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ASTM D4742-02a

(Test Method)

Standard Test Method for Oxidation Stability of Gasoline Automotive Engine Oils by Thin-Film Oxygen Uptake (TFOUT)

Standard Test Method for Oxidation Stability of Gasoline Automotive Engine Oils by Thin-Film Oxygen Uptake (TFOUT)

SIGNIFICANCE AND USE
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.8 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.
This test method is intended to be used as a bench screening test and quality control tool for lubricating base oil manufacturing, especially for re-refined lubricating base oils. This test method is useful for quality control of oxidation stability of re-refined oils from batch to batch.
This test method is useful for screening formulated oils prior to engine tests. Within similar additive chemistry and base oil types, the ranking of oils in this test appears to be predictive of ranking in engine tests. When oils having completely different additive chemistry or base oil type are compared, oxidation stability results may not reflect the actual engine test result.
Other oxidation stability test methods have demonstrated that soluble metal catalyst supplies are very inconsistent and they have significant effects on the test results. Thus, for test comparisons, the same source and same batch of metal naphthenates shall be used.
Note 2—It is also recommended as a good research practice not to use different batches of the fuel component in test comparisons.
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 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.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are provided for information purposes only.

General Information

Status
Historical
Publication Date
09-Apr-2002
ICS
75.080 - Petroleum products in general
75.100 - Lubricants, industrial oils and related products
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.09.0G - Oxidation Testing of Engine Oils
Current Stage
Ref Project

Relations

Replaces
ASTM D4742-02 - Standard Test Method for Oxidation Stability of Gasoline Automotive Engine Oils by Thin-Film Oxygen Uptake (TFOUT)
Effective Date
10-Apr-2002
Replaced By
ASTM D4742-08 - Standard Test Method for Oxidation Stability of Gasoline Automotive Engine Oils by Thin-Film Oxygen Uptake (TFOUT)
Effective Date
15-Oct-2008
Referred By
ASTM D7098-21 - Standard Test Method for Oxidation Stability of Lubricants by Thin-Film Oxygen Uptake (TFOUT) Catalyst B
Effective Date
10-Apr-2002
Referred By
ASTM D2272-22 - Standard Test Method for Oxidation Stability of Steam Turbine Oils by Rotating Pressure Vessel
Effective Date
10-Apr-2002

