Vacancy ion-exclusion chromatography of inorganic acids on a weakly acidic cation-exchange resin column

Vacancy ion-exclusion chromatography (VIEC) for inorganic acids such as H2SO4, HCl, H3PO4, HNO3, HI and HF is tested on a polymethacrylate-based weakly acidic cation-exchange resin column in the H+-form. That is, mixture of inorganic acids in the mobile phase is adsorbed to the resin phase passing through the separation column, and each vacant peak induced by injecting water is determined. Retention times are dependent on the degrees of retention for each analyte in the resin phase. In VIEC, well-shaped peaks of inorganic acids are produced, leading to efficient separations. However, retention behaviors of inorganic acids were strongly affected by the concentrations of the acids in the mobile phase. Sulfosalicylic acid was mixed with inorganic acids in the mobile phase prior to the introduction of a separation column in order to obtain the well-resolutions in the lower concentrations of the acids. By using this method, the separations of inorganic acids could be achieved in the range of 0.01–1 mM, and the linear ranges could be extended over two-orders of magnitude. This is considered since the protonated carboxylic groups fixed on the resin phase were increased with increasing the acid concentrations in the mobile phase, and the penetration effects for the acids to the resin phase were thus enhanced. The detection limits (S/N = 3) were below 1.0 μM for all analyte acids. Precision values for retention times were below 0.32% and for peak area were below 0.91%.