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ASTM D6594-04

(Test Method)

Standard Test Method for Evaluation of Corrosiveness of Diesel Engine Oil at 135°C

Standard Test Method for Evaluation of Corrosiveness of Diesel Engine Oil at 135°C

SCOPE
1.1 This test method covers testing 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.

General Information

Status
Historical
Publication Date
31-Oct-2003
ICS
75.100 - Lubricants, industrial oils and related products
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.B0.02 - Heavy Duty Engine Oils
Current Stage
Ref Project

Relations

Replaces
ASTM D6594-03 - Standard Test Method for Evaluation of Corrosiveness of Diesel Engine Oil at 135<sup>o</sup>C
Effective Date
01-Nov-2003
Replaced By
ASTM D6594-04a - Standard Test Method for Evaluation of Corrosiveness of Diesel Engine Oil at 135&#176;C
Effective Date
01-Nov-2004
Referred By
ASTM D6923-23 - Standard Test Method for Evaluation of Engine Oils in a High Speed, Single-Cylinder Diesel Engine—Caterpillar 1R Test Procedure
Effective Date
01-Nov-2003
Referred By
ASTM D4485-22e1 - Standard Specification for Performance of Active API Service Category Engine Oils
Effective Date
01-Nov-2003
Referred By
ASTM D6750-23 - Standard Test Methods for Evaluation of Engine Oils in a High-Speed, Single-Cylinder Diesel Engine—1K Procedure (0.4 % Fuel Sulfur) and 1N Procedure (0.04 % Fuel Sulfur)
Effective Date
01-Nov-2003

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ASTM D6594-04 - Standard Test Method for Evaluation of Corrosiveness of Diesel Engine Oil at 135&#176;C
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
An American National Standard
Designation:D6594–04
Standard Test Method for
1
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
2
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
3
information, refer to the research report of this test method.
1. Scope 2. Referenced Documents
4
1.1 This test method covers testing diesel engine lubricants 2.1 ASTM Standards:
to determine their tendency to corrode various metals, specifi- D 130 Test Method for Detection of Copper Corrosion from
cally alloys of lead and copper commonly used in cam Petroleum Products by the Copper Strip Tarnish Test
followers and bearings. D 5185 Test Method for Determination of Additive Ele-
1.2 The values stated in SI units are to be regarded as the ments, Wear Metals, and Contaminants in Used Lubricat-
standard. ing Oils and Determination of Selected Elements in Base
1.3 This standard does not purport to address all of the Oils by Inductively Coupled Plasma Atomic Emission
safety concerns, if any, associated with its use. It is the Spectrometry (ICP-AES)
responsibility of the user of this standard to establish appro- D 5844 Test Method for Evaluation of Automotive Engine
5
priate safety and health practices and determine the applica- Oils for Inhibition of Rusting (Sequence IID)
bility of regulatory limitations prior to use. D 6557 Test Method for Evaluation of the Rust Preventive
Characteristics of Automotive Engine Oils
E 691 Practice for Conducting an Inter-Laboratory Study to
Determine the Precision of a Test Method
3. Terminology
3.1 Definitions:
1
This test method is under the jurisdiction of ASTM Committee D02 on
3.1.1 corrosion, n—the chemical or electrochemical reac-
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
tion between a material, usually a metal surface, and its
D02.B0 on Automotive Lubricants.
environment that can produce a deterioration of the material
Current edition approved May 1, 2004. Published June 2004. Originally
approved in 2000. Last previous edition approved in 2003 as D 6594–03.
2
The ASTM Test Monitoring Center will update changes in this test method by
means of Information Letters. This edition incorporates revisions contained in all
4
Information Letters through 03-1. Information Letters may be obtained from the For referenced ASTM standards, visit the ASTM website, www.astm.org, or
ASTM Test Monitoring Center, 6555 Penn Ave., Pittsburgh, PA 15206-4489, contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Attention: Administrator. Standards volume information, refer to the standard’s Document Summary page on
3
Supporting data have been filed at ASTM International Headquarters and may the ASTM website.
5
be obtained by requesting Research Report RR: D02–1443. Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D6594–04
and its properties. D5844
3.1.2 developer, n—of an ASTM test method, the assigned
ASTM group, working under the supervision of its governing
subcommittee and main committee, that formats the test
method in accordance with the Form and Style for ASTM
Standards, and continually refines the test method.
3.1.3 developer, n—of a test procedure, an individual or
organization that selects the test apparatus and operating
conditions.
3.1.4 non-reference oil, n—any oil other th
...

