ASTM D6514-03(2019)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
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.
1. Scope B1 Specification for Hard-Drawn Copper Wire
D445 Test Method for Kinematic Viscosity of Transparent
1.1 This test method covers a procedure for evaluating the
and Opaque Liquids (and Calculation of Dynamic Viscos-
oxidation of inhibited lubricants in the presence of air, copper,
ity)
and iron metals.
D664 Test Method for Acid Number of Petroleum Products
1.2 This test method was developed and is used to evaluate
by Potentiometric Titration
the high temperature oxidation stability and deposit forming
D943 Test Method for Oxidation Characteristics of Inhibited
tendencyofoilsforsteamandgasturbines.Ithasbeenusedfor
Mineral Oils
testing other lubricants made with mineral oil and synthetic
D974 Test Method for Acid and Base Number by Color-
basestocks for compressors, hydraulic pumps, and other
Indicator Titration
applications, but these have not been used in cooperative
D3339 Test Method forAcid Number of Petroleum Products
testing.
by Semi-Micro Color Indicator Titration
1.3 The values stated in SI units are to be regarded as D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
standard. No other units of measurement are included in this
standard. D4871 Guide for Universal Oxidation/Thermal Stability
Test Apparatus
1.4 This standard does not purport to address all of the
D5846 Test Method for Universal Oxidation Test for Hy-
safety concerns, if any, associated with its use. It is the
draulic and Turbine Oils Using the Universal Oxidation
responsibility of the user of this standard to establish appro-
Test Apparatus
priate safety, health, and environmental practices and deter-
2.2 British Standards:
mine the applicability of regulatory limitations prior to use.
BS 1829 Specification for Carbon Steel, alternate to Speci-
Identified hazardous chemicals are listed in Section 7. Before
fication A510
usingthistestmethod,refertosuppliers’safetylabels,Material
2.3 Institute of Petroleum Standard:
Safety Data Sheets and other technical literature.
IP2546 Practice for Sampling of Petroleum Products;Alter-
1.5 This international standard was developed in accor-
nate to Practice D4057
dance with internationally recognized principles on standard-
2.4 ASTM Adjunct
ization established in the Decision on Principles for the
Oxidation Cell Varnish Standard
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
3. Terminology
Barriers to Trade (TBT) Committee.
3.1 Definitions of Terms Specific to This Standard:
2. Referenced Documents
3.1.1 Universal Oxidation Test—the apparatus and proce-
dures described in Guide D4871.
2.1 ASTM Standards:
A510 Specification for General Requirements forWire Rods
4. Summary of Test Method
and Coarse Round Wire, Carbon Steel (Metric) A0510_
4.1 After determining the viscosity at 40 °C and acid
A0510M
number of a sample, a test specimen is stressed at 155 °C for
96 h.After cooling, the test specimen is vacuum filtered for the
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.
CurrenteditionapprovedMay1,2019.PublishedJuly2019.Originallyapproved Available from British Standards Institution (BSI), 389 Chiswick High Rd.,
in 2000. Last previous edition approved in 2014 as D6514 – 03 (2014). DOI: London W4 4AL, U.K., http://www.bsigroup.com.
10.1520/D6514-03R19. Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or U.K., http://www.energyinst.org.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Available from ASTM International Headquarters. Order Adjunct No.
Standards volume information, refer to the standard’s Document Summary page on ADJD6514. Names of suppliers in the United Kingdom can be obtained from the
the ASTM website. Institute of Petroleum. Two master standards are held by the IP for reference.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6514 − 03 (2019)
determination of the total insolubles formed during the test. recognized, however, that correlation between results of this
Total insolubles are reported as low, medium, or high. test method and the oxidation stability of an oil in field service
can vary markedly with field service conditions and with
4.2 The viscosity and the acid number of the filtrate are
various oils.
determined and compared with the initial values to ascertain
any increase in those values. Both the change in acid number
5.3 ThistestmethodisdesignedtocomplimentTestMethod
and the increase in viscosity at 40 °C are reported.
D5846 and is intended for evaluation of fluids which do not
degrade significantly within a reasonable period of time at
4.3 The glass cell in which the test specimen was stressed is
135 °C.
rinsed with heptane and dried. Residual deposits are compared
withASTMAdjunct ADJD6514, and the results are reported.
