by George E. Totten, Ph.D

This is a timeline of the history of Committee D02 on Petroleum Products and Lubricants and key moments in the history of the petroleum (and related) industries. For an abridged, designed version from the June 2004 issue of ASTM Standardization News magazine, click here.

To 1899 1900-1919 1920-1939
1940-1959 1960-1979 1980-2004
Print Version
1980 The National Security Act of 1980 mandates that all gasoline be blended with a minimum of 10 percent grain alcohol, or “gasohol.” The requirement will subsequently be scuttled.

1980 ASTM D 3764, Practice for Validation of Process Stream Analyzer Systems, is issued and is the first D02 practice dealing with the validation of process analyzers.

1981 ASTM Special Technical Publication (STP) 751, Distillate Fuel Stability and Cleanliness, is issued.

1982 Subcommittee D02.07 begins work on a laboratory test method to evaluate low-temperature pumpability, that will result in the issuance of D 5133, Method for Low Temperature, Low Shear Rate, Viscosity/ Temperature Dependence of Lubricating Oils Using a Temperature-Scanning Technique, in 1991. D 5133 will go on to be used as a required OEM specification by the International Lubricant and Standardization Approval Committee (ILSAC) in their ILSAC GF-2 specification.

1984 ASTM Special Technical Publication (STP) 878, Marine Fuels, is issued.

1985 The U.S. government cancels the “synfuels” project due to low prices.

1985 The first standard specification for engine oils, ASTM D 4485, Specification for Performance of Engine Oils, is issued.

1986 The primary phase-out of leaded gasoline in the United States is completed.

1986 ASTM Subcommittee J on Aviation Fuels organizes the first technical training course on aviation fuels. By 2004, this course will have been taught more than 56 times to more than 1,600 students in 13 countries and 20 cities. This is the first of the ASTM Technical and Professional Training Program courses.

1987 The first standard specification for two-stroke cycle gasoline engine oils, ASTM D 4681, Specification for Lubricants for Two-Stroke-Cycle Spark-Ignition Gasoline Engines (TSC-4), and the first standard engine test method for two-stroke cycle gasoline engine oils, ASTM D 4682, Specification for Miscibility with Gasoline and Fluidity of Two-Stroke-Cycle Gasoline Engine Lubricants, are issued.

1987 Subcommittee B on Automotive Lubricants is the first to implement facilitation of its monitored standards by forming a section and paying facilitators out of funds derived from reference oil sales for monitored test methods.

1988 To address the need for specifications relating to gasoline-ethanol blends, D02 issues D 4806, Specification for Denatured Fuel Ethanol for Blending with Gasolines for Use as Automotive Spark-Ignition Engine Fuel. To further address the need to cover other oxygenates and properties such as cetane number, metal corrosion, water tolerance, drivability, and federal regulations, ASTM D 4814, Specification for Automotive Spark-Ignition Engine Fuel, is also issued this year. For the first time, D02 recognizes an engine fuel standard not based solely on a straight hydrocarbon product (gasoline). These methods will be followed by others that address automotive spark-ignition engine fuel performance.

1988 ASTM Special Technical Publication (STP) 1005, Distillate Fuel: Contamination, Storage, and Handling, is issued.

1989 ASTM D 4953, Method for Vapor Pressure of Gasoline and Gasoline-Oxygenate Blends (Dry Method), is issued in response to problems with water interacting with gasoline-oxygenate blends when testing in accordance with D 323 (see 1930).

1989 Although used for 30 years for the development of industrial and automotive fluid lubricants, the first standardized FZG gear test is ASTM D 4998, Test Method for Evaluating Wear Characteristics of Tractor Hydraulic Fluids, issued this year, which evaluates gear wear applicable to tractor hydraulic fluids. The FZG gear test machine is the only ASTM test machine that uses an actual gear set as the consumable test piece. In 1991, ASTM D 5182, Test Method for Evaluating the Scuffing (Scoring) Load Capacity of Oils, which evaluates gear oils, will be published. By 2004, this test will be under consideration by the military as a replacement for its Ryder gear test.

1989 ASTM D02.92, the Coordinating Subcommittee on Interlaboratory Crosscheck Programs (ILCP), is established to address laboratories’ desire and need to participate in certification programs that evaluate laboratory proficiency, also called interlaboratory crosschecks (see 1993).

1989 ASTM D 4950, Classification and Specification for Automotive Service Greases, is approved and published. The approval of this method culminates approximately 20 years of joint effort by ASTM, the National Lubricating Grease Institute, and the Society of Automotive Engineers to develop a standard that will be analogous to the American Petroleum Institute engine-oil classification. Several additional test methods are developed and standardized as part of the effort to develop D 4950.

