ASTM D4310-98
(Test Method)Standard Test Method for Determination of the Sludging and Corrosion Tendencies of Inhibited Mineral Oils
Standard Test Method for Determination of the Sludging and Corrosion Tendencies of Inhibited Mineral Oils
SCOPE
1.1 This test method covers the tendency of inhibited mineral oil based steam turbine lubricants and mineral oil based anti-wear hydraulic oils to corrode copper catalyst metal and to form sludge during oxidation in the presence of oxygen, water, and copper and iron metals at an elevated temperature. The test method is also used for testing circulating oils having a specific gravity less than that of water and containing rust and oxidation inhibitors. Note 1-During round robin testing copper and iron in the oil, water and sludge phases were measured. However, the values for the total iron were found to be so low (that is, below 0.8 mg), that statistical analysis was inappropriate. The results of the cooperative test program are available.
1.2 This test method is a modification of Test Method D943 where the oxidation stability of the same kinds of oils is determined by following the acid number of oil. The number of test hours required for the oil to reach an acid number of 2.0 mg KOH/g is the oxidation lifetime .
1.3 The values stated in acceptable metric units are to be regarded as the 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. For specific precautionary statements, see 7.3, 7.4, 7.5, 7.6, 7.7, 7.10, and X1.15.
General Information
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Standards Content (Sample)
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An American National Standard
Designation: D 4310 – 98
Standard Test Method for
Determination of the Sludging and Corrosion Tendencies of
Inhibited Mineral Oils
This standard is issued under the fixed designation D 4310; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope D 329 Specification for Acetone
D 770 Specification for Isopropyl Alcohol
1.1 This test method is used to evaluate the tendency of
D 874 Test Method for Sulfated Ash from Lubricating Oils
inhibited mineral oil based steam turbine lubricants and min-
and Additives
eral oil based anti-wear hydraulic oils to corrode copper
D 943 Test Method for Oxidation Characterististics of In-
catalyst metal and to form sludge during oxidation in the
hibited Mineral Oils
presence of oxygen, water, and copper and iron metals at an
D 1193 Specification for Reagent Water
elevated temperature. The test method is also used for testing
D 4057 Practice for Manual Sampling of Petroleum and
circulating oils having a specific gravity less than that of water
Petroleum Products
and containing rust and oxidation inhibitors.
E 1 Specification for ASTM Thermometers
NOTE 1—During round robin testing copper and iron in the oil, water 10
2.2 IP Standard:
and sludge phases were measured. However, the values for the total iron
Specification for IP Standard Thermometers
were found to be so low (that is, below 0.8 mg), that statistical analysis
2.3 British Standard:
was inappropriate. The results of the cooperative test program are
BS 1829
available.
1.2 This test method is a modification of Test Method D 943
3. Terminology
where the oxidation stability of the same kinds of oils is
3.1 Definition:
determined by following the acid number of oil. The number of
3.1.1 sludge—a precipitate or sediment from oxidized min-
test hours required for the oil to reach an acid number of 2.0
eral oil and water.
mg KOH/g is the oxidation lifetime.
1.3 The values stated in acceptable metric units are to be
4. Summary of Test Method
regarded as the standard.
4.1 An oil sample is contacted with oxygen in the presence
1.4 This standard does not purport to address all of the
of water and an iron-copper catalyst at 95°C for 1000 h. The
safety concerns, if any, associated with its use. It is the
weight of insoluble material is determined gravimetrically by
responsibility of the user of this standard to establish appro-
filtration of the oxidation tube contents through 5-μm pore size
priate safety and health practices and determine the applica-
filter disks. The total amount of copper in the oil, water, and
bility of regulatory limitations prior to use. For specific
sludge phases is also determined.
precautionary statements, see Section 7 and X1.1.5.
NOTE 2—Optionally, some operators may choose to: (a) assess the
2. Referenced Documents
change in weight of the catalyst coil, or (b) determine the acid number at
1000 h, or both. The acid number may serve as a criterion to determine if
2.1 ASTM Standards:
measurement of insoluble material is warranted. Normally, further testing
A 510 Specification for General Requirements for Wire
is not recommended on a highly oxidized oil (that is an oil which has
Rods and Coarse Round Wire, Carbon Steel
attained an acid number >2.0 mg KOH/gm). Instructions for these optional
B 1 Specification for Hard-Drawn Copper Wire
1 5
This test method is under the jurisdiction of ASTM Committee D-2 on Annual Book of ASTM Standards, Vol 06.04.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Annual Book of ASTM Standards, Vol 05.01.
D02.09 on Oxidation. Annual Book of ASTM Standards, Vol 11.01.
Current edition approved June 10, 1998. Published October 1998. Originally Annual Book of ASTM Standards, Vol 05.02.
published as D 4310 – 83. Last previous edition D 4310 – 95. Annual Book of ASTM Standards, Vol 14.03.
