Low-Level Sulfur in Fuel Determination Using Monochromatic WD XRF—ASTM D 7039-04

A monochromatic wavelength dispersive X-ray fluorescence (MWDXRF) technique has been successfully developed for measuring low-level sulfur in fuel. In this technique, two doubly curved crystal (DCC) optics were used to provide monochromatic excitation and fixed channel wavelength dispersive analysis. Using highly efficient DCC optics, compact bench top MWDXRF analyzers for sulfur analysis have been successfully produced. A new ASTM standard test method for low-level sulfur determination in diesel and gasoline, D7039-04, has been developed based on this technique. Data for ultra-low-sulfur fuel were collected and analyzed using this new method. In this paper, the results of repeatability, reproducibility, and bias are presented and discussed. The repeatability for 10-ppm sulfur fuel was shown to be around 1 ppm. The pooled limit of quantification (PLOQ) for ultra-low-sulfur diesel was found to be less than 1.5 ppm in this study. The reproducibility of 15-ppm sulfur diesel fuel was determined to be better than 3 ppm (95 % confident level). The limit of detection for a single analyzer was found to be 0.36 ppm. The effect of matrix composition was investigated. The correction due to matrix for low-level sulfur diesel and gasoline is generally not significant.