ASTM D6594-20e1

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Designation: D6594 − 20
Standard Test Method for
Evaluation of Corrosiveness of Diesel Engine Oil at 135 °C
This standard is issued under the fixed designation D6594; 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.
ε NOTE—Editorially updated TMC governance information in June 2022.
INTRODUCTION
Any properly equipped laboratory, without outside assistance, can use the procedure described in
this test method. However, theASTM Test Monitoring Center (TMC) provides reference oils and an
assessmentofthetestresultsobtainedonthoseoilsbythelaboratory(seeAnnexA1).Bythesemeans,
the laboratory will know whether their use of the test method gives results statistically similar to those
obtainedbyotherlaboratories.Furthermore,variousagenciesrequirethatalaboratoryutilizetheTMC
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* 1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This test method covers testing diesel engine lubricants
ization established in the Decision on Principles for the
to determine their tendency to corrode various metals, specifi-
Development of International Standards, Guides and Recom-
cally alloys of lead and copper commonly used in cam
mendations issued by the World Trade Organization Technical
followers and bearings.
Barriers to Trade (TBT) Committee.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
2. Referenced Documents
standard.
2.1 ASTM Standards:
1.3 This standard does not purport to address all of the
D130 Test Method for Corrosiveness to Copper from Petro-
safety concerns, if any, associated with its use. It is the
leum Products by Copper Strip Test
responsibility of the user of this standard to establish appro-
D5185 Test Method for Multielement Determination of
priate safety, health, and environmental practices and deter-
Used and Unused Lubricating Oils and Base Oils by
mine the applicability of regulatory limitations prior to use.
Inductively Coupled Plasma Atomic Emission Spectrom-
etry (ICP-AES)
D5844 Test Method for Evaluation of Automotive Engine
This test method is under the jurisdiction of ASTM Committee D02 on
Oils for Inhibition of Rusting (Sequence IID) (Withdrawn
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
2003)
Subcommittee D02.B0.02 on Heavy Duty Engine Oils.
Current edition approved May 1, 2020. Published May 2020. Originally
D6557 Test Method for Evaluation of Rust Preventive Char-
approved in 2000. Last previous edition approved in 2019 as D6594 – 19a. DOI:
acteristics of Automotive Engine Oils
10.1520/D6594-20E01.
The ASTM Test Monitoring Center will update changes in this test method by
means of Information Letters. This edition incorporates revisions contained in all
Information Letters through 19-2. Information Letters may be obtained from the For referenced ASTM standards, visit the ASTM website, www.astm.org, or
ASTM Test Monitoring Center, 203 Armstrong Drive, Freeport, PA 16229, contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Attention: Director. Standards volume information, refer to the standard’s Document Summary page on
Supporting data have been filed at ASTM International Headquarters and may the ASTM website.
beobtainedbyrequestingResearchReportRR:D02-1443.ContactASTMCustomer The last approved version of this historical standard is referenced on
Service at service@astm.org. www.astm.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D6594 − 20
3. Terminology 6. Apparatus
3.1 Definitions: 6.1 The main apparatus consists of the following items of
standard wall borosilicate glassware as shown in Figs. 1-6.
3.1.1 corrosion, n—the chemical or electrochemical reac-
tion between a material, usually a metal surface, and its 6.1.1 Main Sample Tube, Fig. 1.
6.1.2 Sample Tube Head, Fig. 2.
environment that can produce a deterioration of the material
and its properties. D5844 6.1.3 Air Tube, Fig. 3.
6.1.4 Thermocouple Tube, Fig. 4.
3.1.2 developer, n—of an ASTM test method, the assigned
6.1.5 Condenser, Allihn Type, Fig. 5.
ASTM group, working under the supervision of its governing
6.1.6 Assembled Apparatus, Fig. 6.
subcommittee and main committee, that formats the test
method in accordance with the Form and Style for ASTM
6.2 Additional glassware items and assembly accessories
Standards, and continually refines the test method. needed are:
6.2.1 Hanger (for metal specimens), of stainless steel,
3.1.3 developer, n—of a test procedure, an individual or
having the dimensions listed in Fig. 7.
organization that selects the test apparatus and operating
6.2.2 Adapter, polytetrafluoroethylene for 10/18 joint for
conditions.
sealing of the air tube to the sample tube head.