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ASTM D4742-02a - Standard Test Method for Oxidation Stability of Gasoline Automotive Engine Oils by Thin-Film Oxygen Uptake (TFOUT)ASTM D4742-02a - Standard Test Method for Oxidation Stability of Gasoline Automotive Engine Oils by Thin-Film Oxygen Uptake (TFOUT)
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ASTM D4742-02a - Standard Test Method for Oxidation Stability of Gasoline Automotive Engine Oils by Thin-Film Oxygen Uptake (TFOUT)
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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: D 4742 – 02a
Standard Test Method for
Oxidation Stability of Gasoline Automotive Engine Oils by
1
Thin-Film Oxygen Uptake (TFOUT)
This standard is issued under the fixed designation D4742; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope D2272 Test Method for Oxidation Stability of Steam Tur-
4
bine Oils by Rotating Pressure Vessel
1.1 This test method evaluates the oxidation stability of
D4057 Practice for Manual Sampling of Petroleum and
engine oils for gasoline automotive engines. This test, run at
6
Petroleum Products
160°C,utilizesahighpressurereactorpressurizedwithoxygen
7
E1 Specification for ASTM Thermometers
along with a metal catalyst package, a fuel catalyst, and water
inapartialsimulationoftheconditionstowhichanoilmaybe
3. Terminology
subjected in a gasoline combustion engine. This test method
3.1 Definitions of Terms Specific to This Standard:
can be used for engine oils with viscosity in the range from 4
2 2 3.1.1 break point—the precise point of time at which rapid
mm /s (cSt) to 21 mm /s (cSt) at 100°C, including re-refined
oxidation of the oil begins.
oils.
3.1.2 oxidation induction time—thetimeuntiltheoilbegins
1.2 Thistestmethodisnotasubstitutefortheenginetesting
tooxidizeatarelativelyrapidrateasindicatedbythedecrease
of an engine oil in established engine tests, such as Sequence
of oxygen pressure.
IIID.
3.1.3 oxygen uptake—oxygen absorbed by oil as a result of
1.3 The values stated in SI units are to be regarded as the
oil oxidation.
standard. The values given in parentheses are provided for
information purposes only.
4. Summary of Test Method
1.4 This standard does not purport to address all of the
4.1 Thetestoilismixedinaglasscontainerwiththreeother
safety concerns, if any, associated with its use. It is the
liquids that are used to simulate engine conditions: (1)an
responsibility of the user of this standard to establish appro-
oxidized/nitrated fuel component (AnnexA2), (2) a mixture of
priate safety and health practices and determine the applica-
solublemetalnaphthenates(lead,copper,iron,manganese,and
bility of regulatory limitations prior to use. For specific
tin naphthenates (Annex A3)), and (3) Type II reagent water.
warning statements, see Sections 7 and 8.
4.2 The glass container holding the oil mixture is placed in
2. Referenced Documents ahighpressurereactorequippedwithapressuregage.Thehigh
pressurereactorissealed,chargedwithoxygentoapressureof
2.1 ASTM Standards:
620 kPa (90 psig), and placed in an oil bath at 160°C at an
A314 Specification for Stainless Steel Billets and Bars for
2 angle of 30° from the horizontal. The high pressure reactor is
Forging
rotatedaxiallyataspeedof100r/minformingathinfilmofoil
B211 Specification for Aluminum and Aluminum-Alloy
3 within the glass container resulting in a relatively large
Bar, Rod, and Wire
oil-oxygen contact area.
D664 TestMethodforAcidNumberofPetroleumProducts
4
by Potentiometric Titration
NOTE 1—Apressure sensing device can be used in place of a pressure
5
D1193 Specification for Reagent Water gage.
4.3 The pressure of the high pressure reactor is recorded
continuously from the beginning of the test and the test is
1 terminated when a rapid decrease of the high pressure reactor
This test method is under the jurisdiction of ASTM Committee D02 on
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee pressure is observed (Point B, Fig. A1.2). The period of time
D02.09 on Oxidation.
thatelapsesbetweenthetimewhenthehighpressurereactoris
Current edition approved April 10, 2002. Published July 2002. Originally
placedintheoilbathandthetimeatwhichthepressurebegins
published as D4742–88. Last previous edition D4742–02.
2
Annual Book of ASTM Standards, Vol 01.03.
3
Annual Book of ASTM Standards, Vol 02.02.
4 6
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 05.02.
5 7
Annual Book of ASTM Standards, Vol 11.01. Annual Book of ASTM Standards, Vol 14.03.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D 4742 – 02a
FIG. 1 Schematic Drawing of Oxidation Test Apparatus
todecreaserapidlyiscalledtheoxidationinductiontimeandis predictive of ranking in engine tests. When oils having
used as a measure of the relative oil oxidation stability. completely different additive chemistry or base oil type are
compared, oxidation stability results may not reflect the actual
5. Significance and Use
engine test result.
5.1 This test method is
...

