ASTM D6514-03(2014)
(Test Method)Standard Test Method for High Temperature Universal Oxidation Test for Turbine Oils
Standard Test Method for High Temperature Universal Oxidation Test for Turbine Oils
SIGNIFICANCE AND USE
5.1 Degradation of fluid lubricants because of oxidation or thermal breakdown can result in fluid thickening or in the formation of acids or insoluble solids and render the fluid unfit for further use as a lubricant.
5.2 This test method can be used for estimating the oxidation stability of oils. It can function as a formulation screening tool, specification requirement, quality control measurement, or as a means of estimating remaining service life. It shall be recognized, however, that correlation between results of this test method and the oxidation stability of an oil in field service can vary markedly with field service conditions and with various oils.
5.3 This test method is designed to compliment Test Method D5846 and is intended for evaluation of fluids which do not degrade significantly within a reasonable period of time at 135°C.
SCOPE
1.1 This test method covers a procedure for evaluating the oxidation of inhibited lubricants in the presence of air, copper, and iron metals.
1.2 This test method was developed and is used to evaluate the high temperature oxidation stability and deposit forming tendency of oils for steam and gas turbines. It has been used for testing other lubricants made with mineral oil and synthetic basestocks for compressors, hydraulic pumps, and other applications, but these have not been used in cooperative testing.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety 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.
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Designation: D6514 − 03 (Reapproved 2014)
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, Liquid Fuels, and Lubricantsand is the direct responsibility of
D02.09.0C on Oxidation of Turbine Oils.
Current edition approved Oct. 1, 2014. Published December 2014. Originally Available from British Standards Institute (BSI), 389 Chiswick High Rd.,
approved in 2000. Last previous edition approved in 2008 as D6514 – 03 (2008). London W4 4AL, U.K.
DOI: 10.1520/D6514-03R14. 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 (2014)
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-
and for temperature and flow control shall be acceptable,
tion stability of oils. It can function as a formulation screening
provided they are shown to maintain temperature and gas flow
tool, specification requirement, quality control measurement,
within the standard’s specified limits.
or as a means of estimating remaining service life. It shall be
recognized, however, that correlation between results of this 6.1.2 Holes in the aluminum block to accommodate the test
test method and the oxidation stability of an oil in field service cells shall provide 1.0 mm maximum clearance for 38-mm
can vary markedly with field service conditions and with outside diameter glass tubes. The test cells shall fit into the
various oils. block to a depth of 225 6 5 mm.
FIG. 1 Heating Block
D6514 − 03 (2014)
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.
6.4 Oxidation Cell, borosilicate glass, as shown in Fig. 2,
andasfurtherdescribedinGuideD4871.Thisconsistsofatest
cell of borosilicate glass, standard wall, 38 mm outside
FIG. 3 Basic Head
diameter, 300 6 5-mm length, with open end fitted with a
34/45 standard-taper, ground-glass outer joint.
6,7
D4871. Alternate apparatus designs for sample heating, and
6.5 Gas Inlet Tube, as shown in Fig. 2, and as further
for temperature and flow control shall be acceptable provided
described in Guide D4871. This consists of an 8-mm outside
theyareshowntomaintaintemperatureandgasflowwithinthe
diameter glass tube, 455 6 5 mm long, lower end with fused
specified limits.
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.
6.8 Drying Oven, explosion proof model recommended.
6.6 Basic Head, as shown in Fig. 3, and as further described
7. Reagents and Materials
in Guide D4871.This is an air condenser, with 34/45 standard-
taper, ground-glass inner joint, opening for gas inlet tube,
7.1 Reagent grade chemicals shall be used in all tests.
septum port for sample withdrawal, and exit tube to conduct
Unless otherwise indicated, it is intended that all reagents
off-gases and entrained vapors. Overall length shall be 125 6
conform to the specifications of the Committee on Analytical
5 mm.
Reagents of the American Chemical Society, where such
specifications are available. Other grades may be used, pro-
6.7 Test precision was developed using the universal
vided it is first ascertained that the reagent is of sufficiently
oxidation/thermal stability test apparatus described in Guide
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
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 (2014)
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,47mmindiameterpore
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
lowing the end of a test. Drain the used oil completely. Rinse
not recommended.
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
use.
8.1 ASTM Oxidation Cell Varnish Standards (ADJD6514 )
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 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
NOTE 2—One procedure for preparing clean catalyst wire is to cut 0.50
an angle of 45°. When any evidence of fading is observed,
6 0.01 m lengths of wire. Hold one end of the wire tightly with a pair of
particularly at the left-hand of the plaque, it is suggested that
clean pliers or in a vise while cleaning with the abrasive cloth. Reverse
the one that is more faded with respect to the other be
ends of the wire and repeat.Alternatively, clean a longer length of wire (3
discarded.
to 5 m) and then cut 0.50 6 0.01 m lengths from the clean wire.
8.1.1.1 Alternatively, place a 20 mm ( ⁄4 in.) opaque strip
10.3 Preparation of Catalyst Coil
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
Designation: D6514 − 03 (Reapproved 2008) D6514 − 03 (Reapproved 2014)
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
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.
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 (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 Test Method for Universal Oxidation Test for Hydraulic and Turbine Oils Using the Universal Oxidation Test Apparatus
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 D4057
2.4 ASTM Adjunct
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 D4871.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
D02.09.0C on Oxidation of Turbine Oils.
Current edition approved Dec. 1, 2008Oct. 1, 2014. Published February 2009 December 2014. Originally approved in 2000. Last previous edition approved in 20032008
as D6514D6514 – 03 (2008).–03. DOI: 10.1520/D6514-03R08.10.1520/D6514-03R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM 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
D6514 − 03 (2014)
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 The glass cell in which the test specimen was stressed is rinsed with heptane and dried. Residual deposits are compared with
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 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 , 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:
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. 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. 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. 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
6.7 Test precision was developed using the universal oxidation/thermal stability test apparatus described in Guide 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.
6.8 Drying Oven, explosion proof model recommended.
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.
D6514 − 03 (2014)
FIG. 1 Heating Block
FIG. 2 Oxidation Cell
D6514 − 03 (2014)
FIG. 3 Basic Head
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
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, 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, 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.
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 is C & 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.
The sole source of supply of Nochromix Reagent known to the committee at this time is Godax Laboratories, 720-B Erie Ave., Takoma Park, MD 20192.
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.
D6514 − 03 (2014)
8. Corrosion Standards
8.1 ASTM Oxidation Cell Varnish Standards (ADJD6514 ) consist of reproductions in color of typical oxidation cell internal
surfaces representing increasing degrees of staining, the reproductions being encased in plastic in the form of a plaque.
8.1.1 Keep the plastic-encased printed ASTM Oxidation Cell Varnish Standards (ADJD6514 ) protected from light 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.
8.1.1.1 Alternatively, place a 20 mm ( ⁄4 in.) opaque strip (masking tape) across the top of the colored portion of the plaque when
initially purchased. At intervals, remove the opaque strip and observe. When there is any evidence of fading of the exposed portion,
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 D4057 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 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 24–h soak at room
7,11
temperature with cleaning reagent, rinse thoroughly with tap water, then distilled water and allow to dry at room temperature
or in an
...
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