Standard Test Method for Evaluation of Corrosiveness of Diesel Engine Oil at 121°C

SCOPE
1.1 This test method is used to test diesel engine lubricants to determine their tendency to corrode various metals, specifically alloys of lead and copper commonly used in cam followers and bearings. Correlation with field experience has been established.
1.2 The values stated in acceptable SI units are to be regarded as the standard.
1.3 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. Specific hazard statements are given in 5.3.1, 6.6, 6.7, 6.8, 6.9, 6.10, 6.11, 7.1.1, 7.1.2, 7.1.5, and 7.4.1.

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ASTM D5968-00a - Standard Test Method for Evaluation of Corrosiveness of Diesel Engine Oil at 121°C
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5968 – 00a An American National Standard
Standard Test Method for
Evaluation of Corrosiveness of Diesel Engine Oil
This standard is issued under the fixed designation D 5968; 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.
INTRODUCTION
The method described in this test method is based on the gas turbine lubricant corrosion and
oxidation test described in Federal Test Method Standard 791, Method 5308. Because this test method
relates to corrosion in diesel engines rather than in gas turbines, temperatures, metal coupons, and
certain parts of the test procedure were modified to be more appropriate for heavy duty diesel engines.
The method described in this test method can be used by any properly equipped laboratory, without
outside assistance. However, the ASTM Test Monitoring Center (TMC) provides reference oils and
an assessment of the test results obtained on those oils by the laboratory (see Annex A1). By these
means, the laboratory will know whether their use of the test method gives results statistically similar
to those obtained by other laboratories. Furthermore, various agencies require that a laboratory utilize
the TMC services in seeking qualification of oils against specifications. For example, the U.S. Army
imposes such a requirement in connection with several Army engine lubricating oil specifications.
Accordingly, this test method is written for use by laboratories that utilize the TMC services.
Laboratories that choose not to use those services may simply ignore those portions of the test method
that refer to the TMC.
This test method may be modified by means of Information Letters issued by the TMC. In addition,
the TMC may issue supplementary memoranda related to the method (see Annex A1). For other
information, refer to the research report on the Cummins Bench Corrosion Test.
1. Scope responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.1 This test method is used to test diesel engine lubricants
bility of regulatory limitations prior to use. Specific hazard
to determine their tendency to corrode various metals, specifi-
statements are given in 5.3.1, 6.6, 6.7, 6.8, 6.9, 6.10, 6.11,
cally alloys of lead and copper commonly used in cam
7.1.1, 7.1.2, 7.1.5, and 7.4.1.
followers and bearings. Correlation with field experience has
been established.
2. Referenced Documents
1.2 The values stated in acceptable SI units are to be
2.1 ASTM Standards:
regarded as the standard.
D 130 Test Method for Detection of Copper Corrosion from
1.3 This standard does not purport to address all of the
Petroleum Products by the Copper Strip Tarnish Test
safety concerns, if any, associated with its use. It is the
D 4636 Test Method for Corrosiveness and Oxidation Sta-
bility of Hydraulic Oils, Aircraft Turbine Engine Lubri-
cants, and Other Highly Refined Oils
This test method is under the jurisdiction of ASTM Committee D02 on
D 5185 Determination of Additive Elements, Wear Metals,
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
and Contaminants in Used Lubricating Oils and Determi-
D02.B0.02 on Heavy Duty Engine Oils.
Current edition approved Nov. 10, 2000. Published November 2000. Originally
nation of Selected Elements in Base Oils by Inductively
published as D 5968 – 98. Last previous edition D 5968 – 00.
Coupled Plasma Atomic Emission Spectrometry (ICP-
ASTM Test Monitoring Center, 6555 Penn Ave., Pittsburgh, PA 15206-4489,
AES)
Telephone: (412) 365-1000, Fax: (412) 365-1045 (reference oil test telephone
reports), Fax: (412) 365-1047 (other messages), Telephone Oil Assignments: (412)
E 691 Practice for Conducting an Inter-Laboratory Study to
365-1004. 8
Determine the Precision of a Test Method
Available from ASTM Headquarters. Request RR:D02-1322. The research
report and this test method are supplemented by Information Letters and Memo-
randa issued by the ASTM Test Monitoring Center. This edition incorporates
revisions contained in all information letters through No. 00–1. Users of this test Annual Book of ASTM Standards, Vol 05.01.
method shall contact the ASTM Test Monitoring Center to obtain the most recent of Discontinued, Test Method D 4636 served as the basis for this test method. See
these. 1994 Annual Book of ASTM Standards, Vol 05.03.
4 7
Wang, J. C., and Cusano, C. M., “Development of A Bench Test to Detect Oils Annual Book of ASTM Standards, Vol 05.03.
