Designation: D6514 − 03 (Reapproved 2008)

Standard Test Method for

High Temperature Universal Oxidation Test for Turbine Oils1
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 D974 Test Method for Acid and Base Number by Color-
1.1 This test method covers a procedure for evaluating the Indicator Titration
oxidation of inhibited lubricants in the presence of air, copper, D3339 Test Method for Acid Number of Petroleum Products
and iron metals. by Semi-Micro Color Indicator Titration
D4057 Practice for Manual Sampling of Petroleum and
1.2 This test method was developed and is used to evaluate Petroleum Products
the high temperature oxidation stability and deposit forming D4871 Guide for Universal Oxidation/Thermal Stability
tendency of oils for steam and gas turbines. It has been used for Test Apparatus
testing other lubricants made with mineral oil and synthetic D5846 Test Method for Universal Oxidation Test for Hy-
basestocks for compressors, hydraulic pumps, and other appli- draulic and Turbine Oils Using the Universal Oxidation
cations, but these have not been used in cooperative testing. Test Apparatus
1.3 The values stated in SI units are to be regarded as 2.2 British Standards:3
standard. No other units of measurement are included in this BS 1829 Specification for Carbon Steel, alternate to Speci-
standard. fication A510
1.4 This standard does not purport to address all of the 2.3 Institute of Petroleum Standard:4
safety concerns, if any, associated with its use. It is the IP 2546 Practice for Sampling of Petroleum Products; Alter-
responsibility of the user of this standard to establish appro- nate to Practice D4057
priate safety and health practices and determine the applica- 2.4 ASTM Adjunct5
bility of regulatory limitations prior to use. IDENTIFIED HAZARD- Oxidation Cell Varnish Standard
OUS CHEMICALS ARE LISTED IN SECTION 7. BEFORE USING THIS TEST
METHOD, REFER TO SUPPLIERS’ SAFETY LABELS, MATERIAL SAFETY
3. Terminology
DATA SHEETS AND OTHER TECHNICAL LITERATURE.
3.1 Definitions of Terms Specific to This Standard:
2. Referenced Documents 3.1.1 Universal Oxidation Test—the apparatus and proce-
2.1 ASTM Standards:2 dures described in Guide D4871.
A510 Specification for General Requirements for Wire Rods
and Coarse Round Wire, Carbon Steel 4. Summary of Test Method
B1 Specification for Hard-Drawn Copper Wire 4.1 After determining the viscosity at 40°C and acid number
D445 Test Method for Kinematic Viscosity of Transparent of a sample, a test specimen is stressed at 155°C for 96 h. After
and Opaque Liquids (and Calculation of Dynamic Viscos- cooling, the test specimen is vacuum filtered for the determi-
ity) nation of the total insolubles formed during the test. Total
D664 Test Method for Acid Number of Petroleum Products insolubles are reported as low, medium, or high.
by Potentiometric Titration 4.2 The viscosity and the acid number of the filtrate are
D943 Test Method for Oxidation Characteristics of Inhibited determined and compared with the initial values to ascertain
Mineral Oils any increase in those values. Both the change in acid number
and the increase in viscosity at 40°C are reported.
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricantsand is the direct responsibility of D02.09.0C on
Oxidation of Turbine Oils.
3
Current edition approved Dec. 1, 2008. Published February 2009. Originally Available from British Standards Institute (BSI), 389 Chiswick High Rd.,
approved in 2000. Last previous edition approved in 2003 as D6514–03. DOI: London W4 4AL, U.K.
4
10.1520/D6514-03R08. Available from Institute of Petroleum (IP), 61 New Cavendish St., London,
2
For referenced ASTM standards, visit the ASTM website, [Link], or WIG 7AR, U.K.
5
contact ASTM Customer Service at service@[Link]. 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.