1989 ASTM D 4951, Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES), is issued. D 4951 will become one of the two most widely used methods for such analysis in virtually all oil analysis laboratories worldwide, along with D 5185, Method for Determination of Additive Elements, Wear Metals, and Contaminants in Used Lubricating Oils and Determination of Selected Elements in Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry, which will be published in 1991. The use of these two standards will reduce the time required for multi-element analysis from several days, using wet chemistry, to a few minutes, using the ICP-AES methods.

1990 The first standard engine test for engine oils, ASTM D 5119, Method for Evaluation of Automotive Engine Oils in the CRC L-38 Spark-Ignition Engine, is published.

1990 The D02.93 Coordinating Subcommittee on International Standards and Related Activities is formed.

1990 ASTM Committees D02 and E13 on Molecular Spectroscopy and Chromatography kick off a collaboration on multivariate infrared analyzers.

1990 A worldwide round robin is conducted to develop a cold-cranking simulator test very close to the same temperatures actually used for the engine-cranking test. This work results in the issuance of ASTM D 5293, Method for Apparent Viscosity of Engine Oils between 5° and -30°C Using the Cold-Cranking Simulator. This helps the Society of Automotive Engineers (SAE) to establish meaningful low-temperature cranking limits for SAE W grade oils.

1991 ASTM D 5188, Method for Vapor-Liquid Ratio Temperature Determination of Fuels (Evacuated Chamber Method), D 5190, Method for Vapor Pressure of Petroleum Products (Automatic Method), and D 5191, Method for Vapor Pressure of Petroleum Products (Mini Method), are issued.

1992 ASTM D 5236, Method for Distillation of Heavy Hydrocarbon Mixtures (Vacuum Potstill Method), is published.

1992 Hydraulic fluids are often used in environments where flammability of the fluid is a safety concern, therefore, ASTM D 5306, Method for Linear Flame Propagation Rate of Lubricating Oils and Hydraulic Fluids, is approved. This standard measures the propagation rate of a flame and is an indication of the relative ignitability of the fluid.

1993 D2PP Software for calculating statistical precision obtained in the interlaboratory studies conducted in D02 committees is published. Virtually all D02 crosschecks use this software for data analysis. This is one of the most important milestones in the committee’s history.

1993 ASTM D 5482, Method for Vapor Pressure of Petroleum Products (Mini Method-Atmospheric), is published.

1993 The Interlaboratory Crosscheck Program (see 1989) is launched, and a major milestone is achieved as evidenced by the wide popularity of this program around the world. It is truly an international program with 45 percent of the participating laboratories from outside the United States. By 2004, more than 700 laboratories, many of which are from outside of North America, will have participated in 18 programs.

1994 The first standardized test for evaluating metalworking fluids using actual metalworking tools, ASTM D 5619, Method for Comparing Metal Removal Fluids Using the Tapping Torque Test Machine, is issued.

1994 The Data Communications Committee is formed within the D02 Subcommittee B Test Monitoring Board to standardize industry protocols for electronic data transfer.

1994 E 1655, Practice for Calibration of Multivariate IR Analyzers, is the first fruit of the D02/E13 collaboration (see 1990).

1994 Committee D02 begins to add mandatory quality-control sections to numerous standards to improve the data reliability in routine petroleum products testing.

1994 ASTM Subcommittee D02.04 on Hydrocarbon Analysis plays a key role in developing new or improved test methods to meet the gasoline regulatory requirements of the U.S. Environmental Protection Agency and the California Air Resources Board. The endeavor includes large multi-method round robins to study test methods, the writing of new test methods, and revision of existing test methods. Close attention is paid to improving the precision of test methods. The test methods developed from this effort include:
• D 5769, Method for Determination of Benzene, Toluene, and Total Aromatics in Finished Gasolines by Gas Chromatography/Mass Spectrometry — standardizes total aromatics analysis in the United States and will be adopted by the EPA.
• D 3606, Method for Determination of Benzene and Toluene in Finished Motor and Aviation Gasoline by Gas Chromatography — precision of method for benzene improved; will be adopted by the EPA.
• D 4815, Method for Determination of MTBE, ETBE, TAME, DIPE, Tertiary-Amyl Alcohol and C1 to C4 Alcohols in Gasoline by Gas Chromatography — rewritten, and precision increased by a factor of three for MTBE and other oxygenates; will be adopted by CARB and allowed by the EPA as an alternative method.
• D 1319, Method for Hydrocarbon Types in Liquid Petroleum Products by Fluorescent Indicator Adsorption — new precision obtained for oxygenated gasolines; method also improved by eliminating depentanization step and inclusion of guidelines on how to improve method optimally; will be used by CARB for a time and will remain in use by the EPA for total olefins and alternative total aromatics.
• D 5599, Method for Determination of Oxygenates in Gasoline by Gas Chromatography and Oxygen Selective Flame Ionization Detection — new GC/OFID method for oxygenates developed; will become the EPA’s primary method for total oxygenates.
• D 5580, Method for Determination of Oxygenates in Gasoline by Gas Chromatography and Oxygen Selective Flame Ionization Detection — new method for benzene and total aromatics developed with excellent precision; will be adopted by CARB for total aromatics and benzene regulation.

