ASTM D6514-03(2008)
(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
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.
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.
This test method is designed to compliment Test Method D 5846 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 and health 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.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation: D6514 − 03(Reapproved 2008)
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 D943 Test Method for Oxidation Characteristics of Inhibited
Mineral Oils
1.1 This test method covers a procedure for evaluating the
D974 Test Method for Acid and Base Number by Color-
oxidation of inhibited lubricants in the presence of air, copper,
Indicator Titration
and iron metals.
D3339 Test Method forAcid Number of Petroleum Products
1.2 This test method was developed and is used to evaluate
by Semi-Micro Color Indicator Titration
the high temperature oxidation stability and deposit forming
D4057 Practice for Manual Sampling of Petroleum and
tendencyofoilsforsteamandgasturbines.Ithasbeenusedfor
Petroleum Products
testing other lubricants made with mineral oil and synthetic
D4871 Guide for Universal Oxidation/Thermal Stability
basestocks for compressors, hydraulic pumps, and other
Test Apparatus
applications, but these have not been used in cooperative
D5846 Test Method for Universal Oxidation Test for Hy-
testing.
draulic and Turbine Oils Using the Universal Oxidation
1.3 The values stated in SI units are to be regarded as Test Apparatus
standard. No other units of measurement are included in this
2.2 British Standards:
standard.
BS 1829 Specification for Carbon Steel, alternate to Speci-
fication A510
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
2.3 Institute of Petroleum Standard:
responsibility of the user of this standard to establish appro-
IP2546 Practice for Sampling of Petroleum Products;Alter-
priate safety and health practices and determine the applica-
nate to Practice D4057
bility of regulatory limitations prior to use. IDENTIFIED HAZARD- 5
2.4 ASTM Adjunct
OUS CHEMICALS ARE LISTED IN SECTION 7.BEFORE USING THIS TEST
Oxidation Cell Varnish Standard
METHOD, REFER TO SUPPLIERS’ SAFETY LABELS,MATERIAL SAFETY
DATA SHEETS AND OTHER TECHNICAL LITERATURE.
3. Terminology
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:
dures described in Guide D4871.
A510 Specification for General Requirements forWire Rods
and Coarse Round Wire, Carbon Steel
4. Summary of Test Method
B1 Specification for Hard-Drawn Copper Wire
4.1 Afterdeterminingtheviscosityat40°Candacidnumber
D445 Test Method for Kinematic Viscosity of Transparent
ofasample,atestspecimenisstressedat155°Cfor96h.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
determined and compared with the initial values to ascertain
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.
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.
10.1520/D6514-03R08. Available from Institute of Petroleum (IP), 61 New Cavendish St., London,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or WIG 7AR, U.K.
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(Reapproved 2008)
any increase in those values. Both the change in acid number
and the increase in viscosity at 40°C are reported.
D6514 − 03 (2008)
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
withASTMAdjunct ADJD6514, 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 Testcellsaremaintainedatconstantelevatedtempera-
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,
provided they are shown to maintain temperature and gas flow
recognized, however, that correlation between results of this
test method and the oxidation stability of an oil in field service within the standard’s specified limits.
6.1.2 Holes in the aluminum block to accommodate the test
can vary markedly with field service conditions and with
various oils. cells shall provide 1.0 mm maximum clearance for 38-mm
FIG. 1 Heating Block
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
thetestoilsintheheatingblockat155 60.5°Cfortheduration
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:
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
full scale.
FIG. 3 Basic Head
6.4 Oxidation Cell, borosilicate glass, as shown in Fig. 2,
andasfurtherdescribedinGuideD4871.Thisconsistsofatest
6,7
cell of borosilicate glass, standard wall, 38 mm outside
D4871. 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.
theyareshowntomaintaintemperatureandgasflowwithinthe
specified limits.
6.5 Gas Inlet Tube, as shown in Fig. 2, and as further
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
7. Reagents and Materials
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.
