ASTM D7111-16

Standard Test Method for Determination of Trace Elements in Middle Distillate Fuels by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

SIGNIFICANCE AND USE
5.1 Trace elemental analysis is used to indicate the level of contamination of middle distillate fuels. Trace metals in turbine fuels can cause corrosion and deposition on turbine components at elevated temperatures. Some diesel fuels have specification limit requirements for trace metals to guard against engine deposits. Trace level copper in middle distillate aviation turbine fuel can significantly accelerate thermal instability of the fuel, leading to oxidation and production of detrimental insoluble deposits in the engine.  
5.2 Gas turbine fuel oil Specification D2880 provides recommended upper limits for five trace metals (calcium, lead, sodium, potassium, and vanadium). Military specification MIL-DTL-16884 for naval distillate fuel sets requirements for maximum concentrations of the same five metals. Both specifications designate Test Method D3605, an atomic absorption/flame emission method, for the quantitative analysis of four of the metals. Test Method D3605 does not cover potassium. This test method provides an alternative to Test Method D3605, covers potassium and a number of additional elements.  
5.3 There are several sources of multi-element contamination of naval distillate fuel. Sea water is pumped into the diesel fuel tanks (as ballast) to trim ships. Also, some of the oilers (fuel supply ships) have dirty tanks. Corrosion products come from unlined tanks, piping, pumps, and heat exchangers.
SCOPE
1.1 This test method covers the determination of selected elements in middle distillate fuels by inductively coupled plasma atomic emission spectrometry (ICP-AES). The specific elements are listed in Table 1. The concentration range of this test method is approximately 0.1 mg/kg to 2.0 mg/kg. The test method may be used for concentrations outside of this range; however, the precision statements may not be applicable. Middle distillate fuels covered in this test method have all distillation fractions contained within the boiling range of 150 °C to 390 °C. This includes, but is not limited to, diesel fuels and aviation turbine fuels.  
1.2 This test method is not intended to analyze insoluble particulates. However, very small particulate matter (smaller than a micrometre) will be carried into the plasma and be included in the quantitative analysis.  
1.3 This test method may give a result that is higher than the true value if an analyte is present in the sample in a form which is sufficiently volatile. For example, hexamethyldisiloxane will generate a biased high result for silicon.  
1.4 The values stated in SI units are to be regarded as 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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 30-Nov-2016
• ICS: 75.160.20 - Liquid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

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: D7111 − 16
Standard Test Method for
Determination of Trace Elements in Middle Distillate Fuels
by Inductively Coupled Plasma Atomic Emission
1
Spectrometry (ICP-AES)
This standard is issued under the fixed designation D7111; 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* D3605 Test Method for Trace Metals in Gas Turbine Fuels
by Atomic Absorption and Flame Emission Spectroscopy
1.1 This test method covers the determination of selected
D4057 Practice for Manual Sampling of Petroleum and
elements in middle distillate fuels by inductively coupled
Petroleum Products
plasma atomic emission spectrometry (ICP-AES). The specific
D4306 Practice for Aviation Fuel Sample Containers for
elements are listed in Table 1. The concentration range of this
Tests Affected by Trace Contamination
test method is approximately 0.1 mg⁄kg to 2.0 mg/kg. The test
D5185 Test Method for Multielement Determination of
method may be used for concentrations outside of this range;
Used and Unused Lubricating Oils and Base Oils by
however, the precision statements may not be applicable.
Inductively Coupled Plasma Atomic Emission Spectrom-
Middle distillate fuels covered in this test method have all
etry (ICP-AES)
distillation fractions contained within the boiling range of
D6299 Practice for Applying Statistical Quality Assurance
150 °C to 390 °C. This includes, but is not limited to, diesel
and Control Charting Techniques to Evaluate Analytical
fuels and aviation turbine fuels.
Measurement System Performance
1.2 This test method is not intended to analyze insoluble
D6792 Practice for Quality System in Petroleum Products
particulates. However, very small particulate matter (smaller
and Lubricants Testing Laboratories
than a micrometre) will be carried into the plasma and be
D7260 Practice for Optimization, Calibration, and Valida-
included in the quantitative analysis.
tion of Inductively Coupled Plasma-Atomic Emission
Spectrometry (ICP-AES) for ElementalAnalysis of Petro-
1.3 Thistestmethodmaygivearesultthatishigherthanthe
truevalueifananalyteispresentinthesampleinaformwhich leum Products and Lubricants
is sufficiently volatile. For example, hexamethyldisiloxane will
2.2 Military Standard:
3
generate a biased high result for silicon.
MIL-DTL-16884 Fuel, Naval Distillate
1.4 The values stated in SI units are to be regarded as
3. Terminology
standard.
1.5 This standard does not purport to address all of the 3.1 Definitions:
3.1.1 calibration, n—the determination of the values of the
safety concerns, if any, associated with its use. It is the
significant parameters by comparison with values indicated by
responsibility of the user of this standard to establish appro-
a set of reference standards.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
3.1.2 calibration curve, n—the graphical or mathematical
representation of a relationship between the assigned (known)
2. Referenced Documents
values of standards and the measured responses from the
2
2.1 ASTM Standards:
measurement system.
D2880 Specification for Gas Turbine Fuel Oils
3.1.3 calibration standard, n—a standard having an ac-
cepted value (reference value) for use in calibrating a measure-
1
This test method is under the jurisdiction of ASTM Committee D02 on
ment instrument or system.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
3.1.4 detection limit, n—a stated limiting value that desig-
Current edition approved Dec. 1, 2016. Published December 2016. Originally
nates the lowest concentration that can be determined with
approved in 2005. Last previous edition approved in 2015 as D7111 – 15a. DOI:
10.1520/D7111-16. confidence and that is specific to the analytical procedure used.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
3
the ASTM website. Available online at http://quicksearch.dla.mil or http://assistdocs.com
*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

