ASTM D4636-99(2004)e1

Standard Test Method for Corrosiveness and Oxidation Stability of Hydraulic Oils, Aircraft Turbine Engine Lubricants, and Other Highly Refined Oils

SIGNIFICANCE AND USE
This test method simulates the environment encountered by fully formulated lubricating fluids in actual service and uses an accelerated oxidation rate to permit measurable results to be obtained in a reasonable time. The use of metals provides catalytic reactive surfaces of those materials commonly found in real systems. The high temperature and air agitation help accelerate the oxidation reactions that are expected to occur. Moisture in the air adds another realistic condition that encourages oil breakdown by facilitating acid formation.
Interpretation of results should be done by comparison with data from oils of known field performance. The accelerated conditions likely will cause one or more of the following measurable effects: mass change and corroded appearance of some metals; change of viscosity; increase in acid number; measurable reaction products in the form of sludge; and mass loss of oil due to evaporation.
This test method is most suitable for oils containing oxidation and corrosion inhibitors. Without such ingredient(s), the severe test conditions will yield rather drastic changes to the oil.
SCOPE
1.1 This test method covers the testing of hydraulic oils, aircraft turbine engine lubricants, and other highly refined oils to determine their resistance to oxidation and corrosion degradation and their tendency to corrode various metals. Petroleum and synthetic fluids may be evaluated using moist or dry air with or without metal test specimens.
1.2 This test method consists of a standard test procedure, an alternative Procedure 1, and an alternative Procedure 2. As there are variations possible with this test method, it will be up to the particular specification to establish the conditions required. In addition to temperature, the variables to specify if other than those of the standard procedure or alternative Procedure 1 or 2 are: test time, air flow and humidity, sample frequency, test fluid quantity, and metal specimen(s).
1.3 The values stated in SI units are to be regarded as standard. The values in parentheses are for information only.
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.

General Information

• Status: Historical
• Publication Date: 30-Apr-2004
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.09.0D - Oxidation of Lubricants

Relations

• Replaces: ASTM D4636-99 - Standard Test Method for Corrosiveness and Oxidation Stability of Hydraulic Oils, Aircraft Turbine Engine Lubricants, and Other Highly Refined Oils
• Effective Date: 01-May-2004

