• Reichstädter, Marek

Abstract

This work studies development of Diffusive Gradients in Thin films (DGT) technique for determination of mercury (Hg) and other trace metals and further application possibilities of this technique. In this work, the DGT technique is developed for the determination of Hg and other trace metals in various liquid media. Two different Hg-specific ion-exchange resins were evaluated for application in the DGT technique – Purolite S924 and Cysteine-Modified Amino-Propyl silica (CAPS). The Purolite S924 is commercially available chelating resin, the CAPS resin was prepared under laboratory conditions by glutaraldehyde-mediated immobilisation of cysteine onto 3-aminopropyl functionalised silica. Both resins showed promising application potential in the DGT technique thanks to their reliable performance in solutions of a broad range of pH and ionic strength. The performance of the DGTs with the new resins was compared with the performance of the DGTs with the commonly used Chelex-100 and 3-mercaptopropyl silica resins.The major advantage of the S924 and CAPS resin is the ability of simultaneous assessment of Hg and other trace metals (Cu, Ni, Pb, Cd, Co). Due to different requirements on the resins used in the DGT technique for Hg and other trace metals, the DGT technique or simultaneous quantitative determination of Hg and other trace metals was not reported yet. Until now, the assessment of Hg and other trace metals have been performed by two separated types of the DGT samplers – one for Hg and one for other trace metals. That increased the number of samples produced and consumables used. The DGT technique with the CAPS resin was used for determination of metals in Oostende and Zeebrugge marine harbours in the Belgian coastal zone. Although the DGT technique was originally introduced as an environmental analysis tool, the application of the DGT technique in food analysis was also studied in this work. The performance of the DGT technique was validated in fish sauces and the effective diffusion coefficients of Hg and trace metals in the fish sauce were determined. Subsequently, the DGT technique was successfully applied to determine the concentration of mercury and other trace metals in fish sauce samples. To compare the new analytical procedure using DGT technique, fish sauces were also analysed directly by thermal decomposition gold amalgamation atomic absorption spectrometry (TD-AAS) and also after microwave decomposition by sector field inductively coupled plasma mass spectrometry (SF-ICP-MS). Due to the preconcentration ability of the DGT technique, lower detection limits were achieved in comparison with the TD-AAS or the SF-ICP-MS. Moreover, the wear and corrosion of metal parts of the analytical instruments were eliminated by the ability of the DGT technique to separate the trace metals from the complex matrix of fish sauce.

Topics

• impedance spectroscopy
• corrosion
• thin film
• gold
• strength
• resin
• atomic absorpion spectrometry
• thermal decomposition
• spectrometry
• Mercury
• inductively coupled plasma mass spectrometry