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 D6514 − 03 (2008)
4.3 The glass cell in which the test specimen was stressed is 5.3 This test method is designed to compliment Test Method
rinsed with heptane and dried. Residual deposits are compared D5846 and is intended for evaluation of fluids which do not
with ASTM Adjunct ADJD6514,5 and the results are reported. degrade significantly within a reasonable period of time at
135°C.
5. Significance and Use
5.1 Degradation of fluid lubricants because of oxidation or 6. Apparatus
thermal breakdown can result in fluid thickening or in the 6.1 Heating Block, as shown in Fig. 1, and as further
formation of acids or insoluble solids and render the fluid unfit described in Guide D4871, to provide a controlled constant
for further use as a lubricant. temperature for conducting the test.
5.2 This test method can be used for estimating the oxida- 6.1.1 Test cells are maintained at constant elevated tempera-
tion stability of oils. It can function as a formulation screening ture by means of a heated aluminum block which surrounds
tool, specification requirement, quality control measurement, each test cell. Alternate apparatus designs for sample heating
or as a means of estimating remaining service life. It shall be and for temperature and flow control shall be acceptable,
recognized, however, that correlation between results of this provided they are shown to maintain temperature and gas flow
test method and the oxidation stability of an oil in field service within the standard’s specified limits.
can vary markedly with field service conditions and with 6.1.2 Holes in the aluminum block to accommodate the test
various oils. cells shall provide 1.0 mm maximum clearance for 38-mm

FIG. 1 Heating Block

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 D6514 − 03 (2008)
outside diameter glass tubes. The test cells shall fit into the
block to a depth of 225 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 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 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:
[Link] 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
full scale.
6.4 Oxidation Cell, borosilicate glass, as shown in Fig. 2, FIG. 3 Basic Head
and as further described in Guide D4871. This consists of a test
cell of borosilicate glass, standard wall, 38 mm outside D4871.6,7 Alternate apparatus designs for sample heating, and
diameter, 300 6 5-mm length, with open end fitted with a for temperature and flow control shall be acceptable provided
34/45 standard-taper, ground-glass outer joint. they are shown to maintain temperature and gas flow within the
6.5 Gas Inlet Tube, as shown in Fig. 2, and as further specified limits.
described in Guide D4871. This consists of an 8-mm outside 6.8 Drying Oven, explosion proof model recommended.
diameter glass tube, 455 6 5 mm long, lower end with fused
capillary 1.5-mm inside diameter. The capillary bore shall be 7. Reagents and Materials
15 6 1 mm long. The lower tip is cut at a 45° angle. 7.1 Reagent grade chemicals shall be used in all tests.
6.6 Basic Head, as shown in Fig. 3, and as further described Unless otherwise indicated, it is intended that all reagents
in Guide D4871. This is an air condenser, with 34/45 standard- conform to the specifications of the Committee on Analytical
taper, ground-glass inner joint, opening for gas inlet tube, Reagents of the American Chemical Society, where such
septum port for sample withdrawal, and exit tube to conduct specifications are available.8 Other grades may be used, pro-
off-gases and entrained vapors. Overall length shall be 125 6 vided it is first ascertained that the reagent is of sufficiently
5 mm. high purity to permit its use without lessening the accuracy of
the determination.
6.7 Test precision was developed using the universal
oxidation/thermal stability test apparatus described in Guide 7.2 Catalyst Coil (comprised of the following):7,9
7.2.1 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 A510, is preferred. Similar wire conforming to
British Standard BS 1829 is also satisfactory.

6
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, IL 60554-9585. Glassware for the Universal Oxidation test apparatus is also
available from W.A. Sales, Ltd., 419 Harvester Ct., Wheeling, IL 60090.
7
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 1, which you may attend.
8
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.
9
The sole source of supply of prepared catalyst coils for use with this test
method known to the committee at this time is C & P Catalyst, P.O. Box 520984,
FIG. 2 Oxidation Cell Tulsa, OK 74152.

