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ASTM D128-98(2019)

(Test Method)

Standard Test Methods for Analysis of Lubricating Grease

Standard Test Methods for Analysis of Lubricating Grease

SIGNIFICANCE AND USE
4.1 These test methods can be used to identify and estimate the amount of some of the constituents of lubricating greases. These test methods are applicable to many, but not all, greases.  
4.2 Composition should not be considered as having any direct bearing on service performance unless such correlation is established.  
Note 2: Details on other test methods for grease analysis can be found in other reference material.4,5,6
SCOPE
1.1 These test methods for analysis cover greases of the conventional type, which consist essentially of petroleum oil and soap. The constituents that can be determined are soap, unsaponifiable matter (petroleum oil, and so forth), water, free alkalinity, free fatty acid, fat, glycerin, and insolubles.  
Note 1: Any of the test methods described herein are best used by an experienced grease analyst who may also be able to make appropriate adaptations of the techniques as occasion requires.  
1.2 A supplementary test method is provided in Appendix X1. This test method is intended primarily for application to greases containing thickeners that are essentially insoluble in n-hexane, and to greases that cannot be analyzed by conventional methods because of the presence of such constituents as nonpetroleum fluids or nonsoap-type thickeners, or both. In some cases, these constituents can react with strong acid or alkaline solutions.  
1.3 These test methods appear in the following order:    
Sections  
Ash Determination  
7 – 11  
Insolubles, Soap, Fat, Petroleum Oil,
and Unsaponifiable Matter  
12 – 20  
Free Alkali and Free Acid  
21 – 23  
Water  
24  
Glycerin (Quantitative)  
25 – 29  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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.  
1.6 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.

General Information

Status
Published
Publication Date
30-Jun-2019
ICS
75.100 - Lubricants, industrial oils and related products
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.G0.01 - Chemical and General Laboratory Tests
Current Stage
Ref Project

Relations

Refers
ASTM D217-16 - Standard Test Methods for Cone Penetration of Lubricating Grease
Effective Date
01-Oct-2016
Refers
ASTM D445-16 - Standard Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)
Effective Date
15-Dec-2016
Refers
ASTM D217-19 - Standard Test Methods for Cone Penetration of Lubricating Grease
Effective Date
01-May-2019
Refers
ASTM D217-19a - Standard Test Methods for Cone Penetration of Lubricating Grease
Effective Date
01-Jul-2019
Refers
ASTM D445-14 - Standard Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)
Effective Date
01-Jul-2014
Refers
ASTM D445-14e1 - Standard Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)
Effective Date
01-Jul-2014
Refers
ASTM D473-07(2017) - Standard Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method
Effective Date
01-Jun-2017

