ASTM D7412-21
(Test Method)Standard 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
Standard 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
SIGNIFICANCE AND USE
5.1 Antiwear additives are commonly used in petroleum and hydrocarbon based lubricants to prevent machinery wear by forming a chemical barrier activated by frictional heat. Antiwear additives that are phosphate based can be measured by FT-IR spectroscopy using the phosphate absorption band. Initially, phosphate antiwear additives will decompose and form a protective film by binding to metal surfaces and through oxidative mechanisms, and so a decrease in the level of phosphate antiwear additive relative to that in the new oil is expected during normal machinery operation. Subsequently, significant depletion of phosphate antiwear additives due to oxidation or hydrolysis can occur when the lubricant is subjected to high temperatures and high levels of moisture. This usually occurs prior to the point where the oxidation of the lubricant begins to accelerate, making trending of phosphate antiwear additives a useful indicator of the lubricant’s remaining in-service life. Monitoring of phosphate antiwear additive depletion 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 D5185), physical property tests (Test Methods D445 and D2896) and other FT-IR oil analysis methods for oxidation (Test Method D7414), sulfate by-products (Test Method D7415), and nitration (Test Method D7624), which also assess elements of the oil’s condition, see Refs (1-6).
SCOPE
1.1 This test method covers monitoring phosphate antiwear additives in in-service petroleum and hydrocarbon based lubricants such as various types of engine oils, hydraulic oils, and other lubricants that are formulated for protection against wear. Typical phosphate antiwear additives include zinc dialkyldithiophosphates, trialkyl phosphates, and triaryl phosphates.
1.2 This test method uses Fourier Transform Infrared (FT-IR) spectrometry for monitoring of phosphate antiwear additive depletion in in-service petroleum and hydrocarbon based lubricants as a result of normal machinery operation. Monitoring the depletion of phosphate antiwear additives in in-service lubricants can indicate unusual wear or severe operating conditions of the machine. This test method is designed as a fast, simple spectroscopic check for monitoring of phosphate antiwear additives 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 phosphate antiwear additives in the oil.
1.3 Acquisition of FT-IR spectral data for measuring phosphate antiwear additives in in-service oil and lubricant samples is described in Practice D7418. In this test method, measurement and data interpretation parameters for phosphate antiwear additives 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 phosphate antiwear additives in 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 centimeter).
1.4.3 In either case, maintenance action limits should be determined through statistical analysis, history of the same or simila...
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Designation: D7412 − 21
Standard 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)
1
Spectrometry
This standard is issued under the fixed designation D7412; 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* value for a single measurement or, alternatively, can be based
2
on a rate of change of the response measured, see Ref (1).
1.1 This test method covers monitoring phosphate antiwear
1.4.1 For direct trend analysis, values are recorded directly
additives in in-service petroleum and hydrocarbon based lubri-
fromabsorptionspectraandreportedinunitsofabsorbanceper
cants such as various types of engine oils, hydraulic oils, and
0.1 mm pathlength.
otherlubricantsthatareformulatedforprotectionagainstwear.
1.4.2 For differential trend analysis, values are recorded
Typical phosphate antiwear additives include zinc dialkyl-
from the differential spectra (spectrum obtained by subtraction
dithiophosphates, trialkyl phosphates, and triaryl phosphates.
of the absorption spectrum of the reference oil from that of the
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 of phosphate antiwear addi-
timeter).
tive depletion in in-service petroleum and hydrocarbon based
1.4.3 In either case, maintenance action limits should be
lubricants as a result of normal machinery operation. Monitor-
determined through statistical analysis, history of the same or
ing the depletion of phosphate antiwear additives in in-service
similar equipment, round robin tests or other methods in
lubricants can indicate unusual wear or severe operating
conjunction with the correlation of changes in the level of
conditions of the machine. This test method is designed as a
phosphate antiwear additives to equipment performance.
fast, simple spectroscopic check for monitoring of phosphate
NOTE 1—It is not the intent of this test method to establish or
antiwear additives in in-service petroleum and hydrocarbon
recommendnormal,cautionary,warning,oralertlimitsforanymachinery.
based lubricants with the objective of helping diagnose the
Suchlimitsshouldbeestablishedinconjunctionwithadviceandguidance
operational condition of the machine based on measuring the
from the machinery manufacturer and maintenance group.
level of phosphate antiwear additives in the oil.
1.5 This test method is for petroleum and hydrocarbon
1.3 Acquisition of FT-IR spectral data for measuring phos- based lubricants and is not applicable for ester based oils,
including polyol esters or phosphate esters.
phate antiwear additives in in-service oil and lubricant samples
is described in Practice D7418. In this test method, measure-
1.6 The values stated in SI units are to be regarded as
mentanddatainterpretationparametersforphosphateantiwear
standard. No other units of measurement are included in this
additives using both direct trend analysis and differential
standard.
-1
(spectral subtraction) trend analysis are presented.
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
safety concerns, if any, associated with its use. It is the
changes associated with phosphate antiwear additives in in-
responsibility of the user of this standard to establish appro-
service petroleum and hydrocarbon based lubricants. Warnings
priate safety, health, and environmental practices and deter-
or alarm limits can be set on the basis of a fixed minimum
mine the applicability of regulatory limitations prior to use.
1.8 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1
This test method is under the jurisdiction of ASTM Committee D02 on
ization established in the Decision on Principles for the
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.
Current edition approved Dec. 1, 2021. Published January 2022. Originally
2
approved in 2009. Last previous edition approved in 2018 as D7412 – 18. DOI: The boldface numbers in parentheses refer to a list of references at the end of
10.1520/D7412-21. this standard.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Ba
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D7412 − 18 D7412 − 21
Standard 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)
1
Spectrometry
This standard is issued under the fixed designation D7412; 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*
1.1 This test method covers monitoring phosphate antiwear additives in in-service petroleum and hydrocarbon based lubricants
such as various types of engine oils, hydraulic oils, and other lubricants that are formulated for protection against wear. Typical
phosphate antiwear additives include zinc dialkyldithiophosphates, trialkyl phosphates, and triaryl phosphates.
1.2 This test method uses Fourier Transform Infrared (FT-IR) spectrometry for monitoring of phosphate antiwear additive
depletion in in-service petroleum and hydrocarbon based lubricants as a result of normal machinery operation. Monitoring the
depletion of phosphate antiwear additives in in-service lubricants can indicate unusual wear or severe operating conditions of the
machine. This test method is designed as a fast, simple spectroscopic check for monitoring of phosphate antiwear additives 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 phosphate antiwear additives in the oil.
1.3 Acquisition of FT-IR spectral data for measuring phosphate antiwear additives in in-service oil and lubricant samples is
described in Practice D7418. In this test method, measurement and data interpretation parameters for phosphate antiwear additives
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 phosphate antiwear additives in 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
2
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 centimeter).
1
This test method is under the jurisdiction of ASTM Committee D02 on 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.
Current edition approved Jan. 1, 2018Dec. 1, 2021. Published March 2018January 2022. Originally approved in 2009. Last previous edition approved in 20092018 as
D7412 – 09.D7412 – 18. DOI: 10.1520/D7412-18.10.1520/D7412-21.
2
The boldface numbers in parentheses refer to a list of references at the end of this standard.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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D7412 − 21
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 changes in the level of phosphate antiwear
additives 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
1.6.1 Except
...
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