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ASTM D6792-23c(Practice)
Standard Practice for Quality Management Systems in Petroleum Products, Liquid Fuels, and Lubricants Testing Laboratories

SIGNIFICANCE AND USE
4.1 A petroleum products, liquid fuels, and lubricants testing laboratory plays a crucial role in product quality management and customer satisfaction. It is essential for a laboratory to provide quality data. This document provides guidance for establishing and maintaining a quality management system in a laboratory.  
4.1.1 The word ‘customer’ can refer to both customers internal and external to the laboratory or organization.
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1.1 This practice covers the establishment and maintenance of the essentials of a quality management system in laboratories engaged in the analysis of petroleum products, liquid fuels, and lubricants. It is designed to be used in conjunction with Practice D6299.
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ASTM D1159-23(Test Method)
Standard Test Method for Bromine Numbers of Petroleum Distillates and Commercial Aliphatic Olefins by Electrometric Titration

SIGNIFICANCE AND USE
5.1 The bromine number is useful as a measure of aliphatic unsaturation in petroleum samples. When used in conjunction with the calculation procedure described in Annex A2, it can be used to estimate the percentage of olefins in petroleum distillates boiling up to approximately 315 °C (600 °F).  
5.2 The bromine number of commercial aliphatic monoolefins provides supporting evidence of their purity and identity.
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1.1 This test method3 covers the determination of the bromine number of the following materials:  
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90 % Distillation Point, °C (°F)  
Bromine Number, max3    
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205 to 327 (400 to 626)  
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1.1.2 Commercial olefins that are essentially mixtures of aliphatic mono-olefins and that fall within the range of 95 to 165 bromine number (see Note 1). This test method has been found suitable for such materials as commercial propylene trimer and tetramer, butene dimer, and mixed nonenes, octenes, and heptenes. This test method is not satisfactory for normal alpha-olefins.  
Note 1: These limits are imposed since the precision of this test method has been determined only up to or within the range of these bromine numbers.  
1.2 The magnitude of the bromine number is an indication of the quantity of bromine-reactive constituents, not an identification of constituents; therefore, its application as a measure of olefinic unsaturation should not be undertaken without the study given in Annex A1.  
1.3 For petroleum hydrocarbon mixtures of bromine number less than 1.0, a more precise measure for bromine-reactive constituents can be obtained by using Test Method D2710. If the bromine number is less than 0.5, then Test Method D2710 or the comparable bromine index methods for industrial aromatic hydrocarbons, Test Methods D1492 or D5776 must be used in accordance with their respective scopes. The practice of using a factor of 1000 to convert bromine number to bromine index is not applicable for these lower values of bromine number.  
1.4 The values stated in SI units are to be regarded as the standard.  
1.4.1 Exception—The values given in parentheses are for information only.  
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ASTM D2983-23(Test Method)
Standard Test Method for Low-Temperature Viscosity of Automatic Transmission Fluids, Hydraulic Fluids, and Lubricants using a Rotational Viscometer

SIGNIFICANCE AND USE
5.1 The low-temperature, low-shear-rate viscosity of automatic transmission fluids, gear oils, torque and tractor fluids, and industrial and automotive hydraulic oils (see Appendix X4) are of considerable importance to the proper operation of many mechanical devices. Measurement of the viscometric properties of these oils and fluids at low temperatures is often used to specify their acceptance for service. This test method is used in a number of specifications.  
5.2 Initially this test method was developed to determine whether an automatic transmission fluid (ATF) would meet OEM low temperature performance criterion originally defined using a particular model viscometer.6, 7 The viscosity range covered in the original ATF performance correlation studies was from less than 1000 mPa·s to more than 60 000 mPa·s. The success of the ATF correlation and the development of this test method has over time been applied to other fluids and lubricants such as gear oils, hydraulic fluids, and so forth.  
5.3 Procedures A, B, C, and D of this test method describe how to measure apparent viscosity directly without the errors associated with earlier techniques that extrapolated experimental viscometric data obtained at higher temperatures.
Note 1: Low temperature viscosity values obtained by either interpolation or extrapolation of oils may be subject to errors caused by gelation and other forms of non-Newtonian response to spindle speed and torque.  
5.4 Procedures A, B, C, and D; If viscosity measurements are difficult to stabilize or a noticeable decrease in viscosity is seen at a constant speed between an initial measurement made during the 5 s to 10 s after the spindle rotation commences and the stabilized measurement between 60 s and 180 s, then this most likely indicates time-dependent, structural breakdown in the fluid. Some formulated fluid types may form wax structures when soaked at or below a certain low temperature which varies among fluids. The rotating spindle ...
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1.1 This test method covers the use of rotational viscometers with an appropriate torque range and specific spindle for the determination of the low-shear-rate viscosity of automatic transmission fluids, gear oils, hydraulic fluids, and some lubricants. This test method covers the viscosity range of 300 mPa·s to 900 000 mPa·s  
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1.4.2 The viscosity data used for Procedure D precision study was from 6400 mPa·s to 256 000 mPa·s at test temperatures of –26 °C and –40 °C.  
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5.1 This test simulates a type of severe field service in which corrosion-promoting moisture in the form of condensed water vapor accumulates in the axle assembly. This may happen as a result of volume expansion and contraction of the axle lubricant and the accompanied breathing in of moisture-laden air through the axle vent. The test screens lubricants for their ability to prevent the expected corrosion.  
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ASTM D6224-23(Practice)
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4.1 This practice is intended to help users, particularly power plant operators, maintain effective control over their mineral lubricating oils and lubrication monitoring program. This practice may be used to perform oil changes based on oil condition and test results rather than on the basis of service time or calendar time. It is intended to save operating and maintenance expenses.  
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1.2 This practice does not cover the monitoring of lubricating oil for steam and gas turbines. Rather, it is intended to complement Practice D4378.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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ASTM D5707-23(Test Method)
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5.1 This test method can be used to determine wear properties and coefficient of friction of lubricating greases at selected temperatures and loads specified for use in applications where high-speed vibrational or start-stop motions are present for extended periods of time under initial high Hertzian point contact pressures. This test method has found application in qualifying lubricating greases used in constant velocity joints of front-wheel-drive automobiles and for lubricating greases used in roller bearings. Users of this test method should determine whether results correlate with field performance or other applications.
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Note 1: Optimol Instruments supplies an upgrade kit to allow SRVI/II-machines to operate with 1600 N, if needed.  
1.2 This test method can also be used for determining a fluid lubricant's ability to protect against wear and its coefficient of friction under similar test conditions.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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ASTM E2412-23a(Practice)
Standard Practice for Condition Monitoring of In-Service Lubricants by Trend Analysis Using Fourier Transform Infrared (FT-IR) Spectrometry

