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ASTM D7963-14

(Test Method)

Standard Test Method for Determination of Contamination Level of Fatty Acid Methyl Esters in Middle Distillate and Residual Fuels Using Flow Analysis by Fourier Transform Infrared Spectroscopy—Rapid Screening Method

Standard Test Method for Determination of Contamination Level of Fatty Acid Methyl Esters in Middle Distillate and Residual Fuels Using Flow Analysis by Fourier Transform Infrared Spectroscopy—Rapid Screening Method

SIGNIFICANCE AND USE
5.1 The present and growing international governmental requirements to add Fatty Acid Methyl Esters (FAME) to diesel fuel has had the unintended side-effect of leading to potential FAME contamination of fuels in multi-fuel transport facilities such as cargo tankers and pipelines, and industry wide concerns. This has led to a requirement to measure contamination levels in diesel and other fuels to assist custody transfer issues.  
5.2 Analytical methods have been developed with the capability of measuring down to  
5.3 A similar procedure, Test Method D7797, is available for AVTUR in the range 20 mg/kg to 150 mg/kg. Test Method D7797 uses the same apparatus, with a specific model developed for AVTUR.
SCOPE
1.1 This test method specifies a rapid screening method using flow analysis by Fourier Transform Infrared (FA-FTIR) spectroscopy with partial least squares (PLS) processing for the quantitative determination of the fatty acid methyl ester (FAME) contamination of middle distillates, in the range of 20 mg/kg to 1000 mg/kg, and of middle distillates and residual fuels, following dilution, for levels above 0.1 %.
Note 1: Annex A2 describes a dilution procedure to significantly expand the measurement range above 1000 mg/kg for distillates and to enable measurement of residual oils
Note 2: This test method detects all FAME components, with peak IR absorbance at approximately 1749 cm-1 and C8 to C22 molecules, as specified in standards such as D6751 and EN 14214. The accuracy of the test method is based on the molecular mass of C16 to C18 FAME species; the presence of other FAME species with different molecular masses could affect the accuracy.
Note 3: Additives such as antistatic agents, antioxidants, and corrosion inhibitors are measured with the FAME by the FTIR spectrometer. However any potential interference effects of these additives are eliminated by the flow analysis processing.
Note 4: Precision for middle distillate and residual fuel is provided in preliminary form at this time, details are given in Appendix X1.
Note 5: The scope of this test method does not include aviation turbine fuel which is addressed by Test Method D7797.  
1.2 All stated values are in SI units.  
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.

General Information

Status
Historical
Publication Date
30-Sep-2014
ICS
75.160.20 - Liquid fuels
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.14 - Stability, Cleanliness and Compatibility of Liquid Fuels
Current Stage
Ref Project

Relations

Replaced By
ASTM D7963-19 - Standard Test Method for Determination of Contamination Level of Fatty Acid Methyl Esters in Middle Distillate and Residual Fuels Using Flow Analysis by Fourier Transform Infrared Spectroscopy—Rapid Screening Method
Effective Date
01-Jun-2019
Referred By
ASTM D8274-20a - Standard Test Method for Determination of Biodiesel (Fatty Acid Methyl Esters) Content in Diesel Fuel Oil by Portable Rapid Mid-Infrared Analyzer
Effective Date
01-Oct-2014

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ASTM D7963-14 - Standard Test Method for Determination of Contamination Level of Fatty Acid Methyl Esters in Middle Distillate and Residual Fuels Using Flow Analysis by Fourier Transform Infrared Spectroscopy—Rapid Screening MethodASTM D7963-14 - Standard Test Method for Determination of Contamination Level of Fatty Acid Methyl Esters in Middle Distillate and Residual Fuels Using Flow Analysis by Fourier Transform Infrared Spectroscopy—Rapid Screening Method
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ASTM D7963-14 - Standard Test Method for Determination of Contamination Level of Fatty Acid Methyl Esters in Middle Distillate and Residual Fuels Using Flow Analysis by Fourier Transform Infrared Spectroscopy—Rapid Screening Method
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Standards Content (Sample)