Copyright by ASTM Int'l (all rights reserved); 3

 D6514 − 03 (2008)
7.2.2 Electrolytic Copper Wire, 1.63 mm in diameter (No. 9. Sampling
14 American Wire Gage or No. 16 Imperial Standard Wire 9.1 Samples for this test can come from laboratory blends,
Gage), 99.9 % purity, conforming to Specification B1, is tanks, drums, small containers, or operating equipment. There-
preferred. fore, use the applicable apparatus and techniques described in
7.3 Acetone, reagent grade. (Warning—Flammable. Health Practice D4057 or IP 2546 to obtain suitable samples.
hazard.) 9.2 Special precautions to preserve the integrity of a sample
7.4 Heptane, reagent grade. (Warning—Flammable. Health will not normally be required. It is good practice to avoid
hazard.) undue exposure of samples to sunlight or strong direct light.
7.5 Propan-2-ol (iso-Propyl Alcohol) , reagent grade. Fluid samples which are not homogeneous on visual inspection
(Warning—Flammable. Health hazard.) shall be rejected and fresh samples obtained.
7.6 Isooctane, reagent grade. (Warning—Flammable. 10. Preparation of Apparatus
Health hazard.)
10.1 Cleaning Glassware:
7.7 Abrasive Cloth, silicon carbide, 100-grit with cloth 10.1.1 Clean new glassware by washing with a hot detergent
backing. solution (using a bristle brush) and rinse thoroughly with tap
7.8 Whatman Filter Paper, No. 41, 47–mm diameter. water. If any visible deposits remain, soaking with a hot
7.9 Membrane Filters, white, plain, 47 mm in diameter pore detergent solution has proven helpful. After final cleaning, by
size 8 µm. Millipore SC membrane filters (MF-type, cellulose 24–h soak at room temperature with cleaning reagent,7,11 rinse
ester),7,10 or equivalent have been found satisfactory. thoroughly with tap water, then distilled water and allow to dry
at room temperature or in an oven. Following the final distilled
7.10 Air, dry. water rinse, an iso-propyl alcohol or acetone rinse will hasten
7.11 Cleaning Reagent, either Nochromix7,11 (Warning drying at room temperature.
—Health hazard. Corrosive. Harmful if inhaled) or Micro7,12 10.1.2 Used glassware should be cleaned immediately fol-
solution. lowing the end of a test. Drain the used oil completely. Rinse
all glassware with heptane to remove traces of oil. Then clean
NOTE 1—Because of extreme hazards, chromic acid cleaning solution is
not recommended. the glassware by the procedure described in 9.1.1 before later
use.
8. Corrosion Standards 10.2 Cleaning Catalyst:
8.1 ASTM Oxidation Cell Varnish Standards (ADJD65145) 10.2.1 Clean equal lengths (0.50 6 0.01 m) of iron and
consist of reproductions in color of typical oxidation cell copper wire with wads of absorbed cotton wet with heptane or
internal surfaces representing increasing degrees of staining, isooctane. Follow by abrasion with silicon carbide cloth until
the reproductions being encased in plastic in the form of a fresh metal surfaces are exposed. Then wipe with dry absorbent
plaque. cotton until all loose particles of metal and abrasive have been
8.1.1 Keep the plastic-encased printed ASTM Oxidation removed. In following operations, handle the catalyst with
Cell Varnish Standards (ADJD65145) protected from light to clean gloves (cotton, rubber, or plastic) to prevent contact with
avoid the possibility of fading. Inspect for fading by comparing the skin.
two different plaques, one of which has been carefully pro-
NOTE 2—One procedure for preparing clean catalyst wire is to cut 0.50
tected from light (new). Observe both sets in diffuse daylight 6 0.01 m lengths of wire. Hold one end of the wire tightly with a pair of
(or equivalent) first from a point directly above and then from clean pliers or in a vise while cleaning with the abrasive cloth. Reverse
an angle of 45°. When any evidence of fading is observed, ends of the wire and repeat. Alternatively, clean a longer length of wire (3
particularly at the left-hand of the plaque, it is suggested that to 5 m) and then cut 0.50 6 0.01 m lengths from the clean wire.
the one that is more faded with respect to the other be 10.3 Preparation of Catalyst Coil :
discarded. 10.3.1 Twist the iron and copper wires tightly together at
[Link] Alternatively, place a 20 mm (3 ⁄4 in.) opaque strip one end for three twists. With the two wires parallel, wind the
(masking tape) across the top of the colored portion of the wires around a cylindrical mandrel to produce a single coil 16
plaque when initially purchased. At intervals, remove the mm in inside diameter. The mandrel described in Test Method
opaque strip and observe. When there is any evidence of fading D943 is satisfactory, but other cylindrical metal or wood stock
of the exposed portion, it is suggested that the standards be may be used. Remove the coil from the mandrel and secure the
replaced. free ends with three twists. Bend the twisted ends to conform
8.1.2 If the surface of the plastic cover shows excessive to the shape of the spiral coil. Stretch the coil to produce a
scratching, it is suggested that the plaque be replaced. finished coil with an overall length of 80 6 8 mm.7 ,9
10.3.2 Store the catalyst coil in a dry, inert atmosphere until
10
use. For storage up to 24 h, the coil can be stored in heptane.
The sole source of supply of the apparatus known to the committee at this time
is Millipore Filter Corp., Bedford, MA. Before use, inspect stored coils to ensure that no corrosion
11
The sole source of supply of Nochromix Reagent known to the committee at products or contaminating materials are present.
this time is Godax Laboratories, 720-B Erie Ave., Takoma Park, MD 20192.
12
The sole source of supply of Micro known to the committee at this time is 10.4 Use a fresh catalyst coil for each test. Do not reuse
International Products Corp., P.O. Box 70, Burlington, NJ 08016. coils.