Corrosive to Engine Components,” SAE Technical Paper No. 940790, 1994. Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5968
2.2 U.S. Federal Test Method Standards:
Federal Test Method Standard 791, Method 5308.7 Corro-
siveness and Oxidation Stability of Light Oils (Metal
Squares)
3. Summary of Test Method
3.1 Four metal coupons of copper, lead, tin, and phosphor
bronze are immersed in a measured amount of engine oil. The
oil, at an elevated temperature, is blown with air for a period of
time. When the test is completed, the coupons and the stressed
oil are examined to detect corrosion.
3.2 An industrial reference oil is tested with each group of
tests to verify test acceptability.
4. Significance and Use
4.1 This test method is intended to simulate the corrosion
process of non-ferrous metals in diesel lubricants. The corro-
sion process under investigation is that believed to be induced
primarily by inappropriate lubricant chemistry rather than
lubricant degradation or contamination. This test method has
been found to correlate with an extensive fleet database
containing corrosion-induced cam and bearing failures.
5. Apparatus
FIG. 2 Sample Tube Head
5.1 The main apparatus consists of the following items of
standard wall borosilicate glassware as shown in Figs. 1-6.
5.1.1 Main Sample Tube, Fig. 1.
5.1.2 Sample Tube Head, Fig. 2.
5.1.3 Air Tube, Fig. 3.
Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700
Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
FIG. 3 Air Tube
5.1.4 Thermocouple Tube, Fig. 4.
5.1.5 Condenser, Allihn Type, Fig. 5.
5.1.6 Assembled Apparatus, Fig. 6.
5.2 Additional glassware items and assembly accessories
needed are:
5.2.1 Spacers (for metal specimen), of borosilicate glass,
standard wall, 9-mm outside diameter, 6-mm length.
5.2.2 Oil Sampling Tube, Borosilicate Glass, 4-mm outside
diameter, with sampling end approximately 600 mm to reach
FIG. 1 Sample Tube into main sample tube. Tube is bent U-shape with exit end
D 5968
FIG. 4 Thermocouple Tube
FIG. 6 Assembled Apparatus
5.3 Other items and equipment are:
5.3.1 Heating Bath, constant temperature control within6
0.5°C (61°F) of test temperature with an immersion depth of
2506 20 mm. Oil or aluminum baths are recommended.
(Warning—There are exposed hot surfaces on apparatus.
Avoid skin contact by use of protective equipment.)
5.3.2 Hood Ventilation, to adequately remove fumes during
heating.
5.3.3 Air Supply, dry air, with a dew point of − 68°C
(−90°F) maximum and free of reactive contaminants.
5.3.4 Flowmeter, capable of measuring 10 6 1 L/h.
5.3.5 Balance, analytical sensitivity 0.1 mg.
5.3.6 Balance, Laboratory, 2500-g capacity, 0.1-g sensitiv-
ity.
5.3.7 Microscope, with 20-diameter magnification.
5.3.8 Assembly Fixture, wood slotted to hold coupons
squares (assembly as shown in Fig. 7) for tying with wire.
5.3.9 When air needs to be conditioned there is a need for an
air drier. The method used is optional provided the air
FIG. 5 Condenser, Allihn Type characteristics of 5.3.3 are attained. For drying, a satisfactory
method is the use of a glass column containing 8-mesh
anhydrous calcium sulfate with a column diameter such that
fitted by a one-hole stopper to a 25-mL filtering flask. Exit end
velocity of air does not exceed 1.2 m/min.
may be any convenient length.
5.3.10 Oven, optional, to dry glassware at elevated tempera-
10,11
5.2.3 Adapter, Polytetrafluoroethylene for 10/18 joint
ture.
for sealing of air tube to sample tube head.
5.3.11 Forceps, stainless steel.
5.3.12 Thermocouple.
5.3.13 Brush, short-bristled, stiff (old-style typewriter clean-
A satisfactory source for this item is Kontes Glass Co., Vineland, NJ 08360.
ing brush or equivalent).
The sole source of supply of the apparatus known to the committee at this time
is noted in the adjoining footnote. If you are aware of alternative suppliers, please
6. Reagents and Materials
provide this information to ASTM Headquarters. Your comments will receive
6.1 Purity of Reagents—Use reagent grade chemicals in all
careful consideration at a meeting of the responsible technical committee, which
you may attend. tests. Unless otherwise indicated it is intended that all reagents
D 5968
6.8 Glassware Cleaning Solution, mix 35 mL of saturated
sodium dichromate (aqueous) solution and 1000 mL of con-
centrated sulfuric acid. (Warning—Causes severe burns.)
11,15
6.9 Carbon Remover for Glassware, Oakite Stripper
R-8. (Warning—Corrosive, causes severe burns.)
6.10 Tetrahydrofuran.(Warning—Toxic and flammable.
Health hazard.)
6.11 Naphtha, Aromatic.(Warning—Flammable. Health
hazard.)
6.12 Filter Paper.
6.13 Kimwipe Tissues, or similar.
6.14 Industrial Reference Oil.
7. Preparation of Apparatus
7.1 Cleaning of Glassware from Previous Run:
7.1.1 Rinse all glassware items and the air tube adapter with
degreasing solvent to remove residual oil, and air dry.