7.1 Reagent grade chemicals shall be used in all tests.
Unless otherwise indicated, it is intended that all reagents
6.6 Basic Head, as shown in Fig. 3, and as further described
conform to the specifications of the Committee on Analytical
in Guide D4871.This is an air condenser, with 34/45 standard-
Reagents of the American Chemical Society, where such
taper, ground-glass inner joint, opening for gas inlet tube,
specifications are available. Other grades may be used, pro-
septum port for sample withdrawal, and exit tube to conduct
vided it is first ascertained that the reagent is of sufficiently
off-gases and entrained vapors. Overall length shall be 125 6
high purity to permit its use without lessening the accuracy of
5 mm.
the determination.
6.7 Test precision was developed using the universal
7,9
7.2 Catalyst Coil (comprised of the following):
oxidation/thermal stability test apparatus described in Guide
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.
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 (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,reagentgrade.(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.
Fluidsampleswhicharenothomogeneousonvisualinspection
7.5 Propan-2-ol (iso-Propyl Alcohol) , reagent grade.
shall be rejected and fresh samples obtained.
(Warning—Flammable. Health hazard.)
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 Cleannewglasswarebywashingwithahotdetergent
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
detergent solution has proven helpful. After final cleaning, by
7.9 Membrane Filters,white,plain,47mmindiameterpore
7,11
24–h soak at room temperature with cleaning reagent, rinse
size 8 µm. Millipore SC membrane filters (MF-type, cellulose
7,10 thoroughly with tap water, then distilled water and allow to dry
ester), or equivalent have been found satisfactory.
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
7.11 Cleaning Reagent, either Nochromix (Warning drying at room temperature.
7,12
10.1.2 Used glassware should be cleaned immediately fol-
—Health hazard. Corrosive. Harmful if inhaled) or Micro
solution. lowing the end of a test. Drain the used oil completely. Rinse
all glassware with heptane to remove traces of oil. Then clean
NOTE1—Becauseofextremehazards,chromicacidcleaningsolutionis
the glassware by the procedure described in 9.1.1 before later
not recommended.
use.
8. Corrosion Standards
10.2 Cleaning Catalyst:
8.1 ASTM Oxidation Cell Varnish Standards (ADJD6514 ) 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
freshmetalsurfacesareexposed.Thenwipewithdryabsorbent
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 (ADJD6514 ) protected from light to clean gloves (cotton, rubber, or plastic) to prevent contact with
avoidthepossibilityoffading.Inspectforfadingbycomparing
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
to 5 m) and then cut 0.50 6 0.01 m lengths from the clean wire.
particularly at the left-hand of the plaque, it is suggested that
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
8.1.1.1 Alternatively, place a 20 mm ( ⁄4 in.) opaq
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
An American National Standard
Designation:D6514–03 Designation: D 6514 – 03 (Reapproved 2008)
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 (´) indicates an editorial change since the last revision or reapproval.
1. 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.
1.3The values stated in SI units are to be regarded as the standard.
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 and health 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.
2. Referenced Documents
2.1 ASTM Standards:
A 510 Specification for General Requirements for Wire Rods and Coarse Round Wire, Carbon Steel
B1 Specification for Hard-Drawn Copper Wire
D 445 Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and the Calculation of Dynamic Viscosity)
D 664 Test Method for Acid Number of Petroleum Products by Potentiometric Titration
D 943 Test Method for Oxidation Characteristics of Inhibited Mineral Oils
D 974 Test Method for Acid and Base Number by Color-Indicator Titration
D 3339 Test Method for Acid Number of Petroleum Products by Semi-Micro Color Indicator Titration
D 4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D 4871 Guide for Universal Oxidation/Thermal Stability Test Apparatus
D 5846 TestMethodforUniversalOxidationTestforHydraulicandTurbineOilsUsingtheUniversalOxidationTestApparatus
2.2 British Standards:
BS 1829 Specification for Carbon Steel, alternate to Specification A 510
2.3 Institute of Petroleum Standard:
IP 2546 Practice for Sampling of Petroleum Products; Alternate to Practice D 4057
2.4 ASTM Adjunct
ADJD6514 Oxidation Cell Varnish Standard
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 Universal Oxidation Test—the apparatus and procedures described in Guide D 4871.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of D02.09.0C on Oxidation
of Turbine Oils.