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5.1 Periodic sampling and analysis of lubricants have long been used as a means to determine overall machinery health. Atomic emission (AE) and atomic absorption (AA) spectroscopy are often employed for wear metal analysis (for example, Test Method D5185). A number of physical property tests complement wear metal analysis and are used to provide information on lubricant condition (for example, Test Methods D445, D2896, and D6304). Molecular analysis of lubricants and hydraulic fluids by FT-IR spectroscopy produces direct information on molecular species of interest, including additives, fluid breakdown products and external contaminants, and thus complements wear metal and other analyses used in a condition monitoring program (1, 2-6).
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1.1 This practice covers the use of FT-IR in monitoring additive depletion, contaminant buildup and base stock degradation in machinery lubricants, hydraulic fluids and other fluids used in normal machinery operation. Contaminants monitored include water, soot, ethylene glycol, fuels and incorrect oil. Oxidation, nitration and sulfonation of base stocks are monitored as evidence of degradation. The objective of this monitoring activity is to diagnose the operational condition of the machine based on fault conditions observed in the oil. Measurement and data interpretation parameters are presented to allow operators of different FT-IR spectrometers to compare results by employing the same techniques.  
1.2 This practice is based on trending and distribution response analysis from mid-infrared absorption measurements. While calibration to generate physical concentration units may be possible, it is unnecessary or impractical in many cases. Warning or alarm limits (the point where maintenance action on a machine being monitored is recommended or required) can be determined through statistical analysis, history of the same or similar equipment, round robin tests or other methods in conjunction with correlation to equipment performance. These warning or alarm limits can be a fixed maximum or minimum value for comparison to a single measurement or can also be based on a rate of change of the response measured (1) .2 This practice describes distributions but does not preclude using rate-of-change warnings and alarms.
Note 1: It is not the intent of this practice to establish or recommend normal, cautionary, warning or alert limits for any machinery. Such limits should be established in conjunction with advice and guidance from the machinery manufacturer and maintenance group.  
1.3 Spectra and distribution profiles presented herein are for illustrative purposes only and are not to be construed as representing or establishing lubricant or machinery guidelines.  
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1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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ASTM D7216-23(Test Method)
Standard Test Method for Determining Automotive Engine Oil Compatibility with Typical Seal Elastomers

