ASTM D6810-21
(Test Method)Standard Test Method for Measurement of Hindered Phenolic Antioxidant Content in Non-Zinc Turbine Oils by Linear Sweep Voltammetry
Standard Test Method for Measurement of Hindered Phenolic Antioxidant Content in Non-Zinc Turbine Oils by Linear Sweep Voltammetry
SIGNIFICANCE AND USE
5.1 The quantitative determination of hindered phenol antioxidants in a new turbine oil measures the amount of this material that has been added to the oil as protection against oxidation. Beside phenols, turbine oils can be formulated with other antioxidants such as amines which can extend the oil life. In used oil, the determination measures the amount of original (phenolic) antioxidant remaining after oxidation have reduced its initial concentration. This test method 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. Nor does it measure the overall stability of an oil, which is determined by the total contribution of all species present. 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 Practices D6224 and D4378), having the capability of measuring remaining oxidative life of the used oil.
5.1.1 This test method is applicable to non-zinc turbine oils. These are refined mineral oils containing rust and oxidation inhibitors, but not antiwear additives. This test method has not yet been established with sufficient precision for antiwear oils.
5.2 This test method is also suitable for manufacturing control and specification acceptance.
5.3 When a voltammetric analysis is obtained for a turbine oil inhibited with a typical hindered phenol antioxidant, there is an increase in the current of the produced voltammogram between 3 s to 5 s (or 0.3 V to 0.6 V applied voltage) (see Note 1) in the basic test solution (Fig. 1—x-axis 1 second = 0.1 V). Hindered phenol antioxidants detected by voltammetric analysis include, but are not limited to, 2,6-di-tert-butyl-4-methylphenol; 2,6-di-tert-butylphenol and 4,4'-meth...
SCOPE
1.1 This test method covers the voltammetric determination of hindered phenol antioxidants in new or in-service non-zinc turbine oils in concentrations from 0.0075 % by weight up to concentrations found in new oils by measuring the amount of current flow at a specified voltage in the produced voltammogram.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
1.4 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.
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Designation: D6810 − 21
Standard Test Method for
Measurement of Hindered Phenolic Antioxidant Content in
1
Non-Zinc Turbine Oils by Linear Sweep Voltammetry
This standard is issued under the fixed designation D6810; 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* for Auxiliary Power Plant Equipment
D6447 Test Method for Hydroperoxide Number of Aviation
1.1 This test method covers the voltammetric determination
Turbine Fuels by Voltammetric Analysis
of hindered phenol antioxidants in new or in-service non-zinc
D6971 Test Method for Measurement of Hindered Phenolic
turbine oils in concentrations from 0.0075 % by weight up to
and Aromatic Amine Antioxidant Content in Non-zinc
concentrations found in new oils by measuring the amount of
Turbine Oils by Linear Sweep Voltammetry
current flow at a specified voltage in the produced voltammo-
gram.
3. Terminology
1.2 The values stated in SI units are to be regarded as
3.1 For definitions of terms used in this method, refer to
standard. No other units of measurement are included in this
Terminology D4175.
standard.
1.3 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
4.1 A measured quantity of sample is dispensed into a vial
responsibility of the user of this standard to establish appro-
containing a measured quantity of alcohol-based electrolyte
priate safety, health, and environmental practices and deter-
solution and containing a layer of sand. When the vial is
mine the applicability of regulatory limitations prior to use.
shaken, the hindered phenol antioxidants and other solution
1.4 This international standard was developed in accor-
soluble oil components present in the sample are extracted into
dance with internationally recognized principles on standard-
the solution and the remaining droplets suspended in the
ization established in the Decision on Principles for the
solution are agglomerated by the sand. The sand/droplet
Development of International Standards, Guides and Recom-
suspension is allowed to settle out and the hindered phenol
mendations issued by the World Trade Organization Technical
antioxidants dissolved in the solution are quantified by volta-
Barriers to Trade (TBT) Committee.
mmetric analysis. The results are calculated and reported as
weight percent of antioxidant or as millimoles (mmol) of
2. Referenced Documents
antioxidant per litre of sample for prepared and fresh oils and
2
2.1 ASTM Standards:
as a percent remaining antioxidant for used oils.
