ASTM D7343 Standard Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods for Elemental Analysis of Petroleum Products and Lubricants
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 the standard.

1.6.1 Exception - The values given in parentheses are for information only.

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 and health 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.

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
D5059 Test Methods for Lead 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 Measurement System Performance
D6334 Test Method for Sulfur in Gasoline by Wavelength Dispersive X-Ray Fluorescence
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

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.