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ASTM D3524-14

(Test Method)

Standard Test Method for Diesel Fuel Diluent in Used Diesel Engine Oils by Gas Chromatography

Standard Test Method for Diesel Fuel Diluent in Used Diesel Engine Oils by Gas Chromatography

SIGNIFICANCE AND USE
5.1 Some fuel dilution of the engine oil may take place during normal operation. However, excessive fuel dilution is of concern in terms of possible performance problems. This method provides a means to determine the magnitude of the fuel dilution, providing the user with the ability to predict performance and to take appropriate action.
SCOPE
1.1 This test method covers the use of gas chromatography to determine the amount of diesel fuel in used engine lubricating oil. This test is limited to SAE 30 oil. The diesel fuel diluent is analyzed at concentrations up to 12 mass %.Note 1—This test method may be applicable to higher viscosity grade oils. However, such oils were not included in the program used to develop the precision statement.  
1.2 This test method is limited to gas chromatographs equipped with flame ionization detectors and temperature programmable ovens. Note 2—The use of other detectors and instrumentation has been reported. However, the precision statement applies only when the instrumentation specified is employed.  
1.3 There is some overlap of the boiling ranges of diesel fuel and SAE 30 engine oils. Moreover, the boiling range of SAE 30 oils from various sources can vary appreciably. As a result, the calibration can be altered by as much as 2 %, in terms of fuel dilution. When testing unknown or mixed brands of used engine oil, it should be realized that the precision of the method may be poorer than the precision obtained when calibrating with a new oil representative of the used oil being tested.  
1.4 The values stated in SI units are to be regarded as the standard. The values stated in inch-pound units are for information only.  
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 and health practices and determine the applicability of regulatory requirements prior to use.

General Information

Status
Historical
Publication Date
30-Apr-2014
ICS
75.100 - Lubricants, industrial oils and related products
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.B0 - Automotive Lubricants
Current Stage
Ref Project

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ASTM D3524-14 - Standard Test Method for Diesel Fuel Diluent in Used Diesel Engine Oils by Gas ChromatographyASTM D3524-14 - Standard Test Method for Diesel Fuel Diluent in Used Diesel Engine Oils by Gas Chromatography
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ASTM D3524-14 - Standard Test Method for Diesel Fuel Diluent in Used Diesel Engine Oils by Gas Chromatography
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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: D3524 − 14
Standard Test Method for
Diesel Fuel Diluent in Used Diesel Engine Oils by Gas
1
Chromatography
This standard is issued under the fixed designation D3524; 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.
1. Scope 2. Referenced Documents
2
1.1 This test method covers the use of gas chromatography 2.1 ASTM Standards:
to determine the amount of diesel fuel in used engine lubricat- D4626 Practice for Calculation of Gas Chromatographic
ing oil. This test is limited to SAE 30 oil. The diesel fuel Response Factors
diluent is analyzed at concentrations up to 12 mass %. E260 Practice for Packed Column Gas Chromatography
NOTE 1—This test method may be applicable to higher viscosity grade
E355 Practice for Gas ChromatographyTerms and Relation-
oils. However, such oils were not included in the program used to develop
ships
the precision statement.
E594 Practice for Testing Flame Ionization Detectors Used
1.2 This test method is limited to gas chromatographs
in Gas or Supercritical Fluid Chromatography
equipped with flame ionization detectors and temperature
E1510 Practice for Installing Fused Silica Open Tubular
programmable ovens.
Capillary Columns in Gas Chromatographs
NOTE 2—The use of other detectors and instrumentation has been
reported. However, the precision statement applies only when the instru- 3. Terminology
mentation specified is employed.
3.1 Definitions:
1.3 There is some overlap of the boiling ranges of diesel
3.1.1 For definition of gas chromatography terms, refer to
fuel and SAE 30 engine oils. Moreover, the boiling range of
Practice E355.
SAE 30 oils from various sources can vary appreciably. As a
3.2 Definitions of Terms Specific to This Standard:
result, the calibration can be altered by as much as 2 %, in
3.2.1 fuel dilution, n—the amount, expressed as a
terms of fuel dilution. When testing unknown or mixed brands
percentage, of diesel fuel found in engine lubricating oil.
ofusedengineoil,itshouldberealizedthattheprecisionofthe
3.2.1.1 Discussion—Fuel dilution may be the result of
method may be poorer than the precision obtained when
engine wear or improper performance.
calibrating with a new oil representative of the used oil being
3.2.2 fuel diluent, n—in used oil analysis, is the unburned
tested.
fuel components that enter the engine crankcase causing
1.4 The values stated in SI units are to be regarded as the
dilution of the oil.
standard. The values stated in inch-pound units are for infor-
3.2.2.1 Discussion—In this method, the fuel diluent compo-
mation only.
nents being determined are from diesel fuel.
1.5 This standard does not purport to address all of the
3.3 Abbreviations:
safety concerns, if any, associated with its use. It is the
3.3.1 Acommonabbreviationofhydrocarboncompoundsis
responsibility of the user of this standard to establish appro-
to designate the number of carbon atoms in the compound. A
priate safety and health practices and determine the applica-
prefix is used to indicate the carbon chain form, while a
bility of regulatory requirements prior to use.
subscripted suffix denotes the number of carbon atoms.
For example: normal decane n–C
10
iso-tetradecane i–C
14
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
2
Subcommittee D02.B0 on Automotive Lubricants. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2014. Published May 2014. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1976. Last previous edition approved in 2004 as D3524 – 04, which Standards volume information, refer to the standard’s Document Summary page on
was withdrawn January 2013 and reinstated May 2014. DOI: 10.1520/D3524-14. the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D3524 − 14
4. Summary of Test Method temperature required. Connection of the column to the sample
inlet system must be such that no temperature zones below the
4.1 Gas chromatographic techniques are used for analyzing
column temperature (cold spots) exist.
the samples, by adding a known percentage of n-decane as an
internal standard, in order to determine the mass percent of 6.2 Data Acquisition System:
diesel fuel in the lubricating oil. A calibration curve is 6.2.1 Integrator—Means must be provid
...

