ASTM D4310-10(2015)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4310 − 10 (Reapproved 2015)
Standard Test Method for
Determination of Sludging and Corrosion Tendencies of
Inhibited Mineral Oils
This standard is issued under the fixed designation D4310; 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 tional information. Users should be aware that selling mercury
and/or mercury containing products into your state or country
1.1 This test method covers and is used to evaluate the
may be prohibited by law.
tendency of inhibited mineral oil based steam turbine lubri-
1.6 This standard does not purport to address all of the
cants and mineral oil based anti-wear hydraulic oils to corrode
safety concerns, if any, associated with its use. It is the
copper catalyst metal and to form sludge during oxidation in
responsibility of the user of this standard to establish appro-
thepresenceofoxygen,water,andcopperandironmetalsatan
priate safety and health practices and determine the applica-
elevated temperature. The test method is also used for testing
bility of regulatory limitations prior to use. For specific
circulating oils having a specific gravity less than that of water
warning statements, see Section 7 and X1.1.5.
and containing rust and oxidation inhibitors.
NOTE 1—During round robin testing copper and iron in the oil, water
2. Referenced Documents
and sludge phases were measured. However, the values for the total iron
2.1 ASTM Standards:
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 A510 Specification for General Requirements forWire Rods
available (see Section 16).
and Coarse Round Wire, Carbon Steel
B1 Specification for Hard-Drawn Copper Wire
1.2 This test method is a modification of Test Method D943
D664 Test Method for Acid Number of Petroleum Products
where the oxidation stability of the same kinds of oils is
by Potentiometric Titration
determinedbyfollowingtheacidnumberofoil.Thenumberof
D874 Test Method for Sulfated Ash from Lubricating Oils
test hours required for the oil to reach an acid number of
and Additives
2.0 mg KOH/g is the oxidation lifetime.
D943 Test Method for Oxidation Characteristics of Inhibited
1.3 Procedure A of this test method requires the determina-
Mineral Oils
tion and report of the weight of the sludge and the total amount
D1193 Specification for Reagent Water
of copper in the oil, water, and sludge phases. Procedure B
D3339 Test Method forAcid Number of Petroleum Products
requires the sludge determination only. The acid number
by Semi-Micro Color Indicator Titration
determination is optional for both procedures.
D4057 Practice for Manual Sampling of Petroleum and
1.4 The values stated in SI units are to be regarded as
Petroleum Products
standard. No other units of measurement are included in this
E1 Specification for ASTM Liquid-in-Glass Thermometers
standard.
2.2 Energy Institute Standard:
Specification for IP Standard Thermometers
1.5 WARNING—Mercury has been designated by many
2.3 British Standard:
regulatory agencies as a hazardous material that can cause
BS 1829 Reference Tables for Iron v. Constantan Thermo-
central nervous system, kidney and liver damage. Mercury, or
couples
its vapor, may be hazardous to health and corrosive to
materials.Cautionshouldbetakenwhenhandlingmercuryand
3. Terminology
mercury containing products. See the applicable product Ma-
3.1 Definitions:
terial Safety Data Sheet (MSDS) for details and EPA’s
website—http://www.epa.gov/mercury/faq.htm—for addi-
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
This test method is under the jurisdiction of ASTM Committee D02 on Standards volume information, refer to the standard’s Document Summary page on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of the ASTM website.
Subcommittee D02.09.0C on Oxidation of Turbine Oils. Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR,
Current edition approved Oct. 1, 2015. Published December 2015. Originally U.K., http://www.energyinst.org.
approved in 1983. Last previous edition approved in 2010 as D4310 – 10. DOI: Available from British Standards Institution (BSI), 389 Chiswick High Rd.,
10.1520/D4310-10R15. London W4 4AL, U.K., http://www.bsigroup.com.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4310 − 10 (2015)
3.1.1 sludge—a precipitate or sediment from oxidized min- included in the design, this viewing window shall be fitted with
eral oil and water. a suitable opaque cover and be kept closed when no observa-
tion is being made.
4. Summary of Test Method 6.2.1.2 If glass heating baths are used, the bath shall be
wrapped with aluminum foil or other opaque material.