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.
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Designation: D4636 – 99 (Reapproved 2004)
Standard Test Method for
Corrosiveness and Oxidation Stability of Hydraulic Oils,
Aircraft Turbine Engine Lubricants, and Other Highly
Refined Oils
This standard is issued under the fixed designation D4636; 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.
This standard has been approved for use by agencies of the Department of Defense.
´ NOTE—Warning notes were editorially moved into the standard text in May 2004.
INTRODUCTION
This test method is the result of combining Federal Test Methods 5307.2 and 5308.7. Features and
detailsofbothofthesetestmethodsareincluded,butthenewtestmethodisbasicallyMethod5307.2
expanded to include Method5308.7.
1. Scope 2. Referenced Documents
1.1 This test method covers the testing of hydraulic oils, 2.1 ASTM Standards:
aircraft turbine engine lubricants, and other highly refined oils D91 Test Method for Precipitation Number of Lubricating
to determine their resistance to oxidation and corrosion degra- Oils
dationandtheirtendencytocorrodevariousmetals.Petroleum D445 Test Method for Kinematic Viscosity of Transparent
and synthetic fluids may be evaluated using moist or dry air and Opaque Liquids (and Calculation of Dynamic Viscos-
with or without metal test specimens. ity)
1.2 This test method consists of a standard test procedure, D664 Test Method forAcid Number of Petroleum Products
an alternative Procedure 1, and an alternative Procedure 2.As by Potentiometric Titration
therearevariationspossiblewiththistestmethod,itwillbeup D1193 Specification for Reagent Water
to the particular specification to establish the conditions D3339 Test Method for Acid Number of Petroleum Prod-
required. In addition to temperature, the variables to specify if ucts by Semi-Micro Color Indicator Titration
other than those of the standard procedure or alternative 2.2 U.S. Federal Test Method Standards:
Procedure 1 or 2 are: test time, air flow and humidity, sample Method5307.2 Corrosiveness and Oxidation Stability of
frequency, test fluid quantity, and metal specimen(s). Aircraft Turbine Engine Lubricants
1.3 The values stated in SI units are to be regarded as Method5308.7 Corrosiveness and Oxidation Stability of
standard. The values in parentheses are for information only. Light Oils (Metal Squares)
1.4 This standard does not purport to address all of the MIL-S-13282 Refined Silver (99.95) (P07015)
safety concerns, if any, associated with its use. It is the 2.3 Other Standards:
responsibility of the user of this standard to establish appro- AMS 4616 Silicon Iron Bronze (C65900)
priate safety and health practices and determine the applica- AMS 4908 TitaniumAlloy—(8% Mn)Annealed (R56080)
bility of regulatory limitations prior to use. AMS 6490 Steel (M50) (T11350)
QQ-A-671 Cadmium Anod (L01900)
QQ-C-576 Copper Electrolytic Tough Pitch (ETP)
(C11000)
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method is under the jurisdiction of ASTM Committee D02 on contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee Standards volume information, refer to the standard’s Document Summary page on
D02.09.0D on Oxidation of Lubricants. the ASTM website.
Current edition approved May 17, 2004. Published May 2004. Originally AvailablefromStandardizationDocumentsOrderDesk,Bldg.4SectionD,700
approved in 1986. Withdrawn 1994 and reinstated January 1997. Last previous Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
edition approved in 1999 as D4636–99. DOI: 10.1520/D4636-99R04E01. See ASTM DS56, Metal and Alloys in the Unified Numbering System.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D4636 – 99 (2004)
QQ-M-44 MagnesiumAlloyAZ31B Condition H24 or H26 accelerate the oxidation reactions that are expected to occur.
(M11311) Moisture in the air adds another realistic condition that
QQ-S-698 Low-Carbon Steel 1010, CR Temper No. 4 or 5 encourages oil breakdown by facilitating acid formation.
(G10100) 4.2 Interpretation of results should be done by comparison
QQ-A-250/4 Aluminum Alloy 2024 T-3 or T-4 (A92024) with data from oils of known field performance. The acceler-
ated conditions likely will cause one or more of the following
3. Summary of Test Method
measurable effects: mass change and corroded appearance of
3.1 This test method consists of a standard test procedure some metals; change of viscosity; increase in acid number;
measurable reaction products in the form of sludge; and mass
(see 10.1), an alternative Procedure 1 (see 10.2), and an
alternative Procedure 2 (see 10.3).The standard test procedure loss of oil due to evaporation.