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ASTM D128-98(2019) - Standard Test Methods for Analysis of Lubricating Grease
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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.
Designation: D128 − 98 (Reapproved 2019)
Standard Test Methods for
1
Analysis of Lubricating Grease
This standard is issued under the fixed designation D128; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
1.1 These test methods for analysis cover greases of the
Barriers to Trade (TBT) Committee.
conventional type, which consist essentially of petroleum oil
and soap. The constituents that can be determined are soap,
2. Referenced Documents
unsaponifiable matter (petroleum oil, and so forth), water, free
2
alkalinity, free fatty acid, fat, glycerin, and insolubles.
2.1 ASTM Standards:
D95 Test Method for Water in Petroleum Products and
NOTE 1—Any of the test methods described herein are best used by an
Bituminous Materials by Distillation
experienced grease analyst who may also be able to make appropriate
adaptations of the techniques as occasion requires. D156 Test Method for Saybolt Color of Petroleum Products
(Saybolt Chromometer Method)
1.2 A supplementary test method is provided in Appendix
D217 Test Methods for Cone Penetration of Lubricating
X1. This test method is intended primarily for application to
Grease
greases containing thickeners that are essentially insoluble in
D445 Test Method for Kinematic Viscosity of Transparent
n-hexane, and to greases that cannot be analyzed by conven-
and Opaque Liquids (and Calculation of Dynamic Viscos-
tional methods because of the presence of such constituents as
ity)
nonpetroleum fluids or nonsoap-type thickeners, or both. In
D473 Test Method for Sediment in Crude Oils and Fuel Oils
some cases, these constituents can react with strong acid or
by the Extraction Method
alkaline solutions.
D804 Terminology Relating to Pine Chemicals, Including
1.3 These test methods appear in the following order:
Tall Oil and Related Products
Sections
D1078 Test Method for Distillation Range of Volatile Or-
Ash Determination 7–11
ganic Liquids
Insolubles, Soap, Fat, Petroleum Oil, 12–20
and Unsaponifiable Matter D1193 Specification for Reagent Water
Free Alkali and Free Acid 21–23
D1353 Test Method for Nonvolatile Matter in Volatile Sol-
Water 24
vents for Use in Paint, Varnish, Lacquer, and Related
Glycerin (Quantitative) 25–29
Products
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
3. Terminology
standard.
3.1 Definitions:
1.5 This standard does not purport to address all of the
3.1.1 asphalt, n—a dark brown-to-black cementitious mate-
safety concerns, if any, associated with its use. It is the
rial in which the predominating constituents are bitumens.
responsibility of the user of this standard to establish appro-
3.1.1.1 Discussion—Asphalt can be a natural product or a
priate safety, health, and environmental practices and deter-
material obtained from petroleum processing.
mine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accor-
3.1.2 candle pitch, n—a dark brown-to-black, tarry or solid,
dance with internationally recognized principles on standard-
by-product residue from soap and candle stock manufacture,
ization established in the Decision on Principles for the
refiningofvegetableoils,refiningofwoolgrease,orrefiningof
refuse animal fats.
1
These test methods are under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and are the direct responsibility
2
of Subcommittee D02.G0.01 on Chemical and General Laboratory Tests. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 1, 2019. Published August 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ɛ1
approved in 1922. Last previous edition approved in 2014 as D128 – 98 (2014) . Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D0128-98R19. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D128 − 98 (2019)
3.1.3 cup grease, n—any lubricating grease having physical 3.1.11 neutralization number, n—of petroleum oil, the qua
...

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5.1 This test method is used to assess the ability of grease to prevent corrosion in rolling bearings operated in the presence of distilled water, sodium chloride solution, or synthetic sea water. It is used for development and specification purposes.
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ASTM D4742-23(Test Method)
Standard Test Method for Oxidation Stability of Gasoline Automotive Engine Oils by Thin-Film Oxygen Uptake (TFOUT)