4.1 An oil sample is contacted with oxygen in the presence
6.2.1.3 Bright light entering the test cell from directly
of water and an iron-copper catalyst at 95 °C for 1000 h. The
overhead can be eliminated by use of an opaque shield.
weight of insoluble material is determined gravimetrically by
filtration of the oxidation tube contents through 5 µm pore size 6.3 Flowmeter, with a flow capacity of at least 3 L of
filter disks. The total amount of copper in the oil, water, and oxygen/hour, and an accuracy of 60.1 L⁄h.
sludge phases is also determined for ProcedureA. Procedure B
6.4 Heating Bath Thermometer—ASTM Solvents Distilla-
requires the sludge determination. The copper determination is
tion Thermometer having a range from 72 °C to 126°C and
not required. The acid number determination is optional for
conforming to the requirements for Thermometer 40C as
both procedures.
prescribed in Specification E1, or for Thermometer 70C as
prescribed in Specifications for IP Standard Thermometers.
NOTE 2—Optionally, some operators may choose to: (1) assess the
change in weight of the catalyst coil, or (2 ) determine the acid number at
Alternatively, temperature–measuring devices of equal or bet-
1000 h, or both. The acid number may serve as a criterion to determine if
ter accuracy may be used.
measurement of insoluble material is warranted. Normally, further testing
is not recommended on a highly oxidized oil (that is an oil which has 6.5 Oxidation Cell Thermometer,havingarangefrom80 °C
attained an acid number >2.0 mg KOH/g). Instructions for these optional
to 100 °C, graduated in 0.1 °C, total length—250 mm, stem
tests are not included in this test method.
diameter—6.0 mm to 7.0 mm, calibrated for 76 mm immer-
sion. Temperature measuring devices such as liquid-in-glass
5. Significance and Use
thermometers, thermocouples, or platinum resistance ther-
5.1 Insoluble material may form in oils that are subjected to mometers that provide equivalent or better accuracy and
oxidizing conditions.
precision that cover the temperature range, may be used.
5.2 Significant formation of oil insolubles or metal corro-
6.6 Wire Coiling Mandrel, as shown in Fig. 2.
sion products, or both, during this test may indicate that the oil
6.7 Thermometer Bracket, for holding the oxidation cell
will form insolubles or corrode metals, or both, during field
thermometer, of 18-8 stainless steel, having the dimensions
service. However, no correlation with field service has been
shown in Fig. 3.The thermometer is held in the bracket by two
established.
fluoro-elastomer O-rings of approximately 5 mm inside diam-
eter. Alternatively, thin stainless steel wire may be used.
6. Apparatus
6.8 Abrasive Cloth, silicon carbide, 100-grit with cloth
6.1 Oxidation Cell, of borosilicate glass, as shown in Fig. 1,
backing.
consisting of a test tube, condenser, and oxygen delivery tube.
6.9 Flexible Tubing, poly vinyl chloride approximately
The test tube has a calibration line at 300 mL (maximum error
1 3
6.4 mm ( ⁄4 in.) inside diameter with a ⁄32 in. wall for delivery
1 mL). This calibration applies to the test tube without inserts
of oxygen to the oxidation cell.
at 20 °C.
6,7
6.10 Membrane Filters, white,plain,47 mmor90 mmin
6.2 Heating Bath: Liquid Bath or Metal Block, thermostati-
diameter, pore size 5 µm.
cally controlled, capable of maintaining the oil sample in the
6,8
oxidation cell at a temperature of 95 °C 6 0.2 °C, fitted with a
6.11 Filter Holder, 47 mm or 90 mm, consisting of a
suitable stirring device to provide a uniform temperature
borosilicate glass funnel and a funnel base with a coarse grade
throughout the bath, and large enough to hold the desired
(40 µm to 60 µm) fritted-glass filter support or stainless steel
number of oxidation cells immersed in the heating bath to a
screen support such that the filter can be clamped between the
depth of 390 mm 6 10 mm and in the heating liquid itself to a
ground-glass sealing surfaces of the funnel and its base by
depth of 355 mm 6 10 mm.
means of a metal clamp.
6.2.1 Studies have suggested that direct sunlight or artificial
6,9
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
more of the following ways:
6.2.1.1 Use of heated liquid baths that are designed and If you are aware of alternative suppliers, please provide this information to
ASTM International Headquarters. Your comments will receive careful consider-
constructed of metal, or combinations of metals and other
ation at a meeting of the responsible technical committee, which you may attend.
suitable opaque materials, that prevent light from entering the
The sole source of supply of the Millipore SM membrane filters (MF-type,
test cell from the sides is preferred. If a viewing window is
cellulose esters) known to the committee at this time is Millipore Filter Corp.,
Bedford, MA.