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: D7963 − 14
Standard Test Method for
Determination of Contamination Level of Fatty Acid Methyl
Esters in Middle Distillate and Residual Fuels Using Flow
Analysis by Fourier Transform Infrared Spectroscopy—
1
Rapid Screening Method
This standard is issued under the fixed designation D7963; 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 specifies a rapid screening method 2.1 ASTM Standards:
using flow analysis by Fourier Transform Infrared (FA-FTIR) D1298 Test Method for Density, Relative Density, or API
spectroscopywithpartialleastsquares(PLS)processingforthe Gravity of Crude Petroleum and Liquid Petroleum Prod-
quantitative determination of the fatty acid methyl ester ucts by Hydrometer Method
(FAME) contamination of middle distillates, in the range of D4052 Test Method for Density, Relative Density, and API
20 mg⁄kgto1000 mg⁄kg,andofmiddledistillatesandresidual Gravity of Liquids by Digital Density Meter
fuels, following dilution, for levels above 0.1 %. D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
NOTE 1—Annex A2 describes a dilution procedure to significantly
D4177 Practice for Automatic Sampling of Petroleum and
expand the measurement range above 1000 mg/kg for distillates and to
Petroleum Products
enable measurement of residual oils
NOTE 2—This test method detects all FAME components, with peak IR
D6751 Specification for Biodiesel Fuel Blend Stock (B100)
-1
absorbance at approximately 1749 cm and C to C molecules, as
8 22
for Middle Distillate Fuels
specified in standards such as D6751 and EN 14214. The accuracy of the
D7797 Test Method for Determination of the Fatty Acid
test method is based on the molecular mass of C to C FAME species;
16 18
Methyl Esters Content of Aviation Turbine Fuel Using
thepresenceofotherFAMEspecieswithdifferentmolecularmassescould
Flow Analysis by Fourier Transform Infrared Spectros-
affect the accuracy.
NOTE 3—Additives such as antistatic agents, antioxidants, and corro-
copy – Rapid Screening Method
sion inhibitors are measured with the FAME by the FTIR spectrometer.
E1655 Practices for Infrared Multivariate Quantitative
However any potential interference effects of these additives are elimi-
Analysis
nated by the flow analysis processing.
3
2.2 CEN Standard:
NOTE 4—Precision for middle distillate and residual fuel is provided in
preliminary form at this time, details are given in Appendix X1. EN 14214 Automotive Fuels—Fatty Acid Methyl Esters
NOTE 5—The scope of this test method does not include aviation
(FAME) for Diesel Engines—Requirements and Test
turbine fuel which is addressed by Test Method D7797.
Methods
4
1.2 All stated values are in SI units.
2.3 Energy Institute Standards:
IP 583 Test Method for Determination of the Fatty Acid
1.3 This standard does not purport to address all of the
Methyl Esters Content of Aviation Turbine Fuel Using
safety concerns, if any, associated with its use. It is the
Flow Analysis by Fourier Transform Infrared
responsibility of the user of this standard to establish appro-
Spectroscopy—Rapid Screening Method
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contactASTM Customer Service at service@astm.org. ForAnnual Book ofASTM
Standards volume information, refer to the standard’s Document Summary page on
1
This test method is under the jurisdiction of ASTM Committee D02 on the ASTM website.
3 rd
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Available from theAmerican National Standards Institute (ANSI) 25W43 St,
th
Subcommittee D02.14 on Stability and Cleanliness of Liquid Fuels. 4 Floor. New York, NY 10036.
4
Current edition approved Oct. 1, 2014. Published October 2014. DOI: 10.1520/ Available from the Energy Institute, 61 New Cavendish Street, London,
D7963-14. W1G7AR, U.K. www.energyinst.org.uk.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7963 − 14
3. Terminology 6. Apparatus
3.1 Definitions: 6.1 Automatically controlled, closely integrated instrument
3.1.1 FAME, n—fatty acid methyl esters, also known as comprising a FTIR spectrometer witha2mmeffective optical
biodiesel. path length flow-through cell, computer controlled pump,
sorbent cartridge holder, control and interface electronics, test
3.1.1.1 Discussion—Used as a component in auto
...