Current edition approved May 10, 2003. Published July 2003. Originally approved in 2000. Last previous edition approved in 2002 as D6514–02.
Current edition approved Dec. 1, 2008. Published February 2009. Originally approved in 2000. Last previous edition approved in 2003 as D 6514–03.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from British Standards Institute (BSI), 389 Chiswick High Rd., London W4 4AL, U.K.
Available from Institute of Petroleum (IP), 61 New Cavendish St., London, WIG 7AR, U.K.
Available from ASTM International Headquarters. Order Adjunct No. ADJD6514. Names of suppliers in the United Kingdom can be obtained from the 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.
D 6514 – 03 (2008)
4. Summary of Test Method
4.1 After determining the viscosity at 40°C and acid 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 determination of the total insolubles formed during the test. Total insolubles
are reported as low, medium, or high.
4.2 The viscosity and the acid number of the filtrate are determined and compared with the initial values to ascertain any
increase in those values. Both the change in acid number and the increase in viscosity at 40°C are reported.
4.3 Theglasscellinwhichthetestspecimenwasstressedisrinsedwithheptaneanddried.Residualdepositsarecomparedwith
ASTM Adjunct ADJD6514, and the results are reported.
5. 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 D 5846 and is intended for evaluation of fluids which do not
degrade significantly within a reasonable period of time at 135°C.
6. Apparatus
6.1 Heating Block, as shown in Fig. 1, and as further described in Guide D 4871, to provide a controlled constant temperature
for conducting the test.
6.1.1 Test cells are maintained at constant elevated temperature by means of a heated aluminum block which surrounds each
test cell. Alternate apparatus designs for sample heating and for temperature and flow control shall be acceptable, provided they
are shown to maintain temperature and gas flow within the standard’s specified limits.
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 6 5 mm.
6.2 Temperature Control System , as shown at lower left in Fig. 1, and as further described in Guide D4871,D 4871, 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,D 4871, 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:
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 full scale.
6.4 Oxidation Cell, borosilicate glass, as shown in Fig. 2, and as further described in Guide D4871.D 4871. This consists of a
test cell of borosilicate glass, standard wall, 38 mm outside diameter, 300 6 5-mm length, with open end fitted with a 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.D 4871. This consists of an 8-mm outside
diameter glass tube, 455 6 5 mm long, lower end with fused 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.
6.6 Basic Head, as shown in Fig. 3, and as further described in Guide D4871.D 4871. This is an air condenser, with 34/45
standard-taper, ground-glass inner joint, opening for gas inlet tube, septum port for sample withdrawal, and exit tube to conduct
off-gases and entrained vapors. Overall length shall be 125 6 5 mm.
6.7 Test precision was developed using the universal oxidation/thermal stability test apparatus described in Guide
6,7
D4871.D 4871. Alternate apparatus designs for sample heating, and for temperature and flow control shall be acceptable
provided they are shown to maintain temperature and gas flow within the specified limits.
6.8 Drying Oven, explosion proof model recommended.
7. Reagents and Materials
7.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents conform to the
specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are
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.
If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a
meeting of the responsible technical committee , which you may attend.
D 6514 – 03 (2008)
FIG. 1 Heating Block
FIG. 2 Oxidation Cell
D 6514 – 03 (2008)
FIG. 3 Basic Head
available. Other grades may be used, provided 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):
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,A 510, is preferred. Similar wire conforming to
British Standard BS 1829 is also satisfactory.
7.2.2 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 B1,B 1, is preferred.
7.3 Acetone, reagent grade. (Warning—Flammable. Health hazard.)
7.4 Heptane, reagent grade. (Warning—Flammable. Health hazard.)
7.5 Propan-2-ol (iso-Propyl Alcohol) , reagent grade. (Warning—Flammable. Health hazard.)
7.6 Isooctane, reagent grade. (Warning—Flammable. Health hazard.)
7.7 Abrasive Cloth, silicon carbide, 100-grit with cloth backing.
7.8 Whatman Filter Paper, No. 41, 47–mm diameter.
7.9 Membrane Filters, white, plain, 47 mm in diameter pore size 8 µm. Millipore SC membrane filters (MF-type, cellulose
7,10
ester), or equivalent have been found satisfactory.
