RESUMEN
This work describes development of a flow injection (FI) system for determination of iodide, based on the chemiluminescence (CL) reaction between iodine and luminol. Iodide in the sample zone is oxidized to iodine. Employment of a gas-diffusion (GD) unit allows for selective detection of the generated CL (425nm). Preliminary results showed for concentrations of less than 2mgL(-1), that signals were irreproducible and that the calibration was not linear. In order to solve these problems, a method of 'membrane conditioning' was investigated, in which iodide stream was continuously merged with oxidant to generate I(2) that conditioned the GD membrane and tubing. This minimized surface interaction between the active surface and the I(2) generated from the samples, thus improving both precision and sensitivity. By employing membrane conditioning, it has been possible to reliably detect concentrations down to 0.1mgL(-1). At the optimized condition, an excellent linear calibration (r(2) = 0.999) was obtained from 0.1 to 1.0mgL(-1). The method was successfully applied to determine iodide in some pharmaceutical products such as potassium iodide tablets and a liquid patent medicine. However, for vitamin tablets, ascorbic acid was found to interfere seriously by causing a negative signal.
RESUMEN
In this work, we have modified the technique of all injection analysis (AIA) by changing the position of the detector. The detection is then located as a part of the circulatory loop. With this new detector position, we could monitor for many numbers of circulation. The sensitivity was improved by using the cumulative signal data obtained when the number of circulation rounds was increased. The dilution effect using this new detector location was also less than that with the previous system. We employed a four-channel peristaltic pump to aspirate four types of liquids into the system together at one time. The AIA method was then developed for determination of phosphorus in soils and sediment extracts. The method was optimized for the new harmonized scheme of extraction that has been developed by the European Commission.