2 10
Available from ASTM Headquarters. Request RR: D02-1291 issued July 14, Available from The Institute of Petroleum, 61 New Cavendish St., London
1992. WIM, 8AR, England.
3 11
Annual Book of ASTM Standards, Vol 01.03. Available from British Standards Institute, 2 Park St., London, England
Annual Book of ASTM Standards, Vol 02.03. WIA285.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D4310–98
tests are not included in this test method.
consisting of a test tube, condenser, and oxygen delivery tube.
The test tube has a calibration line at 300 mL (maximum error
5. Significance and Use
1 mL). This calibration applies to the test tube without inserts
5.1 Insoluble material may form in oils that are subjected to
at 20°C.
oxidizing conditions.
6.2 Heating Bath, thermostatically controlled, capable of
5.2 Significant formation of oil insolubles or metal corro-
maintaining the oil sample in the oxidation cell at a tempera-
sion products, or both, during this test may indicate that the oil
ture of 95 6 0.2°C, fitted with a suitable stirring device to
will form insolubles or corrode metals, or both, during field
provide a uniform temperature throughout the bath, and large
service. However, no correlation with field service has been
enough to hold the desired number of oxidation cells immersed
established.
in the heating bath to a depth of 390 6 10 mm and in the
6. Apparatus
heating liquid itself to a depth of 355 6 10 mm.
6.1 Oxidation Cell, of borosilicate glass, as shown in Fig. 1,
All dimensions are in millimetres (inches)
NOTE 1—The oxidation test tube has a calibration line at 300 ml. This calibration applies to the test tube alone at 20°C.
NOTE 2—Open tube ends to be ground and fire-polished.
FIG. 1 Oxidation Cell
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
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D4310–98
6.2.1 Studies have suggested that direct sunlight or artificial 6.12 Weighing Bottle, cylindrical body with ground-glass
light may adversely influence the results of this test. To stopper; approximate inside diameter 45 mm, height of body
minimize effects of light exposure on the lubricant being 65 mm, capacity 60 mL.
tested, light shall be excluded from the lubricant by one or 6.13 Vacuum Source, to provide pressure reduction to 13.3
more of the following ways: 6 0.7 kPa (100 6 5 mm Hg) absolute pressure.
6.14 Cooling Vessel—A desiccator or other type of tightly
6.2.1.1 Use of heated liquid baths that are designed and
covered vessel for cooling the weighing vessels before weigh-
constructed of metal, or combinations of metals and other
ing. The use of a drying agent is not recommended.
suitable opaque materials, that prevent light from entering the
6.15 Drying Oven, capable of maintaining a temperature of
test cell from the sides is preferred. If a viewing window is
105 6 2°C.
included in the design, this viewing window shall be fitted with
6.16 Forceps, having unserrated tips.
a suitable opaque cover and be kept closed when no observa-
6.17 Syringe, 50-mL Luer-Lok with 12-in. needle.
tion is being made.
6.18 Separatory Funnels, with a capacity of 1000 mL.
6.2.1.2 If glass heating baths are used, the bath shall be
6.19 Rubber Policeman.
wrapped with aluminum foil or other opaque material.
6.2.1.3 Bright light entering the test cell from directly
7. Reagents and Materials
overhead can be eliminated by use of an opaque shield.
7.1 Purity of Reagents—Reagent grade chemicals shall be
6.3 Flowmeter, with a flow capacity of at least 3 L of
used in all tests. Unless otherwise indicated, it is intended that
oxygen/hour, and an accuracy of 60.1 L/h.
all reagents conform to the specifications of the Committee on
6.4 Heating Bath Thermometer—ASTM Solvents Distilla-
Analytical Reagents of the American Chemical Society where
tion Thermometer having a range from 72 to 126°C and
such specifications are available. Other grades may be used,
conforming to the requirements for Thermometer 40C as
provided it is first ascertained that the reagent is of sufficiently
prescribed in Specification E 1, or for Thermometer 70C as
high purity to permit its use without lessening the accuracy of
prescribed in Specifications for IP Standard Thermometers.
the determination.
Alternatively, temperature–measuring devices of equal or bet-
7.2 Purity of Water—Unless otherwise indicated, references
ter accuracy may be used.
to water shall be understood to mean reagent water as defined
6.5 Oxidation Cell Thermometer, having a range from 80
by Type II of Specification D 1193.
to 100°C, graduated in 0.1°C, total length—250 mm, stem
7.3 Acetone (Warning—Health hazard, flammable.),
diameter—6.0 to 7.0 mm, calibrated for 76-mm immersion.
99.5 % Grade, conforming to Specification D 329.
