An automatic back titration method for microchemical analysis

摘要

An automatic back titration method for microchemical analysis is introduced, which is based on conventional volumetric analysis's principle and the use of flow injection analysis apparatus for the automation and microminiatur-ization of the process. The sample and a known, but excess amount of a calibrated reagent solution are injected and propelled into a titration cell. where their reaction takes place. The excess of the reagent is then titrated With a titrant containing an indicator and the end point is monitored photometrically. Since homogeneous mixing in the titration cell is obtained magnetically in the whole process, there is a linear relationship between the analyte's concentration and the volume of the titrant consumed. Nickel in the range of 10-70 g 1↑(-1) is determined by the above method, in which 30 μl of sample and 500 μl of EDTA are injected and the excess of EDTA is titrated with a standard zinc salt solution containing xylenol orange which could be blocked by nickel ion m a direct titration. This method is characteristic of low sample and reagent consumption, high sampling rate as high as 45 samples h↑(-1), negligible effect of sample's viscosity, small carry-over effect (lower than 0.14%l. and very good precision, whose relative standard deviations are as small as 0.24%. # 1997 Elsevier Science B.V.