ASTM D943-04a(2010)e1
(Test Method)Standard Test Method for Oxidation Characteristics of Inhibited Mineral Oils
Standard Test Method for Oxidation Characteristics of Inhibited Mineral Oils
SIGNIFICANCE AND USE
This test method is widely used for specification purposes and is considered of value in estimating the oxidation stability of lubricants, especially those that are prone to water contamination. It should be recognized, however, that correlation between results of this method and the oxidation stability of a lubricant in field service may vary markedly with field service conditions and with various lubricants. The precision statement for this method was determined on steam turbine oils.
Note 1—Furthermore, in the course of testing a lubricant by this method, other signs of deterioration, such as sludge formation or catalyst coil corrosion, may appear that are not reflected in the calculated oxidation lifetime. The subcommittee responsible for this method is investigating the application of alternative criteria for evaluation of lubricants using this test apparatus. Test Method D4310 is now available for sludge measurement.
SCOPE
1.1 This test method covers the evaluation of the oxidation stability of inhibited steam-turbine oils in the presence of oxygen, water, and copper and iron metals at an elevated temperature. This test method is limited to a maximum testing time of 10 000 h. This test method is also used for testing other oils, such as hydraulic oils and circulating oils having a specific gravity less than that of water and containing rust and oxidation inhibitors.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.2.1 Exception—The values in parentheses in the figures are provided for information for those using old equipment based on non-SI units.
1.3 WARNINGMercury has been designated by many regulatory agencies as a hazardous material that can cause central nervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s websitehttp://www.epa.gov/mercury/faq.htmfor additional information. Users should be aware that selling mercury and/or mercury containing products into your state or country may be prohibited by law.
1.4 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. For specific warning statements, see Section 6.
General Information
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Standards Content (Sample)
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
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Designation: D943 − 04a (Reapproved 2010) BS 2000-280:1999
Standard Test Method for
Oxidation Characteristics of Inhibited Mineral Oils
This standard is issued under the fixed designation D943; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
ε NOTE—Updated Scope with regard to SI units and added mercury caveat editorially in October 2010.
1. Scope 2. Referenced Documents
1.1 This test method covers the evaluation of the oxidation
2.1 ASTM Standards:
stability of inhibited steam-turbine oils in the presence of A510 Specification for General Requirements forWire Rods
oxygen, water, and copper and iron metals at an elevated
and Coarse Round Wire, Carbon Steel
temperature. This test method is limited to a maximum testing B1 Specification for Hard-Drawn Copper Wire
time of 10 000 h.This test method is also used for testing other
D664 Test Method for Acid Number of Petroleum Products
oils,suchashydraulicoilsandcirculatingoilshavingaspecific by Potentiometric Titration
gravitylessthanthatofwaterandcontainingrustandoxidation
D1193 Specification for Reagent Water
inhibitors. D3244 Practice for Utilization of Test Data to Determine
Conformance with Specifications
1.2 The values stated in SI units are to be regarded as
D3339 Test Method forAcid Number of Petroleum Products
standard. No other units of measurement are included in this
by Semi-Micro Color Indicator Titration
standard.
D4057 Practice for Manual Sampling of Petroleum and
1.2.1 Exception—The values in parentheses in the figures
Petroleum Products
are provided for information for those using old equipment
D4310 Test Method for Determination of Sludging and
based on non-SI units.
Corrosion Tendencies of Inhibited Mineral Oils
1.3 WARNING—Mercury has been designated by many
D5770 Test Method for Semiquantitative Micro Determina-
regulatory agencies as a hazardous material that can cause
tion of Acid Number of Lubricating Oils During Oxida-
central nervous system, kidney and liver damage. Mercury, or
tion Testing
its vapor, may be hazardous to health and corrosive to
E1 Specification for ASTM Liquid-in-Glass Thermometers
materials.Cautionshouldbetakenwhenhandlingmercuryand
2.2 Energy Institute Standards:
mercury containing products. See the applicable product Ma-
Specifications for IP Standard Thermometers
terial Safety Data Sheet (MSDS) for details and EPA’s
website—http://www.epa.gov/mercury/faq.htm—for addi-
2.3 British Standard:
tional information. Users should be aware that selling mercury BS 1829
and/or mercury containing products into your state or country
may be prohibited by law.
3. Summary of Test Method
1.4 This standard does not purport to address all of the
3.1 The oil sample is contacted with oxygen in the presence
safety concerns, if any, associated with its use. It is the
ofwaterandaniron-coppercatalystat95°C.Thetestcontinues
responsibility of the user of this standard to establish appro-
until the measured acid number of the oil is 2.0 mg KOH/g or
priate safety and health practices and determine the applica-
above. The number of test hours required for the oil to reach
bility of regulatory limitations prior to use. For specific
2.0 mg KOH/g is the “oxidation lifetime.”
warning statements, see Section 6.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method is under the jurisdiction of ASTM Committee D02 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Standards volume information, refer to the standard’s Document Summary page on
Subcommittee D02.09.0C on Oxidation of Turbine Oils. the ASTM website.