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 D6514 − 03 (2008)
11. Procedure from the test cell. Do not attempt to dislodge insolubles from
11.1 Measure the initial acid number of the oils to be tested the coil, gas inlet tube, or oxidation tube.
by Test Method D664, D3339, or D974 and the initial viscosity 11.14 Rinse both filters with sufficient heptane till the fluid
at 40°C by Test Method D445. passing through the filters is completely colorless. With the
vacuum applied, remove the clamp and funnel from the filter
11.2 Adjust the heating block to a temperature high enough
membrane and funnel base. Rinse the surface of the membrane
to maintain the oil in the oxidation test cell at 155 6 0.5°C. The
with a gentle stream of heptane, directing the stream from the
155 6 0.5° setting is predetermined with a calibrated thermom-
edge towards the center so as to remove final traces of oil from
eter or thermocouple sitting on the bottom of a test cell
the membrane. Maintain the vacuum for a short time to remove
containing 100 g test fluid with 3.0 6 0.5 L/h dry air flowing
final traces of heptane. Transfer the membranes to the identical
through the fluid.
weighing vessels used in the initial weighing and dry for at
11.3 Place the catalyst coil and gas inlet tube in the test cell. least 1 h in the oven at 105°C. Allow to cool for at least 1 h and
Obtain the total weight, W1, of these three components to the determine the weights of the No. 41 Whatman filter, W2a, and
nearest 0.1 mg. The components may be weighed either the 8 µm filter membrane, W3a, to the nearest 0.1 mg.
separately or together.
11.15 Dry the test cell plus gas delivery tube plus catalyst
11.4 Remove the gas inlet tube and weigh 100 6 1 g of test coil in an oven at 70°C for at least 1 h. Allow to cool for at least
fluid into the oxidation test cell 1 h and determine the combined weight of these three
11.5 Fit the gas inlet tube and basic head into the test cell so components, W1a.
that the tip of the gas inlet tube rests on the bottom of the test 11.16 Determine the acid number of the oxidized oil filtrate
cell inside the catalyst coil. A PTFE sleeve may be used when according to the same procedure used in 11.1.
inserting the basic condenser head into the cell. No grease is to 11.17 Determine the viscosity of the oxidized oil filtrate at
be used in the ground glass joint. 40°C according to Test Method D445.
11.6 Place the test cell into the preheated constant tempera- 11.18 Compare test cell appearance to the ASTM Oxidation
ture block. Cell Varnish Standards (ADJD65145). Hold both the cell and
11.7 Connect a gas delivery tube from the flow control the standard in such a manner that light reflected from them at
system to the gas inlet tube and adjust the flowmeter control to an angle of approximately 45° will be observed.
deliver dry air at 3 6 0.5 l/h. Record this time as the start of the
test. 12. Calculations
11.8 Recheck the air flow and temperature after the test is 12.1 Total weight of insoluble material:
underway and at least once daily during the test. Adjust to Total Insolubles, mg: ~ W 1a 2 W 1 ! 1 ~ W 2a 2 W 2 ! 1 ~ W 3a 2 W 3 ! (1)
maintain the air flow and temperature as needed. Total Weight, mg Report
30 or lower low
NOTE 3—Exhaust gases need not be collected. Vent exhaust gases greater than 30 but less than 100 medium
properly. 100 or more high
11.9 After 96 h, shut off the temperature and air flow. 12.2 Change in Acid Number (AN) :
Remove the gas inlet tube supporting the catalyst coil and Change in AN 5 ANf 2 ANi (2)
remove the test cell from the heating block. Wash gas inlet tube
with sufficient heptane to remove all test fluid and set it aside where:
in a clean location. ANf = final AN.
ANi = initial AN.
11.10 Allow sample to cool for a minimum of 16 but no
longer than 72 h 12.3 Percent Increase in Viscosity at 40°C:
11.11 Dry a No. 41 Whatman filter and an 8 µm filter % Increase in Viscosity @ 407C ~ V f 2 V i ! /V i 3 100 (3)
membrane in an oven at 70°C for 1 h and cool in a desiccator. where:
Using weighing vessel, obtain the weight of the No. 41
Vf = final viscosity.
Whatman filter, W2, and the 8 µm filter membrane, W3, each to Vi = initial viscosity.
the nearest 0.1 mg.
11.12 Filter the oil first through the preweighed No. 41 13. Interpretation
Whatman filter paper and then in a separate filtration apparatus 13.1 Interpret the oxidation stabilization of the sample
through the 8 µm membrane filter. Transfer the filtrate into a accordingly as the appearance of the oxidation cell agrees with
clean 250 mL beaker and set aside for acid number and one of the varnishes of the ASTM Oxidation Cell Varnish
viscosity determinations. Standard (ADJD65145).
11.13 Reassemble the Whatman filtration apparatus. Rinse 13.1.1 When the appearance of the oxidation cell is in the
the oxidation cell plus catalyst coil with sufficient 100 mL obvious transition state between that indicated by any two
portions of heptane to ensure complete transfer of loose adjacent standard varnishes, judge the sample by the more
insolubles to the Whatman filter and removal of all test fluid varnished standard color.