6.6 Wire Coiling Mandrel, as shown in Fig. 2 .
7.4 Cleaning Reagent, cleaning by a 24-h soak at room
temperature in either Nochromix (Warning—Corrosive,
6.7 Thermometer Bracket, for holding the oxidation cell
health hazard) or in Micro solution.
thermometer, of 18-8 stainless steel, having the dimensions
7.5 n-Heptane, Reagent grade. (Warning—Flammable.
shown in Fig. 3 . The thermometer is held in the bracket by two
Harmful if inhaled.)
fluoro-elastomer O-rings of approximately 5-mm inside diam-
7.6 Hydrochloric Acid (Warning—Toxic and corrosive.),
eter. Alternatively, thin stainless steel wire may be used.
concentrated [(36 mass % (relative density 1.19)].
6.8 Abrasive Cloth, silicon carbide, 100-grit with cloth
7.7 Isopropyl Alcohol (Warning—Flammable.), conform-
backing.
ing to Specification D 770.
6.9 Flexible Tubing, poly vinyl chloride approximately 6.4-
7.8 Catalyst Wires:
1 3
mm ( ⁄4-in.) inside diameter with a ⁄32-in. wall for delivery of
7.8.1 Low-Metalloid Steel Wire, 1.59 mm (0.0625 in.) in
oxygen to the oxidation cell.
diameter (No. 16 Washburn and Moen Gage).
6.10 Membrane Filters, white, plain, 47 mm in diameter,
7.8.2 Electrolytic Copper Wire, 1.63 mm (0.064 in.) in
pore size 5 μm.
diameter (No. 16 Imperial Standard Wire Gage or No. 14
6.11 Filter Holder, 47 mm, consisting of a borosilicate
glass funnel and a funnel base with a coarse grade (40 to
60-μm) fritted-glass filter support or stainless steel screen
Fisher 3-415 weighing bottle, size G, available from Fisher Scientific Co.,
support such that the filter can be clamped between the
Pittsburgh, PA., or equivalent, has been found satisfactory for this purpose.
ground-glass sealing surfaces of the funnel and its base by Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
means of a metal clamp.
listed by the American Chemical Society, see Analar 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.
12 18
A summary of the results of these studies is available from ASTM Headquar- Nochromix is available from Godax Laboratories, Inc., 720-B Erie Avenue,
ters. Request RR:D02-1365. Takoma Park, MD 20912.
13 19
Brooklyn Thermometer No. 21276-RM, available from Brooklyn Thermom- Micro is available from International Products Corp., P.O. Box 70, Burlington,
eter Co., Farmingdale, NY, or equivalent has been found satisfactory for this NJ 08016.
purpose. Carbon steel wire, soft bright annealed and free from rust of Grade 1008 as
Millipore SM membrane filters (MF-type, cellulose esters), available from described in Specification A 510 is satisfactory. Similar wire conforming to BS1829,
Millipore Filter Corp., Bedford MA, or equivalent have been found satisfactory. is also satisfactory. If these steels are not available, other equivalent steels may be
Millipore Pyrex XX-10-047-00 or XX-10-047-30 filter holder, available from used, provided they are found to be satisfactory in comparative tests using this Test
Millipore Filter Corp., or equivalent have been found satisfactory for this purpose. Method D 4310.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D4310–98
American Wire Gage), 99.9 % purity, conforming to Specifi- 7.9 Detergent, water-soluble.
cation B 1. Soft copper wire of an equivalent grade may also be 7.10 Oxygen—(Warning—Oxygen vigorously accelerates
used. combustion) 99.5 % minimum purity, with pressure regulation
NOTE 3—Alternatively, suitably prepared catalyst coils may be pur-
chased from a supplier. Alconox has been found satisfactory for this purpose.
FIG. 2 Mandrel for Winding Catalyst Coils
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D4310–98
All dimensions are in millimetres (inches).
Material: 18-8 Stainless Steel. 22 Gage (0.792 mm).
FIG. 3 Thermometer Bracket
adequate to maintain a constant flow of gas through the equal length of copper wire with wads of absorbent cotton wet
apparatus. The use of a two-stage pressure regulator on tank with n-heptane and follow by abrasion with abrasive cloth until
oxygen is recommended.
a fresh metal surface is exposed. Then wipe with dry absorbent
cotton until all loose particles of metal and abrasive have been
8. Sampling
removed. In subsequent operations handle the catalyst wires
8.1 Samples for this test can come from tanks, drums, small
with clean gloves (cotton, rubber, or plastic) to prevent contact
containers, or even operating equipment. Therefore, use the
with the skin.
applicable apparatus and techniques described in Test Method
9.2 Preparation of Catalyst Coil—Twist the iron and copper
D 4057.
wires tightly together at one end for three turns and then wind
8.2 For one single determination the minimum required
them simultaneously alongside each other on a threaded
sample size is 300 mL.
mandrel (see Fig. 2), inserting the iron wire in the deeper
9. Preparation of Apparatus thread. Remove the coil from the mandrel, twist the free ends
of the iron and copper wires together for three turns, and bend
9.1 Cleaning
...
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