1994 Subcommittee D02.12 on Environmental Standards for Lubricants is formed to address critical problems in the industry by developing standards or modifying existing methods for the measurement of new areas of lubricant performance such as lubricant classification and assessment of biodegradability, ecotoxicity and bioaccumulation. The subcommittee will develop standards such as D 6081, Practice for Aquatic Toxicity Testing of Lubricants: Sample Preparation and Results Interpretation; D 6384, Terminology Relating to Biodegradability and Ecotoxicity of Lubricants; and ASTM D 6731, Method for Determining the Aerobic, Aquatic Biodegradability of Lubricants or Lubricant Components in a Closed Respirometer.

1995 First full-scale test for gear oils, ASTM D 5704, Method for Evaluation of the Thermal and Oxidative Stability of Lubricating Oils Used for Manual Transmissions and Final Drive Axles, is developed.

1995 A symposium on the tribology of hydraulic pump testing is held on Dec. 4-5. Papers from the symposium will be published in Special Technical Publication (STP) 1310, Tribology of Hydraulic Pump Testing (see 1999).

1996 Eco-evaluated fluids have become a major topic in the fluid power industry and by this year two very complex standards are approved: ASTM D 6006, Guide for Assessing Biodegradability of Hydraulic Fluids, and D 6046, Classification of Hydraulic Fluids for Environmental Impact.

1997 The first standard test for the direct measurement of the effect of engine oils on fuel economy, ASTM D 6202, Method for Automotive Engine Oils on the Fuel Economy of Passenger Cars and Light-Duty Trucks in the Sequence VIA Spark Ignition Engine, is issued.

1997 Coordinating Subcommittees 94 and 95 are created out of CS 91, the General Coordinating Committee. CS 94 is the Coordinating Subcommittee on Quality Assurance and Statistics, which serves as the central resource on statistics and quality assurance practices for D02. The principle function of CS 95 Subcommittee on Terminology is the maintenance of the terminology compendium ASTM D 4175, Terminology Relating to Petroleum, Petroleum Products, and Lubricants.

1997 ASTM D 6122, Practice for Validation of Multivariate Process Infrared Spectrophotometers, is issued.

1997 ASTM D 6158, Specification for Mineral Hydraulic Oils, is issued and defines the physical, chemical, and performance requirements of the four more common mineral base hydraulic fluids (HH (non-inhibited refined mineral oil), HL (refined mineral oil with improved rust protection and oxidation stability), HM (improved antiwear properties), and HV (improved viscosity-temperature properties)). This specification was developed over several years and is a significant accomplishment. ASTM D 6158 provides an overview of both the requirements and testing results to be reported.

1997 ASTM D 6200, Method for Determination of Cooling Characteristics of Quench Oils by Cooling Curve Analysis, is issued for cooling curve characterization of petroleum-based quench oils. This method will be followed by ASTM D 6482, Method for Determination of Cooling Characteristics of Aqueous Polymer Quenchants by Cooling Curve Analysis with Agitation (Tensi Method), and D 6549, Method for Determination of Cooling Characteristics of Quenchants by Cooling Curve Analysis with Agitation (Drayton Unit), which are used for cooling curve characterization of both petroleum and aqueous-polymer quenchants. The latter two standards are the only methods of this kind in the world and are global standards. These methods were developed in collaboration with the Quenching and Cooling Committees of ASM International and International Federation for Heat Treatment and Surface Engineering.

1997 High VI improved hydraulic fluids often contain high viscosity index improvers, which may shear down with use and reduce the in-service viscosity of the fluid. ASTM D 6080, Practice for Defining the Viscosity Characteristics of Hydraulic Fluids, is developed to address this situation. New fluids are subjected to controlled testing to determine the degraded viscosity and are then reclassified according to viscosities at both low and high temperatures. The advantage of such a system is that users can ascertain if a fluid is sufficiently shear-stable for their application.

1998 The publication of ASTM D 6299, Practice for Applying Statistical Quality Assurance Techniques to Evaluate Analytical Measurement System Performance, provides a standardized approach and control chart techniques for D02 test methods for quality analysis.

1998 Publication of ASTM D 6300, Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lubricants, which is a conversion of Research Report (RR) D02:1007 methodology into ASTM standard practice format; this standard is technically harmonized with ISO 4259.

