ASTM D7751-16

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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 14-Dec-2016
• 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)

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
Designation: D7751 − 16
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* 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This test method covers the quantitative determination
D4057 Practice for Manual Sampling of Petroleum and
of additive elements in unused lubricating oils and additive
Petroleum Products
packages, as shown in Table 1.
D4177 Practice for Automatic Sampling of Petroleum and
1.2 Additivepackagesrequiredilutionwithacontamination
Petroleum Products
free diluent (base oil) prior to analysis. The dilution factor has
D6299 Practice for Applying Statistical Quality Assurance
to be calculated from the expected concentrations to bring the
and Control Charting Techniques to Evaluate Analytical
concentrationsforallelementsintotherangeslistedinTable1.
Measurement System Performance
D6300 Practice for Determination of Precision and Bias
1.3 Some lubrication oils will contain higher concentrations
Data for Use in Test Methods for Petroleum Products and
than the maximum concentrations listed in Table 1. These
Lubricants
samples require dilution with a contamination free diluent
D6792 Practice for Quality System in Petroleum Products
(base oil) prior to analysis. The dilution factor has to be
and Lubricants Testing Laboratories
calculated from the expected concentrations to bring the
D7343 Practice for Optimization, Sample Handling,
concentrationsforallelementsintotherangeslistedinTable1.
Calibration, and Validation of X-ray Fluorescence Spec-
1.4 This test method is limited to the use of energy
trometry Methods for Elemental Analysis of Petroleum
dispersive X-ray fluorescence (EDXRF) spectrometers em-
Products and Lubricants
ploying an X-ray tube for excitation in conjunction with the
E1621 Guide for ElementalAnalysis by Wavelength Disper-
ability to separate the signals of adjacent elements by using a
sive X-Ray Fluorescence Spectrometry
3
high resolution semiconductor detector.
2.2 ISO Standards:
ISO 4259 Determination and application of precision data in
1.5 This test method uses inter-element correction factors
relation to methods of test
calculated from a fundamental parameters (FP) approach or
from another matrix correction method.
3. Terminology
1.6 The values stated in SI units are to be regarded as
3.1 Definitions:
standard. No other units of measurement are included in this
3.1.1 energy dispersive X-ray spectrometry, n—XRF spec-
standard.
trometry applying energy dispersive selection of radiation.
1.6.1 The preferred concentration units are mg/kg or mass
3.2 Abbreviations:
%.
3.2.1 EDXRF—Energy Dispersive X-ray Fluorescence
1.7 This standard does not purport to address all of the Spectrometry.
safety concerns, if any, associated with its use. It is the
3.2.2 FP—Fundamental Parameters.
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4.1 A specimen is placed in the X-ray beam, and the
appropriate regions of its spectrum are measured to give the
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 Dec. 15, 2016. Published February 2017. Originally the ASTM website.
ɛ1
3
approved in 2011. Last previous edition approved in 2014 as D7751 – 14 . Available from International Organization for Standardization (ISO), 1, ch. de
DOI:10.1520/D7751-16. la Voie-Creuse, CP 56, CH-1211 Geneva 20, Switzerland, http://www.iso.org.
*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 ----------------------
D7751 − 16
TABLE 1 Elements and Range of Applicability
spectrometer. (Warning—Exposure to excessive quantities of
Element PLOQ in mass % Max Concentration in X-radiation is injurious to health. The operator needs to take
mass %
appropriate actions to avoid exposing any part of their body,
Magnesium 0.018 0.10
not only to primary X-rays, bu
...

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.
´1
Designation: D7751 − 14 D7751 − 16
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
ε NOTE—Table 4 was corrected editorially in November 2015.
1. 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. The pooled limit of quantitation of this test method as obtained by statistical analysis of interlaboratory test
results is 0.02 % for magnesium, 0.003 % for phosphorus, 0.002 % for sulfur, 0.001 % for chlorine, 0.003 % for calcium, 0.001 %
for zinc, and 0.002 % for molybdenum.
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
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 Dec. 1, 2014Dec. 15, 2016. Published January 2015February 2017. Originally approved in 2011. Last previous edition approved in 20122014
ɛ1
as D7751 – 12.14 DOI:10.1520/D7751-14E01. DOI:10.1520/D7751-16.
*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 ----------------------
D7751 − 16
TABLE 1 Elements and Range of Applicability
Element Concentration
Range in mass %
Magnesium 0.02 to 0.4
Phosphorous 0.003 to 0.25
Sulfur 0.002 to 1.5
Chlorine 0.001 to 0.4
Calcium 0.003 to 1.0
Zinc 0.001 to 0.25
Molybdenum 0.002 to 0.05
TABLE 1 Elements and Range of Applicability
Element PLOQ in mass % Max Concentration in
mass %
Magnesium 0.018 0.10
Phosphorous 0.024 0.125
Sulfur 0.008 1.94
Chlorine 0.0007 0.05
Calcium 0.002 0.44
Zinc 0.040 0.143
Molybdenum 0.004 0.047
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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lubricants
D6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories
D7343 Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods
for Elemental Analysis of Petroleum Products and Lubricants
E1621 Guide for Elemental Analysis by Wavelength Dispersive X-Ray Fluorescence Spectrometry
3
2.2 ISO Standards:
ISO 4259 Determination and application
...