SIGNIFICANCE AND USE
5.1 Some engine oil formulations have been shown to lack compatibility with certain elastomers used for seals in automotive engines. These deleterious effects on the elastomer are greatest with new engine oils (that is, oils that have not been exposed to an engine’s operating environment) and when the exposure is at elevated temperatures.  
5.2 This test method requires that non-reference oil(s) be tested in parallel with a reference oil known to be aggressive for some parameters under service conditions. This relative  compatibility permits decisions on the anticipated or predicted performance of the non-reference oil in service.  
5.3 Elastomer materials can show significant variation in physical properties, not only from batch to batch but also within a sheet and from sheet to sheet. Results obtained with the reference oil are submitted by the test laboratories to the TMC to allow it to update continually the total and within-laboratory standard deviation estimates. These estimates, therefore, incorporate effects of variations in the properties of the reference elastomers on the test variability.  
5.4 This test method is suitable for specification compliance testing, quality control, referee testing, and research and development.  
5.5 The reference elastomers, reference oil, and the physical properties involved in this test method address the specific requirements of engine oils. Although other tests exist for compatibility of elastomers with liquids, these are considered too generalized for engine oils.
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1.1 This test method covers quantitative procedures for the evaluation of the compatibility of automotive engine oils with several reference elastomers typical of those used in the sealing materials in contact with these oils. Compatibility is evaluated by determining the changes in volume, Durometer A hardness, and tensile properties when the elastomer specimens are immersed in the oil for a specified time and temperature.  
1.2 Effective sealing action requires that the physical properties of elastomers used for any seal have a high level of resistance to the liquid or oil in which they are immersed. When such a high level of resistance exists, the elastomer is said to be compatible with the liquid or oil.
Note 1: The user of this test method should be proficient in the use of Test Methods D412 (tensile properties), D471 (effect of rubber immersion in liquids), D2240 (Durometer hardness), and D5662 (gear oil compatibility with typical oil seal elastomers), all of which are involved in the execution of the operations of this test method.  
1.3 This test method provides a preliminary or first order evaluation of oil/elastomer compatibility only. Because seals might be subjected to static or dynamic loads, or both, and they can operate over a range of conditions, a complete evaluation of the potential sealing performance of any elastomer-oil combination in any service condition usually requires tests additional to those described in this test method.  
1.4 The several reference elastomer formulations specified in this test method were chosen to be representative of those used in both heavy-duty diesel engines (detailed in Annex A1) and passenger-car spark-ignition engines (the latter are covered in Annex A2). The procedures described in this test method can, however, also be used to evaluate the compatibility of automotive engine oils with different elastomer types/formulations or different test durations and temperatures to those employed in this test method.
Note 2: In such cases, the precision and bias statement in Section 12 does not apply. In addition to agreeing acceptable limits of precision, where relevant, the user and supplier should also agree:  (1) test temperatures and immersion times to be used; (2) the formulations and typical properties of the elastomers; and (3) the sourcing and quality control of the elastomer sheets.
Note 3: The TMC may also issue In...

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SIGNIFICANCE AND USE
5.1 Trending the wear, contamination, consistency, and oxidative properties of a lubricating grease is a crucial part of condition-monitoring programs. Changes in these properties or deviations from the new grease can be indicative of problems within the lubricated component, such as the mixing of incompatible thickener types, excessive wear or contaminant levels, or significant depletion of antioxidant levels. These test methods also makes it possible to develop trends that can be used to predict failures before they occur and allow for corrective action to be taken.
SCOPE
1.1 This test method covers the determination and evaluation of flow properties, wear levels, contaminants, and oxidative condition of new and in-service lubricating grease.  
1.2 This test method provides guidance on evaluating in-service grease samples, NLGI grades 00 to 3, for wear, consistency, contamination, and oxidation.  
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3.1 Exception—The exception to this will be where units of references were developed by the developers of the test equipment and necessary to report the results of the test.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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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ASTM
ASTM D7922-23(Test Method)
Standard Test Method for Determination of Glycol for In-Service Engine Oils by Gas Chromatography

SIGNIFICANCE AND USE
5.1 Some glycol/antifreeze dilution of in-service engine oil is normal under typical operating conditions. However, excessive glycol dilution can lead to decreased performance, premature wear, or sudden engine failure. This test method provides a means of quantifying the level of glycol based antifreeze dilution, allowing the user to take necessary action.
SCOPE
1.1 This test method covers the determination of glycol based antifreeze for in-service engine oil by derivative headspace/gas chromatography.  
1.2 Sample is derivatized in-situ directly in a headspace sampling vial prior to vapor phase extraction and injection into a gas chromatograph.  
1.3 The chemistry of the derivatization is unique to the detection of the molecules of ethylene glycol and 1,2-propylene glycol. 1,3-propylene glycol could also be detected but is not used in any known anti-freeze at this time. Other coolant analyses are beyond the scope of this test method.  
1.4 The derivatization process does not affect glycol breakdown products such as glycolate and formate and hence the presence of these compounds in the oil will not be quantified.  
1.5 The test method concentration range is from 50 µg/g to 1000 µg/g. Lower levels are possible by method modifications. Higher levels are possible through sample dilution.  
1.6 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.8 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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