1998 Subcommittee D02.14 on Stability and Cleanliness of Liquid Fuels is formed. The subcommittee’s oxidative stability tests are related to storage stability. The group also oversees thermal stability, compatibility and cleanliness tests for fuels. The other subcommittee dealing exclusively with various aspects of stability is Subcommittee D02.09 on Oxidation, which covers lubricants, greases and hydraulic fluids.

1999 A symposium on hydraulic failure analysis is held Dec. 5-6; papers from the symposium will be published in Special Technical Publication (STP) 1339, Hydraulic Failure Analysis: Fluids, Components, and System Effects.

1999 ASTM D 6469, Guide for Microbial Contamination in Fuels and Fuel Systems, is published.

1999 ASTM D 6377, Method for Determination of Vapor Pressure of Crude Oil: VPCRx (Expansion Method), and D 6378, Method for Determination of Vapor Pressure (VPx) of Petroleum Products, Hydrocarbons, and Hydrocarbon-Oxygenate Mixtures (Triple Expansion Method), are issued. ASTM D 6450, Test Method for Flash Point by Continuously Closed Cup (CCCFP) Tester, is also issued, which does not rely on the use of the human eye to detect the flash point and instead, utilizes the pressure increase when a flash occurs.

2000 The European Union bans leaded gasoline.

2000 A new interlaboratory cross-check program for crude oils is launched. Analysis of crude oils is more challenging than most refined products, and their addition to the program represents a major step in improving the precision of test methods.

2000 The first D02 test method that uses intermediate precision rather than repeatability in its precision statement is approved and published: ASTM D 6593, Test Method for Evaluation of Automotive Engine Oils for Inhibition of Deposit Formation in a Spark-Ignition Internal Combustion Engine Fueled with Gasoline and Operated Under Low-Temperature, Light-Duty Conditions.

2001 Publication of ASTM D 6708, Practice for Statistical Assessment and Improvement of the Expected Agreement Between Two Test Methods that Purport to Measure the Same Property of a Material, a standardized approach to assess relative bias between standard test methods.

2001 One of the largest interlaboratory studies ever undertaken in D02 is conducted to determine low levels of sulfur in gasolines and in diesels. It involves four test methods, 70 laboratories and 32 samples. More than 6,000 data points are collected. The new precision data obtained is expected to define the regulatory compliance for low levels of sulfur of fuels in the future.

2001 ASTM D 6666, Guide for Evaluation of Aqueous Polymer Quenchants and D 6710, Guide for Evaluation of Hydrocarbon-Based Quench Oil, are issued; they are the only standards of this kind available covering both petroleum and aqueous-polymer quenchants.

2002 Publication of D 6792, Guide for a Quality System in Petroleum Products and Lubricants Testing Laboratories, the first total quality management standard for petroleum labs. This is the first standard of its kind issued by D02 for benchmarking a laboratory’

2002 ASTM D 6546, Test Methods and Suggested Limits for Determining the Compatibility of Elastomer Seals for Industrial Hydraulic Fluid Applications, is approved. This guide relates to the compatibility of hydraulic fluids with O-ring elastomers, which are used extensively for sealing in hydraulic components. The information from these tests can be used to anticipate expected service quality.

2002 To help fluid users and developers understand the suitability of a fluid for its intended use, ASTM D 6813, Guide for Performance Evaluation of Hydraulic Fluids for Piston Pumps, is published. This is a very thorough and useful guide for selecting test methods that are available to determine specific performance characteristics.

2003 ASTM D 6973, Method for Indicating Wear Characteristics of Petroleum Hydraulic Fluids in a High Pressure Constant Volume Vane Pump - 35 VQ, is approved, which uses a larger and higher-pressure vane pump relative to the vane pump used in ASTM D 2882 (see 1970).

2002 Subcommittee D02.96 on In-Service Lubricant Testing and Condition Monitoring Services is formed.

2003 Publication of the Fuels and Lubricants Handbook: Technology, Properties, Performance, and Testing. This near-encyclopedic tome provides in-depth discussion of a large range of fuels and lubricants and the test methods used in determining their properties and performance characteristics. It is the most comprehensive treatise on the subject to have been published in more than 40 years.

2004 D2PP software is issued as an adjunct to D 6300 (see 1998), as standardized controlled software to execute the D 6300 statistical algorithms.

2004 A new interlaboratory cross-check program for sulfur determination of ultra-low sulfur in diesel fuels is launched. It will use four methods designated by the U.S. Environmental Protection Agency (EPA) for regulatory compliance, and will use samples with 15 parts per million or less of sulfur. As ultra-low sulfur fuels become mandatory on the roadways, the importance of this new initiative is sure to grow.

Posted June 2004

To 1899 1900-1919 1920-1939
1940-1959 1960-1979 1980-2004

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