A sequential injection lab-on-valve (LOV) unit, integrating a miniaturized electrochemical flow cell (EFC), has been constructed for the determination of trace amounts of Se (IV) by employing cathodic stripping voltammetry (CSV) technique. The procedure is carried out on a mercury film coated glassy carbon electrode. The analyte solution and electrolyte solution were continuously aspirated and merged in the holding coil (HC) by using a single syringe pump, which were afterwards pushed into the EFC, where the peak current was generated during the subsequent deposition/stripping procedure and measured as the basis of quantification. Assay parameters were optimized in order to achieve the best analytical performance, including mercury film preparation, supporting electrolyte composition, deposition potential and deposition time, and flow variables in the LOV. By loading a sample volume of 500 microL, a linear calibration graph was derived within 1-600 microg L(-1), and a detection limit (3b) of 0.11 microgL(-1) was achieved along with a sampling frequency of 20 h(-1). By integrating the EFC into the LOV unit, the assembling system not only minimized the sample/reagent consumption and waste generation, but also enhanced the sampling frequency. The work itself extended the applications of electrochemical detection techniques and provided a good platform for Se (IV) electrochemical analysis.
"Flow based methods provide automation for sample preparation and detection. Flow based techniques incorporating with hydride generation-atomic absorption spectrometry (Zhang and Adeloju 2008; Mena et al. 1999), hydride generation-atomic fluorescence spectrometry (Semenova et al. 2003; Gamiz-Gracia and Luque de Castro 1999), fluorometry (Pedro et al. 2004), spectrometry (Nakano, Yoshii, and Kawashima 2004; Mousavi, Ghiasvand, and Jahanshahi 1998), and voltammetry (Wang et al. 2009) were applied for determination of selenium in various samples such as food, pharmaceutical, and environmental samples. "
[Show abstract][Hide abstract] ABSTRACT: A precise, accurate, and reliable flow-batch spectrophotometric method for the determination of selenium (IV) was developed using o-phenylenediamine as a reagent with a sequential injection monosegmented flow system incorporating a simple heating unit. The reaction zones of selenium(IV) and o-phenylenediamine were mixed and heated in a chamber at 62°C for 5 minutes. The piaselanol complexes were then detected at a maximum absorption wavelength of 335 nm. In-line single standard calibration and standard addition procedures were developed employing the monosegmented flow technique. Under the optimized conditions, a linear calibration graph in a range of 0.1–4.0 mg L−1 selenium (IV) was obtained with limits of detection and quantitation of 0.01 and 0.1 mg L−1, respectively. Relative standard deviations were 2% [for both 0.1 and 0.5 mg L−1 selenium (IV) (n = 11)]. A sample throughput of 2 h−1 using four standard addition levels was achieved. The developed system was successfully applied to raw selenium-enriched yeast samples. The analyses performed by the developed method agreed well with those obtained from a standard inductively coupled plasma mass spectrometry method.
[Show abstract][Hide abstract] ABSTRACT: This paper presents an overview of the field of electrochemical stripping analysis in flow systems covering developments in the last 12 years (since 1998). The review discusses the flow schemes utilized in stripping analysis, techniques for on-line sample pre-treatment, the main pre-concentration and stripping/detection modes, the most important flow-through cell configurations used and the different types of working electrodes. Finally, applications in inorganic and organic analysis are discussed. Special emphasis is given to different novel approaches developed over the last few years that hold some promise for the future such as the use of the lab-on-a valve (LOV) configuration, microfluidic manifolds, flow-probes for remote sensing, environmentally friendly electrode materials and hyphenation with spectroscopic techniques.
[Show abstract][Hide abstract] ABSTRACT: The lab-on-a-valve (LOV) integrated microdevice has recently attracted much attention as a functional mesofluidic platform for programmable, pressure-driven flow as compared to lab-on-a-chip counterparts. We review the current state of the art of LOV as a versatile front end to column-separation techniques, namely, liquid chromatography (LC), gas chromatography (GC) and capillary electrophoresis (CE) for automatic mesofluidic handling at the low-microliter level, in-line sample processing and introducing the appropriate form of the analyte into the instrument for separation or detection.The open architecture of the LOV monolith unit has been to date exploited to accommodate micro solid-phase extraction in a renewable fashion, the so-called bead-injection analysis, encompassing reversed-phase materials and molecularly imprinted polymers, and in-valve microscale affinity chromatography. A plethora of interfaces have been recently devised for reliable injection of minute, well-defined volumes of analyte-containing solutions into LC,GC or CEWe illustrate these applications with representative examples in environmental and bioanalytical arenas.
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