Standard 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

SIGNIFICANCE AND USE
A large number of compounds, such as aldehydes, ketones, esters, and carboxylic acids, are produced when oils react with atmospheric oxygen. Oxidation is measured using a common FT-IR spectral feature between 1800 and 1670 cm-1 caused by the absorption of the carbonyl group present in most oxidation compounds. These oxidation products may lead to increased viscosity (causing oil thickening problems), acidity (causing acidic corrosion), and formation of sludge and varnish (leading to filter plugging, fouling of critical oil clearances and valve friction). Monitoring of oxidation products is therefore an important parameter in determining overall machinery health 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 and D 6304), base reserve (Test Method D 2896 and D 4739), acid number tests (Test Methods D 664 and D 974) and other FT-IR oil analysis methods for nitration (Practice E 2412), sulfate by-products (Test Method D 7415), 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 oxidation in in-service petroleum and hydrocarbon based lubricants such as in diesel crankcase, motor, hydraulic, gear and compressor oils, as well as other types of lubricants that are prone to oxidation.
1.2 This test method uses Fourier Transform Infrared (FT-IR) spectrometry for monitoring build-up of oxidation products in in-service petroleum and hydrocarbon based lubricants as a result of normal machinery operation. Petroleum and hydrocarbon based lubricants react with oxygen in the air to form a number of different chemical species, including aldehydes, ketones, esters, and carboxylic acids. This test method is designed as a fast, simple spectroscopic check for monitoring of oxidation 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 oxidation in the oil.
1.3 Acquisition of FT-IR spectral data for measuring oxidation in in-service oil and lubricant samples is described in Practice D 7418. In this test method, measurement and data interpretation parameters for oxidation 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 oxidation 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 oxidation 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...

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ASTM D7414-09 - Standard 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
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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: D7414 − 09
Standard Test Method for
Condition Monitoring of Oxidation in In-Service Petroleum
and Hydrocarbon Based Lubricants by Trend Analysis
1
Using Fourier Transform Infrared (FT-IR) Spectrometry
This standard is issued under the fixed designation D7414; 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 1.4.2 For differential trend analysis, values are recorded
from the differential spectra (spectrum obtained by subtraction
1.1 This test method covers monitoring oxidation in in-
of the absorption spectrum of the reference oil from that of the
service petroleum and hydrocarbon based lubricants such as in
in-service oil) and reported in units of 100*absorbance per 0.1
diesel crankcase, motor, hydraulic, gear and compressor oils,
mm pathlength (or equivalently absorbance units per centime-
as well as other types of lubricants that are prone to oxidation.
tre).
1.2 This test method uses Fourier Transform Infrared (FT-
1.4.3 In either case, maintenance action limits should be
IR)spectrometryformonitoringbuild-upofoxidationproducts
determined through statistical analysis, history of the same or
in in-service petroleum and hydrocarbon based lubricants as a
similar equipment, round robin tests or other methods in
result of normal machinery operation. Petroleum and hydro-
conjunction with the correlation of oxidation changes to
carbon based lubricants react with oxygen in the air to form a
equipment performance.
number of different chemical species, including aldehydes,
NOTE 1—It is not the intent of this test method to establish or
ketones, esters, and carboxylic acids. This test method is
recommend normal, cautionary, warning or alert limits for any machinery.
designed as a fast, simple spectroscopic check for monitoring
Suchlimitsshouldbeestablishedinconjunctionwithadviceandguidance
of oxidation in in-service petroleum and hydrocarbon based
from the machinery manufacturer and maintenance group.
lubricants with the objective of helping diagnose the opera-
1.5 This test method is for petroleum and hydrocarbon
tionalconditionofthemachinebasedonmeasuringthelevelof
based lubricants and is not applicable for ester based oils,
oxidation in the oil.
including polyol esters or phosphate esters.
1.3 Acquisition of FT-IR spectral data for measuring oxida-
1.6 The values stated in SI units are to be regarded as
tion in in-service oil and lubricant samples is described in
standard. No other units of measurement are included in this
Practice D7418. In this test method, measurement and data
standard.
interpretation parameters for oxidation using both direct trend
-1
1.6.1 Exception—The unit for wave numbers is cm .
analysis and differential (spectral subtraction) trend analysis
1.7 This standard does not purport to address all of the
are presented.
safety concerns, if any, associated with its use. It is the
1.4 This test method is based on trending of spectral
responsibility of the user of this standard to establish appro-
changes associated with oxidation of in-service petroleum and
priate safety and health practices and determine the applica-
hydrocarbon based lubricants. Warnings or alarm limits can be
bility of regulatory limitations prior to use.
set on the basis of a fixed minimum value for a single
measurement or, alternatively, can be based on a rate of change
2. Referenced Documents
2
of the response measured, see Ref (1).
3
2.1 ASTM Standards:
1.4.1 For direct trend analysis, values are recorded directly
D445 Test Method for Kinematic Viscosity of Transparent
fromabsorptionspectraandreportedinunitsofabsorbanceper
and Opaque Liquids (and Calculation of Dynamic Viscos-
0.1 mm pathlength.
ity)
D664 Test Method for Acid Number of Petroleum Products
1
This test method is under the jurisdiction of ASTM Committee D02 on by Potentiometric Titration
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
D7414-09. 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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