A reliable and sensitive analytical optical method for the determination of phosphorous in oceanographic and environmental materials does not exist. In this work, a novel hydride generation method was used to form phosphine from a sample containing phosphate mixed with 7% sodium borohydride. By heating the mixture to 500 °C, phosphine was reproducibly generated and collected in a cold trap. Phosphine was then introduced into an ICP where several atomic emission lines for phosphorous were observed. Copper emission did not spectrally interfere with phosphorous atomic emission with this hydride generation-ICP-AES method. This hydride generation method allows the use of small sample volumes (< 5 μL).