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5.1 Insoluble material may form in oils that are subjected to oxidizing conditions.  
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SCOPE
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ASTM D4177-22e1(Practice)
Standard Practice for Automatic Sampling of Petroleum and Petroleum Products

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4.1 Representative samples of petroleum and petroleum products are required for the determination of chemical and physical properties, which are used to establish standard volumes, prices, and compliance with commercial terms and regulatory requirements. This practice does not cover sampling of electrical insulating oils and hydraulic fluids. This practice does not address how to sample crude at temperatures below the freezing point of water.
PART I—General
This part is applicable to all petroleum liquid sampling whether it be crude oil or refined products. Review this section before designing or installing any automatic sampling system.
SCOPE
1.1 This practice describes general procedures and equipment for automatically obtaining samples of liquid petroleum and petroleum products, crude oils, and intermediate products from the sample point into the primary container. This practice also provides additional specific information about sample container selection, preparation, and sample handling. If sampling is for the precise determination of volatility, use Practice D5842 (API MPMS Chapter 8.4) in conjunction with this practice. For sample mixing and handling, refer to Practice D5854 (API MPMS Chapter 8.3). This practice does not cover sampling of electrical insulating oils and hydraulic fluids.  
1.2 Table of Contents:    
Section  
INTRODUCTION  
Scope  
1  
Referenced Documents  
2  
Terminology  
3  
Significance and Use  
4  
PART I–GENERAL  
Representative Sampling Components  
5  
Design Criteria  
6  
Automatic Sampling Systems  
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Sampling Location  
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Mixing of the Flowing Stream  
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Proportionality  
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Sample Extractor Grab Volume  
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Containers  
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Sample Handling and Mixing  
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Control Systems  
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Sample System Security  
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Performance Monitoring  
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PART III–REFINED PRODUCTS  
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KEYWORDS  
Keywords  
20  
ANNEXES  
Calculations of the Margin of Error based on Number of Sample Grabs  
Annex A1  
Theoretical Calculations for Selecting the Sampler Probe Location  
Annex A2  
Portable Sampling Units  
Annex A3  
Profile Performance Test  
Annex A4  
Sampler Acceptance Test Data  
Annex A5  
APPENDIXES  
Design Data Sheet for Automatic Sampling System  
Appendix X1  
Comparisons of Percent Sediment and Water versus Unloading Time Period  
Appendix X2  
Sampling Frequency and Sampling System Monitoring Spreadsheet  
Appendix X3  
Sampling System Monitoring—Additional Diagnostics  
Appendix X4  
1.3 Units—The values stated in either SI units or US Customary (USC) units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard. Except where there is no direct SI equivalent, such as for National Pipe Threads/diameters, or tubing.  
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ASTM D4057-22(Practice)
Standard Practice for Manual Sampling of Petroleum and Petroleum Products

SIGNIFICANCE AND USE
4.1 Samples of petroleum and petroleum products are obtained for many reasons, including the determination of chemical and physical properties. These properties may be used for: calculating standard volumes; establishing product value; and often safety and regulatory reporting.  
4.2 There are inherent limitations when performing any type of sampling, any one of which may affect the representative nature of the sample. As examples, a spot sample provides a sample from only one particular point in the tank, vessel compartment, or pipeline. In the case of running or all-level samples, the sample only represents the column of material from which it was taken.  
4.3 Based on the product, and testing to be performed, this practice provides guidance on sampling equipment, container preparation, and manual sampling procedures for petroleum and petroleum products of a liquid, semi-liquid, or solid state, from the storage tanks, flowlines, pipelines, marine vessels, process vessels, drums, cans, tubes, bags, kettles, and open discharge streams into the primary sample container.
SCOPE
1.1 This practice covers procedures and equipment for manually obtaining samples of liquid petroleum and petroleum products, crude oils, and intermediate products from the sample point into the primary container are described. Procedures are also included for the sampling of free water and other heavy components associated with petroleum and petroleum products.  
1.2 This practice also addresses the sampling of semi-liquid or solid-state petroleum products. For the sampling of green petroleum coke, see Practice D8145. For the sampling of calcined petroleum coke, see Practice D6970.  
1.3 This practice provides additional specific information about sample container selection, preparation, and sample handling.  
1.4 This practice does not cover sampling of electrical insulating oils and hydraulic fluids. If sampling is for the precise determination of volatility, use Practice D5842 (API MPMS Chapter 8.4) in conjunction with this practice. For sample mixing and handling, refer to Practice D5854 (API MPMS Chapter 8.3).  
1.5 The procedures described in this practice may also be applicable in sampling most non-corrosive liquid industrial chemicals provided that all safety precautions specific to these chemicals are followed. Also, refer to Practice E300. The procedures described in this practice are also applicable to sampling liquefied petroleum gases and chemicals. Also refer to Practices D1265 and D3700. The procedure for sampling bituminous materials is described in Practice D140. Practice D4306 provides guidance on sample containers and preparation for sampling aviation fuel.  
1.6 Units—The values stated in SI units are to be regarded as the standard. USC units are reflected in parentheses.  
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ASTM D5291-21(Test Method)
Standard Test Methods for Instrumental Determination of Carbon, Hydrogen, and Nitrogen in Petroleum Products and Lubricants

