ASTM D6594-00
(Test Method)Standard Test Method for Evaluation of Corrosiveness of Diesel Engine Oil at 135oC
Standard Test Method for Evaluation of Corrosiveness of Diesel Engine Oil at 135<sup>o</sup>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.
1.2 The values stated in 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.
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Designation: D 6594 – 00 An American National Standard
Standard Test Method for
Evaluation of Corrosiveness of Diesel Engine Oil at 135°C
This standard is issued under the fixed designation D 6594; 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
Any properly equipped laboratory, without outside assistance, can use the procedure described in
this test method. 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 of this test method .
1. Scope ing Oils and Determination of Selected Elements in Base
Oils by Inductively Coupled Plasma Atomic Emission
1.1 This test method is used to test diesel engine lubricants
Spectrometry (ICP-AES)
to determine their tendency to corrode various metals, specifi-
D 5844 Test Method for Evaluation of Automotive Engine
cally alloys of lead and copper commonly used in cam
Oils for Inhibition of Rusting (Sequence IID)
followers and bearings.
D 6557 Test Method forEvaluation of the Rust Preventive
1.2 The values stated in SI units are to be regarded as the
Characteristics of Automotive Engine Oils
standard.
E 691 Practice for Conducting an Inter-Laboratory Study to
1.3 This standard does not purport to address all of the
Determine the Precision of a Test Method
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3. Terminology
priate safety and health practices and determine the applica-
3.1 Definitions:
bility of regulatory limitations prior to use.
3.1.1 corrosion, n—the chemical or electrochemical reac-
2. Referenced Documents tion between a material, usually a metal surface, and its
environment that can produce a deterioration of the material
2.1 ASTM Standards:
and its properties. D 5844
D 130 Test Method for Detection of Copper Corrosion from
3.1.2 developer, n—of an ASTM test method, the assigned
Petroleum Products by the Copper Strip Tarnish Test
ASTM group, working under the supervision of its governing
D 5185 Test Method for Determination of Additive Ele-
subcommittee and main committee, that formats the test
ments, Wear Metals, and Contaminants in Used Lubricat-
method in accordance with the Form and Style for ASTM
Standards, and continually refines the test method.
This test method is under the jurisdiction of ASTM Committee D02 on
3.1.3 developer, n—of a test procedure, an individual or
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.B0 on Automotive Lubricants.
organization that selects the test apparatus and operating
Current edition approved Nov. 10, 2000. Published January 2001.
conditions.
The ASTM Test Monitoring Center will update changes in this test method by
3.1.4 non-reference oil, n—any oil other than a reference
means of Information Letters. This edition incorporates revisions contained in all
Information Letters through 00-1. Information Letters may be obtained from the
ASTM Test Monitoring Center, 6555 Penn Ave., Pittsburgh, PA 15206-4489,
Attention: Administrator.
3 5
Available from ASTM Headquarters. Request the High Temperature Corrosion Annual Book of ASTM Standards, Vol 05.03.
Bench Test Research Report, RR:D02-1443. Annual Book of ASTM Standards, Vol 05.04.
4 7
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 6594
oil; such as a research formulation, commercial oil, or candi-
date oil. D 5844
3.1.5 reference oil, n—an oil of known performance char-
acteristics, used as a basis for comparison. D 5844
3.1.5.1 Discussion—Reference oils are used to calibrate
testing facilities, to compare the performance of other oils, or
to evaluate other materials (such as seals) that interact with
oils.
3.1.6 specimen, n—a piece or portion of a sample used to
make a test.
3.1.7 sponsor, n—of an ASTM test method, an organization
that is responsible for ensuring supply of the apparatus used in
the test procedure portion of the test method.
3.1.7.1 Discussion—In some instances, such as a test
method for chemical analysis, an ASTM working group can be
the sponsor of a test method. In other instances, a company
with a self-interest may or may not be the developer of the test
procedure used within the test method, but is the sponsor of the
test method.
3.1.8 test oil, n—any oil subjected to evaluation in an
established procedure. D 6557
4. Summary of Test Method
4.1 Four metal specimens of copper, lead, tin, and phosphor
FIG. 1 Sample Tube
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 copper specimen and the
stressed oil are examined to detect corrosion and corrosion
products, respectively.