3.1.4 non-reference oil, n—any oil other than a reference
6.3 Other items and equipment are:
oil; such as a research formulation, commercial oil, or candi-
6.3.1 Heatingbath,withconstanttemperaturecontrolwithin
date oil. D5844
60.5 °C of test temperature with an immersion depth of 23 cm
3.1.5 reference oil, n—an oil of known performance
to 35 cm. Oil baths are recommended. (Warning—There are
characteristics, used as a basis for comparison. D5844
exposedhotsurfacesonapparatus.Avoidskincontactbyuseof
3.1.5.1 Discussion—Reference oils are used to calibrate
protective equipment.)
testing facilities, to compare the performance of other oils, or
6.3.2 Ventilation, to adequately remove fumes during heat-
to evaluate other materials (such as seals) that interact with
ing.
oils.
6.3.3 Air Supply, use air from a clean, dry source.
3.1.6 specimen, n—a piece or portion of a sample used to
6.3.3.1 An air drier is required when air needs to be
make a test.
conditioned. The method used is optional provided the air
characteristics of 6.3.3 are attained. For drying, a satisfactory
3.1.7 sponsor, n—of an ASTM test method, an organization
method is the use of a glass column containing 8-mesh
that is responsible for ensuring supply of the apparatus used in
anhydrous calcium sulfate with a column diameter such that
the test procedure portion of the test method.
velocity of air does not exceed 1.2 m⁄min.
3.1.7.1 Discussion—In some instances, such as a test
6.3.4 Flowmeter, capable of measuring 10 L⁄h 6 1 L⁄h.
method for chemical analysis, anASTM 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. D6557
4. Summary of Test Method
4.1 Four metal specimens 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 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. FIG. 1 Sample Tube
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D6594 − 20
FIG. 2 Sample Tube Head
FIG. 4 Thermocouple Tube
FIG. 5 Condenser, Allihn Type
FIG. 3 Air Tube
6.3.8 Thermocouple, or equivalent. Use sheathed thermo-
6.3.5 Syringe, capable of accurately measuring out 100 mL couple when the thermocouple is in direct contact with oil.
of liquid. When a thermocouple well is used, use a sheathed or un-
6.3.6 Oven, optional, to dry glassware at elevated tempera- sheathed thermocouple in the well to control sample tempera-
ture. ture; fill thermocouple well with a heat transfer medium.
6.3.7 Forceps, stainless steel; or gloves (powder free). 6.3.9 Sanding Block and Holder, for specimen preparation.
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D6594 − 20
7.4 Cotton, 100 %.
7.5 Acetone (ACS), sulfur free. (Warning—Flammable.
Health hazard.)
7.6 Glassware Cleaning Solution, Contrad (trademark)
10,8
70. (Warning—Health hazard.)
7.7 Heptane. (Warning—Flammable. Health hazard.)
7.8 Cleaning Solvent—Cyclohexane or heptane, industrial
grade. (Warning—Both are flammable and health hazards.)
7.9 Reference Oil.
8. Preparation of Apparatus
8.1 Cleaning:
8.1.1 Rinse all items and the air tube adapter with cleaning
solvent to remove residual oil, and air-dry.
8.1.2 Wash all glassware items and the air tube adapter with
detergent. Rinse with tap water, distilled water, and dry.
8.1.3 The following more thorough glassware cleaning
procedure can be used, if it is required for a given situation:
8.1.3.1 Fill and immerse all glassware items with glassware
cleaning solution (see 7.6) and soak for 3 h to 16 h.
(Warning—Corrosive, causes severe burns.)
8.1.3.2 Remove glassware from cleaning solution; rinse
several times with tap water, followed by distilled water, and
FIG. 6 Assembled Apparatus
oven-dry.
8.1.3.3 This more thorough glass cleaning procedure is
necessary in a referee situation, unless an alternative glassware
7. Reagents and Materials
cleaning solution is available that is satisfactory to all parties
7.1 Purity of Reagents—Use reagent grade chemicals in all
involved.
tests. Unless otherwise indicated, it is intended that all reagents
8.2 Assembled Apparatus, shown in Fig. 6.
conform to the specifications maintained by the Committee on
Analytical Reagents of the American Chemical Society.
8.3 Preparation of Metal Specimens:
7,8 8.3.1 In all succeeding steps, handle the specimens only
7.2 Metal Specimens
withstainlesssteelforcepsorpowder-freeglovesuntilthefinal
7.2.1 Specimens are 0.081 cm thick by 2.5 cm square,
weighing. If large defects or particles are present on the metal
except the lead specimen, which is 0.157 cm thick. One
specimens, remove them first using coarse sandpaper, followed
specimen from each of the following metal types, each with
by polishing with the 240 and 400-grit abrasive papers, as
two drilled holes (as shown in Fig. 7), is required:
described in 8.3.2.