SIGNIFICANCE AND USE
5.1 This is the first ASTM standard covering the simultaneous determination of carbon, hydrogen, and nitrogen in petroleum products and lubricants.  
5.2 Carbon, hydrogen, and particularly nitrogen analyses are useful in determining the complex nature of sample types covered by this test method. The CHN results can be used to estimate the processing and refining potentials and yields in the petrochemical industry.  
5.3 The concentration of nitrogen is a measure of the presence of nitrogen containing additives. Knowledge of its concentration can be used to predict performance. Some petroleum products also contain naturally occurring nitrogen. Knowledge of hydrogen content in samples is helpful in addressing their performance characteristics. Hydrogen to carbon ratio is useful to assess the performance of upgrading processes.
SCOPE
1.1 These test methods cover the instrumental determination of carbon, hydrogen, and nitrogen in laboratory samples of petroleum products and lubricants. Values obtained represent the total carbon, the total hydrogen, and the total nitrogen.  
1.2 These test methods are applicable to samples such as crude oils, fuel oils, additives, and residues for carbon and hydrogen and nitrogen analysis. These test methods were tested in the concentration range of at least 75 % to 87 % by mass for carbon, at least 9 % to 16 % by mass for hydrogen, and  
1.3 The nitrogen test method is not applicable to light materials or those containing  
1.3.1 However, using Test Method D levels of 0.1 % by mass nitrogen in lubricants could be determined.  
1.4 These test methods are not recommended for the analysis of volatile materials such as gasoline, gasoline-oxygenate blends, or gasoline type aviation turbine fuels.  
1.5 The results of these tests can be expressed as mass % carbon, hydrogen or nitrogen.  
1.6 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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ASTM
ASTM D6304-20(Test Method)
Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fischer Titration

SIGNIFICANCE AND USE
5.1 A knowledge of the water content is important in the manufacturing, purchase, sale, or transfer of petroleum products to help in predicting their quality and performance characteristics.  
5.2 The presence of moisture could lead to premature corrosion and wear, an increase in the debris load resulting in diminished lubrication and premature plugging of filters, an impedance in the effect of additives, and undesirable support of deleterious bacterial growth.
SCOPE
1.1 This test method covers the direct determination of entrained water in petroleum products and hydrocarbons using automated instrumentation. This test method also covers the indirect analysis of water thermally removed from samples and swept with dry inert gas into the Karl Fischer titration cell. Mercaptan, sulfide (S– or H2S), sulfur, and other compounds are known to interfere with this test method (see Section 6). The precision statement of this method covers the nominal range of 20 mg/kg to 25 000 mg/kg for Procedure A, 30 mg/kg to 2100 mg/kg for Procedure B, and 20 mg/kg to 360 mg/kg for Procedure C.  
1.2 This test method is intended for use with commercially available coulometric Karl Fischer reagents and for the determination of water in additives, lube oils, base oils, automatic transmission fluids, hydrocarbon solvents, and other petroleum products. By proper choice of the sample size, this test method may be used for the determination of water from mg/kg to percent level concentrations.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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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