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 D 5854 . 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: D 2622 , D 4294 , D 5059 , D 6334 , D 6443 , D 6445 , D 6481 , D 7039 , D 7212 , and D 7220 and those under the jurisdiction of the Energy Institute s Test Method Standardization Committee: IP 228, IP 336, IP 352, IP 407, IP 433, IP 447, IP 475, IP 489, IP 496, IP 497, IP 503, IP 531, and IP 532.

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 D 4057 or IP 475 to sample these materials. Refer to Practice D 5842 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 D 4057 or IP 475 for detailed sampling procedures.

1.6 The values stated in SI units are to be regarded as the standard. 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.

2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

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

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 and Diesel Fuel 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

Keywords

calibration; EDXRF; regression; validation; WDXRF;

ICS Code

ICS Number Code 71.040.50 (Physicochemical methods of analysis)

DOI: 10.1520/D7343-07

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