Sensitive determination of dissolved sulfide in estuarine water by solid-phase extraction and high-performance liquid chromatography of methylene blue

A sensitive method involving solid-phase extraction and HPLC analysis of methylene blue has been developed to measure nanomolar levels of dissolved sulfide in oxic surface waters. The procedure included 1) a preconcentration step, in which methylene blue generated from sulfide reaction with n,n-dimethyl-p-phenylenediamine in acidic conditions in the presence of ferric ion was absorbed onto Waters tC18 cartridge; and 2) a determination step, in which methylene blue was separated by HPLC in a gradient elution to minimize natural organic matter interference and detected by absorbance. The concentrations of the dissolved sulfide, quantified by standard addition, were about 2.1–4.7 nM in oxic surface waters from Galveston Bay, Texas.