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Abstract: Removal of zinc and cadmium from highly saline solutions by hydroxide precipitation is discussed. Experimental solubilities of zinc and cadmium in highly saline solutions were compared to modeled results obtained using Pitzer’s approach. An amphoteric character of zinc and cadmium and an influence of chloride ion on the concentration of dissolved metals were investigated. In order to avoid errors linked to pH measurements in concentrated aqueous solutions, the method of calibration of glass pH electrodes was developed and evaluated. The method uses easily prepared buffers whose pHs were determined with the Pitzer ion-interaction approach. The presented investigations address two issues of high significance in industrial wastewater treatment, namely: precise pH measurements and rigorous modeling of highly saline wastewaters. The results can be implemented in the treatment of hydrometallurgical wastewaters such as zinc refinery wastewater. Additionally, an implementation of the presented investigations is not limited to wastewater treatment but can easily be extended to other high-chloride metallurgical processes wherein the pH measurements in highly saline streams are required. Graphical Abstract: