Abstract
The optimization of a continuous flow system for electrochemical hydride generation coupled to microwave-induced plasma atomic emission spectrometry (MIP–AES) for the determination of Se is presented. A small electrolytic cell with a porous glassy carbon working electrode was used for hydride generation. When using an Ar MIP operated in a TE101 cavity a detection limit of 0.6 ng mL–1 (3σ) could be achieved. The calibration curve was linear up to 1 µg mL–1. A standard deviation of less than 2% (10 replicate analyses) could be achieved. It was shown that interferences of transition metals are of the same order of magnitude as with a larger electrolysis cell described earlier, and light elements hardly caused any signal depression as tested. It was possible to distinguish between Se(IV) and Se(VI) species and seleno-DL-methionine, because under optimized conditions of an electrolysis current of 10 mA, a microwave power of 210 W, an Ar flow rate of 15 L h–1 and a sample flow rate of 2.5 mL min–1 only Se(IV) was transformed to H2Se and transferred into the plasma. Finally, the possibility of an electrochemical pre-enrichment was shown to enable it to further decrease the detection limit.
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Schermer, S., Jurica, L., Paumard, J. et al. Optimization of electrochemical hydride generation in a miniaturized electrolytic flow cell coupled to microwave-induced plasma atomic emission spectrometry for the determination of selenium. Fresenius J Anal Chem 371, 740–745 (2001). https://doi.org/10.1007/s002160101040
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DOI: https://doi.org/10.1007/s002160101040