Current edition approved Oct. 1, 2010. Published December 2010. Originally Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR,
approved in 1947. Last previous edition approved in 2004 as D943–04a. United Kingdom.
In 1976, this test method ceased to be a joint ASTM-IP standard. DOI: Available from British Standards Institute, 389 Chiswick High Rd., London,
10.1520/D0943-10. W4 4AL, United Kingdom.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D943 − 04a (2010)
NOTE 1—All dimensions are in millimetres (inches).
NOTE 2—The oxidation test tube has a calibration line at 300 mL. This calibration applies to the test tube alone at 20°C.
NOTE 3—Open tube ends to be ground and fire-polished.
FIG. 1 Oxidation Cell
NOTE 1—Furthermore, in the course of testing a lubricant by this
4. Significance and Use
method, other signs of deterioration, such as sludge formation or catalyst
4.1 This test method is widely used for specification pur-
coilcorrosion,mayappearthatarenotreflectedinthecalculatedoxidation
poses and is considered of value in estimating the oxidation lifetime. The subcommittee responsible for this method is investigating
theapplicationofalternativecriteriaforevaluationoflubricantsusingthis
stability of lubricants, especially those that are prone to water
test apparatus. Test Method D4310 is now available for sludge measure-
contamination. It should be recognized, however, that correla-
ment.
tion between results of this method and the oxidation stability
of a lubricant in field service may vary markedly with field
5. Apparatus
service conditions and with various lubricants. The precision
statement for this method was determined on steam turbine 5.1 Oxidation Cell, of borosilicate glass, as shown in Fig. 1,
oils. consisting of a test tube, condenser, and oxygen delivery tube.
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D943 − 04a (2010)
The test tube has a calibration line at 300 mL (maximum error 5.8 Abrasive Cloth, silicon carbide, 100-grit with cloth
1 mL). This calibration applies to the test tube alone at 20°C. backing.
5.2 Heating Bath, thermostatically controlled, capable of 5.9 Syringes, glass, with Luer-Lok locking connectors, 10
maintaining the oil sample in the oxidation cell at a tempera- and 50-mL capacities for sampling, and water additions,
ture of 95 6 0.2°C, fitted with a suitable stirring device to respectively.
provide a uniform temperature throughout the bath, and large
5.10 Syringe Sampling Tube, Grade 304 stainless steel
enoughtoholdthedesirednumberofoxidationcellsimmersed
tubing, 2.11 mm in outside diameter, 1.60 mm in inside
in the heating bath to a depth of 390 6 10 mm and in the
diameter, 559 6 2 mm long, with one end finished at 90° and
heating liquid itself to a depth of 355 6 10 mm.
the other end fitted with a Luer-Lok female connector. The
Luer-Lok connector is preferably of elastomeric material, such
NOTE 2—Metal block heaters meeting the test method requirements
may also be used. It is not known what types of heating baths were used
as polyfluorovinylchloride to provide a good seal with the
7,8
in developing the precision statement.
syringe.
5.2.1 Studies have suggested that direct sunlight or artificial
5.11 Stopper,forLuerfittingofsyringesamplingtube,made
light may adversely influence the results of this test. To 9
of polytetrafluoroethylene or polyfluorovinylchloride.
minimize effects of light exposure on the lubricant being
5.12 Sampling Tube Holder, for supporting the syringe
tested, light shall be excluded from the lubricant by one or
sampling tube, made of methyl methacrylate resin, having the
more of the following ways:
dimensions shown in Fig. 4.
5.2.1.1 Use of heated liquid baths that are designed and
constructed of metal, or combinations of metals and other 5.13 Sampling Tube Spacer, for positioning the end of the
suitable opaque materials, that prevent light from entering the sampling tube above the sampling tube holder, made of a
test cell from the sides is preferred. If a viewing window is length of plastic tubing polyvinyl chloride, polyethylene,
included in the design, this viewing window shall be fitted with polypropylene, or polytetrafluoroethylene having an inside
a suitable opaque cover and be kept closed when no observa- diameter of approximately 3 mm and 51 6 1 mm length.
tion is being made.
5.14 Flexible Tubing, polyvinyl chloride approximately 6.4
5.2.1.2 If glass heating baths are used, the bath shall be
mmininsidediameterwithawallfordeliveryofoxygentothe
wrapped with aluminum foil or other opaque material.
oxidation cell.
5.2.1.3 Bright light entering the test cell from directly
6. Reagents and Materials
overhead can be eliminated by use of an opaque shield.
6.1 Purity of Water—Unless otherwise indicated, references
5.3 Flowmeter, with a capacity of at least 3 L of oxygen/h,
to water shall be understood to mean reagent water as defined
and an accuracy of 6 0.1 L/h.
by Type II of Specification D1193.
