents
free diluent (base oil) prior to analysis. The dilution factor has
2
2.1 ASTM Standards:
to be calculated from the expected concentrations to bring the
D4057 Practice for Manual Sampling of Petroleum and
concentrationsforallelementsintotherangeslistedinTable1.
Petroleum Products
1.3 Some lubrication oils will contain higher concentrations
D4177 Practice for Automatic Sampling of Petroleum and
than the maximum concentrations listed in Table 1. These
Petroleum Products
samples require dilution with a contamination free diluent
D6299 Practice for Applying Statistical Quality Assurance
(base oil) prior to analysis. The dilution factor has to be
and Control Charting Techniques to Evaluate Analytical
calculated from the expected concentrations to bring the
Measurement System Performance
concentrationsforallelementsintotherangeslistedinTable1.
D6300 Practice for Determination of Precision and Bias
Data for Use in Test Methods for Petroleum Products,
1.4 This test method is limited to the use of energy
Liquid Fuels, and Lubricants
dispersive X-ray fluorescence (EDXRF) spectrometers em-
D6792 Practice for Quality Management Systems in Petro-
ploying an X-ray tube for excitation in conjunction with the
leum Products, Liquid Fuels, and Lubricants Testing
ability to separate the signals of adjacent elements by using a
Laboratories
high resolution semiconductor detector.
D7343 Practice for Optimization, Sample Handling,
1.5 This test method uses inter-element correction factors
Calibration, and Validation of X-ray Fluorescence Spec-
calculated from a fundamental parameters (FP) approach or
trometry Methods for Elemental Analysis of Petroleum
from another matrix correction method.
Products and Lubricants
1.6 The values stated in SI units are to be regarded as
E1621 Guide for ElementalAnalysis by Wavelength Disper-
standard. No other units of measurement are included in this
sive X-Ray Fluorescence Spectrometry
standard. 3
2.2 ISO Standards:
1.6.1 The preferred concentration units are mg/kg or mass
ISO 4259 Determination and application of precision data in
%.
relation to methods of test
1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 3. Terminology
responsibility of the user of this standard to establish appro-
3.1 Definitions:
priate safety, health, and environmental practices and deter-
3.1.1 energy dispersive X-ray spectrometry, n—XRF spec-
mine the applicability of regulatory limitations prior to use.
trometry applying energy dispersive selection of radiation.
1.8 This international standard was developed in accor-
3.2 Abbreviations:
dance with internationally recognized principles on standard-
1 2
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Subcommittee D02.03 on Elemental Analysis. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved July 1, 2021. Published August 2021. Originally the ASTM website.
3
approved in 2011. Last previous edition approved in 2016 as D7751 – 16. Available from International Organization for Standardization (ISO), 1, ch. de
DOI:10.1520/D7751-16R21. la Voie-Creuse, CP 56, CH-1211 Geneva 20, Switzerland, http://www.iso.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7751 − 16 (2021)
TABLE 1 Elements and Range of Applicability
calculation of concen
...