ASTM D7343-20
(Practice)Standard Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods for Elemental Analysis of Petroleum Products and Lubricants
Standard Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods for Elemental Analysis of Petroleum Products and Lubricants
SIGNIFICANCE AND USE
3.1 Accurate elemental analyses of samples of petroleum and petroleum products are required for the determination of chemical properties, which are in turn used to establish compliance with commercial and regulatory specifications.
SCOPE
1.1 This practice covers information relating to sampling, calibration and validation of X-ray fluorescence instruments for elemental analysis, including all kinds of wavelength dispersive (WDXRF) and energy dispersive (EDXRF) techniques. This practice includes sampling issues such as the selection of storage vessels, transportation, and sub-sampling. Treatment, assembly, and handling of technique-specific sample holders and cups are also included. Technique-specific requirements during analytical measurement and validation of measurement for the determination of trace elements in samples of petroleum and petroleum products are described. For sample mixing, refer to Practice D5854. Petroleum products covered in this practice are considered to be a single phase and exhibit Newtonian characteristics at the point of sampling.
1.2 Applicable Test Methods—This practice is applicable to the XRF methods under the jurisdiction of ASTM Subcommittee D02.03 on Elemental Analysis, and those under the jurisdiction of the Energy Institute’s Test Method Standardization Committee (Table 1). Some of these methods are technically equivalent though they may differ in details (Table 2).
1.3 Applicable Fluids—This practice is applicable to petroleum and petroleum products with vapor pressures at sampling and storage temperatures less than or equal to 101 kPa (14.7 psi). Use Practice D4057 or IP 475 to sample these materials. Refer to Practice D5842 when sampling materials that also require Reid vapor pressure (RVP) determination.
1.4 Non-applicable Fluids—Petroleum products whose vapor pressure at sampling and sample storage conditions are above 101 kPa (14.7 psi) and liquefied gases (that is, LNG, LPG, etc.) are not covered by this practice.
1.5 Sampling Methods—The physical sampling and methods of sampling from a primary source are not covered by this guide. It is assumed that samples covered by this practice are a representative sample of the primary source liquid. Refer to Practice D4057 or IP 475 for detailed sampling procedures.
1.6 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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.
General Information
- Status
- Published
- Publication Date
- 30-Jun-2020
- Technical Committee
- D02 - Petroleum Products, Liquid Fuels, and Lubricants
- Drafting Committee
- D02.03 - Elemental Analysis
Relations
- Effective Date
- 01-Mar-2024
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Nov-2023
- Refers
ASTM D5842-23 - Standard Practice for Sampling and Handling of Fuels for Volatility Measurement - Effective Date
- 01-Oct-2023
- Refers
ASTM D5842-19 - Standard Practice for Sampling and Handling of Fuels for Volatility Measurement - Effective Date
- 01-Nov-2019
- Effective Date
- 01-Aug-2019
- Effective Date
- 01-Aug-2019
- Effective Date
- 01-May-2019
- Effective Date
- 01-May-2019
- Effective Date
- 01-Jul-2018
- Effective Date
- 15-Dec-2017
- Effective Date
- 15-Nov-2017
- Effective Date
- 01-Jul-2017
- Effective Date
- 01-May-2017
- Effective Date
- 01-Jan-2017
Overview
ASTM D7343-20 defines a standardized practice for the optimization, sample handling, calibration, and validation of X-ray fluorescence (XRF) spectrometry methods for elemental analysis of petroleum products and lubricants. This standard applies to both wavelength dispersive (WDXRF) and energy dispersive (EDXRF) XRF techniques. Accurate elemental analysis is critical to determine chemical properties, regulate product quality, and ensure compliance with various commercial and regulatory specifications.
This standard addresses issues such as proper sample handling, preparation, storage, instrument calibration, and validation of analytical results. By following ASTM D7343-20, laboratories can improve the reliability and comparability of their elemental analysis results using XRF technology in petroleum and lubricant industries.
Key Topics
Sampling and Sample Preparation
- Guidance on selecting appropriate storage vessels and transportation methods to minimize contamination.
- Instructions for assembling and managing sample holders and films specific to XRF analysis.
- Emphasis on clean lab practices, blank sample analyses, and contamination control.
Applicable Fluids and Limitations
- Covers petroleum products and lubricants with vapor pressure ≤101 kPa (14.7 psi) at sampling/storage temperatures.
- Not suitable for products exceeding this vapor pressure, such as LNG and LPG.
- Assumes samples are of single phase and have Newtonian characteristics.
Instrument Setup and Measurement
- Detailed requirements for WDXRF and EDXRF instrument verification, quality control, and optimal parameter settings.
- Addressing common instrument interferences and the use of standards/blanks for bias correction.
- Procedures for sample cup preparation, leak checks, and immediate measurement for sensitive or volatile samples.
Calibration and Validation
- Regression techniques for calibration, with methods to handle background correction, line overlap, and matrix effects.
- Importance of quality control samples, routine validation checks, and compliance with statistical quality control practices.
Applications
The ASTM D7343-20 standard practice is essential in various contexts:
Refineries and Analytical Laboratories
- Routine testing of feedstocks and finished petroleum products for trace elements such as sulfur, lead, vanadium, and nickel.
- Ensures compliance with environmental regulations, fuel standards, and commercial contracts.
Lubricant Blending & Quality Control
- Analysis of additives (e.g., zinc, phosphorus, calcium) in lubricating oils for product formulation and performance monitoring.
Research and Development
- Supporting development of new petroleum products by providing accurate elemental composition data to inform product design.
Regulatory and Certification Compliance
- Assisting in meeting requirements for national and international fuel and lubricant quality, including environmental limits on sulfur or lead.
