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On-line electrochemically controlled solid-phase extraction coupled to electrospray and inductively coupled plasma mass spectrometry
Uppsala University, Teknisk-naturvetenskapliga vetenskapsområdet, Chemistry, Department of Chemistry.
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Manuscript (Other academic)
URN: urn:nbn:se:uu:diva-93085OAI: oai:DiVA.org:uu-93085DiVA: diva2:166455
Available from: 2005-05-03 Created: 2005-05-03 Last updated: 2010-01-13Bibliographically approved
In thesis
1. Development and Investigations of Novel Sample Preparation Techniques: Electrochemical Extraction and Evaluation of Miniaturized Analytical Devices Coupled to Mass Spectrometry
Open this publication in new window or tab >>Development and Investigations of Novel Sample Preparation Techniques: Electrochemical Extraction and Evaluation of Miniaturized Analytical Devices Coupled to Mass Spectrometry
2005 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Different sample preparation steps prior to a detection method are often essential in analytical chemistry. In this thesis, both static extractions and on-line coupled solid-phase extractions have been studied in combination with different detection techniques. Aspects of performing sample preparations in miniaturized analytical devices and the development of poly(dimethylsiloxane) (PDMS) microchips are discussed. Polypyrrole was also evaluated as an electrochemically controllable stationary phase for solid-phase microextraction (SPME) and solid-phase extraction (SPE).

The first part of this thesis describes the extraction of an organic compound from a very complex solid matrix utilizing the pressurized-fluid extraction (PFE) technique. The presented results show that PFE is easily optimized and enables rapid extractions and extracts relatively free from interferences.

An integrated three-electrode device, which enabled electrochemical (EC) SPME under potential control, was developed. With this device, both anions and cations could be extracted employing two types of polypyrrole films. Planar micro band electrodes positioned at the end of a capillary were also used to electrochemically extract and detect anions in a miniaturized flow system. Different analyte concentrations and preconcentration times were examined, and good linear correlations were found between the extraction time and the detection response. The on-line coupling of a thin layer EC cell, with a polypyrrole coated working electrode, to different mass spectrometric (MS) techniques is also described and evaluated. The results show that EC-SPE, employing polypyrrole as stationary phase, can be used as a preconcentration step prior to detection.

In addition, this thesis describes the development and on-line coupling of a microelectrode array equipped PDMS microchip with an integrated graphite electrospray emitter to electrospray ionization (ESI) MS. The system enabled short transfer times and an EC conversion efficiency of 30% at a flow rate of 0.5 μL/min. The on-line EC/ESI-MS experiments were significantly simplified using a wireless Bluetooth battery-powered EC instrument.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2005. 51 p.
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 54
Analytical chemistry, Electrochemical extraction, Solid-phase microextraction, Solid-phase extraction, Microchip, Mass spectrometry, Polypyrrole, Pressurized-fluid extraction, Preconcentration, Electrospray ionization, Analytisk kemi
National Category
Analytical Chemistry
urn:nbn:se:uu:diva-5807 (URN)91-554-6256-1 (ISBN)
Public defence
2005-06-02, Room B41, BMC, Uppsala Biomedical Center, Uppsala, 13:15
Available from: 2005-05-03 Created: 2005-05-03Bibliographically approved

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