Standard Guide for Measurement of Remaining Primary Antioxidant Content In In-Service Industrial Lubricating Oils by Linear Sweep Voltammetry

SIGNIFICANCE AND USE
The quantitative determination of remaining antioxidants for in-service industrial oils by measuring the amount of these additives that have been added to the oil as protection against oxidation. Industrial lubricants, such as turbine oils, compressor oils, gear oils, hydraulic oils, bearing lubricants and greases can be formulated with a wide variety of antioxidants types such as phenols and amines (as primary antioxidants), which are working synergistically and therefore all important to be monitored individually. For in-service oils, the LSV determines and compares the amount of original primary antioxidants remaining after oxidation have reduced its initial concentration.
This guide covers procedures for primary antioxidants such as amines and phenols, as described by Test Method D6971 and D6810.
LSV is not designed or intended to detect all of the antioxidant intermediates formed during the thermal and oxidative stressing of the oils, which are recognized as having some contribution to the remaining useful life of the used or in-service oil. In order to measure the overall stability of an oil (including contribution of intermediates present), and before making final judgment on the remaining useful life of the used oil (which might result in the replacement of the oil reservoir), it is advised to perform additional analytical techniques (in accordance with Practice D4378 and Practice D6224).
This guide is applicable to a wide range of industrial oils, both mineral or synthetic based, which can contain rust and oxidation inhibitors, antiwear additives such as zinc dialkyl dithiophosphates on gear oils, circulating oils, transmission oils and other industrial lubricating oils.
The test is also suitable for manufacturing control and specification acceptance.
When a voltammetric analysis is obtained for a industrial lubricant inhibited with at least one type of antioxidant, there is an increase in the current of the produced voltammogram between 5 to 8 s ...
SCOPE
1.1 This guide covers the voltammetric analysis for qualitative measurements of primary antioxidants in new or in-service type industrial lubricants detectable in concentrations as low as 0.0075 mass percent up to concentrations found in new oils by measuring the amount of current flow at a specified voltage in the produced voltammogram.
1.2 This guide can be used as a resource for a condition monitoring program to track the oxidative health of a range of industrial lubricants which contain primary antioxidants. In order to avoid excessive degradation of the base-oil, these primary antioxidants play a major role to protect the lubricants against thermal-oxidative degradation. This guide can help users with interpretation and troubleshooting results obtained using linear sweep voltammetry (LSV).
1.3 When used as part of oil condition monitoring practices, it is important to apply trend analysis to monitor the antioxidant depletion rate relative to a baseline sample rather than use voltammetry for an absolute measurement of the antioxidant concentration. The trending pattern provides a proactive means to identify the level of oil degradation or abnormal changes in the condition of the in-service lubricant.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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.

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30-Nov-2009
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ASTM D7590-09e1 - Standard Guide for Measurement of Remaining Primary Antioxidant Content In In-Service Industrial Lubricating Oils by Linear Sweep Voltammetry
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´1
Designation: D7590 − 09
StandardGuide for
Measurement of Remaining Primary Antioxidant Content In
In-Service Industrial Lubricating Oils by Linear Sweep
1
Voltammetry
This standard is issued under the fixed designation D7590; 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
´ NOTE—Corrected figure placement and numbering editorially in March 2011.
INTRODUCTION
Under normal thermal and oxidative working conditions, which degrade the chemical composition
of the oil’s basestock and gradually deplete the oil’s additive package, good oil condition monitoring
procedures are necessary to determine and planning corrective actions before the oil properties
changes have passed their warning limits.Antioxidant monitoring practices are a vital part of modern
oil condition monitoring practices to achieve lubrication excellence. This guide addresses the correct
guidelines for voltammetric data interpretation.
1. Scope 1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This guide covers the voltammetric analysis for quali-
responsibility of the user of this standard to establish appro-
tative measurements of primary antioxidants in new or in-
priate safety and health practices and determine the applica-
service type industrial lubricants detectable in concentrations
bility of regulatory limitations prior to use.
as low as 0.0075 mass percent up to concentrations found in
newoilsbymeasuringtheamountofcurrentflowataspecified
2. Referenced Documents
voltage in the produced voltammogram.
2
2.1 ASTM Standards:
1.2 This guide can be used as a resource for a condition
D1193 Specification for Reagent Water
monitoring program to track the oxidative health of a range of
D4057 Practice for Manual Sampling of Petroleum and
industrial lubricants which contain primary antioxidants. In
Petroleum Products
order to avoid excessive degradation of the base-oil, these
D4378 Practice for In-Service Monitoring of Mineral Tur-
primary antioxidants play a major role to protect the lubricants
bine Oils for Steam and Gas Turbines
against thermal-oxidative degradation. This guide can help
D6224 PracticeforIn-ServiceMonitoringofLubricatingOil
users with interpretation and troubleshooting results obtained
for Auxiliary Power Plant Equipment
using linear sweep voltammetry (LSV).
D6304 Test Method for Determination of Water in Petro-
1.3 When used as part of oil condition monitoring practices,
leum Products, Lubricating Oils, and Additives by Cou-
it is important to apply trend analysis to monitor the antioxi-
lometric Karl Fischer Titration
dant depletion rate relative to a baseline sample rather than use
D6810 Test Method for Measurement of Hindered Phenolic
voltammetry for an absolute measurement of the antioxidant
Antioxidant Content in Non-Zinc Turbine Oils by Linear
concentration.The trending pattern provides a proactive means
Sweep Voltammetry
to identify the level of oil degradation or abnormal changes in
D6971 Test Method for Measurement of Hindered Phenolic
the condition of the in-service lubricant.
and Aromatic Amine Antioxidant Content in Non-zinc
1.4 The values stated in SI units are to be regarded as Turbine Oils by Linear Sweep Voltammetry
standard. No other units of measurement are included in this D7214 Test Method for Determination of the Oxidation of
standard.
1 2
This guide is under the jurisdiction of ASTM Committee D02 on Petroleum For referenced ASTM standards, visit the ASTM website, www.astm.org, or
ProductsandLubricantsandisthedirectresponsibilityofSubcommitteeD02.09.0C contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
on Oxidation of Turbine Oils. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Dec. 1, 2009. Published February 2010. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D7590 − 09
Used Lubricants by FT-IR Using Peak Area Increase 4.2 ASTM International has two standards, Test Method
Calculation D6810 and D6971, that shall enable the measurement of the
3
remaining phenolic and aminic type of antioxidants. No
2.2 ISO Standards:
standard test method has been developed for the detection of
ISO 4406.2 Hydraulic fluid power -- Fluids -- Method for
other type of antioxidants by linear voltammetry, although
coding the level of contamination by solid particles
4 LSV also has detection capabilities for these types of second
...

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