4.2 A reference oil is tested with each group of tests to
verify test acceptability.
5. Significance and Use
5.1 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.
6. Apparatus
6.1 The main apparatus consists of the following items of
standard wall borosilicate glassware as shown in Figs. 1-6.
6.1.1 Main Sample Tube, Fig. 1.
6.1.2 Sample Tube Head, Fig. 2.
6.1.3 Air Tube, Fig. 3.
6.1.4 Thermocouple Tube, Fig. 4.
6.1.5 Condenser, Allihn Type, Fig. 5.
6.1.6 Assembled Apparatus, Fig. 6.
FIG. 2 Sample Tube Head
6.2 Additional glassware items and assembly accessories
needed are:
6.2.1 Hanger (for metal specimens), of stainless steel, hav- of 250 6 20 mm. Oil baths are recommended. (Warning—
ing the dimensions listed in Fig. 7. There are exposed hot surfaces on apparatus. Avoid skin
6.2.2 Adapter, polytetrafluoroethylene for 10/18 joint for contact by use of protective equipment.)
sealing of the air tube to the sample tube head. 6.3.2 Ventilation, to adequately remove fumes during heat-
6.3 Other items and equipment are: ing.
6.3.1 Heating bath, with constant temperature control within 6.3.3 Dry Air Supply, with a dew point of −68°C.
6 0.5°C (6 1°F) of test temperature with an immersion depth 6.3.3.1 When air needs to be conditioned an air drier is
D 6594
FIG. 5 Condenser, Allihn Type
FIG. 3 Air Tube
FIG. 6 Assembled Apparatus
FIG. 4 Thermocouple Tube
6.3.7 Oven, optional, to dry glassware at elevated tempera-
required. The method used is optional provided the air char-
ture.
acteristics of 6.3.3 are attained. For drying, a satisfactory
6.3.8 Forceps, stainless steel; or gloves (powder free).
method is the use of a glass column containing 8-mesh
6.3.9 Thermocouple, or equivalent. Use sheathed thermo-
anhydrous calcium sulfate with a column diameter such that
couple when used directly in contact with oil. Use unsheathed
velocity of air does not exceed 1.2 m/min.
thermocouple when thermocouple well is used; fill thermo-
6.3.4 Flowmeter, capable of measuring 10 6 1 L/h.
couple well with a heat transfer medium.
6.3.5 Balance, with a capacity of 2500 g and sensitivity of
6.3.10 Sanding Block and Holder, for specimen preparation.
0.1 g.
7. Reagents and Materials
6.3.6 Syringe, capable of accurately measuring out 100 mL
of liquid. 7.1 Purity of Reagents—Use reagent grade chemicals in all
D 6594
NOTE 1—All dimensions in mm.
FIG. 7 Specimen Hanger
tests. Unless otherwise indicated, it is intended that all reagents 7.8 Degreasing Solvent, (THF recommended).
conform to the specifications maintained by the Committee on 7.9 Naphtha, Aromatic. (Warning—Flammable. Health
Analytical Reagents of the American Chemical Society . hazard.)
9,10 2
7.2 Metal Specimens 7.10 Reference Oil .
7.2.1 Specimens are 0.081 cm thick by 2.5 cm square,
8. Preparation of Apparatus
except that lead specimen that is 0.178 cm thick. One specimen
from each of the following metal types, each with two drilled
8.1 Cleaning of Glassware:
holes, is required:
8.1.1 Rinse all glassware items and the air tube adapter with
7.2.1.1 Copper (R401-A),
degreasing solvent to remove residual oil, and air-dry.
7.2.1.2 Lead (R401-lead),
8.1.2 Wash all glassware items and the air tube adapter with
7.2.1.3 Tin (R401-tin), and
detergent. Rinse with tap water, distilled water, and dry.
7.2.1.4 Phosphor Bronze (R401-PBz).
8.1.3 Store all items in a dust-free cabinet until needed for
7.3 Abrasive Paper , 240-grit aluminum oxide and 400-grit
test. If stored longer than one week, rinse again with distilled
silicon carbide. Do not use iron-containing abrasives such as
water before use, and dry.
natural emery.