7.10 Air, dry.
7,11 7,12
7.11 Cleaning Reagent, either Nochromix (Warning —Health hazard. Corrosive. Harmful if inhaled) or Micro solution.
NOTE 1—Because of extreme hazards, chromic acid cleaning solution is not recommended.
8. Corrosion Standards
8.1 ASTM Oxidation Cell Varnish Standards (ADJD6514)(ADJD6514 ) consist of reproductions in color of typical oxidation
cellinternalsurfacesrepresentingincreasingdegreesofstaining,thereproductionsbeingencasedinplasticintheformofaplaque.
8.1.1 Keeptheplastic-encasedprintedASTMOxidationCellVarnishStandards(ADJD6514)(ADJD6514 )protectedfromlight
to avoid the possibility of fading. Inspect for fading by comparing two different plaques, one of which has been carefully protected
from light (new). Observe both sets in diffuse daylight (or equivalent) first from a point directly above and then from an angle of
45°. When any evidence of fading is observed, particularly at the left-hand of the plaque, it is suggested that the one that is more
faded with respect to the other be discarded.
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, Tulsa, OK
74152.
The sole source of supply of the apparatus known to the committee at this time is Millipore Filter Corp., Bedford, MA.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of D02.09.0C on Oxidation
of Turbine Oils.
Current edition approved Dec. 1, 2008. Published February 2009. Originally approved in 2000. Last previous edition approved in 2003 as D 6514–03.
The sole source of supply of Micro known to the committee at this time is International Products Corp., P.O. Box 70, Burlington, NJ 08016.
D 6514 – 03 (2008)
8.1.1.1 Alternatively,placea20mm( ⁄4in.)opaquestrip(maskingtape)acrossthetopofthecoloredportionoftheplaquewhen
initiallypurchased.Atintervals,removetheopaquestripandobserve.Whenthereisanyevidenceoffadingoftheexposedportion,
it is suggested that the standards be replaced.
8.1.2 If the surface of the plastic cover shows excessive scratching, it is suggested that the plaque be replaced.
9. Sampling
9.1 Samples for this test can come from laboratory blends, tanks, drums, small containers, or operating equipment. Therefore,
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 will not normally be required. It is good practice to avoid undue
exposure of samples to sunlight or strong direct light. Fluid samples which are not homogeneous on visual inspection shall be
rejected and fresh samples obtained.
10. Preparation of Apparatus
10.1 Cleaning Glassware:
10.1.1 Cleannewglasswarebywashingwithahotdetergentsolution(usingabristlebrush)andrinsethoroughlywithtapwater.
If any
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
An American National Standard
Designation:D6514–02 Designation: D 6514 – 03 (Reapproved 2008)
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.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. 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.
1.3The values stated in SI units are to be regarded as standard.
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 and health practices and determine the applicability of regulatory
limitations prior to use.Identified hazardous chemicals are listed in Sections Section 7.37, 7.4 and 7.5. Before using this
standard,test method, refer to suppliers’ safety labels, Material Safety Data Sheets and other technical literature.
2. Referenced Documents
2.1 ASTM Standards:
A510 Specification for General Requirements for Wire Rods and Coarse Round Wire, Carbon Steel
B1 Specification for Hard-Drawn Copper Wire
D445 Test Method for Kinematic Viscosity of Transparent and Opaque Liquids Test Method for Kinematic Viscosity of
Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)
D664 Test Method for Acid Number of Petroleum Products by Potentiometric Titration
D943 Test Method for Oxidation Characteristics of Inhibited Mineral Oils
D974 Test Method for Acid and Base Number by Color-Indicator Titration
D3339 Test Method for Acid Number of Petroleum Products by Semi-Micro Color Indicator Titration
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4871 Guide for Universal Oxidation/Thermal Stability Test Apparatus
D5846 TestMethodforUniversalOxidationTestforHydraulicandTurbineOilsUsingtheUniversalOxidationTestApparatus
2.2 British Standards:
BS 1829 Specification for Carbon Steel, alternate to Specification A510
2.3 Institute of Petroleum Standard:
IP 2546 Practice for Sampling of Petroleum Products; Alternate to Practice D 4057
2.4 ASTM Adjunct
ASTM Oxidation Cell Varnish Standard
This standard is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of D02.09 on Oxidation of
Lubricants.