Related Standards
ASTM D7343-20 is designed for use alongside key XRF test methods and sampling protocols, including but not limited to:
- ASTM D2622 - Wavelength Dispersive XRF for Sulfur in Petroleum Products
- ASTM D4294 - Energy Dispersive XRF for Sulfur in Petroleum Products
- ASTM D4927, D4929 - Elemental analysis in lubricants and organic chlorides in crude oil
- ASTM D6376, D6443, D6481, D7039, D7212, D7220, D7751, D7757, D8127, D8252 - Additional methods for measuring various elements in petroleum and lubricant matrices
- ASTM D4057, Practice D5842, Practice D5854 - Guidelines for sampling and handling liquid petroleum products, including mixing and volatility measurement
- Referenced Energy Institute (EI/IP) Methods - Complementary procedures for specific analytes and product types
Conclusion
By adhering to ASTM D7343-20, laboratories ensure optimal sample handling, accurate calibration, and robust validation in XRF elemental analysis of petroleum products and lubricants. This standard enables confidence in data quality, supports regulatory compliance, and enhances the reliability of results across global supply chains in the petroleum and lubricant sectors.
Keywords: ASTM D7343, XRF spectrometry, elemental analysis, petroleum products, lubricants, WDXRF, EDXRF, calibration, sample handling, validation, sulfur analysis, lubricant additives, quality control.
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Frequently Asked Questions
ASTM D7343-20 is a standard published by ASTM International. Its full title is "Standard Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods for Elemental Analysis of Petroleum Products and Lubricants". This standard covers: SIGNIFICANCE AND USE 3.1 Accurate elemental analyses of samples of petroleum and petroleum products are required for the determination of chemical properties, which are in turn used to establish compliance with commercial and regulatory specifications. SCOPE 1.1 This practice covers information relating to sampling, calibration and validation of X-ray fluorescence instruments for elemental analysis, including all kinds of wavelength dispersive (WDXRF) and energy dispersive (EDXRF) techniques. This practice includes sampling issues such as the selection of storage vessels, transportation, and sub-sampling. Treatment, assembly, and handling of technique-specific sample holders and cups are also included. Technique-specific requirements during analytical measurement and validation of measurement for the determination of trace elements in samples of petroleum and petroleum products are described. For sample mixing, refer to Practice D5854. Petroleum products covered in this practice are considered to be a single phase and exhibit Newtonian characteristics at the point of sampling. 1.2 Applicable Test Methods—This practice is applicable to the XRF methods under the jurisdiction of ASTM Subcommittee D02.03 on Elemental Analysis, and those under the jurisdiction of the Energy Institute’s Test Method Standardization Committee (Table 1). Some of these methods are technically equivalent though they may differ in details (Table 2). 1.3 Applicable Fluids—This practice is applicable to petroleum and petroleum products with vapor pressures at sampling and storage temperatures less than or equal to 101 kPa (14.7 psi). Use Practice D4057 or IP 475 to sample these materials. Refer to Practice D5842 when sampling materials that also require Reid vapor pressure (RVP) determination. 1.4 Non-applicable Fluids—Petroleum products whose vapor pressure at sampling and sample storage conditions are above 101 kPa (14.7 psi) and liquefied gases (that is, LNG, LPG, etc.) are not covered by this practice. 1.5 Sampling Methods—The physical sampling and methods of sampling from a primary source are not covered by this guide. It is assumed that samples covered by this practice are a representative sample of the primary source liquid. Refer to Practice D4057 or IP 475 for detailed sampling procedures. 1.6 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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.
SIGNIFICANCE AND USE 3.1 Accurate elemental analyses of samples of petroleum and petroleum products are required for the determination of chemical properties, which are in turn used to establish compliance with commercial and regulatory specifications. SCOPE 1.1 This practice covers information relating to sampling, calibration and validation of X-ray fluorescence instruments for elemental analysis, including all kinds of wavelength dispersive (WDXRF) and energy dispersive (EDXRF) techniques. This practice includes sampling issues such as the selection of storage vessels, transportation, and sub-sampling. Treatment, assembly, and handling of technique-specific sample holders and cups are also included. Technique-specific requirements during analytical measurement and validation of measurement for the determination of trace elements in samples of petroleum and petroleum products are described. For sample mixing, refer to Practice D5854. Petroleum products covered in this practice are considered to be a single phase and exhibit Newtonian characteristics at the point of sampling. 1.2 Applicable Test Methods—This practice is applicable to the XRF methods under the jurisdiction of ASTM Subcommittee D02.03 on Elemental Analysis, and those under the jurisdiction of the Energy Institute’s Test Method Standardization Committee (Table 1). Some of these methods are technically equivalent though they may differ in details (Table 2). 1.3 Applicable Fluids—This practice is applicable to petroleum and petroleum products with vapor pressures at sampling and storage temperatures less than or equal to 101 kPa (14.7 psi). Use Practice D4057 or IP 475 to sample these materials. Refer to Practice D5842 when sampling materials that also require Reid vapor pressure (RVP) determination. 1.4 Non-applicable Fluids—Petroleum products whose vapor pressure at sampling and sample storage conditions are above 101 kPa (14.7 psi) and liquefied gases (that is, LNG, LPG, etc.) are not covered by this practice. 1.5 Sampling Methods—The physical sampling and methods of sampling from a primary source are not covered by this guide. It is assumed that samples covered by this practice are a representative sample of the primary source liquid. Refer to Practice D4057 or IP 475 for detailed sampling procedures. 1.6 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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.