4.3 This test method is most suitable for oils containing
uses washer-shaped metal specimens stacked on the air tube,
200 mL of test oil, 10 L/h air flow rate, and periodic test oil oxidation and corrosion inhibitors. Without such ingredient(s),
the severe test conditions will yield rather drastic changes to
withdrawal and evaluation. Alternative Procedure 1 uses
washer-shaped metal specimens, 165 mLof test oil, 10 L/h air the oil.
flow rate, and no periodic test oil sampling. Alternative
5. Apparatus
Procedure 2 uses square metal specimens tied together resting
5.1 The main apparatus consists of the following items of
vertically in the large glass tube, 100 mL of test oil, 5 L/h air
standard wall borosilicate glassware as shown in Figs. 1-5:
flow rate, and no periodic test oil sampling.
5.1.1 Main Sample Tube (Fig. 1).
NOTE 1—Flow rates other than those listed in this test method may be
5.1.2 Sample Tube Head (Fig. 2).
required by various specifications; if they are so used, the modification to
the test method should be stated in the test report.
3.2 Alarge glass tube containing a sample of oil and metal
specimens is placed in a constant temperature bath and heated
for the specified number of hours while air is passed through
the oil to provide agitation and a source of oxygen. Typically,
temperaturesofthebathusedarefrom100°C(212°F)to360°C
(680°F). Weighed metal specimens are placed in the tube
during the test. Corrosiveness of the oil is determined by loss
in metal mass, and microscopic examination of the sample
metal surface(s). Oil samples are withdrawn from the test oil
and checked for changes in viscosity and acid number as a
result of the oxidation reactions.
3.3 MetalsusedinthebasictestandalternativeProcedure1
are titanium, magnesium, steel (two types), bronze, silver, and
aluminum. Metals used in alternative Procedure 2 are copper,
steel, aluminum, magnesium, and cadmium. Other metals may
be specified.
3.4 Sampling of the oil for analysis is done periodically
throughout the test. Alternatively, no periodic samples are
taken and a final viscosity and acid number are determined for
comparison with those of the original untested oil.
3.5 At the end of the test, the amount of sludge present in
the oil remaining in the same tube is determined by centrifu-
gation. Also, the quantity of oil lost during the test is
determined gravimetrically.
3.6 Airisuseddryinthestandardtest.Ahumidifiermaybe
used to provide controlled moist air, if required.
4. Significance and Use
4.1 Thistestmethodsimulatestheenvironmentencountered
byfullyformulatedlubricatingfluidsinactualserviceanduses
anacceleratedoxidationratetopermitmeasurableresultstobe
obtained in a reasonable time. The use of metals provides
catalytic reactive surfaces of those materials commonly found
in real systems. The high temperature and air agitation help
FIG. 1 Sample Tube
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D4636 – 99 (2004)
FIG. 2 Sample Tube Head
5.1.3 Air Tube (Fig. 3). exposedhotsurfacesonapparatus.Avoidcontactwithexposed
5.1.4 Condenser, Allihn Type (Fig. 4). skin by use of protective equipment as required.)
5.1.5 Condenser, Allihn Type, Fig. 4 with 71/60 joint.
5.3.2 Hood, ventilation to adequately remove fumes during
5.1.6 Assembled Apparatus (Fig. 5).
heating.
5.2 Additional glassware items and assembly accessories
5.3.3 Air Supply, free of reactive contaminants. For dry air,
needed are:
dew point is −68°C (−90°F) maximum; for moist air, moisture
5.2.1 Spacers (for Metal Specimen), of borosilicate glass,
is 10 6 1 mg water/L air, standard conditions of 21°C
standard wall, 9-mm outside diameter, 6-mm length.
(70°F)/105 kPa (1 atm).
5.2.2 Oil Sampling Tube, Borosilicate Glass, 4-mm outside
5.3.4 Flowmeter, capable of measuring 10 6 1 L/h at same
diameter, with sampling end approximately 600 mm to reach
standard conditions as in 5.3.3.
into the main sample tube. The tube is bent U-shape with exit
5.3.5 Balance, analytical, sensitivity 0.1 mg.
end fitted by a one-hole stopper to a 25-mLfiltering flask.The
5.3.6 Balance, Laboratory, 2500-g capacity, 0.1-g sensitiv-
exit end may be any convenient length.
ity.
5.2.3 Adapter, polytetrafluoroethylene for 10/18 joint for
5.3.7 Centrifuge, capable of relative force of 840 6 40
sealing of air tube to sample tube head.
relative centrifugal force at the tip of the tubes.
5.3 Other items and equipment are:
5.3.8 Centrifuge Tubes,TestMethodD91,cone-shaped,100
5.3.1 Heating Bath, constant temperature within 60.5°C
mL.
(61°F) of test temperature with an immersion depth of 250 6
20 mm. Oil baths or aluminum block baths are recommended,
5.3.9 Microscope, with 20-diameter magnification.
but above 220°C (428°F), use aluminum block bath or other
