The principal appeal of ion chromatography (IC) as an analytical technique lies in the ability to rapidly analyze a mixture of ions of widely varying concentrations and properties in a single elution. It is therefore not surprising that IC has been considered as a potentially powerful technique for the complete analysis of all electroless nickel (EN) solution anions. However, the use of the technique has been hampered by the similar ion exchange selectivity coefficients of many of the EN solution anions, making it difficult to achieve effective separation of all the EN bath anions on an ion chromatography column. This article addresses the separation issue and describes a method that has been developed for separating the organic acid anions commonly found in an electroless nickel bath from the inorganic anions. By using a high-capacity anion exchange column and carefully selecting a mixed isocratic-gradient elution with sodium hydroxide, the separation and quantification of all the component anions in a surrogate electroless nickel solution (hypophosphite, orthophosphite, sulfate, propanoic and succinic acid) were achieved. The analysis of trivalent anions such as citrate and orthophosphate was also shown to be possible.