D1193 Specification for Reagent Water
4.2 Voltammetric analysis is a technique that applies
D4057 Practice for Manual Sampling of Petroleum and
electro-analytic methods when a sample to be analyzed is
Petroleum Products
mixed with an electrolyte and a solvent and placed within an
D4175 Terminology Relating to Petroleum Products, Liquid
electrolytic cell. Data is obtained by measuring the current
Fuels, and Lubricants
passing through the cell as a function of the potential applied,
D4378 Practice for In-Service Monitoring of Mineral Tur-
and test results are based upon current, voltage and time
bine Oils for Steam, Gas, and Combined Cycle Turbines
relationships at the cell electrodes. The cell consists of a fluid
D6224 PracticeforIn-ServiceMonitoringofLubricatingOil
container into which is mounted a small, easily polarized
working electrode, and a large nonpolarizable reference elec-
1
This test method is under the jurisdiction of ASTM Committee D02 on
trode.Thereferenceelectrodeshouldbemassiverelativetothe
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
working electrode so that its behavior remains essentially
Subcommittee D02.09.0C on Oxidation of Turbine Oils.
constant with the passage of small current; that is, it remains
Current edition approved July 1, 2021. Published August 2021. Originally
unpolarized during the analysis period. Additional electrodes,
approved in 2002. Last previous edition approved in 2013 as D6810 – 13. DOI:
10.1520/D6810-21.
auxiliary electrodes, can be added to the electrode system to
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
eliminate the effects of resistive drop for high resistance
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
solutions. In performing a voltammetric analysis, the potential
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. across the electrodes is varied linearly with time, and the
*A Summary of Changes sec
...
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: D6810 − 13 D6810 − 21
Standard Test Method for
Measurement of Hindered Phenolic Antioxidant Content in
1
Non-Zinc Turbine Oils by Linear Sweep Voltammetry
This standard is issued under the fixed designation D6810; 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 the voltammetric determination of hindered phenol antioxidants in new or in-service non-zinc turbine
oils in concentrations from 0.0075 0.0075 % by weight % up to concentrations found in new oils by measuring the amount of
current flow at a specified voltage in the produced voltammogram.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.4 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D4378 Practice for In-Service Monitoring of Mineral Turbine Oils for Steam, Gas, and Combined Cycle Turbines
D6224 Practice for In-Service Monitoring of Lubricating Oil for Auxiliary Power Plant Equipment
D6447 Test Method for Hydroperoxide Number of Aviation Turbine Fuels by Voltammetric Analysis
D6971 Test Method for Measurement of Hindered Phenolic and Aromatic Amine Antioxidant Content in Non-zinc Turbine Oils
by Linear Sweep Voltammetry
3. Terminology
3.1 For definitions of terms used in this method, refer to Terminology D4175.
4. Summary of Test Method
4.1 A measured quantity of sample is dispensed into a vial containing a measured quantity of alcohol-based electrolyte solution
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
D02.09.0C on Oxidation of Turbine Oils.
Current edition approved May 1, 2013July 1, 2021. Published May 2013August 2021. Originally approved in 2002. Last previous edition approved in 20072013 as
D6810D6810 – 13.-07. DOI: 10.1520/D6810-13.10.1520/D6810-21.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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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D6810 − 21
NOTE 1—x-axis = time (seconds) and y-axis is current (arbitrary units). Top line in Fig. 1 is voltammogram of a fresh R&O turbine oil showing valley
indicator before and after standard.
FIG. 1 HinderdHindered Phenol Voltammetric Response in Basic Test Solution with Blank Response Zeroed
and containing a layer of sand. When the vial is shaken, the hindered phenol antioxidants and other solution soluble oil components
present in the sample are extracted into the solution and the remaining droplets suspended in the solution are agglomerated by the
sand. The sand/droplet suspension is allowed to settle out and the hindered phenol antioxidants dissolved in the solution are
quantified by voltammetric analysis. The results are calculated and reported as weight percent of antioxidant or as millimoles
(mmol) of antioxidant per litre of sample for prepared and fresh oils and as a percent remaining antioxidant for used oils.
4.2 Voltammetric analysis is a technique that applies electro-analytic methods when a sample to be analyzed is mixed with an
electrolyte and a solvent and placed w
...
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