ASTM D6514-00

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
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Designation: D 6514 – 00 An American National Standard
Standard Test Method for
High Temperature Universal Oxidation Test for Turbine Oils
This standard is issued under the fixed designation D 6514; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope D 974 Test Method for Acid and Base Number by Color-
Indicator Titration
1.1 This test method covers a procedure for evaluating the
D 3339 Test Method for Acid Number of Petroleum Prod-
oxidation of inhibited lubricants in the presence of air, copper,
ucts by Semi-Micro Color Indicator Titration
and iron metals.
D 4057 Practice for Manual Sampling of Petroleum and
1.2 This test method was developed for, and is used, to
Petroleum Products
evaluate the high temperature oxidation stability and deposit
D 4871 Guide for Universal Oxidation/Thermal Stability
forming tendency of oils for steam and gas turbines. It has been
Test Apparatus
used for testing other lubricants made with mineral oil and
D 5846 Test Method for Universal Oxidation Test for Hy-
synthetic basestocks for compressors, hydraulic pumps, and
draulic and Turbine Oils Using the Universal Oxidation
other applications, but these have not been used in cooperative
Test Apparatus
testing.
2.2 British Standards:
1.3 The values stated in SI units are to be regarded as
BS 1829 Specification for Carbon Steel, alternate to Speci-
standard.
fication A 510
1.4 This standard does not purport to address all of the
2.3 Institute of Petroleum Standard:
safety concerns, if any, associated with its use. It is the
IP 2546 Practice for Sampling of Petroleum Products;
responsibility of the user of this standard to establish appro-
Alternate to Practice D 4057
priate safety and health practices and determine the applica-
2.4 ASTM Adjunct
bility of regulatory limitations prior to use.
ASTM Oxidation Cell Varnish Standard
1.5 Identified hazardous chemicals are listed in Sections 7.2,
7.3 and 7.4. Before using this standard, refer to suppliers’
3. Terminology
safety labels, Material Safety Data Sheets and other technical
3.1 Definitions of Terms Specific to This Standard:
literature.
3.1.1 Universal Oxidation Test—the apparatus and proce-
2. Referenced Documents dures described in Guide D 4871
2.1 ASTM Standards:
4. Summary of Test Method
A 510 Specification for General Requirements for Wire
4.1 An oil sample is exposed to air at elevated temperatures
Rods and Coarse Round Wire, Carbon Steel
3 in the presence of copper and iron metals. The test is run for 96
B 1 Specification for Hard-Drawn Copper Wire
4 h at 155°C after which the viscosity increase, acid number
D 329 Specification for Acetone
increase, and sludge generated are measured. The test cell is
D 445 Test Method for Kinematic Viscosity of Transparent
5 also washed, dried, and compared with the ASTM Oxidation
and Opaque Liquids
Cell Varnish Standard.
D 664 Test Method for Acid Number of Petroleum Products
by Potentiometric Titration
5. Significance and Use
D 770 Specification for Isopropyl Alcohol
5.1 Degradation of fluid lubricants because of oxidation or
D 943 Test Method for Oxidation Characteristics of Inhib-
thermal breakdown can result in fluid thickening or in the
ited Mineral Oils
Annual Book of ASTM Standards, Vol 05.02.
Annual Book of ASTM Standards, Vol 05.03.
1 8
This standard is under the jurisdiction of ASTM Committee D02 on Petroleum Available from British Standards Institute, 2 Park St., London, England
Products and Lubricants and is the direct responsibility of D02.09 on Oxidation. W1A2B5.
Current edition approved Feb. 10, 2000. Published March 2000. Available from Institute of Petroleum, 61 New Cavendish St., London, W.I.,
Annual Book of ASTM Standards, Vol 01.03. England.
3 10
Annual Book of ASTM Standards, Vol 02.03. Available from ASTM Headquarters. Request PCN:ADJD6514.Names of
Annual Book of ASTM Standards, Vol 06.04. suppliers in the United Kingdom can be obtained from the Institute of Petroleum.
Annual Book of ASTM Standards, Vol 05.01. Two master standards are held by the IP for reference.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 6514
formation of acids or insoluble solids and render the fluid unfit 6.3.2 Flowmeters shall have a scale length sufficiently long
for further use as a lubricant. to permit accurate reading and control to within 5 % of full
scale.
