5.1 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 D5185), physical property tests (Test Methods D445 and D2896), base number tests (Test Methods D974 and D4739), and other FT-IR oil analysis methods for nitration (Test Method D7624), oxidation (Test Method D7414), and additive depletion (Test Method D7412), which also assess elements of the oil’s condition, see Refs (1-6).

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 D7418. 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).2

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 Exception—The 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, 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.