Capteur de resine chelatante pour le prelevement la preconcentration et la determination de metaux traces toxiques (Zn, Cd, Hg, Pb) dans les eaux

Abstract

The subject of this article is the elaboration of a catcher of toxic metals (Zn, Cd, Hg, Pb) which enables them to be determined at μg 1 −1 level. It is known that, at these low concentrations, it is advisable to prevent the sample from being altered in any way between the time of taking and the time of analysis; moreover, it is necessary to proceed, on the one hand, to the pre-concentration of the wanted elements and, on the other hand, to the elimination of the main elements present in water and likely to interfere at the time of analytical determination. We therefore made a catcher which makes it possible to achieve these two desired effects by chromatographic separation and to carry out the conditioning of the sample, in the field, in a well-defined, chemical form, stable in time as a small volume in a solid state, easy to carry and to store. The catcher is in the shape of a small, cylindrical capsule (diameter = 29 mm, thickness = 10 mm) in Makrolon (Lexan) whose bases are made of a nylon cloth and which contains a chelating resin load (Chelex-100, 100–200 mesh). At the time of use, the catcher is put into a dismountable filtering-apparatus which permits percolation of the solution containing the wanted metal traces. Then, to proceed to the analytical determination of the elements it is possible to use two methods: analysis in solution after elution; X-ray fluorescence spectrometry, or else activation analysis on the catcher dried and then pelletized when hot in an hydraulic press. The experimentation has included the following points: 1. 1. Determination of the conditions of chromatographic separation on Chelex-100 resin which permits optimal fixation of Zn, Cd, Hg and Pb and the elution of the main elements Ca, Mg and Fe. We chose soda-citrate medium 7.1 · 10 −2 M at pH = 7.00; 2. 2. Determination of the conditions of use of the catcher and its efficiency according to the main elements in the sample of water. The process we chose involves a sample of 1 l. of water which is acidified at pH 1 by concentrated HNO 3 and then filtered through a membrane (0.45 μm). The solid residue is examined by X-ray fluorescence spectrometry. To the filtrate are added 100 ml of soda-citrate buffer 7.1 · 10 −1 M and the pH is set to seven by addition of NaOH. Then the filtrate is percolated through the Chelex-100 resin catcher (flux = 1.5 ml min −1). Then, it is possible to proceed: either to the elution of toxic metals by HNO 2 2M to determine them in solution (atomic absorption spectrophotometry, anodic stripping voltammetry); or to pelletizing of the catcher and to the analytical determination by X-ray fluorescence spectromy or activation analysis. The results of these methods are compared with different water: (1) spring warer: (2) over waters and (3) sea-water. The elution method as well as direct analysis of the pelletized catcher gave satisfactory agreement.