5.2 This test method can be used for estimating the oxida-
tion stability of oils. It can function as a formulation screening 6.3.3 The total system accuracy shall meet or exceed the
tool, specification requirement, quality control measurements, following tolerances:
or as a means of estimating remaining service life. These last 6.3.3.1 Inlet pressure regulator within 0.34 kPa (0.05 psig)
three functions of the test method are expected to be fulfilled of setpoint; total flow control system reproducibility within
once a precision statement has been devised for the procedure. 7 % of full scale; repeatability of measurement within 0.5 % of
It should be recognized, however, that correlation between full scale.
results of this test method and the oxidation stability of an oil 6.4 Oxidation Cell, borosilicate glass, as shown in Fig. 2,
in field service can vary markedly with field service conditions and as further described in Guide D 4871. This consists of a
and with various oils. test cell of borosilicate glass, standard wall, 38 mm outside
5.3 This test method is designed to compliment Test Method diameter, 300 6 5-mm length, with open end fitted with a
D 5846 and is intended for evaluation of fluids which do not 34/45 standard-taper, ground-glass outer joint.
degrade significantly within a reasonable period of time at 6.5 Gas Inlet Tube, as shown in Fig. 2, and as further
135°C. described in Guide D 4871. This consists of an 8-mm outside
diameter glass tube, 455 6 5 mm long, lower end with fused
6. Apparatus
capillary 1.5-mm inside diameter. The capillary bore shall be
15 6 1 mm long. The lower tip is cut at a 45° angle.
6.1 Heating Block, as shown in Fig. 1, and as further
6.6 Basic Head, as shown in Fig. 3, and as further described
described in Guide D 4871, to provide a controlled constant
in Guide D 4871. This is an air condenser, with 34/45 standard-
temperature for conducting the test.
taper, ground-glass inner joint, opening for gas inlet tube,
6.1.1 Test cells are maintained at constant elevated tempera-
septum port for sample withdrawal, and exit tube to conduct
ture by means of a heated aluminum block which surrounds
off-gases and entrained vapors. Overall length shall be 125 6
each test cell. Alternate apparatus designs for sample heating
5 mm.
and for temperature and flow control shall be acceptable,
6.7 Test precision was developed using the universal
provided they are shown to maintain temperature and gas flow
oxidation/thermal stability test apparatus described in Guide
within the standard’s specified limits.
D 4871. Alternate apparatus designs for sample heating, and
6.1.2 Holes in the aluminum block to accommodate the test
for temperature and flow control shall be acceptable provided
cells shall provide 1.0 mm maximum clearance for 38-mm
they are shown to maintain temperature and gas flow within the
outside diameter glass tubes. The test cells shall fit into the
specified limits.
block to a depth of 225 6 5 mm.
6.8 Drying Oven, explosion proof.
6.2 Temperature Control System, as shown at lower left in
Fig. 1, and as further described in Guide D 4871, to maintain
the test oils in the heating block at 155 6 0.5°C for the duration
of the test.
A standard commercial apparatus has been found satisfactory for the purpose
of this method. This apparatus, including heating block, temperature control system,
6.3 Gas Flow Control System, as shown at the upper left in
flow control system and glassware, is available from Falex Corp., 1020 Airpark
Fig. 1, and as further described in Guide D 4871, to provide dry
Drive, Sugar Grove, IL 60554-9585. Glassware for the Universal Oxidation test
air at a flow rate of 3.0 6 0.5 L/h to each test cell.
apparatus is also available from W.A. Sales, Ltd., 419 Harvester Ct., Wheeling, IL
6.3.1 A gas flow controller is required for each test cell. 60090.
D 6514
FIG. 1 Heating Block
7. Reagents and Materials
7.1 Catalyst Wire.
7.1.1 Low-Metalloid Steel Wire, 1.59 mm in diameter (No.
16 Washburn and Moen Gage). Carbon steel wire, soft bright
annealed and free from rust, of grade 1008 as described in
Specification A 510, is preferred. Similar wire conforming to
British Standard 1829 is also satisfactory.
7.1.2 Electrolytic Copper Wire, 1.63 mm in diameter (No.
14 American Wire Gage or No. 16 Imperial Standard Wire
Gage), 99.9 % purity, conforming to Specification B 1, is
preferred.
7.2 Acetone, conforming to Specification D 329.
(WARNING)—Acetone - Flammable. Health hazard.
7.3 Heptane, reagent grade. (WARNING)—Flammable.
Health hazard.
7.4 Propan-2-ol (iso-Propyl Alcohol), conforming to Speci-
fication D 770. (WARNING)—Flammable. Health hazard.
FIG. 2 Oxidation Cell
7.5 Abrasive Cloth, silicon carbide, 100-grit with cloth
backing. 7.7 Membrane Filters, white, plain, 47 mm in diameter pore
7.6 Whatman Filter Paper, No. 41, 47 mm. size 8 μm. Millipore SC membrane filters (MF-type, cellulose
D 6514
undue exposure of samples to sunlight or strong direct light.
