ASTM D6514-03(2019)e1
(Test Method)Standard Test Method for High Temperature Universal Oxidation Test for Turbine Oils
Standard Test Method for High Temperature Universal Oxidation Test for Turbine Oils
SIGNIFICANCE AND USE
5.1 Degradation of fluid lubricants because of oxidation or thermal breakdown can result in fluid thickening or in the formation of acids or insoluble solids and render the fluid unfit for further use as a lubricant.
5.2 This test method can be used for estimating the oxidation stability of oils. It can function as a formulation screening tool, specification requirement, quality control measurement, or as a means of estimating remaining service life. It shall be recognized, however, that correlation between results of this test method and the oxidation stability of an oil in field service can vary markedly with field service conditions and with various oils.
5.3 This test method is designed to compliment Test Method D5846 and is intended for evaluation of fluids which do not degrade significantly within a reasonable period of time at 135 °C.
SCOPE
1.1 This test method covers a procedure for evaluating the oxidation of inhibited lubricants in the presence of air, copper, and iron metals.
1.2 This test method was developed and is used to evaluate the high temperature oxidation stability and deposit forming tendency of oils for steam and gas turbines. It has been used for testing other lubricants made with mineral oil and synthetic basestocks for compressors, hydraulic pumps, and other applications, but these have not been used in cooperative testing.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Identified hazardous chemicals are listed in Section 7. Before using this test method, refer to suppliers' safety labels, Material Safety Data Sheets and other technical literature.
1.5 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.
General Information
Relations
Standards Content (Sample)
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: D6514 − 03 (Reapproved 2019)
Standard Test Method for
High Temperature Universal Oxidation Test for Turbine Oils
This standard is issued under the fixed designation D6514; 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.
ε NOTE—Editorially updated Footnote 5 in February 2020.
1. Scope A510 Specification for General Requirements forWire Rods
and Coarse Round Wire, Carbon Steel (Metric) A0510_
1.1 This test method covers a procedure for evaluating the
A0510M
oxidation of inhibited lubricants in the presence of air, copper,
B1 Specification for Hard-Drawn Copper Wire
and iron metals.
D445 Test Method for Kinematic Viscosity of Transparent
1.2 This test method was developed and is used to evaluate
and Opaque Liquids (and Calculation of Dynamic Viscos-
the high temperature oxidation stability and deposit forming
ity)
tendencyofoilsforsteamandgasturbines.Ithasbeenusedfor
D664 Test Method for Acid Number of Petroleum Products
testing other lubricants made with mineral oil and synthetic
by Potentiometric Titration
basestocks for compressors, hydraulic pumps, and other
D943 Test Method for Oxidation Characteristics of Inhibited
applications, but these have not been used in cooperative
Mineral Oils
testing.
D974 Test Method for Acid and Base Number by Color-
1.3 The values stated in SI units are to be regarded as Indicator Titration
D3339 Test Method forAcid Number of Petroleum Products
standard. No other units of measurement are included in this
standard. by Semi-Micro Color Indicator Titration
D4057 Practice for Manual Sampling of Petroleum and
1.4 This standard does not purport to address all of the
Petroleum Products
safety concerns, if any, associated with its use. It is the
D4871 Guide for Universal Oxidation/Thermal Stability
responsibility of the user of this standard to establish appro-
Test Apparatus
priate safety, health, and environmental practices and deter-
D5846 Test Method for Universal Oxidation Test for Hy-
mine the applicability of regulatory limitations prior to use.
draulic and Turbine Oils Using the Universal Oxidation
Identified hazardous chemicals are listed in Section 7. Before
Test Apparatus
usingthistestmethod,refertosuppliers’safetylabels,Material
2.2 British Standards:
Safety Data Sheets and other technical literature.
1.5 This international standard was developed in accor- BS 1829 Specification for Carbon Steel, alternate to Speci-
fication A510
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
2.3 Institute of Petroleum Standard:
Development of International Standards, Guides and Recom-
IP2546 Practice for Sampling of Petroleum Products;Alter-
mendations issued by the World Trade Organization Technical
nate to Practice D4057
Barriers to Trade (TBT) Committee. 5
2.4 ASTM Adjunct
Oxidation Cell Varnish Standard
2. Referenced Documents
2.1 ASTM Standards:
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
D02.09.0C on Oxidation of Turbine Oils. Available from British Standards Institution (BSI), 389 Chiswick High Rd.,
CurrenteditionapprovedMay1,2019.PublishedJuly2019.Originallyapproved London W4 4AL, U.K., http://www.bsigroup.com.
in 2000. Last previous edition approved in 2014 as D6514 – 03 (2014). DOI: Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR,
10.1520/D6514-03R19E01. U.K., http://www.energyinst.org.
2 5
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available from ASTM International Headquarters. Order Adjunct No.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM ADJD6514-E-PDF. Names of suppliers in the United Kingdom can be obtained
Standards volume information, refer to the standard’s Document Summary page on from the Institute of Petroleum. Two master standards are held by the IP for
the ASTM website. reference.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D6514 − 03 (2019)
3.1.1 Universal Oxidation Test—the apparatus and proce- 5. Significance and Use
dures described in Guide D4871.