7.2.1.1 Copper (R401-A),
8.3.2 Remove any burrs from the drilled holes with a
7.2.1.2 Lead (R401-lead),
1.5113 mm, #53 (drill wire gauge) drill bit. Using a sanding
7.2.1.3 Tin (R401-tin), and
block with a specimen holder, remove all surface blemishes
7.2.1.4 Phosphor Bronze (R401-PBz).
from both sides and all four edges of each specimen with
7.3 Abrasive Paper, 240-grit aluminum oxide and 400-grit
240-grit abrasive paper. Finish polishing with 400-grit paper
silicon carbide. Do not use iron-containing abrasives such as
wetted by acetone to remove marks from previous polishing.
natural emery.
8.3.2.1 A good technique is to rub the specimen with
longitudinal strokes in a direction perpendicular to that used
with 240-grit paper. Use a different sheet of paper for each
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
metal type.
DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
8.3.2.2 Make sure that the specimen edges are polished in
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
the same manner as the surfaces. Carry out this procedure
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
copeial Convention, Inc. (USPC), Rockville, MD. using normal room lighting and without magnification of the
Obtain metal specimens from Test Engineering, Inc. (TEI), 12718 Cimarron
specimen surface. Do not scribe or otherwise mark the sur-
Path, San Antonio, TX 78249-3423.
faces.
The sole source of supply of the apparatus known to the committee at this time
8.3.3 Store the polished metal specimens in acetone.
is noted in the adjoining footnote. If you are aware of alternative suppliers, please
provide this information toASTM International Headquarters. Your comments will
receive careful consideration at a meeting of the responsible technical committee,
which you may attend.
9 10
Suitable abrasive paper meeting these specifications is included with the metal Contrad 70 is available from Decon Laboratories, Inc., 460 Glennie Circle,
specimens when the specimens are ordered. King of Prussia, PA 19406, (800) 332–6647.
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D6594 − 20
NOTE 1—All dimensions in mm.
FIG. 7 Specimen Hanger
8.3.4 Just prior to a test start, remove each specimen from 10. Test Results
the acetone, and clean all metal dust from the specimen using
10.1 Remove the air tube with the attached specimens from
100 % cotton. Rub with a light-to-medium touch to remove
the sample tube. Do not touch the specimens with hands.
particles but do not polish the specimen further.
Retain the sample tube and test oil for further examination.
8.3.5 Wash specimens in acetone, and allow them to dry in
10.2 Using forceps, wash the copper specimen in heptane,
a desiccator.
and discard the other specimens.
9. Procedure 10.3 Rate the copper specimen for tarnish according to the
Strip Examination, Interpretation, and Report sections of Test
9.1 Add 100 mL 6 1 mL of oil to the sample tube by
Method D130.
syringe.
10.4 Immediately after calibration of the ICP-AES instru-
9.2 Place the specimen hanger onto the air tube, and hang
ment (as specified in Test Method D5185), use Test Method
test specimens on their respective hooks.
D5185 to determine the concentration of copper, lead, and tin
9.2.1 Arrange the specimens on the hanger in the sequence:
in both the new and used oil. No decimal results shall be
lead, copper, tin, and phosphor bronze.
recorded.
9.3 Insert the air tube with the attached specimens into the
10.4.1 Any measured concentration results that round to
sample tube so that the air tube rests on the bottom of the
zero shall be reported as zero.
sample tube.
10.5 Calculations—Change in metal concentration in the
9.4 Place the sample tube head on the sample tube.
used test oil:
9.5 Place the assembled sample tube and condenser into the
∆ C 5 C 2 C (1)
2 1
bath so that the sample tube is submerged 23 cm to 35 cm in
where:
the bath with the test oil temperature set at 135 °C 6 0.5 °C.
∆ C = change in metal concentration before and after test,
9.6 Start the flow of the cooling water through the con-
C = measurement of metal concentration in new test oil
denser jacket.
(as determined in 10.4), and
9.7 To begin testing, connect the source of clean, dry air C = measurement of metal concentration in used test oil
(as determined in 10.4).
5L⁄h 6 0.5 L⁄h to the air tube and allow the air to flow for
168 h. Use a calibrated flow meter in setting airflow rates.
11. Reference Oil Testing
9.8 End of Test—After 168 h at 135 °C, shut off the airflow
11.1 Test a
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