A series of oxo- and sulfido-bridged dinuclear molybdenum(V) complexes, (a) M_O2O₂(μ-O, S) (dte)₂, (b) M_O2O₂(μ-S₃)(dtc)₃, (C) M_O2OS(μ-S₃) (dtc)₃ and (d) M_O2S₂(μ-S₂)(dct)₃ [dtc=S₂CN(n-Bu)₂] were synthesized: (a) by refluxing an aqueous solution containing molyb denum(V) chloride and sodium dibutyldithiocarbamate, (b) and (c) by the reaction among molybdenum(VI) oxide, sodium hydrogensulfide and dibutyldithiocarbamic acid, and (d) by the sulfurization of (a) with diphosphorus pentasulfide, respectively.
These complexes were separated by high-performance liquid chromatography employing a Zorbax SIL column (silica gel) with hexane-ethanol as an eluent and a Unisil C18 column (octadecylsilane) with water-methanol (Fig.1 and 2). Each molybdenum complex was successfully determined on a Zorbax SIL column with hexyl p-hydroxybenzoate as an internal standard hy use of a calibration curve drawn between the raios (Mo complex/standard) of weight and peak area. The coefficient of variation was 0.59∼2.21% and the limit of detection was about 2 ng for S/N=3.

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