Colorimetric analysis based on solid-phase extraction with sedimentable dispersed particulates: demonstration of concept and application for on-site environmental water analysis.

A novel simple and functional colorimetric methodology for on-site environmental water analysis was proposed. This method combines coloration of the analyte and extraction of the colored species on dispersed particulates during their sedimentation in the same container. The whole analysis can be performed within 15 min by comprising the addition of 1 mL of sample solution into a 1.5-mL microtube containing the powders of coloring reagents and the sedimentable fine particulates as an adsorbent. The analyte is determined by comparing the sediment color with the standard color by visual inspection or the color information of the photo image. The potential of this methodology was demonstrated through developing colorimetry for Fe2+ with o-phenanthroline, NO2- by azo-dye formation, HCHO by the MBTH method, and PO43- by the 4-aminoantipyrine method based on the enzyme reactions. The material, size, amount of the adsorbent particles, and other conditions were optimized for each analytes. The advantages of the methodology were as follows: high sensitivity, easy controllability of the sensitivity over the wide range by the amount, size, and material of the particulates, lower interference from the colored matrix components due to obtaining the color data from not the aqueous phase but the sedimented particulates, and acceleration of the color development rate by the particulates as seen in NO2- determination as consequence shorten the operation time. A simple device equipped with twin cells was proposed for on-site analysis which contains two successive different coloring operations. The developed methods were successfully applied to the environmental water samples with the good agreement of the results with those by the usual instrumental methods.

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

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.