ASTM D7343-20 is classified under the following ICS (International Classification for Standards) categories: 71.040.50 - Physicochemical methods of analysis. The ICS classification helps identify the subject area and facilitates finding related standards.
ASTM D7343-20 has the following relationships with other standards: It is inter standard links to ASTM D6481-24, ASTM D6299-23a, ASTM D8252-23, ASTM D5842-23, ASTM D5842-19, ASTM D8252-19e1, ASTM D8252-19, ASTM D5059-14(2019), ASTM D6443-14(2019)e1, ASTM D7212-13(2018), ASTM D6299-17b, ASTM D6299-17a, ASTM D8127-17, ASTM D6334-12(2017), ASTM D6299-17. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
ASTM D7343-20 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
Standards Content (Sample)
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.
Designation: D7343 − 20
Designation: 558/07
Standard Practice for
Optimization, Sample Handling, Calibration, and Validation
of X-ray Fluorescence Spectrometry Methods for Elemental
Analysis of Petroleum Products and Lubricants
This standard is issued under the fixed designation D7343; 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* tion Committee (Table 1). Some of these methods are techni-
cally equivalent though they may differ in details (Table 2).
1.1 This practice covers information relating to sampling,
calibration and validation of X-ray fluorescence instruments
1.3 Applicable Fluids—This practice is applicable to petro-
for elemental analysis, including all kinds of wavelength
leum and petroleum products with vapor pressures at sampling
dispersive (WDXRF) and energy dispersive (EDXRF) tech-
and storage temperatures less than or equal to 101 kPa
niques. This practice includes sampling issues such as the
(14.7 psi). Use Practice D4057 or IP 475 to sample these
selection of storage vessels, transportation, and sub-sampling.
materials. Refer to Practice D5842 when sampling materials
Treatment, assembly, and handling of technique-specific
that also require Reid vapor pressure (RVP) determination.
sample holders and cups are also included. Technique-specific
1.4 Non-applicable Fluids—Petroleum products whose va-
requirements during analytical measurement and validation of
por pressure at sampling and sample storage conditions are
measurement for the determination of trace elements in
above 101 kPa (14.7 psi) and liquefied gases (that is, LNG,
samples of petroleum and petroleum products are described.
LPG, etc.) are not covered by this practice.
For sample mixing, refer to Practice D5854. Petroleum prod-
ucts covered in this practice are considered to be a single phase
1.5 Sampling Methods—The physical sampling and meth-
and exhibit Newtonian characteristics at the point of sampling.
ods of sampling from a primary source are not covered by this
guide. It is assumed that samples covered by this practice are
1.2 Applicable Test Methods—This practice is applicable to
a representative sample of the primary source liquid. Refer to
the XRF methods under the jurisdiction ofASTM Subcommit-
Practice D4057 or IP 475 for detailed sampling procedures.
tee D02.03 on Elemental Analysis, and those under the
jurisdiction of the Energy Institute’s Test Method Standardiza-
1.6 The values stated in SI units are to be regarded as
standard. The values given in parentheses after SI units are
This practice is under the jurisdiction ofASTM Committee D02 on Petroleum
provided for information only and are not considered standard.
Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-
1.7 This standard does not purport to address all of the
mittee D02.03 on Elemental Analysis.
Current edition approved July 1, 2020. Published July 2020. Originally approved
safety concerns, if any, associated with its use. It is the
in 2007. Last previous edition approved in 2018 as D7343 – 18. DOI: 10.1520/
responsibility of the user of this standard to establish appro-
D7343-20.
priate safety, health, and environmental practices and deter-
This practice was jointly prepared by ASTM International and the Energy
Institute. mine the applicability of regulatory limitations prior to use.
*A Summary of Changes section appears at the end of this standard
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
D7343 − 20
TABLE 1 XRF Standard Test Methods for Analysis of Petroleum
D2622 Test Method for Sulfur in Petroleum Products by
Products and Lubricants
Wavelength Dispersive X-ray Fluorescence Spectrometry
Technique Analysis ASTM EI
D4057 Practice for Manual Sampling of Petroleum and
WD-XRF Sulfur in Petroleum Products D2622
Petroleum Products
Additive Elements in Lubricating D4927 IP 407
D4294 Test Method for Sulfur in Petroleum and Petroleum
Oils andAdditives
Lead in Gasoline D5059 IP 228
Products by Energy Dispersive X-ray Fluorescence Spec-
Lead in Gasoline IP 489
trometry
Sulfur in Gasoline D6334
Additive Elements in Lube Oils and D6443 D4927 Test Methods for Elemental Analysis of Lubricant
Additives
and Additive Components—Barium, Calcium,
Vanadium and Nickel IP 433
Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive
Sulfur IP 447
Sulfur inAutomotive Fuels IP 497 X-Ray Fluorescence Spectroscopy
Chlorine and Bromine IP 503
D4929 Test Method for Determination of Organic Chloride
Sulfur in Ethanol as Blending IP 553
Content in Crude Oil
Agent
Si, Cr, Ni, Fe, and Cu in Used IP 560
D5059 Test Methods for Lead and Manganese in Gasoline
Greases
by X-Ray Spectroscopy
Several Metals in Burner Fuels IP 593
D5842 Practice for Sampling and Handling of Fuels for
Derived from Waste Mineral Oils
MWD-XRF Sulfur in Gasoline and Diesel D7039 Volatility Measurement
Silicon in Gasoline and Naphtha D7757