The sole source of supply of the Millipore Pyrex XX-10-047-00 or XX-10-
047-30 filter holder known to the committee at this time is Millipore Filter Corp.,
Supporting data (summary of the results of these studies) have been filed at Bedford, MA.
ASTM International Headquarters and may be obtained by requesting Research The sole source of supply of the Fisher 3-415 weighing bottle, size G, known
Report RR:D02-1365. to the committee at this time is Fisher Scientific Co., Pittsburgh, PA.
D4310 − 10 (2015)
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
6.13 Vacuum Source, to provide pressure reduction to 6.19 Rubber Policeman.
13.3 kPa 6 0.7 kPa (100 mm 6 5 mm Hg) absolute pressure.
6.20 Pipette Bulb.
6.14 Cooling Vessel—A desiccator or other type of tightly
6.21 Syringe, glass or plastic, with Luer-Lok locking
covered vessel for cooling the weighing vessels before weigh-
connector, 10 mL capacity for sampling.
ing. The use of a drying agent is not recommended.
6.15 Drying Oven, capable of maintaining a temperature of 6.22 Syringe Sampling Tube, Grade 304 stainless steel
105 °C 6 2 °C.
tubing, 2.11 mm (0.083 in.) outside diameter, 1.60 mm
(0.063 in.) inside diameter, 559 mm 6 2 mm (24.0 in. 6
6.16 Forceps, having unserrated tips.
0.08 in.) long, with one end finished at 90° and the other end
6.17 Syringe, 50 mL Luer-Lok with 12 in. needle.
fitted with a Luer-Lok female connector.
6.18 Separatory Funnels, with a capacity of 1000 mL.
D4310 − 10 (2015)
FIG. 2 Mandrel for Winding Catalyst Coils
D4310 − 10 (2015)
All dimensions are in millimetres (inches).
Material: 18-8 Stainless Steel. 22 Gauge (0.792 mm).
FIG. 3 Thermometer Bracket
7. Reagents and Materials provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
7.1 Purity of Reagents—Reagent grade chemicals shall be
the determination.
used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specifications of the Committee on
7.2 Purity of Water—Unless otherwise indicated, references
Analytical Reagents of the American Chemical Society where
to water shall be understood to mean reagent water as defined
such specifications are available. Other grades may be used,
by Type II of Specification D1193.
7.3 Acetone—Reagent grade. (Warning—Health hazard,
Reagent Chemicals, American Chemical Society Specifications, American
flammable.)
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.
D4310 − 10 (2015)
7.4 Cleaning Reagent, cleaning by a 24 h soak at room 9.2 Preparation of Catalyst Coil—Twist the iron and copper
6,11
temperature in either Nochromix (Warning—Corrosive, wires tightly together at one end for three turns and then wind
6,12
health hazard) or in Micro solution. them simultaneously alongside each other on a threaded
mandrel (see Fig. 2), inserting the iron wire in the deeper
7.5 n-heptane, Reagent grade. (Warning—Flammable.
thread. Remove the coil from the mandrel, twist the free ends
Harmful if inhaled.)
of the iron and copper wires together for three turns, and bend
7.6 Hydrochloric Acid (Warning—Toxic and corrosive.),
the twisted ends to conform to the shape of the spiral coil. The
concentrated [(36 mass % (relative density 1.19)].
overall length of the finished coil should be 225 mm 65mm
(8.9 in. 6 0.2 in.). If necessary, the coil may be stretched to
7.7 Isopropyl Alcohol—Reagent grade. (Warning—
Flammable.) give the required length (Note 4 and Note 5).
7.8 Catalyst Wires:
NOTE 5—The finished catalyst coil is a double spiral of copper and iron
7.8.1 Low-Metalloid Steel Wire, 1.59 mm (0.0625 in.) in wire, 225 mm 6 5 mm (8.9 in. 6 0.2 in.) overall length and 15.9 mm to
16.5 mm (0.625 in. to 0.650 in.) inside diameter. The turns of wire are
diameter (No. 16 Washburn and Moen Gauge).
evenly spaced, and two consecutive turns of
...