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ASTM D5770-96

(Test Method)

Standard Test Method for Semiquantitative Micro Determination of Acid Number of Lubricating Oils During Oxidation Testing

Standard Test Method for Semiquantitative Micro Determination of Acid Number of Lubricating Oils During Oxidation Testing

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1.1 This test method is a semiquantitative micro method intended for monitoring the changes in acidic constituents occurring in lubricating oils during oxidation testing, when the acid number of such oils falls within the range from 0.02 to 1.0 mg of potassium hydroxide per gram of sample. It is applicable to such oils as turbine oils, hydraulic oils, and other circulating oils.  
Note 1- This test method is a micro version of Test Method D 974 and it produces results similar to that method.  
1.2 This test method is designed for use where sample size is limited. It shall not be used as a replacement for higher precision methods such as Test Methods D 974 or D 664. It shall not be used to monitor oils in-service.  
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.4 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
31-Dec-1995
ICS
75.100 - Lubricants, industrial oils and related products
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.06.0A - Chemical Analysis
Current Stage
Ref Project

Relations

Replaced By
ASTM D5770-02 - Standard Test Method for Semiquantitative Micro Determination of Acid Number of Lubricating Oils During Oxidation Testing
Effective Date
10-Dec-2002

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ASTM D5770-96 - Standard Test Method for Semiquantitative Micro Determination of Acid Number of Lubricating Oils During Oxidation TestingASTM D5770-96 - Standard Test Method for Semiquantitative Micro Determination of Acid Number of Lubricating Oils During Oxidation Testing
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ASTM D5770-96 - Standard Test Method for Semiquantitative Micro Determination of Acid Number of Lubricating Oils During Oxidation Testing
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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.
Designation: D 5770 – 96 An American National Standard
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Semiquantitative Micro Determination of Acid Number of
1
Lubricating Oils During Oxidation Testing
This standard is issued under the fixed designation D 5770; 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.
1. Scope 3. Terminology
1.1 This test method is a semiquantitative micro method 3.1 Definitions:
intended for monitoring the changes in acidic constituents 3.1.1 acid number, n—the quantity of base, expressed in
occurring in lubricating oils during oxidation testing, when the milligrams of potassium hydroxide per gram of sample, that is
acid number of such oils falls within the range from 0.02 to 1.0 required to titrate a sample to a specified endpoint.
mg of potassium hydroxide per gram of sample. It is applicable 3.1.1.1 Discussion—In this test method, the acid number is
to such oils as turbine oils, hydraulic oils, and other circulating calculated from the number of drops required to produce a
oils. change in solution color from blue-green to orange, compared
to the number of drops required to produce an identical color
NOTE 1—This test method is a micro version of Test Method D 974 and
change using a reference standard. Because this is a direct
it produces results similar to that method.
comparison method, the acid number value can be reported in
1.2 This test method is designed for use where sample size
milligrams of potassium hydroxide per gram of sample.
is limited. It shall not be used as a replacement for higher
precision methods such as Test Methods D 974 or D 664. It
4. Summary of Test Method
shall not be used to monitor oils in-service.
4.1 A 2.0-mL portion of the titration solution is titrated with
1.3 The values stated in SI units are to be regarded as the
a sample using a dropping pipet. The number of drops of
standard. The values given in parentheses are for information
sample required to turn the blue-green titration solution to a
only.
persistent orange color is noted.
1.4 This standard does not purport to address all of the
4.2 A second 2.0-mL portion of the titration solution is
safety concerns, if any, associated with its use. It is the
titrated with an acid number reference solution of known acid
responsibility of the user of this standard to establish appro-
number. The number of drops of the reference solution
priate safety and health practices and determine the applica-
required to turn the blue-green titration solution to a persistent
bility of regulatory limitations prior to use.
orange color is noted.
4.3 The estimated acid number of the sample is calculated
2. Referenced Documents
using the acid number of the reference solution and the ratio of
2.1 ASTM Standards:
the number of drops of the reference solution required to effect
D 664 Test Method for Acid Number of Petroleum Products
the color change to the number of drops of the sample required
2
by Potentiometric Titration
for the same change.
D 943 Test Method for Oxidation Characteristics of Inhib-
2
ited Mineral Oils
5. Significance and Use
D 974 Test Method for Acid and Base Number by Color-
5.1 This test method provides a semiquantitative estimate of
2
Indicator Titration
the acid number of lubricating oils obtained from laboratory
D 3339 Test Method for Acid Number of Petroleum Prod-
oxidation tests using smaller amounts of sample than Test
3
ucts by Semi-Micro Color Indicator Titration
Methods D 974, D 664, or D 3339. It has specific application in
D 4871 Guide for Universal Oxidation/Thermal Stability
Test Method D 943 and in Test Method D 4871. This test
4
Test Apparatus
method, therefore, provides a means of monitoring the relative
oxidation of lubricating oils by measuring changes in acid
number, at different time intervals and under various oxidizing
1
This test method is under the jurisdiction of ASTM Committee D-2 on
test conditions.
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
5.2 Since this test method is semiquantitative, each labora-
D02.06.OAon Chemical Analysis.
Current edition approved Dec. 10, 1996. Published February 1997. Originally
tory shall develop its own criteria for each oxidation test
published as D 5770 – 95. Last previous edition D 5770 – 95.
method for determining when to switch from this semiquanti-
2
Annual Book of ASTM Standards, Vol 05.01.
3
tative test method to a more precise test method for acid
Annual Book o
...

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ASTM D6792-23c(Practice)
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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).  
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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.  
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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.  
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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.  
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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  
1.2 This test method was previously titled “Low-Temperature Viscosity of Lubricants Measured by Brookfield Viscometer.” In the lubricant industry, D2983 test results have often been referred to as “Brookfield2 Viscosity” which implies a viscosity determined by this method.  
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1.4.1 The viscosity data used for the precision studies for Procedures A, B, and C covered a range from 300 mPa·s to 170 000 mPa·s at test temperatures of –12 °C, –26 °C, and –40 °C. Appendix X5 includes precision data for –55 °C test temperature and includes samples with viscosities greater 500 000 mPa·s.  
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.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement ar...

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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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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.  
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Note 1: Optimol Instruments supplies an upgrade kit to allow SRVI/II-machines to operate with 1600 N, if needed.  
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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.  
1.4 This practice is designed as a fast, simple spectroscopic check for condition monitoring of in-service lubricants and can be used to assist in the determination of general machinery health through measurement of properties observable in the mid-infrared spectrum such as water, oil oxidation, and others as noted in 1.1. The infrared data generated by this practice is typically used in conjunction with other testing methods. For example, infrared spectroscopy cannot determine wear metal levels or any other type of elemental analysis. The practice as presented is not intended for the prediction of lubricant physical properties (for example, viscosity, total base number, total acid number, etc.). This practice is designed for monitoring in-service lubricants and can aid in the determination of general machinery health and is not designed for the analysis of lubricant composition, lubricant performance or additive package formulations.  
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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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.  
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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.  
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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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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.
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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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