Current edition approved Apr. 10, 2002. Published June 2002. Originally published as D6514–00. Last previous edition D6514–00.
This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of D02.09.0C on Oxidation
of Turbine Oils.
Current edition approved Dec. 1, 2008. Published February 2009. Originally approved in 2000. Last previous edition approved in 2003 as D6514–03.
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM Standards
, Vol 01.03.volume information, refer to the standard’s Document Summary page on the ASTM website.
Annual Book of ASTM Standards, Vol 02.03.
Available from British Standards Institute (BSI), 389 Chiswick High Rd., London W4 4AL, U.K.
Annual Book of ASTM Standards, Vol 05.01.
Available from Institute of Petroleum (IP), 61 New Cavendish St., London, WIG 7AR, U.K.
Annual Book of ASTM Standards, Vol 05.02.
Available from ASTM International Headquarters. Order Adjunct No. ADJD6514. Names of suppliers in the United Kingdom can be obtained from the 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.
D 6514 – 03 (2008)
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 Universal Oxidation Test—the apparatus and procedures described in Guide D4871.
4. Summary of Test Method
4.1An oil sample is exposed to air at elevated temperatures in the presence of copper and iron metals. The test is run for 96 h
at155°Cafterwhichtheviscosityincrease,acidnumberincrease,andsludgegeneratedaremeasured.Thetestcellisalsowashed,
dried, and compared with the ASTM Oxidation Cell Varnish Standard.
4.1 After determining the viscosity at 40°C and acid 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 determination of the total insolubles formed during the test. Total insolubles
are reported as low, medium, or high.
4.2 The viscosity and the acid number of the filtrate are determined and compared with the initial values to ascertain any
increase in those values. Both the change in acid number and the increase in viscosity at 40°C are reported.
4.3 Theglasscellinwhichthetestspecimenwasstressedisrinsedwithheptaneanddried.Residualdepositsarecomparedwith
ASTM Adjunct ADJD6514, and the results are reported.
5. Significance and Use
5.1 Degradationoffluidlubricantsbecauseofoxidationorthermalbreakdowncanresultinfluidthickeningorintheformation
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 measurements, or as a means of estimating remaining service life. These last three
functions of the test method are expected to be fulfilled once a precision statement has been devised for the procedure. It
shouldshallberecognized,however,thatcorrelationbetweenresultsofthistestmethodandtheoxidationstabilityofanoilinfield
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.
6. Apparatus
6.1 Heating Block, as shown in Fig. 1, and as further described in Guide D4871, to provide a controlled constant temperature
for conducting the test.
6.1.1 Test cells are maintained at constant elevated temperature by means of a heated aluminum block which surrounds each
test cell.Alternate apparatus designs for sample heating and for temperature and flow control shall be acceptable, provided they
are shown to maintain temperature and gas flow within the standard’s specified limits.
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 6 5 mm.
6.2 Temperature Control System,asshownatlowerleftinFig.1,andasfurtherdescribedinGuideD4871,D4871,tomaintain
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,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:
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 full scale.
6.4 Oxidation Cell, borosilicate glass, as shown in Fig. 2, and as further described in Guide D4871.D4871. This consists of a
test cell of borosilicate glass, standard wall, 38 mm outside diameter, 300 6 5-mm length, with open end fitted with a 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.D4871. This consists of an 8-mm outside
diameter glass tube, 455 6 5 mm long, lower end with fused 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.
6.6 Basic Head, as shown in Fig. 3, and as further described in Guide D4871.D4871. This is an air condenser, with 34/45
standard-taper, ground-glass inner joint, opening for gas inlet tube, septum port for sample withdrawal, and exit tube to conduct
off-gases and entrained vapors. Overall length shall be 125 6 5 mm.