5.1 Degradation of fluid lubricants because of oxidation or
thermal breakdown can result in fluid thickening or in the
4. Summary of Test Method
formation of acids or insoluble solids and render the fluid unfit
4.1 After determining the viscosity at 40 °C and acid for further use as a lubricant.
number of a sample, a test specimen is stressed at 155 °C for
5.2 This test method can be used for estimating the oxida-
96 h.After cooling, the test specimen is vacuum filtered for the
tion stability of oils. It can function as a formulation screening
determination of the total insolubles formed during the test.
tool, specification requirement, quality control measurement,
Total insolubles are reported as low, medium, or high.
or as a means of estimating remaining service life. It shall be
4.2 The viscosity and the acid number of the filtrate are recognized, however, that correlation between results of this
determined and compared with the initial values to ascertain test method and the oxidation stability of an oil in field service
any increase in those values. Both the change in acid number can vary markedly with field service conditions and with
and the increase in viscosity at 40 °C are reported. various oils.
4.3 The glass cell in which the test specimen was stressed is 5.3 ThistestmethodisdesignedtocomplimentTestMethod
rinsed with heptane and dried. Residual deposits are compared D5846 and is intended for evaluation of fluids which do not
with ASTM Adjunct ADJD6514-E-PDF, and the results are degrade significantly within a reasonable period of time at
reported. 135 °C.
FIG. 1 Heating Block
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D6514 − 03 (2019)
6. Apparatus diameter glass tube, 455 mm 6 5 mm long, lower end with
fused capillary 1.5 mm inside diameter. The capillary bore
6.1 Heating Block, as shown in Fig. 1, and as further
shall be 15 mm 6 1 mm long. The lower tip is cut at a 45°
described in Guide D4871, to provide a controlled constant
angle.
temperature for conducting the test.
6.1.1 Testcellsaremaintainedatconstantelevatedtempera-
6.6 Basic Head, as shown in Fig. 3, and as further described
ture by means of a heated aluminum block which surrounds
in Guide D4871.This is an air condenser, with 34/45 standard-
each test cell. Alternate apparatus designs for sample heating
taper, ground-glass inner joint, opening for gas inlet tube,
and for temperature and flow control shall be acceptable,
septum port for sample withdrawal, and exit tube to conduct
provided they are shown to maintain temperature and gas flow
off-gasesandentrainedvapors.Overalllengthshallbe125 mm
within the standard’s specified limits.
6 5 mm.
6.1.2 Holes in the aluminum block to accommodate the test
6.7 Test precision was developed using the universal
cells shall provide 1.0 mm maximum clearance for 38 mm
outside diameter glass tubes. The test cells shall fit into the oxidation/thermal stability test apparatus described in Guide
6,7
D4871. Alternate apparatus designs for sample heating, and
block to a depth of 225 mm 6 5 mm.
for temperature and flow control shall be acceptable provided
6.2 Temperature Control System, as shown at lower left in
theyareshowntomaintaintemperatureandgasflowwithinthe
Fig. 1, and as further described in Guide D4871, to maintain
specified limits.
the test oils in the heating block at 155 °C 6 0.5 °C for the
duration of the test.
6.8 Drying Oven, explosion proof model recommended.
6.3 Gas Flow Control System, as shown at the upper left in
Fig. 1, and as further described in Guide D4871, to provide dry 7. Reagents and Materials
air at a flow rate of 3.0 L⁄h 6 0.5 L⁄h to each test cell.
7.1 Reagent grade chemicals shall be used in all tests.
6.3.1 A gas flow controller is required for each test cell.
Unless otherwise indicated, it is intended that all reagents
6.3.2 Flowmeters shall have a scale length sufficiently long
conform to the specifications of the Committee on Analytical
to permit accurate reading and control to within 5 % of full
Reagents of the American Chemical Society, where such
scale.
6.3.3 The total system accuracy shall meet or exceed the
following tolerances:
6.3.3.1 Inlet pressure regulator within 0.34 kPa (0.05 psig)
of setpoint; total flow control system reproducibility within
7 % of full scale; repeatability of measurement within 0.5 % of The sole source of supply of the standard commercial apparatus, including
heating block, temperature control system, flow control system, and glassware,
full scale.
known to the committee at this time is Falex Corp., 1020 Airpark Drive, Sugar
6.4 Oxidation Cell, borosilicate glass, as shown in Fig. 2, Grove, IL60554-9585. Glassware for the Universal Oxidation test apparatus is also
available from W.A. Sales, Ltd., 419 Harvester Ct., Wheeling, IL 60090.
andasfurtherdescribedinGuideD4871.Thisconsistsofatest
If you are aware of alternative suppliers, please provide this information to
cell of borosilicate glass, standard wall, 38 mm outside
ASTM International Headquarters. Your comments will receive careful consider-
diameter, 300 mm 6 5 mm length, with open end fitted with a
ation at a meeting of the responsible technical committee , which you may attend.