(Warning—Harmful if inhaled.)
7.1.2 Fill or immerse the sample tube, air tube, and the
9-mm glass spacers in carbon remover at room temperature
until carbonaceous deposits are removed. Water rinse after
removal. (Warning—Corrosive, causes severe burns.)
7.1.3 Wash all glassware items and the air tube adapter with
,
11 16
detergent. Rinse with water to remove detergent, and dry.
7.1.4 Store all items in a dust free cabinet until needed for
test. If stored longer than one week, rinse again with distilled
water before use, and dry.
FIG. 7 Arrangement of Metal Coupons
7.1.5 A more elaborate glass cleaning procedure can be
used, if it is for a given situation. This cleaning procedure is
conform to the specifications of the Committee on Analytical
necessary in a referee situation unless a cleaning solution can
Reagents of the American Chemical Society where such
be used which is satisfactory to all parties involved. Fill and
specifications are available.
immerse all glassware items with glassware cleaning solution
,
11 13
6.2 Metal Specimens:
and soak for 3 to 16 h. (Warning—Corrosive, causes severe
6.2.1 Coupons, 0.081 cm thick by 2.5 cm square, one each,
burns.)
with two drilled holes (as shown in Fig. 7), as follows:
7.1.6 Remove glassware from cleaning solution, rinse sev-
6.2.1.1 Copper (R401-A),
eral times with tap water, followed by distilled water, and oven
6.2.1.2 Lead (R401-lead),
dry.
6.2.1.3 Tin (R401-tin), and
7.2 Cleaning of Glassware (New):
6.2.1.4 Phosphor Bronze (R401-LEADz).
7.2.1 Proceed as in 7.1.3 and 7.1.6 in that order (omit 7.1.1,
6.3 Nichrome Wire, clean (for tying coupons together).
7.1.2, 7.1.4, and 7.1.5).
6.4 Abrasive Paper, 240 grit aluminum oxide and 400 grit
7.3 Assembly—Assemble as shown in Fig. 6 using only the
silicon-carbide. Do not use iron-containing abrasives such as
test oil to lubricate glass joints during assembly.
natural emery.
7.4 Preparation of Metal Specimens:
6.5 Cotton, absorbent.
7.4.1 Wash a length of the metal tying wire with tetrahy-
6.6 Acetone (ACS), sulfur-free. (Warning—Flammable.
drofuran and acetone and allow to dry. (Warning—This and
Health hazard.
the following preparation processes should be performed under
6.7 Degreasing Solvents, Trichlorotrifluorethane or 1,1,1-
a fume hood.)
trichloroethane. (Warning—Harmful if inhaled.)
7.4.2 The metal squares are prepared as follows:
7.4.2.1 Using the 240 grit abrasive paper, remove all surface
blemishes from both sides and all four edges of each square,
and any burrs from the drilled holes. Finish polishing with 400
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
grit paper wetted by acetone to remove marks from previous
listed by the American Chemical Society, see Analar Standards for Laboratory
polishing. A good technique is to place abrasive paper on a flat
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
surface, then rub the specimen with longitudinal strokes in a
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD.
Satisfactory metal specimens may be obtained from: Test Engineering, Inc.
(TEI), 12718 Cimarron Path, San Antonio, TX 78249-3423. This is the only coupon Oakite Stripper R-8 is available from Oakite Products, Inc., 50 Valley Rd.,
source to be used for obtaining a valid reference run and data for certification. Berkeley Heights, NJ 07922. It has been found satisfactory for this purpose.
14 16
Suitable abrasive paper meeting these specifications is included with the metal A detergent found satisfactory is Alconox made by Alconox, Inc., 215 Park
coupons from the source indicated in 6.2. Ave. S., New York, NY 10003.
D 5968
direction perpendicular to that used with 240 grit paper. Use a 8.4.1 Using forceps, wash each square individually in tet-
different sheet of paper for each metal type. rahydrofuran.
8.4.2 Repeat the washing, using fresh tetrahydrofuran,
7.4.2.2 In all succeeding steps, handle the squares only with
tongs or filter paper until the final weighing. If large defects or scrubbing the squares with the short-bristled brush until the
tetrahydrofuran shows no additional discoloration. Use a piece
particles are present on the metal coupons, course sand paper
should be used first to remove them; this is followed by of Kimwipe, dampened with acetone, to rub and wipe the
coupons repeatedly until the tissue remains clean after wiping.
polishing with the 240 and 400 grit abrasive paper.
(1) Store the polished metal coupon in tetrahydrofuran and Allow the squares to air-dry. The reaction products that are to
be removed by this cleaning process may tend to have a
proceed until all coupons are polished.
stronger affinity to the bronze material, and therefore may be
(2) Remove each square from the tetrahydrofura
...

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