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

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 oil’s condition, see Refs (1-6)
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 v...

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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
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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: 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)
1
Spectrometry
This standard is issued under the fixed designation D7415; 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 1.4.1 For direct trend analysis, values are recorded directly
fromabsorptionspectraandreportedinunitsofabsorbanceper
1.1 This test method covers monitoring sulfate by-products
0.1 mm pathlength.
in in-service petroleum and hydrocarbon based diesel crank-
1.4.2 For differential trend analysis, values are recorded
case engine and motor oils that have a sulfur content of greater
from the differential spectra (spectrum obtained by subtraction
than 500 ppm. This test method should not be employed when
of the absorption spectrum of the reference oil from that of the
low-sulfur fuels are used for combustion.
in-service oil) and reported in units of 100*absorbance per
1.2 This test method uses Fourier Transform Infrared (FT-
0.1 mm pathlength (or equivalently absorbance units per cen-
IR) spectrometry for monitoring build-up of sulfate by-
timetre).
products in in-service petroleum and hydrocarbon based lubri-
1.4.3 In either case, maintenance action limits should be
cants as a result of normal machinery operation. Sulfate
determined through statistical analysis, history of the same or
by-products can result from the introduction of sulfur from
similar equipment, round robin tests or other methods in
combustion or from the oxidation of sulfur-containing base oil
conjunction with the correlation of sulfate by-product changes
additives. This test method is designed as a fast, simple
to equipment performance.
spectroscopic check for monitoring of sulfate by-products in
NOTE 1—It is not the intent of this test method to establish or
in-service petroleum and hydrocarbon based lubricants with
recommend normal, cautionary, warning or alert limits for any machinery.
the objective of helping diagnose the operational condition of
Suchlimitsshouldbeestablishedinconjunctionwithadviceandguidance
the machine based on measuring the level of sulfate by-
from the machinery manufacturer and maintenance group.
products in the oil.
1.5 This test method is for petroleum and hydrocarbon
1.3 Acquisition of FT-IR spectral data for measuring sulfate
based lubricants and is not applicable for ester based oils,
by-products in in-service oil and lubricant samples is described
including polyol esters or phosphate esters.
in Practice D7418. In this test method, measurement and data
1.6 The values stated in SI units are to be regarded as
interpretation parameters for sulfate by-products using both
standard. No other units of measurement are included in this
directtrendanalysisanddifferential(spectralsubtraction)trend
standard.
analysis are presented.
-1
1.6.1 Exception—The unit for wave numbers is cm .
1.4 This test method is based on trending of spectral
1.7 This standard does not purport to address all of the
changes associated with sulfate by-products of in-service
safety concerns, if any, associated with its use. It is the
petroleum and hydrocarbon based lubricants. Warnings or
responsibility of the user of this standard to establish appro-
alarm limits can be set on the basis of a fixed minimum value
priate safety and health practices and determine the applica-
for a single measurement or, alternatively, can be based on a
bility of regulatory limitations prior to use.
2
rate of change of the response measured, see Ref (1).
2. Referenced Documents
3
2.1 ASTM Standards:
1
This test method is under the jurisdiction of ASTM Committee D02 on
D445 Test Method for Kinematic Viscosity of Transparent
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.96.03 on FTIR Testing Practices and Techniques Related to
In-Service Lubricants.
3
Current edition approved July 1, 2009. Published August 2009. DOI: 10.1520/ For referenced ASTM standards, visit the ASTM website, www.astm.org, or
D7415-09. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
The boldface numbers in parentheses refer to a list of references at the end of Standards volume information, refer to the standard’s Document Summary page on
this standard. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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