Fluid samples which are not homogeneous on visual inspection
should not be used.
10. Preparation of Apparatus
10.1 Cleaning Glassware:
10.1.1 Clean new glassware by washing with a hot detergent
solution (using a bristle brush) and rinse thoroughly with tap
water. If any visible deposits remain, soaking with a hot
detergent solution has proven helpful. After final cleaning by
soaking with a suitable cleaning solution rinse thoroughly
with tap water, then distilled water and allow to dry at room
temperature or in an oven. Following the final distilled water
rinse, an iso-propyl alcohol or acetone rinse will hasten drying
at room temperature.
10.1.2 Used glassware should be cleaned immediately fol-
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
use.
FIG. 3 Basic Head
10.2 Cleaning Catalyst
10.2.1 Clean equal lengths (0.50 6 0.01m) of iron and
ester), or equivalent have been found satisfactory.
copper wire with wads of absorbed cotton wet with heptane or
7.8 Air, dry with dew point temperature of −60°C.
other saturated paraffinic solvent of comparable boiling point.
Follow by abrasion with silicon carbide cloth until fresh metal
8. Corrosion Standards
surfaces are exposed. Then wipe with dry absorbent cotton
8.1 ASTM Oxidation Cell Varnish Standards consist of
until all loose particles of metal and abrasive have been
reproductions in color of typical oxidational cell internal
removed. In following operations, handle the catalyst with
surfaces representing increasing degrees of staining, the repro-
clean gloves (cotton, rubber, or plastic) to prevent contact with
ductions being encased in plastic in the form of a plaque.
the skin.
8.1.1 Keep the plastic-encased printed ASTM Oxidation
10.2.2 One procedure for preparing clean catalyst wire is to
Cell Varnish Standards protected from light to avoid the
cut 0.50 6 0.01 m lengths of wire. Hold one end of the wire
possibility of fading. Inspect for fading by comparing two
tightly with a pair of clean pliers or in a vise while cleaning
different plaques, one of which has been carefully protected
with the abrasive cloth. Reverse ends of the wire and repeat.
from light (new). Observe both sets in diffuse daylight (or
10.2.3 Alternately, clean a longer length of wire (3 to 5 m)
equivalent) first from a point directly above and then from an
and then cut 0.50 6 0.01 m lengths from the clean wire.
angle of 45°. When any evidence of fading is observed,
10.3 Preparation of Catalyst Coil:
particularly at the left-hand of the plaque, it is suggested that
10.3.1 Twist the iron and copper wires tightly together at
the one that is more faded with respect to the other be
one end for three twists. With the two wires parallel, wind the
discarded.
wires around a cylindrical mandrel to produce a single coil 16
8.1.1.1 Alternatively, place a 20 mm ( ⁄4 in.) opaque strip
mm in inside diameter. The mandrel described in Test Method
(masking tape) across the top of the colored portion of the
D 943 is satisfactory, but other cylindrical metal or wood stock
plaque when initially purchased. At intervals, remove the
may be used. Remove the coil from the mandrel and secure the
opaque strip and observe. When there is any evidence of fading
free ends with three twists. Bend the twisted ends to conform
of the exposed portion, it is suggested that the standards be
to the shape of the spiral coil. Stretch the coil to produce a
replaced.
finished coil with an overall length of 80 6 8 mm.
8.1.2 If the surface of the plastic cover shows excessive
10.3.2 Store the catalyst coil in a dry, inert atmosphere until
scratching, it is suggested that the plaque be replaced.
use. For storage up to 24 h, the coil can be stored in heptane.
Before use, inspect stored coils to ensure that no corrosion
9. Sampling
products or contaminating materials are present.
9.1 Samples for this test can come from laboratory blends,
10.4 Use a fresh catalyst coil for each test. Do not reuse
tanks, drums, small containers, or operating equipment. There-
coils.
fore, use the applicable apparatus and techniques described in
Practice D 4057 or IP 2546 to obtain suitable samples.
9.2 Special precautions to preserve the integrity of a sample
Nochromix Reagent, available from Godax Laboratories, 720-B Erie Ave.,
will not normally be required. It is good practice to avoid
Takoma Park, MD 20192, has been found satisfactory for this purpose. Because of
extreme hazards, chromic acid cleaning solution is not recommended.
Prepared catalyst coils for use with this method are available fromC&P
Available from Millipore Filter Corp., Bedford, MA. Catalyst, P.O. Box 520984, Tulsa, OK 74152.
D 6514
11. Procedure membrane and funnel base. Rinse the surface of the membrane
with a gentle stream of heptane, directing the stream from the
11.1 Measure the initial acid number of the oils t
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