Determination of ultra-micro amounts of sulfur in igneous rocks by spectrofluorimetry using 2-(o-hydroxyphenyl) benzoxazole derivatization and tin(II)-strong phosphoric acid-assisted reduction

A new and very sensitive method was developed for the determination of ultra-micro amounts of sulfur in igneous rock samples. The sulfur compounds in an igneous rock sample are reduced and released in the form of hydrogen sulfide by heating with a tin(II)-strong phosphoric acid (SPA) reagent. The liberated hydrogen sulfide is carried by a flow of nitrogen into a copper(II) absorbing solution to obtain a precipitate of copper(II) sulfide. The remaining copper(II) ion forms a chelate with 2-(o-hydroxyphenyl)benzoxazole (HPB) and quenches the fluorescence of HPB. The amount of sulfide is determined by measuring the HPB fluorescence intensity. The optimum reaction conditions were stoichiometrically investigated. By the present method using 0.1–0.2 g of rock sample, ultramicro amounts of sulfur (0.1–12.8 μg) could be quantitatively separated, collected, and determined with a relative standard deviation of 1.37% for a sample containing 5.7 μg of sulfur (95% confidence level).