D5854 Practice for Mixing and Handling of Liquid Samples
Organic Chloride in Crude Oil D4929 C
of Petroleum and Petroleum Products
ED-XRF Sulfur in Petroleum Products D4294 IP 336
Sulfur in Gasoline D6445 D6299 Practice for Applying Statistical Quality Assurance
Additive Elements in Lubricating D6481
and Control Charting Techniques to Evaluate Analytical
Oils
Measurement System Performance
Sulfur inAutomotive Fuels D7212 IP 531
Sulfur inAutomotive Fuels D7220 IP 532
D6334 Test Method for Sulfur in Gasoline by Wavelength
Additive Elements in Lubricating D7751
Dispersive X-Ray Fluorescence
Oils
D6376 Test Method for Determination of Trace Metals in
Lead in Gasoline IP 352
Sulfur inAutomotive Fuels IP 496
Petroleum Coke by Wavelength Dispersive X-ray Fluo-
Low Sulfur inAutomotive Fuels IP 600
rescence Spectroscopy
MED-XRF Organic Chloride in Crude Oil D4929 C
D6443 TestMethodforDeterminationofCalcium,Chlorine,
ED-XRF Organic Chloride in Crude Oil D4929 C
Copper, Magnesium, Phosphorus, Sulfur, and Zinc in
Unused Lubricating Oils and Additives by Wavelength
TABLE 2 Technically Equivalent XRF Test Methods for Petroleum
Dispersive X-ray Fluorescence Spectrometry (Mathemati-
A
Products and Lubricants
cal Correction Procedure)
Analysis ASTM EI Other
D6445 Test Method for Sulfur in Gasoline by Energy-
Sulfur by WD-XRF D2622 DIN 51400T6;
Dispersive X-ray Fluorescence Spectrometry (Withdrawn
JIS K3541
Additive Elements by WE- D4927 IP 407 DIN 51391T2 2009)
XRF
D6481 Test Method for Determination of Phosphorus,
Lead in Gasoline D5059 IP 228
Sulfur, Calcium, and Zinc in Lubrication Oils by Energy
Sulfur by ED-XRF D4294 IP 336 ISO 8754
Sulfur inAutomotive Fuels D7212 IP 531
Dispersive X-ray Fluorescence Spectroscopy
Sulfur inAutomotive Fuels D7220 IP 532
D7039 Test Method for Sulfur in Gasoline, Diesel Fuel, Jet
A
Nadkarni, R. A., Guide to ASTM Test Methods for the Analysis of Petroleum
Fuel, Kerosine, Biodiesel, Biodiesel Blends, and
Products and Lubricants, 2nd edition, ASTM International, West Conshohocken,
Gasoline-Ethanol Blends by Monochromatic Wavelength
PA, 2007.
Dispersive X-ray Fluorescence Spectrometry
D7212 Test Method for Low Sulfur inAutomotive Fuels by
Energy-Dispersive X-ray Fluorescence Spectrometry Us-
ing a Low-Background Proportional Counter
1.8 This international standard was developed in accor-
D7220 Test Method for Sulfur in Automotive, Heating, and
dance with internationally recognized principles on standard-
Jet Fuels by Monochromatic Energy Dispersive X-ray
ization established in the Decision on Principles for the
Fluorescence Spectrometry
Development of International Standards, Guides and Recom-
D7751 Test Method for Determination ofAdditive Elements
mendations issued by the World Trade Organization Technical
in Lubricating Oils by EDXRF Analysis
Barriers to Trade (TBT) Committee.
D7757 Test Method for Silicon in Gasoline and Related
Products by Monochromatic Wavelength Dispersive
2. Referenced Documents
X-ray Fluorescence Spectrometry
2.1 ASTM Standards:
D8127 Test Method for Coupled Particulate and Elemental
Analysis using X-ray Fluorescence (XRF) for In-Service
Lubricants
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
D7343 − 20
D8252 Test Method for Vanadium and Nickel in Crude and location for storage while awaiting analysis. This area, when-
Residual Oil by X-ray Spectrometry ever possible, should not contain samples that could contami-
nate those requiring trace element analysis.
2.2 Energy Institute Standards:
4.1.2 All laboratory equipment used specifically for trace
IP 228 Determination of lead content of gasoline—X-ray
element analysis should be free of any source of contamina-
spectrometric method
tion.This may require that specific equipment be used only for
IP 336 Determination of sulfur content—Energy-dispersive
trace element analysis.
X-ray fluorescence method
4.1.3 Analyses of blank samples are highly recommended.
IP 352 Determination of lead content of automotive
4.1.4 Sample preparation should be carried out in a clean
gasoline—Energy-dispersive X-ray fluorescence spec-
area. This area should use surfaces that can be decontaminated
trometry method
easily if a spillage occurs.
IP407 Determinationofbarium,calcium,phosphorus,sulfur
4.1.5 Operators should wear clean, fresh, protective gloves
and zinc by wavelength dispersive X-ray fluorescence
for sample preparation for trace element analysis. Tests should
spectrometry
be run to confirm that the gloves do not contain interfering
IP 433 Determination of vanadium and nickel content—
elements or elements of interest, since they may cause con-
Wavelength dispersive X-ray fluorescence spectrometry
tamination. The development of clean area sample handling
IP447 Determination of sulfur content—Wavelength disper-
protocols is encouraged.
sive X-ray fluorescence spectrometry
IP 475 Methods of test for petroleum and its products
5. Sample Preparation
IP 489 Determination of low lead contents in gasolines—
NOTE 1—In Test Method D4929 C, the sample is distilled to obtain a
Wavelength dispersive X-ray fluorescence spectrometry
naphtha cut, which is washed with caustic and then water. The washed
IP 496 Determination of sulfur content of automotive
fraction is then used for alternate XRF measurements.
fuels—Energy-dispersive X-ray fluorescence spectrom-
5.1 Choice of Sample Carrier—XRF testing requires a
etry
sample cell and a support film to hold the liquid sample in
IP 497 Determination of sulfur content of automotive
place during analysis.The choice of the sample cell or cup, the
fuels—Wavelength dispersive X-ray fluorescence spec-
material in which it is held, and the type of support film used
trometry
can all influence the result.