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D7111−16
TABLE 1 Elements and Recommended Wavelengths TABLE 2 Internal Standards, Recommended Wavelengths, and
Approximate Use Concentrations
Element Wavelengths, nm
Internal Wavelength, Concentrati
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D7111 − 15a D7111 − 16
Standard Test Method for
Determination of Trace Elements in Middle Distillate Fuels
by Inductively Coupled Plasma Atomic Emission
1
Spectrometry (ICP-AES)
This standard is issued under the fixed designation D7111; 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*
1.1 This test method covers the determination of selected elements in middle distillate fuels by inductively coupled plasma
atomic emission spectrometry (ICP-AES). The specific elements are listed in Table 1. The concentration range of this test method
is approximately 0.1 mg ⁄kg to 2.0 mg/kg. The test method may be used for concentrations outside of this range; however, the
precision statements may not be applicable. Middle distillate fuels covered in this test method have all distillation fractions
contained within the boiling range of 150 °C to 390 °C. This includes, but is not limited to, diesel fuels and aviation turbine fuels.
1.2 This test method is not intended to analyze insoluble particulates. However, very small particulate matter (smaller than a
micrometre) will be carried into the plasma and be included in the quantitative analysis.
1.3 This test method may give a result that is higher than the true value if an analyte is present in the sample in a form which
is sufficiently volatile. For example, hexamethyldisiloxane will generate a biased high result for silicon.
1.4 The values stated in SI units are to be regarded as standard.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved July 1, 2015Dec. 1, 2016. Published August 2015December 2016. Originally approved in 2005. Last previous edition approved in 2015 as
D7111 – 15.D7111 – 15a. DOI: 10.1520/D7111-15A.10.1520/D7111-16.
TABLE 1 Elements and Recommended Wavelengths
Element Wavelengths, nm
Aluminum 308.215, 396.153
Barium 455.403, 493.408
Calcium 393.366
Chromium 267.716, 283.563
Cobalt 228.615, 236.375, 238.892
Copper 324.752
Iron 259.939
Lithium 670.784
Lead 220.353, 224.688, 283.306
Magnesium 279.553
Manganese 257.610
Molybdenum 202.030, 204.597, 281.616
Nickel 221.648, 341.476
Phosphorus 177.495, 178.287,
185.944, 214.914, 213.618
Palladium 340.458, 342.124
Platinum 214.423
Potassium 766.490
Sodium 588.995
Silicon 251.611
Silver 328.068
Strontium 407.771
Tin 283.999, 189.991
Titanium 334.940
Vanadium 310.230
Zinc 213.857
*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 ----------------------
D7111 − 16
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
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D2880 Specification for Gas Turbine Fuel Oils
D3605 Test Method for Trace Metals in Gas Turbine Fuels by Atomic Absorption and Flame Emission Spectroscopy
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4306 Practice for Aviation Fuel Sample Containers for Tests Affected by Trace Contamination
D5185 Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils by Inductively
Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories
D7260 Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry
(ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
2.2 Military Standard:
3
MIL-DTL-16884 Fuel, Naval Distillate
3. Terminology
3.1 Definitions:
3.1.1 calibration, n—the determination of the values of the significant parameters by comparison with values indicated by a set
of reference standards.
3.1.2 calibration curve, n—the graphical or mathematical
...