SIGNIFICANCE AND USE
5.1 This test method is used to evaluate oxidation stability of lubricating base oils with additives in the presence of chemistries similar to those found in gasoline engine service. Test results on some ASTM reference oils have been found to correlate with sequence IIID engine test results in hours for a 375 % viscosity increase.5 The test does not constitute a substitute for engine testing, which measures wear, oxidation stability, volatility, and deposit control characteristics of lubricants. Properly interpreted, the test may provide input on the oxidation stability of lubricants under simulated engine chemistry.  
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SCOPE
1.1 This test method evaluates the oxidation stability of engine oils for gasoline automotive engines. This test, run at 160 °C, utilizes a high pressure reactor pressurized with oxygen along with a metal catalyst package, a fuel catalyst, and water in a partial simulation of the conditions to which an oil may be subjected in a gasoline combustion engine. This test method can be used for engine oils with viscosity in the range from 4 mm2/s (cSt) to 21 mm2/s (cSt) at 100 °C, including re-refined oils.  
1.2 This test method is not a substitute for the engine testing of an engine oil in established engine tests, such as Sequence IIID.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3.1 Exception—Pressure units are provided in psig, and dimensions are provided in inches in Annex A1, because these are the industry accepted standard and the apparatus is built according to the figures shown.  
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5.1 The four-ball wear-test method can be used to determine the relative wear-preventing properties of greases under the test conditions and if the test conditions are changed the relative ratings may be different. No correlation has been established between the four-ball wear test and field service. The test method cannot be used to differentiate between Extreme Pressure (EP) and Non-Extreme Pressure (Non-EP) Greases.4
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5.1 This is an accelerated engine oil test, performed in a standardized, calibrated, stationary single-cylinder diesel engine that gives a measure of (1) piston and ring groove deposit forming tendency, (2) piston, ring, and liner scuffing and (3) oil consumption. The test is used in the establishment of diesel engine oil specification requirements as cited in Specification D4485 for appropriate API Performance Category C oils (API 1509). The test method can also be used in diesel engine oil development.
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Scope  
1  
Referenced Documents  
2  
Terminology  
3  
Summary of Test Method  
4  
Significance and Use  
5  
Apparatus and Installation  
6  
Intake Air System  
6.2.1  
Exhaust System  
6.2.2  
Fuel System  
6.2.3  
Oil Consumption System  
6.2.4  
Engine Oil System  
6.2.5  
Engine Coolant System  
6.2.6  
Engine Instrumentation  
6.2.7  
Reagents and Materials  
7  
Oil Samples  
8  
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9  
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Complete Engine Inspection  
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Engine Measurements and Inspections  
9.6  
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Valve Guide Bushings  
9.8  
Fuel Injector  
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Piston and Rings  
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Compression Ratio  
9.12  
Engine Timing  
9.13  
Engine Coolant System Cleaning Procedure  
9.14  
Calibration and Standardization  
10  
Test Cell Instrumentation  
10.1  
Instrumentation Standards  
10.2  
Coolant Flow  
10.3  
Fuel Injectors  
10.4  
Air Flow  
10.5  
Intake Air Barrel  
10.6  
Fuel Filter  
10.7  
Oil Scale Flow Rates  
10.8  
Test Stand Calibration  
10.9  
Re-calibration Requirements  
10.9.1  
Extending Test Stand Calibration Period  
10.9.2  
Test Run Numbering  
10.10  
Humidity Calibration Requirements  
10.11  
Calibration of Piston Deposit Raters  
10.12  
Procedure  
11  
Engine Break-in Procedure  
11.1  
Cool-down Procedure  
11.2  
Warm-up Procedure  
11.3  
Shutdowns and Lost Time  
11.4  
Periodic Measurements  
11.5  
Engine Control Systems  
11.6  
Engine Coolant  
11.6.1  
Engine Fuel System  
11.6.2  
Engine Oil Temperature  
11.6.3  
Exhaust Pressure  
11.6.4  
Intake Air  
11.6.5  
Post-Test Procedures  
11.7  
Piston Ring Side Clearances  
11.7.1  
Piston Ratings  
11.7.2  
Ring Gap End Increase  
11.7.3  
Cylinder Liner Wear  
11.7.4  
Cylinder Liner Bore Polish  
11.7.5  
Photographs  
11.7.6  
Calculation and Interpretation of Results  
12  
Test Validity  
12.1  
Calculations  
12.4  
Quality Index  
12.4.1  
Oil Consumption  
12.4.2  
Report  
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1.1 This test method covers and is required to evaluate the performance of engine oils intended to satisfy certain American Petroleum Institute (API) C service categories (included in Specification D4485). It is performed in a laboratory using a standardized high-speed, single-cylinder diesel engine.4 Piston and ring groove deposit-forming tendency and oil consumption is measured. The piston, the rings, and the liner are also examined for distress and the rings for mobility.  
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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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Being an engine test method, this standard does have definite hazards that require safe practices (see Appendix X2 on Safety).  
1.4 The following is the Table of Contents:    
Section  
Scope  
1  
Referenced Documents  
2  
Terminology  
3  
Summary of Test Method  
4  
Significance and Use  
5  
Apparatus and Installation  
6  
Intake Air System  
6.2.1  
Exhaust System  
6.2.2  
Fuel System  
6.2.3  
Oil Consumption System  
6.2.4  
Engine Oil System  
6.2.5  
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6.2.5.1  
Oil Sample Valve  
6.2.5.2  
Engine Coolant System  
6.2.6  
Engine Instrumentation  
6.2.7  
Reagents and Materials  
7  
Oil Samples  
8  
Preparation of Apparatus  
9  
General Engine Assembly Practices  
9.1  
Complete Engine Inspection  
9.2  
Copper Components  
9.3  
Engine Lubricant System Flush  
9.4  
Engine Piston Cooling Jets  
9.5  
Engine Measurements and Inspections  
9.6  
Cylinder Head  
9.7  
Valve Guide Bushings  
9.8  
Fuel Injector  
9.9  
Piston and Rings  
9.10  
Cylinder Liner  
9.11  
Compression Ratio  
9.12  
Engine Timing  
9.13  
Engine Coolant System Cleaning Procedure  
9.14  
Calibration and Standardization  
10  
Test Cell Instrumentation  
10.1  
Instrumentation Standards  
10.2  
Coolant Flow  
10.3  
Re-calibration Requirements  
10.4  
Fuel Injectors  
10.5  
Air Flow  
10.6  
Intake Air Barrel  
10.7  
Fuel Filter  
10.8  
Oil Scale Flow Rates  
10.9  
Calibration of Test Stands  
10.10  
Extending Test Stand Calibration Period  
10.11  
Test Run Numbering  
10.13  
Humidity Calibration Requirements  
10.14  
Calibration of Piston Deposit Raters  
10.15  
Procedure  
11  
Engine Break-in Procedure  
11.1  
Cool-down Procedure  
11.2  
Warm-up Procedure  
11.3  
Shutdowns and Lost Time  
11.4  
Periodic Measurements  
11.5  
Engine Control Systems  
11.6  
Engine Coolant  
11.6.1  
Engine Fuel System  
11.6.2  
Engine Oil Temperature  
11.6.3  
Exhaust Pressure  
11.6.4  
Intake Air  
11.6.5  
Post-Test Procedures  
11.7  
Piston Ring Side Clearances  
11.7.1  
Piston Ratings  
11.7.2  
Referee Ratings  
11.7.3  
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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)