IP 503 Determination of chlorine and bromine content—
5.1.1 Sample Cell—The most common cell is a plastic cup,
Wavelength dispersive X-ray fluorescence spectrometry
ofwhichvariousdesignsareavailable.Thesedesignsallowfor
IP 531 Determination of sulfur content of automotive
a variety of sample types to be measured either in a liquid or
fuels—Low-background proportional counter energy-
powder form. It is important to check that the cup type used is
dispersive X-ray fluorescence spectrometry method
best suited for the compositions of samples to be analyzed.
IP 532 Determination of the sulfur content of automotive
Liquid sample cups usually have a seal that ensures the film is
fuels—Polarized X-ray fluorescence spectrometry
sealed to a level above that of the liquid in the cell and that the
IP 553 Ethanol as a Blending Component for Petrol—
film is taut with no wrinkles.
Determination of Sulfur Content—WDXRF Method
5.1.1.1 Within XRF spectrometers heat is produced, both
IP 560 Determination of Silicon, Chromium, nickel, Iron,
from the spectrometer components themselves and from the
and Copper in Used Greases—WDXRF Method
interaction of X-rays with the sample. Petroleum products that
IP 593 Determination of Pb, Ni, Cr, Cu, Zn, As, Cd, Tl, Sb,
are not stable due to volatility should only be placed into
Co, Mn, and V in Burner Fuels derived from Waste
vented sample cups or special sealed sample cups specifically
Mineral Oils—WDXRF Method
designed for volatile samples (see 8.3).
IP 600 Petroleum Products—Determination of Low Sulfur
5.1.1.2 The cup size may be important. Depending on the
Content of Automotive Fuels—EDXRF Spectrometry
film type used to support the liquid, different films will sag due
to the weight of sample and relax due to chemical interaction,
3. Significance and Use
or heat, or both. To reduce this sagging effect, the smallest
3.1 Accurate elemental analyses of samples of petroleum
diameter sample cups should be used. Cups with diameters
and petroleum products are required for the determination of
well in excess of the area detected by the spectrometer are
chemical properties, which are in turn used to establish
likely to increase errors due to sagging.
compliance with commercial and regulatory specifications.
5.1.1.3 A number of petroleum products require heating to
ensurehomogenizationpriortoanalysisortoenabletransferto
4. Sample Handling
the sample cell; examples include fuel oils and wax products.
4.1 It is necessary to use precautions to minimize the
The sample cup should be able to withstand the temperature
possibility of contamination of trace elemental analysis
used in this process. In general, most plastic sample cells
samples. Good laboratory practices in this area include:
should withstand temperatures up to 70 °C.
4.1.1 Samples received by the laboratory and required for
5.1.2 Sample Cell Holder—Many manufacturers recom-
trace element analysis should be stored in a designated specific
mend metal holders to hold sample cups while they are
transferred into the XRF instrument. These holders can be
made from aluminum, stainless steel, or other materials. It is
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
U.K., http://www.energyinst.org.uk. important to recognize that these represent a potential spectral
D7343 − 20
contamination to the analysis either if the spectrometer is to (4) This test does not need to be repeated for every
determine an analyte that the holder is made from or if the measurement when the analyst is certain that the film and the
material from the holder causes an interference with the material to be analyzed are compatible.
analyte. Generally, this is not a problem for elements with 5.1.3.6 Use of Multiple Films—A common method of en-
atomic number <30. For elements with atomic number >30 it suringthatspectrometersarenotcontaminatedbyleakingfilms
is advisable to check the potential contamination from the is to use a second film in the sample cup holder of the
sample cup holder using a blank. instrument.Thisprovidesahighlevelofsecurity,andformany
systems is essential to avoiding costly down times if a sample
5.1.3 Sample Support Films—Many support films are avail-
should leak. The use of this second film will increase both the
able from both XRF instrument manufacturers and accessory
detection limits as well as the errors of measurement. Some
suppliers. It is important to examine the film types specified in
petroleum products can permeate through polymer films and,
any method being used. There are four criteria that should be
while this may not be a problem for any single analysis, the
considered when selecting a X-ray transmission sample sup-
buildup on a second protective film in some cases may cause
port film:
drift of analysis results. When trace level determinations are
(1) Thickness of film,
required and the optimum performance in both precision and
(2) Composition of film,
detection limit are required, the use of secondary films should
(3) Chemical and physical resistance of film to the liquid
be given careful consideration. If they are considered essential,
intend for analysis, and
they should be inspected or replaced for every analysis as part
(4) Element contaminants contained within the film.
of standard operating procedures.
5.1.3.1 Film thickness typically ranges from 2 µ to6µfor
most applications. Consideration should be given to the varia-
6. Sample Stability
tions in thickness from batch to batch of films. For thinner
films,therelativevarianceinfilmthicknessisoftenhigherthan 6.1 Sample stability during measurement is essential for
that of the thicker films, thus precision of analysis can be accurate determinations. Pay particular care, since a sample
affected more if thinner films are used. One way to avoid this can undergo physical change during analysis. An example of
is to recalibrate or adjust calibrations using monitors each time this is catalyst residues in fuel oils that can settle during
a new batch of film is used. measurement. When this type of situation can occur or is
suspected, maintaining constant masses, heating times (in the
5.1.3.2 Film types are composed of different polymer ma-
case of fuel oils), mixing times, transfer time from preparation
terials.Thosecontainingoxygenornitrogenwillabsorblighter
to measurement, and the determination of low atomic number
elements more than those that do not. Examples of oxygen and
elements first in a sequential analysis scheme should be used.
nitrogen containing polymers are polyester and polyamide. For
the determination of elements lighter than sulfur, these films
6.2 This procedure will not eliminate the particulate settling
should be avoided in favor of polymers containing only carbon
problem; filtering of such samples may be needed before
and hydrogen, provided that the film is not attacked by the
analysis.
sample.