34/45 standard-taper, ground-glass outer joint.
6.5 Gas Inlet Tube, as shown in Fig. 2, and as further
described in Guide D4871. This consists of an 8 mm outside
FIG. 2 Oxidation Cell FIG. 3 Basic Head
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D6514 − 03 (2019)
specifications are available. Other grades may be used, pro- 8.1.1 Keep the plastic-encased printed ASTM Oxidation
vided it is first ascertained that the reagent is of sufficiently Cell Varnish Standards (ADJD6514 ) protected from light to
high purity to permit its use without lessening the accuracy of avoidthepossibilityoffading.Inspectforfadingbycomparing
the determination. two different plaques, one of which has been carefully pro-
7,9 tected from light (new). Observe both sets in diffuse daylight
7.2 Catalyst Coil (comprised of the following):
(or equivalent) first from a point directly above and then from
7.2.1 Low-Metalloid Steel Wire, 1.59 mm in diameter (No.
an angle of 45°. When any evidence of fading is observed,
16 Washburn and Moen Gage). Carbon steel wire, soft bright
particularly at the left-hand of the plaque, it is suggested that
annealed and free from rust, of grade 1008 as described in
the one that is more faded with respect to the other be
Specification A510, is preferred. Similar wire conforming to
discarded.
British Standard BS 1829 is also satisfactory.
8.1.1.1 Alternatively, place a 20 mm ( ⁄4 in.) opaque strip
7.2.2 Electrolytic Copper Wire, 1.63 mm in diameter (No.
(masking tape) across the top of the colored portion of the
14 American Wire Gage or No. 16 Imperial Standard Wire
plaque when initially purchased. At intervals, remove the
Gage), 99.9 % purity, conforming to Specification B1,is
opaquestripandobserve.Whenthereisanyevidenceoffading
preferred.
of the exposed portion, it is suggested that the standards be
7.3 Acetone, reagent grade. (Warning—Flammable. Health
replaced.
hazard.)
8.1.2 If the surface of the plastic cover shows excessive
scratching, it is suggested that the plaque be replaced.
7.4 Heptane,reagentgrade.(Warning—Flammable.Health
hazard.)
9. Sampling
7.5 Propan-2-ol (iso-Propyl Alcohol), reagent grade.
(Warning—Flammable. Health hazard.) 9.1 Samples for this test can come from laboratory blends,
tanks, drums, small containers, or operating equipment.
7.6 Isooctane, reagent grade. (Warning—Flammable.
Therefore, use the applicable apparatus and techniques de-
Health hazard.)
scribed in Practice D4057 or IP 2546 to obtain suitable
7.7 Abrasive Cloth, silicon carbide, 100 grit with cloth
samples.
backing.
9.2 Special precautions to preserve the integrity of a sample
7.8 Whatman Filter Paper, No. 41, 47 mm diameter.
will not normally be required. It is good practice to avoid
undue exposure of samples to sunlight or strong direct light.
7.9 Membrane Filters,white,plain,47 mmindiameterpore
Fluidsampleswhicharenothomogeneousonvisualinspection
size 8 µm. Millipore SC membrane filters (MF-type, cellulose
7,10
shall be rejected and fresh samples obtained.
ester), or equivalent have been found satisfactory.
7.10 Air, dry.
10. Preparation of Apparatus
7,11
7.11 Cleaning Reagent, either Nochromix (Warning—
7,12 10.1 Cleaning Glassware:
Health hazard. Corrosive. Harmful if inhaled) or Micro
10.1.1 Cleannewglasswarebywashingwithahotdetergent
solution.
solution (using a bristle brush) and rinse thoroughly with tap
NOTE1—Becauseofextremehazards,chromicacidcleaningsolutionis
water. If any visible deposits remain, soaking with a hot
not recommended.
detergent solution has proven helpful. After final cleaning, by
7,11
24 h soak at room temperature with cleaning reagent, rinse
8. Corrosion Standards
thoroughly with tap water, then distilled water and allow to dry
8.1 ASTM Oxidation Cell Varnish Standards (ADJD6514 )
at room temperature or in an oven. Following the final distilled
consist of reproductions in color of typical oxidation cell
water rinse, an iso-propyl alcohol or acetone rinse will hasten
internal surfaces representing increasing degrees of staining,
drying at room temperature.
the reproductions being encased in plastic in the form of a
10.1.2 Used glassware should be cleaned immediately fol-
plaque.
lowing the end of a test. Drain the used oil completely. Rinse
all glassware with heptane to remove traces of oil. Then clean
the glassware by the procedure described in 9.1.1 before later
Reagent Chemicals, American Chemical Society Specifications, American
use.
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory 10.2 Cleaning Catalyst:
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
10.2.1 Clean equal lengths (0.50 m 6 0.01 m) of iron and
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
copper wire with wa
...
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