6. Apparatus
5. Significance and Use
6.1 Heating Block, as shown in Fig. 1, and as further
5.1 Degradation of fluid lubricants because of oxidation or
described in Guide D4871, to provide a controlled constant
thermal breakdown can result in fluid thickening or in the
temperature for conducting the test.
formation of acids or insoluble solids and render the fluid unfit
6.1.1 Testcellsaremaintainedatconstantelevatedtempera-
for further use as a lubricant.
ture by means of a heated aluminum block which surrounds
each test cell. Alternate apparatus designs for sample heating
5.2 This test method can be used for estimating the oxida-
tion stability of oils. It can function as a formulation screening and for temperature and flow control shall be acceptable,
tool, specification requirement, quality control measurement, provided they are shown to maintain temperature and gas flow
or as a means of estimating remaining service life. It shall be within the standard’s specified limits.
FIG. 1 Heating Block
D6514 − 03 (2019)
6.1.2 Holes in the aluminum block to accommodate the test
cells shall provide 1.0 mm maximum clearance for 38 mm
outside diameter glass tubes. The test cells shall fit into the
block to a depth of 225 mm 6 5 mm.
6.2 Temperature Control System, as shown at lower left in
Fig. 1, and as further described in Guide D4871, to maintain
the test oils in the heating block at 155 °C 6 0.5 °C for the
duration of the test.
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
air at a flow rate of 3.0 L⁄h 6 0.5 L⁄h to each test cell.
6.3.1 A gas flow controller is required for each test cell.
6.3.2 Flowmeters shall have a scale length sufficiently long
to permit accurate reading and control to within 5 % of full
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
FIG. 3 Basic Head
full scale.
6.4 Oxidation Cell, borosilicate glass, as shown in Fig. 2,
andasfurtherdescribedinGuideD4871.Thisconsistsofatest
cell of borosilicate glass, standard wall, 38 mm outside
6.7 Test precision was developed using the universal
diameter, 300 mm 6 5 mm length, with open end fitted with a oxidation/thermal stability test apparatus described in Guide
6,7
34/45 standard-taper, ground-glass outer joint.
D4871. Alternate apparatus designs for sample heating, and
for temperature and flow control shall be acceptable provided
6.5 Gas Inlet Tube, as shown in Fig. 2, and as further
theyareshowntomaintaintemperatureandgasflowwithinthe
described in Guide D4871. This consists of an 8 mm outside
specified limits.
diameter glass tube, 455 mm 6 5 mm long, lower end with
fused capillary 1.5 mm inside diameter. The capillary bore 6.8 Drying Oven, explosion proof model recommended.
shall be 15 mm 6 1 mm long. The lower tip is cut at a 45°
angle. 7. Reagents and Materials
6.6 Basic Head, as shown in Fig. 3, and as further described
7.1 Reagent grade chemicals shall be used in all tests.
in Guide D4871.This is an air condenser, with 34/45 standard- Unless otherwise indicated, it is intended that all reagents
taper, ground-glass inner joint, opening for gas inlet tube,
conform to the specifications of the Committee on Analytical
septum port for sample withdrawal, and exit tube to conduct Reagents of the American Chemical Society, where such
off-gasesandentrainedvapors.Overalllengthshallbe125 mm
specifications are available. Other grades may be used, pro-
6 5 mm. vided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
the determination.
7,9
7.2 Catalyst Coil (comprised of the following):
The sole source of supply of the standard commercial apparatus, including
heating block, temperature control system, flow control system, and glassware,
known to the committee at this time is Falex Corp., 1020 Airpark Drive, Sugar
Grove, IL60554-9585. Glassware for the Universal Oxidation test apparatus is also
available from W.A. Sales, Ltd., 419 Harvester Ct., Wheeling, IL 60090.
If you are aware of alternative suppliers, please provide this information to
ASTM International Headquarters. Your comments will receive careful consider-
ation at a meeting of the responsible technical committee , which you may attend.
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
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD.
The sole source of supply of prepared catalyst coils for use with this test
method known to the committee at this time isC&P Catalyst, P.O. Box 520984,
FIG. 2 Oxidation Cell Tulsa, OK 74152.