7. Instrument Set-Up Specific to Technique
5.1.3.3 Chemical resistance is often a compromise with film
type. Often, the best resistance is offered by polymers contain-
7.1 Wavelength Dispersive X-Ray Fluorescence (WDXRF):
ing oxygen or nitrogen. Physical aspects such as temperature
7.1.1 Before using anyWDXRF spectrometer, it is essential
will also be an issue especially if hot liquids are to be
that the instrument is performing to the manufacturer’s speci-
measured. Most film types will withstand temperatures up to
fications. Consult with the manufacturer on how to perform
80 °C,
...
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: D7343 − 18 D7343 − 20
Designation: 558/07
Standard Practice for
Optimization, Sample Handling, Calibration, and Validation
of X-ray Fluorescence Spectrometry Methods for Elemental
Analysis of Petroleum Products and Lubricants
This standard is issued under the fixed designation D7343; 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 practice covers information relating to sampling, calibration and validation of X-ray fluorescence instruments for
elemental analysis, including all kinds of wavelength dispersive (WDXRF) and energy dispersive (EDXRF) techniques. This
practice includes sampling issues such as the selection of storage vessels, transportation, and sub-sampling. Treatment, assembly,
and handling of technique-specific sample holders and cups are also included. Technique-specific requirements during analytical
measurement and validation of measurement for the determination of trace elements in samples of petroleum and petroleum
products are described. For sample mixing, refer to Practice D5854. Petroleum products covered in this practice are considered
to be a single phase and exhibit Newtonian characteristics at the point of sampling.
1.2 Applicable Test Methods—This practice is applicable to the XRF methods under the jurisdiction of ASTM Subcommittee
D02.03 on Elemental Analysis, and those under the jurisdiction of the Energy Institute’s Test Method Standardization Committee
(Table 1). Some of these methods are technically equivalent though they may differ in details (Table 2).
1.3 Applicable Fluids—This practice is applicable to petroleum and petroleum products with vapor pressures at sampling and
storage temperatures less than or equal to 101 kPa (14.7 psi). Use Practice D4057 or IP 475 to sample these materials. Refer to
Practice D5842 when sampling materials that also require Reid vapor pressure (RVP) determination.
1.4 Non-applicable Fluids—Petroleum products whose vapor pressure at sampling and sample storage conditions are above
101 kPa (14.7 psi) and liquefied gases (that is, LNG, LPG, etc.) are not covered by this practice.
1.5 Sampling Methods—The physical sampling and methods of sampling from a primary source are not covered by this guide.
It is assumed that samples covered by this practice are a representative sample of the primary source liquid. Refer to Practice
D4057 or IP 475 for detailed sampling procedures.
1.6 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for
information only and are not considered 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.
This practice 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 June 1, 2018July 1, 2020. Published June 2018July 2020. Originally approved in 2007. Last previous edition approved in 20172018 as
D7343 – 12 (2017).D7343 – 18. DOI: 10.1520/D7343-18.10.1520/D7343-20.
This practice was jointly prepared by ASTM International and the Energy Institute.
*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
D7343 − 20
TABLE 1 XRF Standard Test Methods for Analysis of Petroleum
Products and Lubricants
Technique Analysis ASTM EI
WD-XRF Sulfur in Petroleum Products D2622
Additive Elements in Lubricating D4927 IP 407
Oils and Additives
Lead in Gasoline D5059 IP 228
Lead in Gasoline IP 489
Sulfur in Gasoline D6334
Additive Elements in Lube Oils and D6443
Additives
Vanadium and Nickel IP 433
Sulfur IP 447
Sulfur in Automotive Fuels IP 497
Chlorine and Bromine IP 503
Sulfur in Ethanol as Blending IP 553
Agent
Si, Cr, Ni, Fe, and Cu in Used IP 560
Greases
Several Metals in Burner Fuels IP 593
Derived from Waste Mineral Oils
MWD-XRF Sulfur in Gasoline and Diesel D7039
Silicon in Gasoline and Naphtha D7757
Organic Chloride in Crude Oil D4929 C
ED-XRF Sulfur in Petroleum Products D4294 IP 336
Sulfur in Gasoline D6445
Additive Elements in Lubricating D6481
Oils
Sulfur in Automotive Fuels D7212 IP 531
Sulfur in Automotive Fuels D7220 IP 532
Additive Elements in Lubricating D7751
Oils
Lead in Gasoline IP 352
Sulfur in Automotive Fuels IP 496
Low Sulfur in Automotive Fuels IP 600
MED-XRF Organic Chloride in Crude Oil D4929 C
ED-XRF Organic Chloride in Crude Oil D4929 C
TABLE 2 Technically Equivalent XRF Test Methods for Petroleum
A
Products and Lubricants
Analysis ASTM EI Other
Sulfur by WD-XRF D2622 DIN 51400T6;
JIS K3541
Additive Elements by WE- D4927 IP 407 DIN 51391T2
XRF
Lead in Gasoline D5059 IP 228
Sulfur by ED-XRF D4294 IP 336 ISO 8754
Sulfur in Automotive Fuels D7212 IP 531
Sulfur in Automotive Fuels D7220 IP 532
A
Nadkarni, R. A., Guide to ASTM Test Methods for the Analysis of Petroleum
Products and Lubricants, 2nd edition, ASTM International, West Conshohocken,
PA, 2007.
