Automated exploration and exploitation of flow-injection response surfaces

Abstract

Three-dimensional plots of instrumental responses vs. chemical concentrations or flow parameters have been 1 obtained in an automated manner on a computer-controlled flow-injection methods development system. Consideration of several alternative responses for flow-injection systems is shown to help characterize a chemistry more thoroughly and reveal the best experimental conditions. One may see the effects of individual experimental variables (reagent concentrations, pH, flow-rates, etc.), the interactions of these variables, instrumental factors and limitations of the surface exploration procedure employed. Chemical systems studied were the photometric determination of phosphate, palladium(II), iron(II) and persulfate. The propriety of automated response surface mapping is demonstrated and the efficacies of simplex and grid search approaches to response surface exploration are contrasted. Responses obtained include absorbance at peak maximum, relative standard deviation of maximum absorbance, time from injection to peak maximum and wavelength of maximum absorbance. Higher dimensional response surface representations of peak shape and absorbance spectra are also presented. The results show that the response chosen governs the general shape of the surface and the height at any point. This approach to automated characterization of chemical reactions in flow analysis is critically assessed.