SIGNIFICANCE AND USE
5.1 These are accelerated engine oil tests (known as the 1K and 1N test procedures), performed in a standardized, calibrated, stationary single-cylinder diesel engine using either mass fraction 0.4 % sulfur fuel (1K test) or mass fraction 0.04 % sulfur fuel (1N test), that give a measure of (1) piston and ring groove deposit forming tendency, (2) piston, ring and liner scuffing and (3) oil consumption.  
5.2 The 1K test was correlated with vehicles equipped with certain multi-cylinder direct injection engines used in heavy duty and high speed service prior to 1989, particularly with respect to aluminum piston deposits, and oil consumption, when fuel sulfur was nominally mass fraction 0.4 %. These data are given in Research Report RR:D02-1273.9  
5.3 The 1N test has been used to predict piston deposit formation in four-stroke cycle, direct injection, diesel engines that have been calibrated to meet 1994 U.S. federal exhaust emission requirements for heavy-duty engines operated on fuel containing less than mass fraction 0.05 % sulfur. See Research Report RR:D02-1321.9  
5.4 These test methods are used in the establishment of diesel engine oil specification requirements as cited in Specification D4485 for appropriate API Performance Category oils (API 1509).  
5.5 These test methods are also used in diesel engine oil development.
SCOPE
1.1 These test methods cover the performance of engine oils intended for use in certain diesel engines. They are performed in a standardized high-speed, single-cylinder diesel engine by either the 1K (0.4 % mass fuel sulfur) or 1N (0.04 % mass fuel sulfur) procedure.3 The only difference in the two test methods is the fuel used. Piston and ring groove deposit-forming tendency and oil consumption are measured. Also, the piston, the rings, and the liner are examined for distress and the rings for mobility. These test methods are required to evaluate oils intended to satisfy API service categories CF-4 and CH-4 for 1K, and CG-4 for 1N of Specification D4485.  
1.2 These test methods, although based on the original Caterpillar 1K/1N procedures,3 also embody TMC information letters issued before these test methods were first published. These test methods are subject to frequent change. Until the next revision of these test methods, TMC will update changes in these test methods by the issuance of information letters which shall be obtained from TMC (see Annex A1 – Annex A4).  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3.1 Exception—Where there is no direct SI equivalent such as screw threads, national pipe threads/diameters, tubing size, or single source equipment specified. Also Brake Specific Fuel Consumption is measured in kilograms per kilowatthour.  
1.4 The following is the Table of Contents:    
Section  
Introduction  
Scope  
1  
Referenced documents  
2  
Terminology  
3  
Summary of Test Methods  
4  
Significance and Use  
5  
Apparatus  
6  
General Laboratory Requirements  
6.1  
Test Engine  
6.2  
Test Engine Accessories and Parts  
6.3  
Reagents and Materials  
7  
Test Oil Sample Requirements  
8  
Preparation of Apparatus  
9  
Engine Inspection  
9.1  
Engine Pre-Test Lubrication System Flush  
9.2  
Engine Pre-Test Measurements and Inspections  
9.3  
Engine Assembly  
9.4  
Pressure Testing of Fuel System Assembly  
9.5  
Calibration of Engine Test Stand  
10  
General Requirements and Frequency of Calibration  
10.1  
Runs  
10.2  
Specified Test Parameters  
10.3  
Calibration Test Acceptance Criteria  
10.4  
Action on Rejection of Calibration Test  
10.5  
Test Numbering  
10.6  
Reference Oils  
10.7  
Severity Adjustments  
10.8  
Engine Operating Procedure  
11  
...

