A rapid procedure has been developed for the analysis of orthophosphate, sulfate and chloride in riverine sediment interstitial water samples which have dissolved iron concentrations ranging from 0.5–2 mmol L−1. Interferences caused by the precipitation of iron hydroxides resulting from air oxidation of ferrous iron in the anoxic samples and from the alkaline working pH range (9.0 – 10.5) of the Dionex1ion chromatographic system were eliminated by complexing the iron with cyanide. Orthophosphate concentration values are compared with dissolved reactive phosphate concentration data for the same samples. Orthophosphate concentrations rather than dissolved reactive phosphate concentrations are preferred for phosphate mineral solubility calculations and for phosphorus nutrient measurements.