Abstract
A novel automated liquid/liquid extraction system was developed for the determination of trace contaminants in unalloyed, alloyed and highly alloyed steels and super alloys. In the presented batch extraction system the aqueous phase and the non-water miscible organic phase were brought into close phase contact by high-speed stirring with a magnetic stir bar. Iodide complexes of Ag, Bi, Cd, Pb, Sb, Sn, Tl, and Zn were extracted from aqueous steel digests into 4-methylpentan-2-one (MIBK) containing 20 g L−1 trioctylphosphine oxide. Ag, Bi, Cd, Pb, and Tl were extracted quantitatively whereas the extraction yields of Sb, Sn, and Zn were 83%, 61% and 75% respectively. Using high resolution continuum source flame AAS (HR-CS-FAAS) for analyte quantification the method was validated using 21 certified steel reference materials (CRMs).
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Acknowledgments
The authors wish to acknowledge the support from Boehler Edelstahl GmbH (Kapfenberg, Austria). Mr. Bernhard Pichler is thanked for the helpful discussions and the preparation of several steel dissolutions. The provision of a modified control software for the HR-CS-AAS instrument by Analytik Jena AG is acknowledged. This software modification allows instrument remote control and is now part of the software delivered with new instruments.
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Published in the special issue Analytical Sciences in Austria with Guest Editors G. Allmaier, W. Buchberger, and K. Francesconi.
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Wiltsche, H., Prattes, K. & Knapp, G. A novel approach for an automated liquid/liquid extraction system—principle and application for the determination of several trace contaminants in highly alloyed steels and base alloys. Anal Bioanal Chem 400, 2329–2338 (2011). https://doi.org/10.1007/s00216-011-4666-3
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DOI: https://doi.org/10.1007/s00216-011-4666-3