5.3.10 Assembly Fixture, wood (slotted to hold metal
similar non-oil-type heating medium. (Warning—There are
squares for tying with cord) as shown in Fig. 6.
5.3.11 Cord or Wire, for tying metal squares together.
Suitable cord should be lightweight of cleaned linen, cotton,
An800-mmairtubemaybeusedforalternateProcedure1or2whenusingthe
condenser as opposed to the sample tube head in the standard procedure. nylon, or ceramic fiber; suitable wire is nichrome or tantalum.
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D4636 – 99 (2004)
FIG. 4 Condenser, Allihn Type
FIG. 3 Air Tube
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
5.3.12 Whenairmustbeconditioned,thereisneedforanair
the determination.
drier or humidifier. The method used is optional provided the
air characteristics of 5.3.3 are attained. For drying, a satisfac-
6.2 Purity of Water—Unlessotherwiseindicated,references
tory method is the use of a glass column containing 8-mesh
to water shall be understood to mean reagent water as defined
anhydrous calcium sulfate with a column diameter such that
by Specification D1193. Referee situations require Type II
velocity of air does not exceed 1.2 m/min. For humidifying, a
distilled water defined by Specification D1193.
satisfactory device is included in Appendix X1 to provide the
8, 9
6.3 Metal Specimens:
required moist air.
6.3.1 Washer-Shaped Metal Specimens, 6.35-mm ( ⁄4-in.)
5.3.13 Oven,optional,todryglasswareatelevatedtempera-
inside diameter by 19.05-mm ( ⁄4-in.) outside diameter by 0.81
ture.
mm (0.032 in.) thick in the following metals:
5.3.14 Forceps, stainless steel.
5.3.15 Thermocouple , 70 cm (27.6 in.) sheathed.
5.3.16 Brush, short-bristled, stiff (typewriter-cleaning brush
or equivalent).
Reagent Chemicals, American Chemical Society Specifications , American
6. Reagents and Materials
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
6.1 Purity of Reagents—Reagent grade chemicals shall be
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
used in all tests. Unless otherwise indicated, it is intended that
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
all reagents conform to the specifications of the Committee on
MD.
Analytical Reagents of theAmerican Chemical Society where The sole source of supply of the metal specimens known to the committee at
this time is Metaspec Co., P.O. Box 27702, San Antonio, TX 78227-0707.
If you are aware of alternative suppliers, please provide this information to
ASTM International Headquarters. Your comments will receive careful consider-
A resistance temperature device (RTD) is also acceptable. ation at a meeting of the responsible technical committee , which you may attend.
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D4636 – 99 (2004)
6.3.2 Square-Shaped Metal Specimens (asshowninFig.6),
0.81-mm (0.032-in.) by 25.4-mm (1-in.) square in the follow-
ing metals:
C11000 Copper (ETP)
G10100 Steel Grade 1010
A92024 Aluminum Alloy 2024 T-3 or T-4
M11311 Magnesium AZ31B
L01900 Cadmium Anod
6.4 Abrasive Paper, silicon carbide, various grades, includ-
ing 240 and 400-grit. Many papers, including “wet or dry,”
“waterproof,” or iron-containing abrasives, such as natural
emery are not satisfactory.
6.4.1 Silicon-Carbide Grains, 150 mesh.
6.5 Cotton, absorbent.
6.6 n-Heptane.(Warning—Flammable. Harmful if in-
haled.)
6.7 Acetone.(Warning—Extremely flammable. Vapors
may cause flash-fire.)
6.8 Nitric Acid, concentrated. (Warning—Poison. Corro-
sive. Strong oxidizer.)
6.9 Degreasing Solvents: n-Heptane or toluene.
11, 9
6.10 Carbon Remover for Glassware (Warning—
Causes severe burns.)—Mix 35 mL of saturated sodium
dichromate (aqueous) solution and 1000 mL of concentrated
sulfuric acid. (Warning—Corrosive.)
6.11 Glassware Cleaning Solution (Warning—Causes se-
vere burns.)—Mix 35 mL of MICRO in water or 35 mL of
FIG. 5 Assembled Apparatus
NOCHROMIX and 1000 mL of concentrated sulfuric acid.
6.12 Metal Cleaning Solution—Mix equal parts of 15 g
NaOH per litre of water and 15 g of Na PO per litre of water.
3 4
(Warning—Corrosive.)
7. Hazards
7.1 As this test method investigates the corrosive effect of
oil on metal in an artificial environment, precautions must be
taken to prevent premature oxidation of metal specimens by
stray chemicals during test preparations. The cleaned speci-
mens shall be touched only by surfaces known to be free of
interfering contaminants. Do not touch cleaned specimen(s)
with hands. Maintain clean glassware (see Appendix X2)ina
dust-free cabinet; rinse again and dry if clean glass has been
stored unused for more than a week.
7.2 Heating Bath, n-heptane, toluene, acetone, carbon re-
mover, nitric and sulfuric acids, and sodium h
...