ASTM D6443 - 04(2010)

    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)

    Active Standard ASTM D6443 | Developed by Subcommittee: D02.03

    Book of Standards Volume: 05.03


      Format Pages Price  
    PDF 7 $43.00   ADD TO CART
    Hardcopy (shipping and handling) 7 $43.00   ADD TO CART


    Significance and Use

    Lubricating oils can be formulated with additives, which can act as detergents, anti-oxidants, anti-wear agents, and so forth. Some additives can contain one or more of calcium, copper, magnesium, phosphorus, sulfur, and zinc. This test method can be used to determine if the oils, additives, and additive packages meet specification with respect to content of these elements.

    This test method can also be used to determine if lubricating oils, additives, and additive packages meet specification with respect to chlorine concentration. In this context, specification can refer to contamination.

    This test method is not intended for use on samples that contain some component that significantly interferes with the analysis of the elements specified in the scope.

    This test method can complement other test methods for lube oils and additives, including Test Methods D4628, D4927, D4951, and D5185.

    1. Scope

    1.1 This test method covers the determination of calcium, chlorine, copper, magnesium, phosphorus, sulfur, and zinc in unused lubricating oils, additives, and additive packages by wavelength dispersive X-ray fluorescence spectrometry. Matrix effects are handled with mathematical corrections.

    1.2 For each element, the upper limit of the concentration range covered by this test method is defined by the highest concentration listed in Table 1. Samples containing higher concentrations can be analyzed following dilution.

    1.3 For each element, the lower limit of the concentration range covered by this test method can be estimated by the limit of detection (LOD) (see also 40 CFR 136 Appendix B) or limit of quantification (LOQ), both of which can be estimated from Sr, the repeatability standard deviation. LOD and LOQ values, determined from results obtained in the interlaboratory study on precision, are listed in Table 2.

    1.3.1 LOD and LOQ are not intrinsic constants of this test method. LOD and LOQ depend upon the precision attainable by a laboratory when using this test method.

    1.4 This test method uses regression software to determine calibration parameters, which can include influence coefficients (that is, interelement effect coefficients) (Guide E1361), herein referenced as alphas. Alphas can also be determined from theory using relevant software.

    1.5 Setup of this test method is intended for persons trained in the practice of X-ray spectrometry. Following setup, this test method can be used routinely.

    1.6 The values stated in either SI units or angstrom units are to be regarded separately as 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 and health practices and determine the applicability of regulatory limitations prior to use.


    2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

    ASTM Standards

    D1552 Test Method for Sulfur in Petroleum Products (High-Temperature Method)

    D4057 Practice for Manual Sampling of Petroleum and Petroleum Products

    D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products

    D4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards

    D4628 Test Method for Analysis of Barium, Calcium, Magnesium, and Zinc in Unused Lubricating Oils by Atomic Absorption Spectrometry

    D4927 Test Methods for Elemental Analysis of Lubricant and Additive Components--Barium, Calcium, Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy

    D4951 Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry

    D5185 Test Method for Determination of Additive Elements, Wear Metals, and Contaminants in Used Lubricating Oils and Determination of Selected Elements in Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

    D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance

    E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications

    E1361 Guide for Correction of Interelement Effects in X-Ray Spectrometric Analysis

    Government Standard

    40CFR,136AppendixB, Definition and Procedure for the Determination of the Method Detection Limit--Revision 1.11, pp. 265-267


    UNSPSC Code

    UNSPSC Code 15120000(Lubricants and oils and greases and anticorrosives)


    Referencing This Standard

    DOI: 10.1520/D6443-04R10

    ASTM International is a member of CrossRef.

    Citation Format

    ASTM D6443-04(2010), 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), ASTM International, West Conshohocken, PA, 2010, www.astm.org

    Back to Top