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 D6514 − 03 (2008)
14. Report cal test material would, in the long run, in the normal and
14.1 Total weight of insoluble materials in milligrams. correct operation of the test method, exceed the following
values only in one case in twenty:
14.2 Change in acid number (AN).
Repeatability
14.3 Percent increase in viscosity at 40°C. Sludge 3.4X0.8
Viscosity Change 0.54(X + 1)
14.4 Report the varnishing in accordance with one of the AN Change 0.75(X + 0.1)
classifications listed in Table 1. where: X denotes mean value
15.3 Reproducibility—The difference between two single
15. Precision and Bias and independent results obtained by different operators work-
15.1 The precision of this test method as determined by ing in different laboratories on identical test material would, in
statistical examination of interlaboratory results is as follows: the long run, in the normal and correct operation of the test
method, exceed the following values only in one case in
15.2 Repeatability—The difference between two single and
twenty:
independent results obtained by the same operator with the
Reproducibility
same apparatus under constant operating conditions on identi-
Sludge 7.4X0.8
Viscosity Change 1.59(X + 1)
TABLE 1 Oxidation Cell Varnish Classification AN Change 1.57(X + 0.1)
where: X denotes mean value
Classification Designation DescriptionA
0 no varnish clear
15.4 Bias—The procedure in this test method for measuring
oxidation life of an oil has no bias because the value of the
1 slight varnish clear to light gray-brown oxidation life is defined only in terms of this test method.
2 medium varnish amber to light brown 15.5 In the case of pass/fail data, no generally accepted
method for determining precision or bias is currently available.
3 severe varnish dark brown to dark red and
black with black deposits 16. Keywords
A
The ASTM Oxidation Cell Varnish Standard (ADJD65145) is a colored reproduc-
tion of oxidation cells characteristic of these descriptions. 16.1 high temperature fluid stability test; oils—lubricating;
oxidation stability; turbine oil; universal oxidation test

APPENDIX

(Nonmandatory Information)

X1. PROCEDURE FOR PACKAGING CATALYST COILS

X1.1 Materials X1.1.4 Flushing Tube, stainless steel or glass, approxi-

X1.1.1 Test Tubes, borosilicate glass, 250 mm length, 25 mately 5 mm (3⁄16 in.) outside diameter, 305 mm (12 in.) long,
mm outside diameter, approximately 22 mm inside diameter. to deliver nitrogen to bottom of test tube.
X1.1.2 Caps, for test tubes, polyethylene, cylindrical shape, X1.1.5 Nitrogen Gas, 99.7 % minimum purity.
designed to closely grip outside surface of the test tube.7,13
X1.2 Procedure—Flush a new test tube with nitrogen gas,
X1.1.3 Desiccant Bags, 3-g silica gel granules in paper
using the flushing tube, to blow out any loose particles. The
package, approximately 76 mm (3 in.) long, 51 mm (2 in.)
wide, 3 mm (1⁄8 in.) thick.7,14 tube must be visibly clean and dry. Hold the tube on an angle
and gently slide the catalyst coil into the tube. Add a desiccant
13
bag which has been folded lengthwise to fit in the tube. Insert
The sole source of supply of the apparatus known to the committee at this time
is Caplugs, No. 1-SC, available from Unisco, Inc., 600 Palisode Ave., Englewood
the nitrogen flushing tube down the middle of the test tube, to
Cliffs, NJ. the bottom, and blow nitrogen through the tube for several
14
The sole source of supply of the apparatus known to the committee at this time seconds. Immediately after withdrawing the flushing tube, seal
is Dri-Pax Air Dryers, available from Davison Chemical Div., W.R. Grace and Co.,
Baltimore, MD.
the test tube with a polyethylene cap.

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 D6514 − 03 (2008)
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