Simple solid-phase colorimetry for trace Cr(VI) by combination of complexation with diphenylcarbazide and ion-pair solid-phase extraction with sedimentable dispersed particulates

Anal Sci. 2023 Jun;39(6):857-865. doi: 10.1007/s44211-023-00286-9. Epub 2023 Feb 16.

Abstract

A highly sensitive and simple solid-phase colorimetry for Cr(VI) was proposed. It was based on the ion-pair solid-phase extraction of Cr-diphenylcarbazide (DPC) complex with sedimentable dispersed particulates. The concentration of Cr(VI) was measured from the color tones obtained by image analysis of the photo of sediment. Various conditions, e.g., material and amounts of adsorbent particulates, chemical properties and concentration of counter ions, and pH, were optimized for the formation and quantitative extraction of the complex. In the recommended procedure, 1 mL of sample was put into a 1.5 mL microtube where powder form adsorbent and reagents, i.e., XAD-7HP particles, DPC, sodium dodecyl sulfate, amido sulfuric acid, and sodium chloride had been packed. The analytical operation was completed within 5 min by gently shaking the microtube and allowing it to stand until enough amounts of particulates were deposited to take a picture. Chromium (VI) up to 2.0 ppm was determined, and the detection limit was 0.0034 ppm. The sensitivity was enough to determine Cr(VI) at lower concentrations than the water quality of standard (0.02 ppm). This method was successfully applied to the analysis of simulated industrial wastewater samples. The stoichiometry of the extracted chemical species was also investigated by applying the same equilibrium model as the ion-pair solvent extraction.

Keywords: Chromium (VI); Colorimetry; Ion-pair solid-phase extraction; Sedimentable dispersed particulates; Simple analysis.