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.
2. Referenced Documents
2.1 ASTM Standards:
D2622 Test Method for Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4294 Test Method for Sulfur in Petroleum and Petroleum Products by Energy Dispersive X-ray Fluorescence Spectrometry
D4927 Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur,
and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
D7343 − 20
D4929 Test Method for Determination of Organic Chloride Content in Crude Oil
D5059 Test Methods for Lead and Manganese in Gasoline by X-Ray Spectroscopy
D5842 Practice for Sampling and Handling of Fuels for Volatility Measurement
D5854 Practice for Mixing and Handling of Liquid Samples of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6334 Test Method for Sulfur in Gasoline by Wavelength Dispersive X-Ray Fluorescence
D6376 Test Method for Determination of Trace Metals in Petroleum Coke by Wavelength Dispersive X-ray Fluorescence
Spectroscopy
D6443 Test Method for Determination of Calcium, Chlorine, Copper, Magnesium, Phosphorus, Sulfur, and Zinc in Unused
Lubricating Oils and Additives by Wavelength Dispersive X-ray Fluorescence Spectrometry (Mathematical Correction
Procedure)
D6445 Test Method for Sulfur in Gasoline by Energy-Dispersive X-ray Fluorescence Spectrometry (Withdrawn 2009)
D6481 Test Method for Determination of Phosphorus, Sulfur, Calcium, and Zinc in Lubrication Oils by Energy Dispersive X-ray
Fluorescence Spectroscopy
D7039 Test Method for Sulfur in Gasoline, Diesel Fuel, Jet Fuel, Kerosine, Biodiesel, Biodiesel Blends, and Gasoline-Ethanol
Blends by Monochromatic Wavelength Dispersive X-ray Fluorescence Spectrometry
D7212 Test Method for Low Sulfur in Automotive Fuels by Energy-Dispersive X-ray Fluorescence Spectrometry Using a
Low-Background Proportional Counter
D7220 Test Method for Sulfur in Automotive, Heating, and Jet Fuels by Monochromatic Energy Dispersive X-ray Fluorescence
Spectrometry
D7751 Test Method for Determination of Additive Elements in Lubricating Oils by EDXRF Analysis
D7757 Test Method for Silicon in Gasoline and Related Products by Monochromatic Wavelength Dispersive X-ray Fluorescence
Spectrometry
D8127 Test Method for Coupled Particulate and Elemental Analysis using X-ray Fluorescence (XRF) for In-Service Lubricants
D8252 Test Method for Vanadium and Nickel in Crude and Residual Oil by X-ray Spectrometry
2.2 Energy Institute Standards:
IP 228 Determination of lead content of gasoline—X-ray spectrometric method
IP 336 Determination of sulfur content—Energy-dispersive X-ray fluorescence method
IP 352 Determination of lead content of automotive gasoline—Energy-dispersive X-ray fluorescence spectrometry method
IP 407 Determination of barium, calcium, phosphorus, sulfur and zinc by wavelength dispersive X-ray fluorescence
spectrometry
IP 433 Determination of vanadium and nickel content—Wavelength dispersive X-ray fluorescence spectrometry
IP 447 Determination of sulfur content—Wavelength dispersive X-ray fluorescence spectrometry
IP 475 Methods of test for petroleum and its products
IP 489 Determination of low lead contents in gasolines—Wavelength dispersive X-ray fluorescence spectrometry
IP 496 Determination of sulfur content of automotive fuels—Energy-dispersive X-ray fluorescence spectrometry
IP 497 Determination of sulfur content of automotive fuels—Wavelength dispersive X-ray fluorescence spectrometry
IP 503 Determination of chlorine and bromine content—Wavelength dispersive X-ray fluorescence spectrometry
IP 531 Determination of sulfur content of automotive fuels—Low-background proportional counter energy-dispersive X-ray
fluorescence spectrometry method
IP 532 Determination of the sulfur content of automotive fuels—Polarized X-ray fluorescence spectrometry
IP 553 Ethanol as a Blending Component for Petrol—Determination of Sulfur Content—WDXRF Method
IP 560 Determination of Silicon, Chromium, nickel, Iron, and Copper in Used Greases—WDXRF Method
IP 593 Determination of Pb, Ni, Cr, Cu, Zn, As, Cd, Tl, Sb, Co, Mn, and V in Burner Fuels derived from Waste Mineral
Oils—WDXRF Method
IP 600 Petroleum Products—Determination of Low Sulfur Content of Automotive Fuels—EDXRF Spectrometry
3. Significance and Use
3.1 Accurate elemental analyses of samples of petroleum and petroleum products are required for the determination of chemical
properties, which are in turn used to establish compliance with commercial and regulatory specifications.
4. Sample Handling
4.1 It is necessary to use precautions to minimize the possibility of contamination of trace elemental analysis samples. Good
laboratory practices in this area include:
The last approved version of this historical standard is referenced on www.astm.org.
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, U.K., http://www.energyinst.org.uk.
D7343 − 20
4.1.1 Samples received by the laboratory and required for trace element analysis should be stored in a designated specific
location for storage while awaiting analysis. This area, whenever possible, should not contain samples that could contaminate those
requiring trace element analysis.
4.1.2 All laboratory equipment used specifically for trace element analysis should be free of any source of contamination. This
may require that specific equipment be used only for trace element analysis.