5.4 Heating Bath Thermometer—ASTM Solvents Distilla-
6.2 Purity of Reagents—Reagent grade chemicals shall be
tion Thermometer having a range from 72 to 126°C, and
used in all tests. Unless otherwise indicated, it is intended that
conforming to the requirements for Thermometer 40C as
all reagents conform to the specifications of the Committee on
prescribed in Specification E1, or for Thermometer 70C as
Analytical Reagents of the American Chemical Society where
prescribed in Specifications for IP Standard Thermometers.
such specifications are available. Other grades may be used,
Alternatively, temperature–measuring devices of equal or bet-
provided it is first ascertained that the reagent is of sufficiently
ter accuracy may be used.
high purity to permit its use without lessening the accuracy of
5.5 Oxidation Cell Thermometer, having a range from 80 to
the determination.
100°C, graduated in 0.1°C, total length—250 mm, stem
6,7
6.3 Acetone, reagent grade.(Warning—Health hazard;
diameter—6.0 to 7.0 mm, calibrated for 76-mm immersion.
flammable.)
Alternatively, temperature–measuring devices of equal or bet-
ter accuracy may be used.
6.4 Catalyst Wires:
6.4.1 Low-Metalloid Steel Wire, 1.59 mm in diameter (No.
5.6 Thermometer Bracket, for holding the oxidation cell
16 Washburn and Moen Gage).
thermometer, of 18-8 stainless steel, having the dimensions
shown in Fig. 2.The thermometer is held in the bracket by two
The sole source of supply of syringe needles with polychloro-trifluoroethylene
fluoroelastomer O-rings of approximately 5 mm inside diam-
hub known to the committee at this time is Hamilton Co., catalog number KF-714.
eter. Alternatively, thin stainless steel wire may be used.
Suitable stoppers are available from suppliers of infrared spectrometer sample
cells.
5.7 Wire Coiling Mandrel, as shown in Fig. 3.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory
Supporting data (a summary of these results) have been filed at ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
International Headquarters and may be obtained by requesting Research Report and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
RR:D02-1365. MD.
The sole source of supply of the Brooklyn thermometer No. 21276-RM known Carbon steel wire, soft bright annealed and free from rust, of Grade 1008 as
to the committee at this time is the Brooklyn Thermometer Co., Farmingdale, NY. described in Specification A510 is satisfactory. Similar wire conforming to BS 1829
If you are aware of alternative suppliers, please provide this information to is also satisfactory. If these steels are not available, other equivalent steels may be
ASTM International Headquarters. Your comments will receive careful consider- used, provided they are found to be satisfactory in comparative tests using Test
ation at a meeting of the responsible technical committee, which you may attend. Method D943.
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D943 − 04a (2010)
NOTE 1—All dimensions are in millimetres (inches).
NOTE 2—Material: 18-8 Stainless Steel, 22 Gage (0.792 mm).
FIG. 2 Thermometer Bracket
6.4.2 Electrolytic Copper Wire, 1.63 mm in diameter (No. apparatus. The use of a two-stage pressure regulator on tank
16 Imperial Standard Wire Gage or No. 14 American Wire oxygen is recommended. (Warning—Vigorously accelerates
Gage), 99.9 % purity, conforming to Specification B1. Soft combustion.)
copper wire of an equivalent grade may also be used.
6.10 Cleaning Reagent, cleaning by a 24–h soak at room
7,12
temperature either in Nochromix (Warning—Corrosive.
NOTE 3—Alternatively, suitably prepared catalyst coils may be pur-
7,13
chased from a supplier.
Health Hazard.) or in Micro solution.
6.5 Detergent, water-soluble.
7. Sampling
6.6 n-Heptane, reagent grade. (Warning—Flammable.
7.1 Samples for this test can come from tanks, drums, small
Harmful if inhaled.)
containers, or even operating equipment. Therefore, use the
6.7 Hydrochloric Acid, concentrated [36 mass % (relative
applicable apparatus and techniques described in Practice
density 1.19)]. (Warning—Toxic and corrosive.)
D4057.
6.8 Isopropyl Alcohol, reagent grade. (Warning—
Flammable.) The sole source of supply of Nochromix known to the committee at this time
is Godax Laboratories, Inc., 720-B Erie Ave., Takoma Park, MD 20912.
6.9 Oxygen, 99.5 % minimum purity, with pressure regula-
ThesolesourceofsupplyoftheMicrosolutionknowntothecommitteeatthis
tion adequate to maintain a constant flow of gas through the time is International Products Corp., P.O. Box 70, Burlington, NJ 08016.
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D943 − 04a (2010)
NOTE 1—Dimensions are in millimetres (inches).
FIG. 3 Mandrel for Winding Catalyst Coils
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D943 − 04a (2010)
Remove the coil from the mandrel, twist the free ends of the
iron and copper wires together for three turns, and bend the
twisted ends to conform to the shape of the spiral coil. The
overall length of the finished coil should be 225 6 5 mm. If
necessary, the coil may be stretched to give the required length
(Note 3 and Note 4.)
NOTE 4—The finished catalyst coil is a double spiral of copper and iron
wire, 225 6 5 mm overall length and 15.9 to 16.5 mm inside diameter.
The turns of wire are evenly spaced, and two consecutive turns of the
same wire are 3.96 to 4.22 mm apart, center to center.The mandrel shown
in Fig. 3 is designed to produ
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