6.7 Test precision was developed using the universal oxidation/thermal stability test apparatus described in Guide
,
D4871.D4871. Alternate apparatus designs for sample heating, and for temperature and flow control shall be acceptable
provided they are shown to maintain temperature and gas flow within the specified limits.
Annual Book of ASTM Standards, Vol 05.03.
D 6514 – 03 (2008)
FIG. 1 Heating Block
6.8 Drying Oven, explosion proof. , explosion proof model recommended.
7. Reagents and Materials
7.1 Reagentgradechemicalsshallbeusedinalltests.Unlessotherwiseindicated,itisintendedthatallreagentsconformtothe
specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are
available. Other grades may be used, provided 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 Wire. Catalyst Coil (comprised of the following):
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,A510, is preferred. Similar wire conforming to
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., 1020Airpark 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.
Available from British Standards Institute, 389 Chiswick High Rd., London, W4 4AL, U.K.
If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a
meeting of the responsible technical committee , which you may attend.
Available from Institute of Petroleum, 61 New Cavendish St., London, W1G 7AR, U.K.
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.
AvailablefromASTMInternationalHeadquarters.RequestADJD6514.NamesofsuppliersintheUnitedKingdomcanbeobtainedfromtheInstituteofPetroleum.Two
master standards are held by the IP for reference.
D 6514 – 03 (2008)
FIG. 2 Oxidation Cell
FIG. 3 Basic Head
British Standard BS 1829 is also satisfactory.
7.2.2 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 B1,B1, is preferred.
7.3 Acetone, reagent grade. (Warning—Flammable. Health hazard.)
7.4 Heptane, reagent grade. (Warning—Flammable. Health hazard.)
7.5 Propan-2-ol (iso-Propyl Alcohol) , reagent grade. (Warning—Flammable. Health hazard.)
7.6 Isooctane, reagent grade. (Warning—Flammable. Health hazard.)
7.7 Abrasive Cloth, silicon carbide, 100-grit with cloth backing.
7.7Whatman Filter Paper, No. 41, 47 mm.
7.8 Whatman Filter Paper, No. 41, 47–mm diameter.
7.9 Membrane Filters, white, plain, 47 mm in diameter pore size 8 µm. Millipore SC membrane filters (MF-type, cellulose
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, Tulsa, OK
74152.
D 6514 – 03 (2008)
,
ester), or equivalent have been found satisfactory.
7.9
7.10 Air, dry with dew point temperature of −60°C. , dry.
7,11 7,12
7.11 Cleaning Reagent, either Nochromix (Warning —Health hazard. Corrosive. Harmful if inhaled) or Micro solution.
NOTE 1—Because of extreme hazards, chromic acid cleaning solution is not recommended.
8. Corrosion Standards
8.1 ASTMOxidationCellVarnishStandards(ADJD6514 )consistofreproductionsincoloroftypicaloxidationaloxidationcell
internal surfaces representing increasing degrees of staining, the reproductions being encased in plastic in the form of a plaque.
8.1.1 Keeptheplastic-encasedprintedASTMOxidationCellVarnishStandards(ADJD6514 )protectedfromlighttoavoidthe
possibility of fading. Inspect for fading by comparing two different plaques, one of which has been carefully protected from light
(new). Observe both sets in diffuse daylight (or equivalent) first from a point directly above and then from an angle of 45°.When
any evidence of fading is observed, particularly at the left-hand of the plaque, it is suggested that the one that is more faded with
respect to the other be discarded.
8.1.1.1 Alternatively,placea20mm( ⁄4in.)opaquestrip(maskingtape)acrossthetopofthecoloredportionoftheplaquewhen
initiallypurchased.Atintervals,removetheopaquestripandobserve.Whenthereisanyevidenceoffadingoftheexposedportion,
it is suggested that the standards be replaced.
8.1.2 If the surface of the plastic cover shows excessive scratching, it is suggested that the plaque be replaced.
9. Sampling
9.1 Samples for this test can come from laborat
...
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