ASTM D7415 - 09

    Standard Test Method for Condition Monitoring of Sulfate By-Products in In-Service Petroleum and Hydrocarbon Based Lubricants by Trend Analysis Using Fourier Transform Infrared (FT-IR) Spectrometry

    Active Standard ASTM D7415 | Developed by Subcommittee: D02.96

    Book of Standards Volume: 05.04


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    Significance and Use

    An increase in sulfate material can be an indicator of oil degradation caused by oxidation of sulfur in the oil and sulfur in fuel. It can also indicate the breakdown or oxidation of some key additives in the oil such as antiwear and extreme pressure additives as well as blow-by concerns. As oxidized sulfur from blow-by enters the lubricant, it will consume the overbase additive to generate sulfate by-products. Monitoring of sulfate by-products is therefore an important parameter in determining overall machinery health and in determining additive depletion and should be considered in conjunction with data from other tests such as atomic emission (AE) and atomic absorption (AA) spectroscopy for wear metal analysis (Test Method D 5185), physical property tests (Test Methods D 445, D 2896, and D 6304), base number tests (Test Methods D 974 and D 4739) and other FT-IR oil analysis methods for nitration (Practice E 2412), oxidation (Test Method D 7414), additive depletion (Test Method D 7412), breakdown products and external contaminants (Practice E 2412), which also assess elements of the oils condition, see Refs (1-6)

    1. Scope

    1.1 This test method covers monitoring sulfate by-products in in-service petroleum and hydrocarbon based diesel crankcase engine and motor oils that have a sulfur content of greater than 500 ppm. This test method should not be employed when low-sulfur fuels are used for combustion.

    1.2 This test method uses Fourier Transform Infrared (FT-IR) spectrometry for monitoring build-up of sulfate by-products in in-service petroleum and hydrocarbon based lubricants as a result of normal machinery operation. Sulfate by-products can result from the introduction of sulfur from combustion or from the oxidation of sulfur-containing base oil additives. This test method is designed as a fast, simple spectroscopic check for monitoring of sulfate by-products in in-service petroleum and hydrocarbon based lubricants with the objective of helping diagnose the operational condition of the machine based on measuring the level of sulfate by-products in the oil.

    1.3 Acquisition of FT-IR spectral data for measuring sulfate by-products in in-service oil and lubricant samples is described in Practice D 7418. In this test method, measurement and data interpretation parameters for sulfate by-products using both direct trend analysis and differential (spectral subtraction) trend analysis are presented.

    1.4 This test method is based on trending of spectral changes associated with sulfate by-products of in-service petroleum and hydrocarbon based lubricants. Warnings or alarm limits can be set on the basis of a fixed minimum value for a single measurement or, alternatively, can be based on a rate of change of the response measured, see Ref (1).

    1.4.1 For direct trend analysis, values are recorded directly from absorption spectra and reported in units of absorbance per 0.1 mm pathlength.

    1.4.2 For differential trend analysis, values are recorded from the differential spectra (spectrum obtained by subtraction of the absorption spectrum of the reference oil from that of the in-service oil) and reported in units of 100*absorbance per 0.1 mm pathlength (or equivalently absorbance units per centimetre).

    1.4.3 In either case, maintenance action limits should be determined through statistical analysis, history of the same or similar equipment, round robin tests or other methods in conjunction with the correlation of sulfate by-product changes to equipment performance.

    Note 1—It is not the intent of this test method to establish or recommend normal, cautionary, warning or alert limits for any machinery. Such limits should be established in conjunction with advice and guidance from the machinery manufacturer and maintenance group.

    1.5 This test method is for petroleum and hydrocarbon based lubricants and is not applicable for ester based oils, including polyol esters or phosphate esters.

    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 ExceptionThe unit for wave numbers is cm-1.

    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

    D445 Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)

    D974 Test Method for Acid and Base Number by Color-Indicator Titration

    D2896 Test Method for Base Number of Petroleum Products by Potentiometric Perchloric Acid Titration

    D4739 Test Method for Base Number Determination by Potentiometric Hydrochloric Acid Titration

    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)

    D6304 Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fischer Titration

    D7412 Test Method for Condition Monitoring of Phosphate Antiwear Additives in In-Service Petroleum and Hydrocarbon Based Lubricants by Trend Analysis Using Fourier Transform Infrared (FT-IR) Spectrometry

    D7414 Test Method for Condition Monitoring of Oxidation in In-Service Petroleum and Hydrocarbon Based Lubricants by Trend Analysis Using Fourier Transform Infrared (FT-IR) Spectrometry

    D7418 Practice for Set-Up and Operation of Fourier Transform Infrared (FT-IR) Spectrometers for In-Service Oil Condition Monitoring

    E131 Terminology Relating to Molecular Spectroscopy

    E2412 Practice for Condition Monitoring of In-Service Lubricants by Trend Analysis Using Fourier Transform Infrared (FT-IR) Spectrometry


    ICS Code

    ICS Number Code 75.100 (Lubricants, industrial oils and related products)

    UNSPSC Code

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


    Referencing This Standard

    DOI: 10.1520/D7415-09

    ASTM International is a member of CrossRef.

    Citation Format

    ASTM D7415-09, Standard Test Method for Condition Monitoring of Sulfate By-Products in In-Service Petroleum and Hydrocarbon Based Lubricants by Trend Analysis Using Fourier Transform Infrared (FT-IR) Spectrometry, ASTM International, West Conshohocken, PA, 2009, www.astm.org

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