8.1.4 The following more thorough glassware cleaning
7.4 Cotton, 100 %.
procedure can be used, if it is required for a given situation:
7.5 Acetone (ACS), sulfur free. (Warning—Flammable.
8.1.4.1 Fill and immerse all glassware items with glassware
Health hazard.)
cleaning solution (see 7.6) and soak for 3 to 16 h. (Warning—
,
12 10
7.6 Glassware Cleaning Solution, NOCHROMIX .
Corrosive, causes severe burns.)
(Warning—Causes severe burns.)
8.1.4.2 Remove glassware from cleaning solution; rinse
7.7 Tetrahydrofuran (THF).(Warning—Toxic and flam-
several times with tap water, followed by distilled water, and
mable. Health hazard.)
oven-dry.
8.1.4.3 This more thorough glass cleaning procedure is
8 necessary in a referee situation, unless an alternative glassware
Reagent Chemicals, American Chemical Society Specifications, American
cleaning solution is available which is satisfactory to all parties
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
involved.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
8.2 Assembled Apparatus, shown in Fig. 6.
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC).
8.3 Preparation of Metal Specimens:
Obtain metal specimens from Test Engineering, Inc. (TEI), 12718 Cimarron
Path, San Antonio, TX 78249-3423. 8.3.1 In all succeeding steps, handle the specimens only
The sole source of supply of the apparatus known to the committee at this time
with stainless steel forceps or powder-free gloves until the final
is noted in the adjoining footnote. If you are aware of alternative suppliers, please
weighing. If large defects or particles are present on the metal
provide this information to ASTM Headquarters. Your comments will receive
specimens, remove them first using coarse sandpaper, followed
careful consideration at a meeting of the responsible technical committee, which
you may attend.
by polishing with the 240 and 400-grit abrasive papers, as
Suitable abrasive paper meeting these specifications is included with the metal
described in 8.3.2.
specimens when the specimens are ordered.
12 8.3.2 Using a sanding block with a specimen holder, remove
Obtain NOCHROMIX from Godax Laboratories, Inc., 720-B Erie Avenue,
Takoma Park, MD 20912. all surface blemishes from both sides and all four edges of each
D 6594
specimen with 240-grit abrasive paper. Remove any burrs from 10. Test Results
the drilled holes with a ⁄16 in. drill bit. Finish polishing with
10.1 Remove the air tube with the attached specimens from
400-grit paper wetted by acetone to remove marks from
the sample tube. Do not touch the specimens with hands.
previous polishing.
Retain the sample tube and test oil for further examination.
8.3.2.1 A good technique is to rub the specimen with
10.2 Using forceps or gloves, wash the copper specimen in
longitudinal strokes in direction perpendicular to that used with
tetrahydrofuran, and discard the other specimens.
240-grit paper. Use a different sheet of paper for each metal
10.3 Rate the copper specimen for tarnish according to the
type.
Strip Examination, Interpretation, and Report sections of Test
8.3.2.2 Make sure that the specimen edges are polished in
Method D 130.
the same manner as the surfaces. Carry out this procedure
10.4 Immediately after calibration of the ICP-AES instru-
using normal room lighting and without magnification of the
ment (as specified in Test Method D 5185), use Test Method
specimen surface. Do not scribe or otherwise mark the sur-
D 5185 to determine the concentration of copper, lead, and tin
faces.
in both the new and used oil.
8.3.3 Store the polished metal specimens in tetrahydrofuran.
10.5 Calculations:
8.3.4 Just prior to a test start, remove each specimen from
10.5.1 Evaporation Loss:
the tetrahydrofuran, and clean all metal dust from the specimen
L 5 W 2 W /W 3 100 (1)
@~ ! #
1 2 3
using 100 % cotton. Rub with a light-to-medium touch to
remove particles but do not polish the specimen further.
where:
8.3.5 Wash specimens in tetrahydrofuran and allow them to L = percent evaporation loss,
W = initial weight of air tube, sample tube and contents,
dry in a desiccator.
including test oil,
W = final weight of air tube, sample tube and contents,
9. Procedure
including test oil, and
9.1 Place the specimen hanger onto the air tube and hang
W = initial weight of test oil.
test specimens on their respective hooks.
10.5.2 Change in metal concentration in the used test oil:
9.1.1 Arrange the specimens on the hanger
...
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