✦ LIBER ✦

Electrochemical sample pretreatment coupled on-line with electrospray mass spectrometry for enhanced elemental analysis

✍ Scribed by Jack R. Pretty; Gary J. Van Berkel

Publisher: John Wiley and Sons
Year: 1998
Tongue: English
Weight: 305 KB
Volume: 12
Category: Article
ISSN: 0951-4198
DOI: 10.1002/(sici)1097-0231(19981115)12:21<1644::aid-rcm377>3.0.co;2-7

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✦ Synopsis

The successful coupling of a thin-layer, flow-by electrochemical cell on-line with electrospray mass spectrometry (ES-MS) for electrochemically modulated sample preconcentration and clean up, using copper(II) as the targeted analyte, is demonstrated. Particular requirements for the interfacing of this electrochemical system with ES-MS, the choice of cell and electrode materials, and the solvent and electrolyte requirements are addressed. The transfer of Cu 2 at low mg/L levels from matrices that cannot be analyzed directly by ES-MS, including 100% aqueous solutions containing up to 1% (v/v) HNO 3 and 1% (w/w) NaCl, to a more suitable medium (i.e. CH 3 OH/H 2 O (95/5 v/v) with 5.0 mM ammonium acetate and 0.75% (v/v) acetic acid) via electrochemically controlled reduction (deposition) and oxidation (stripping) of the Cu 2 is demonstrated. Acidic samples and samples containing significant levels of dissolved solids required cell washout times of up to 4.0 min following electrochemical extraction. Nonetheless, analysis time was still less than 8 min per sample. Quantification of 20-50 mg/L Cu 2 in various matrices using standard additions with this electrochemical/ES-MS combination is evaluated. The limitations of this combination in its present state of development and possible future directions are summarized.

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