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ASTM
ASTM D7549-23(Test Method)
Standard Test Method for Evaluation of Heavy-Duty Engine Oils under High Output Conditions—Caterpillar C13 Test Procedure

SIGNIFICANCE AND USE
5.1 This test method assesses the performance of an engine oil with respect to control of piston deposits and maintenance of oil consumption under heavy-duty operating conditions selected to accelerate deposit formation in a turbocharged, intercooled four-stroke-cycle diesel engine equipped with a combustion system that minimizes federally controlled exhaust gas emissions.  
5.2 The results from this test method may be compared against specification requirements to ascertain acceptance.  
5.3 The design of the test engine used in this test method is representative of many, but not all, diesel engines. This factor, along with the accelerated operating conditions, needs to be considered when comparing test results against specification requirements.
SCOPE
1.1 The test method covers a heavy-duty engine test procedure under high output conditions to evaluate engine oil performance with regard to piston deposit formation, piston ring sticking and oil consumption control in a combustion environment designed to minimize exhaust emissions. This test method is commonly referred to as the Caterpillar C13 Heavy-Duty Engine Oil Test.3  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.2.1 Exceptions—Where there are no SI equivalent such as screw threads, National Pipe Treads (NPT), and tubing sizes.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. See Annex A1 for general safety precautions.  
1.4 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 D5770-23(Test Method)
Standard Test Method for Semiquantitative Micro Determination of Acid Number of Lubricating Oils During Oxidation Testing

SIGNIFICANCE AND USE
5.1 This test method provides a semiquantitative estimate of the acid number of lubricating oils obtained from laboratory oxidation tests using smaller amounts of sample than Test Methods D974, D664, or D3339. It has specific application in Test Method D943 and in Test Method D4871. This test 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 test conditions.  
5.2 Since this test method is semiquantitative, each laboratory shall develop its own criteria for each oxidation test method for determining when to switch from this semiquantitative test method to a more precise test method for acid number.
SCOPE
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 mg 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 D974 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 D974 or D664. 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.  
1.3.1 Exception—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, 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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