Analytical Sciences

Abstract − Analytical Sciences, 21(9), 1079 (2005).

Resolution of Biparametric Mixtures Using Bead Injection Spectroscopic Flow-through Renewable Surface Sensors
Department of Physical and Analytical Chemistry, Faculty of Experimental Sciences, University of Jaén, 23071 Jaén, Spain
A new, sensitive and simple bead injection spectroscopy-flow injection analysis (BIS-FIA) sensor with spectrophotometric detection, using a commercially available flow-cell, is described to the determination of biparametric mixtures. As an analytical model, the metallic mixture Cu(II) and Zn(II) has been chosen. The flow-cell (Hellma 138-OS) is filled by injecting in the flow system 300 µl of a homogeneous bead suspension of an anion exchanger gel (Sephadex QAE A-25) previously loaded with the chromogenic reagent 2-carboxyl-2-hydroxy-5-sulfoformazylbenzene (Zincon). A sequential reaction of Cu(II) and Zn(II) with Zincon to form two complexes is performed on the bead sensing support and the absorbance is monitored at 627 nm, after two successive injections from the mixture solution. The sample containing these metal ions is injected into the first carrier (deionized water, pH 5.9), and Cu(II) selectively reacts with Zincon on the beads, developing the analytical signal. Then, 600 µl of 2 M HCl is injected to decompose the complex, and the carrier solution is changed. At pH 11 (second carrier) both Cu(II) and Zn(II) react with the chromogenic reagent, the absorbance now corresponding to both analytes. The eluent is again injected to descompose both complexes. After three analyses the sensing bead surface is not regenerated. Then, beads are automatically discarded from the flow cell by reversal of the flow, and instantaneously transported out of the system. So the procedure exploits the combination of the concepts of flow-through renewable sensors with Bead Injection Spectroscopy. Using a sample volume of 1000 µl, the calibration graph for Cu(II) is linear over the range 0.05 to 1 µg ml-1 and for Zn(II) from 0.1 to 1.8 µg ml-1 in the presence of each other. RSDs (%) lower than 5% are obtained for both analytes. The sensor is satisfactorily applied to individual determination or mixture resolution in waters, pharmaceuticals, soils and human hair samples.