Shake, shut, and go – A fast screening of sulfur in heavy crude oils by high-resolution continuum source graphite furnace molecular absorption spectrometry via GeS molecule detection

Highlights: • Quantification of sulfur in heavy crude oils via GeS molecule • Simple sample preparation as microemulsion • Graphite furnace as robust atomizer for heavy crude oil samples • Calibration with aqueous sulfate standard -- Abstract: A fast and simple method for sulfur quantification in crude oils was developed by using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). For this, heavy crude oil samples were prepared as microemulsion (shake) and injected into a graphite furnace (shut). Finally, the concentration of sulfur was determined by monitoring in situ the transient molecular spectrum of GeS at wavelength 295.205 nm after adding a germanium solution as molecular forming agent (and go). Zirconium dioxide in the form of nanoparticles (45–55 nm) was employed as a permanent modifier of the graphite furnace. Calibration was done with an aqueous solution standard of ammonium sulfate, and a characteristic mass (m₀) of 7.5 ng was achieved. The effectiveness of the proposed method was evaluated analizing, ten heavy crude oil samples with sulfur amounts ranging between 0.3 and 4.5% as well as two NIST standard reference materials, 1620c and 1622e. Results were compared with those obtained by routine ICP-OES analysis, and no statistical relevant differences were found.