4.1.3 Analyses of blank samples are highly recommended.
4.1.4 Sample preparation should be carried out in a clean area. This area should use surfaces that can be decontaminated easily
if a spillage occurs.
4.1.5 Operators should wear clean, fresh, protective gloves for sample preparation for trace element analysis. Tests should be
run to confirm that the gloves do not contain interfering elements or elements of interest, since they may cause contamination. The
development of clean area sample handling protocols is encouraged.
5. Sample Preparation
NOTE 1—In Test Method D4929 C, the sample is distilled to obtain a naphtha cut, which is washed with caustic and then water. The washed fraction
is then used for alternate XRF measurements.
5.1 Choice of Sample Carrier—XRF testing requires a sample cell and a support film to hold the liquid sample in place during
analysis. The choice of the sample cell or cup, the material in which it is held, and the type of support film used can all influence
the result.
5.1.1 Sample Cell—The most common cell is a plastic cup, of which various designs are available. These designs allow for a
variety of sample types to be measured either in a liquid or powder form. It is important to check that the cup type used is best
suited for the compositions of samples to be analyzed. Liquid sample cups usually have a seal that ensures the film is sealed to
a level above that of the liquid in the cell and that the film is taut with no wrinkles.
5.1.1.1 Within XRF spectrometers heat is produced, both from the spectrometer components themselves and from the
interaction of X-rays with the sample. Petroleum products that are not stable due to volatility should only be placed into vented
sample cups or special sealed sample cups specifically designed for volatile samples (see 8.3).
5.1.1.2 The cup size may be important. Depending on the film type used to support the liquid, different films will sag due to
the weight of sample and relax due to chemical interaction, or heat, or both. To reduce this sagging effect, the smallest diameter
sample cups should be used. Cups with diameters well in excess of the area detected by the spectrometer are likely to increase
errors due to sagging.
5.1.1.3 A number of petroleum products require heating to ensure homogenization prior to analysis or to enable transfer to the
sample cell; examples include fuel oils and wax products. The sample cup should be able to withstand the temperature used in this
process. In general, most plastic sample cells should withstand temperatures up to 70 °C.
5.1.2 Sample Cell Holder—Many manufacturers recommend metal holders to hold sample cups while they are transferred into
the XRF instrument. These holders can be made from aluminum, stainless steel, or other materials. It is important to recognize that
these represent a potential spectral contamination to the analysis either if the spectrometer is to determine an analyte that the holder
is made from or if the material from the holder causes an interference with the analyte. Generally, this is not a problem for elements
with atomic number <30. For elements with atomic number >30 it is advisable to check the potential contamination from the
sample cup holder using a blank.
5.1.3 Sample Support Films—Many support films are available from both XRF instrument manufacturers and accessory
suppliers. It is important to examine the film types specified in any method being used. There are four criteria that should be
considered when selecting a X-ray transmission sample support film:
(1) Thickness of film,
(2) Composition of film,
(3) Chemical and physical resistance of film to the liquid intend for analysis, and
(4) Element contaminants contained within the film.
5.1.3.1 Film thickness typically ranges from 2 μ to 6 μ for most applications. Consideration should be given to the variations
in thickness from batch to batch of films. For thinner films, the relative variance in film thickness is often higher than that of the
thicker films, thus precision of analysis can be affected more if thinner films are used. One way to avoid this is to recalibrate or
adjust calibrations using monitors each time a new batch of film is used.
5.1.3.2 Film types are composed of different polymer materials. Those containing oxygen or nitrogen will absorb lighter
elements more than those that do not. Examples of oxygen and nitrogen containing polymers are polyester and polyamide. For the
determination of elements lighter than sulfur, these films should be avoided in favor of polymers containing only carbon and
hydrogen, provided that the film is not attacked by the sample.
5.1.3.3 Chemical resistance is often a compromise with film type. Often, the best resistance is offered by polymers containing
oxygen or nitrogen. Physical aspects such as temperature will also be an issue especially if hot liquids are to be measured. Most
film types will withstand temperatures up to 80 °C, but relaxation of the polymer, especially in wide cups, will affect accuracy and
precision.
D7343 − 20
5.1.3.4 All films contain element contaminants. Before using any film, blanks should be run to ensure that the backgrounds are
not elevated by the existence of a contaminant element present in the film. These contaminant elements will affect detection limits
if they correspond to, or interfere with, the analyte element(s).
5.1.3.5 It is necessary to verify that the sample does not dissolve the film or permeate through it. This is especially important
for gasoline-range samples, when a new product is to be analyzed, or when a new kind of film is used for a sample type. This
verification can be done as follows:
(1) Prepare a specimen cup and fill it with a typical specimen.
(2) Place the cell on a clean tissue and wait for 30 min to 60 min.
(3) Remove the cell, and inspect the tissue and the underside of the film. Both should be dry.
(4) This test does not need to be repeated for every measurement when the analyst is certain that the film and the material to
be analyzed are compatible.
5.1.3.6 Use of Multiple Films—A common method of ensuring that spectrometers are not contaminated by leaking films is to
use a second film in the sample cup holder of the instrument. This provides a high level of security, and for many systems is
essential to avoiding costly down times if a sample should leak. The use of this second film will increase both the detection limits
as well as the errors of measurement. Some petroleum products can permeate through polymer films and, while this may not be
a problem for any single analysis, the buildup on a second protective film in some cases may cause drift of analysis results. When
trace level determinations are required and the optimum performance in both precision and detection limit are required, the use
of secondary films should be given careful consideration. If they are considered essential, they should be inspected or replaced for
every analysis as part of standard operating procedures.
6. Sample Stability
6.1 Sample stability
...
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