D6514 − 03 (2019)
7.2.1 Low-Metalloid Steel Wire, 1.59 mm in diameter (No. opaquestripandobserve.Whenthereisanyevidenceoffading
16 Washburn and Moen Gage). Carbon steel wire, soft bright of the exposed portion, it is suggested that the standards be
annealed and free from rust, of grade 1008 as described in replaced.
Specification A510, is preferred. Similar wire conforming to 8.1.2 If the surface of the plastic cover shows excessive
British Standard BS 1829 is also satisfactory.
scratching, it is suggested that the plaque be replaced.
7.2.2 Electrolytic Copper Wire, 1.63 mm in diameter (No.
14 American Wire Gage or No. 16 Imperial Standard Wire
9. Sampling
Gage), 99.9 % purity, conforming to Specification B1,is
9.1 Samples for this test can come from laboratory blends,
preferred.
tanks, drums, small containers, or operating equipment.
7.3 Acetone, reagent grade. (Warning—Flammable. Health
Therefore, use the applicable apparatus and techniques de-
hazard.)
scribed in Practice D4057 or IP 2546 to obtain suitable
samples.
7.4 Heptane,reagentgrade.(Warning—Flammable.Health
hazard.)
9.2 Special precautions to preserve the integrity of a sample
will not normally be required. It is good practice to avoid
7.5 Propan-2-ol (iso-Propyl Alcohol), reagent grade.
undue exposure of samples to sunlight or strong direct light.
(Warning—Flammable. Health hazard.)
Fluidsampleswhicharenothomogeneousonvisualinspection
7.6 Isooctane, reagent grade. (Warning—Flammable.
shall be rejected and fresh samples obtained.
Health hazard.)
7.7 Abrasive Cloth, silicon carbide, 100 grit with cloth
10. Preparation of Apparatus
backing.
10.1 Cleaning Glassware:
7.8 Whatman Filter Paper, No. 41, 47 mm diameter.
10.1.1 Cleannewglasswarebywashingwithahotdetergent
solution (using a bristle brush) and rinse thoroughly with tap
7.9 Membrane Filters,white,plain,47 mmindiameterpore
water. If any visible deposits remain, soaking with a hot
size 8 µm. Millipore SC membrane filters (MF-type, cellulose
7,10
detergent solution has proven helpful. After final cleaning, by
ester), or equivalent have been found satisfactory.
7,11
24 h soak at room temperature with cleaning reagent, rinse
7.10 Air, dry.
thoroughly with tap water, then distilled water and allow to dry
7,11
7.11 Cleaning Reagent, either Nochromix (Warning—
at room temperature or in an oven. Following the final distilled
7,12
Health hazard. Corrosive. Harmful if inhaled) or Micro
water rinse, an iso-propyl alcohol or acetone rinse will hasten
solution.
drying at room temperature.
10.1.2 Used glassware should be cleaned immediately fol-
NOTE1—Becauseofextremehazards,chromicacidcleaningsolutionis
not recommended. lowing the end of a test. Drain the used oil completely. Rinse
all glassware with heptane to remove traces of oil. Then clean
8. Corrosion Standards
the glassware by the procedure described in 9.1.1 before later
8.1 ASTM Oxidation Cell Varnish Standards (ADJD6514 ) use.
consist of reproductions in color of typical oxidation cell
10.2 Cleaning Catalyst:
internal surfaces representing increasing degrees of staining,
10.2.1 Clean equal lengths (0.50 m 6 0.01 m) of iron and
the reproductions being encased in plastic in the form of a
copper wire with wads of absorbed cotton wet with heptane or
plaque.
isooctane. Follow by abrasion with silicon carbide cloth until
8.1.1 Keep the plastic-encased printed ASTM Oxidation
freshmetalsurfacesareexposed.Thenwipewithdryabsorbent
Cell Varnish Standards (ADJD6514 ) protected from light to
cotton until all loose particles of metal and abrasive have been
avoidthepossibilityoffading.Inspectforfadingbycomparing
removed. In following operations, handle the catalyst with
two different plaques, one of which has been carefully pro-
clean gloves (cotton, rubber, or plastic) to prevent contact with
tected from light (new). Observe both sets in diffuse daylight
the skin.
(or equivalent) first from a point directly above and then from
an angle of 45°. When any evidence of fading is observed, NOTE 2—One procedure fo
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