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ASTM D6792-23c(Practice)
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4.1 A petroleum products, liquid fuels, and lubricants testing laboratory plays a crucial role in product quality management and customer satisfaction. It is essential for a laboratory to provide quality data. This document provides guidance for establishing and maintaining a quality management system in a laboratory.  
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Standard Test Method for Bromine Numbers of Petroleum Distillates and Commercial Aliphatic Olefins by Electrometric Titration

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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.  
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1.4 The values stated in SI units are to be regarded as the standard.  
1.4.1 Exception—The values given in parentheses are for information only.  
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Standard Test Method for Low-Temperature Viscosity of Automatic Transmission Fluids, Hydraulic Fluids, and Lubricants using a Rotational Viscometer

SIGNIFICANCE AND USE
5.1 The low-temperature, low-shear-rate viscosity of automatic transmission fluids, gear oils, torque and tractor fluids, and industrial and automotive hydraulic oils (see Appendix X4) are of considerable importance to the proper operation of many mechanical devices. Measurement of the viscometric properties of these oils and fluids at low temperatures is often used to specify their acceptance for service. This test method is used in a number of specifications.  
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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.  
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1.1 This test method covers the use of rotational viscometers with an appropriate torque range and specific spindle for the determination of the low-shear-rate viscosity of automatic transmission fluids, gear oils, hydraulic fluids, and some lubricants. This test method covers the viscosity range of 300 mPa·s to 900 000 mPa·s  
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1.4.2 The viscosity data used for Procedure D precision study was from 6400 mPa·s to 256 000 mPa·s at test temperatures of –26 °C and –40 °C.  
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5.1 This test simulates a type of severe field service in which corrosion-promoting moisture in the form of condensed water vapor accumulates in the axle assembly. This may happen as a result of volume expansion and contraction of the axle lubricant and the accompanied breathing in of moisture-laden air through the axle vent. The test screens lubricants for their ability to prevent the expected corrosion.  
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Standard Practice for Condition Monitoring of In-Service Lubricants by Trend Analysis Using Fourier Transform Infrared (FT-IR) Spectrometry

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5.1 Periodic sampling and analysis of lubricants have long been used as a means to determine overall machinery health. Atomic emission (AE) and atomic absorption (AA) spectroscopy are often employed for wear metal analysis (for example, Test Method D5185). A number of physical property tests complement wear metal analysis and are used to provide information on lubricant condition (for example, Test Methods D445, D2896, and D6304). Molecular analysis of lubricants and hydraulic fluids by FT-IR spectroscopy produces direct information on molecular species of interest, including additives, fluid breakdown products and external contaminants, and thus complements wear metal and other analyses used in a condition monitoring program (1, 2-6).
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1.1 This practice covers the use of FT-IR in monitoring additive depletion, contaminant buildup and base stock degradation in machinery lubricants, hydraulic fluids and other fluids used in normal machinery operation. Contaminants monitored include water, soot, ethylene glycol, fuels and incorrect oil. Oxidation, nitration and sulfonation of base stocks are monitored as evidence of degradation. The objective of this monitoring activity is to diagnose the operational condition of the machine based on fault conditions observed in the oil. Measurement and data interpretation parameters are presented to allow operators of different FT-IR spectrometers to compare results by employing the same techniques.  
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1.3 Spectra and distribution profiles presented herein are for illustrative purposes only and are not to be construed as representing or establishing lubricant or machinery guidelines.  
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1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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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.  
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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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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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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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