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5.1 This guide is intended for the developers or sponsors of new aviation gasolines or additives to describe the data requirements necessary to support the development of specifications for these new products by ASTM members. The ultimate goal of the data generated in accordance with this guide is to provide an understanding of the performance of the new fuel or additive within the property constraints and compositional bounds of the proposed specification criteria.  
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1.3 These research reports are intended to support the development and issuance of new specifications or specification revisions for these products. Guidance to develop ASTM International standard specifications for aviation gasoline is provided in Subcommittee J on Aviation Fuels Operating Procedures, Annex A6, “Guidelines for the Development and Acceptance of a New Aviation Fuel Specification for Spark-Ignition Reciprocating Engines.”  
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5.1 Some acids can be present in aviation turbine fuels due either to the acid treatment during the refining process or to naturally occurring organic acids. Significant acid contamination is not likely to be present because of the many check tests made during the various stages of refining. However, trace amounts of acid can be present and are undesirable because of the consequent tendencies of the fuel to corrode metals that it contacts or to impair the water separation characteristics of the aviation turbine fuel.  
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1.1 This test method covers the determination of the acidity in aviation turbine fuel in the range from 0.000 mg/g to 0.100 mg/g KOH.  
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5.1 Wear due to excessive friction resulting in shortened life of engine components such as fuel pumps and fuel controls has sometimes been ascribed to lack of lubricity in an aviation fuel.  
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1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address 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.  
1.4 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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5.1 The boiling range distribution of FAMES provides an insight into the composition of product related to the transesterification process. This gas chromatographic determination of boiling range can be used to replace conventional distillation methods for product specification testing with the mutual agreement of interested parties.  
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1.1 This test method covers the determination of the boiling range distribution of fatty acid methyl esters (FAME). This test method is applicable to FAMES (biodiesel, B100) having an initial boiling point greater than 100 °C and a final boiling point less than 615 °C at atmospheric pressure as measured by this test method.  
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1.6 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
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5.2 The design of the engine used in this test method is representative of many, but not all, modern diesel engines. This factor, along with the accelerated operating conditions, shall be considered when extrapolating test results.
SCOPE
1.1 This test method, commonly referred to as the Cummins ISB Test, covers the utilization of a modern, 5.9 L, diesel engine equipped with exhaust gas recirculation and is used to evaluate oil performance with regard to valve-train wear.  
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—SI units are provided for all parameters except where there is no direct equivalent such as the units for screw threads, National Pipe Threads/diameters, tubing size, or where there is a sole source of supply equipment specification.  
1.2.2 See also A7.1 for clarification; it does not supersede 1.2 and 1.2.1.  
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 Table of Contents:    
Section  
Scope  
1  
Referenced Documents  
2  
Terminology  
3  
Summary of Test Method  
4  
Significance and Use  
5  
Apparatus  
6  
Engine Fluids and Cleaning Solvents  
7  
Preparation of Apparatus  
8  
Engine/Stand Calibration and Non-Reference Oil Tests  
9  
Test Procedure  
10  
Calculations, Ratings, and Test Validity  
11  
Report  
12  
Precision and Bias  
13  
Annexes  
Safety Precautions  
Annex A1  
Intake Air Aftercooler  
Annex A2  
The Cummins ISB Engine Build Parts Kit  
Annex A3  
Sensor Locations and Special Hardware  
Annex A4  
External Oil System  
Annex A5  
Cummins Service Publications  
Annex A6  
Specified Units and Formats  
Annex A7  
Oil Analyses  
Annex A8  
Alternate Fuel Approval Process  
Annex A9  
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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