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Complex geometries for electrodes are a great challenge in electrochemical applications. Slurry electrodes have been one example, which use complex flow distributors to improve the charge transfer between the current collector and the slurry particles. Here we use titanium-based flow distributors produced by indirect 3D-printing to improve further the electron transfer from highly conductive flow distributors to the slurry particles for a vanadium redox flow application. The titanium static mixers are directly coated with graphite to increase the activity for vanadium redox reactions. Increasing layers of graphite have shown an optimum for the positive and negative electrolytes. The application of heat treatment on the electrodes improves the anodic and cathodic current peaks drastically. Testing the highly conductive static mixers in a self-made redox flow cell results in 110 mA cm-2 discharge polarization.

RESUMEN

Recently, a new sampling device combining active and passive sampling (APS) was developed for the measurement of time-averaged concentrations of metal species and both polar and non-polar organic contaminants in water. By coupling a diffusion cell (loaded with a set of sorbents selective for different substances) with a small pump and a flow meter, the APS device is able to perform in situ measurements that are independent of the hydrodynamic conditions in the exposure medium. In the present study, the diffusion layer thickness (δ) at the sorbent/solution interface within the diffusion cell was characterised under controlled flow conditions. Laboratory tests indicated that, in the range of flow rates investigated, the average diffusion layer thickness (δ¯) varied from ∼60 to ∼110 µm, depending on the type of substance measured and the position of the sorbent with respect to the flow direction. Due to its ability to maintain an approximately constant δ¯, good to excellent agreement was found between measurements performed with the APS device in non-complexing media and concentrations measured in discrete water samples for all the substances investigated. These results suggest that the APS device could overcome issues affecting the quantitative interpretation of measurements by conventional passive sampling devices and serve as a useful tool for simultaneously monitoring a wide range of contaminants in water.

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RESUMEN

Passive sampling with in situ devices offers several advantages over traditional sampling methods (i.e., discrete spot sampling), however, data interpretation from conventional passive samplers is hampered by difficulties in estimating the thickness of the diffusion layer at the sampler/medium interface (δ), often leading to inaccurate determinations of target analyte concentrations. In this study, the performance of a novel device combining active and passive sampling was investigated in the laboratory. The active-passive sampling (APS) device is comprised of a diffusion cell fitted with a pump and a flowmeter. Three receiving phases traditionally used in passive sampling devices (i.e., chelex resin, Oasis HLB, and silicone rubber), were incorporated in the diffusion cell and allowed the simultaneous accumulation of cationic metals, polar, and non-polar organic compounds, respectively. The flow within the diffusion cell was accurately controlled and monitored, and, combined with diffusion coefficients measurements, enabled the average δ to be estimated. Strong agreement between APS and time-averaged total concentrations measured in discrete water samples was found for most of the substances investigated. Accuracies for metals ranged between 87 and 116%, except Cu and Pb (∼50%), whilst accuracies between 64 and 101%, and 92 and 151% were achieved for polar and non-polar organic compounds, respectively. These results indicate that, via a well-defined in situ preconcentration step, the proposed APS approach shows promise for monitoring the concentration of a range of pollutants in water.

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RESUMEN

A membrane microcontactor suitable to perform liquid-liquid extraction as well as evaporation in order to conduct enrichment steps in sample preparation of organ samples has been designed, fabricated, and characterized. Spacers of 100- or 200-µm high were constructed in a metal substrate with a channel width of 13 mm and the extraction kinetics in these channels was evaluated. The spacers were designed such that at the entrance and exit region a uniform flow distribution could take place and that a uniform flow profile could be guaranteed along the channel, hence allowing a large freedom in sample volume to be processed. The extraction and evaporation kinetic behavior of the device was first evaluated by extraction of a drug candidate (4-(2,5-dimethyl-pyrrol-1-y1)-2-hydroxybenzoic acid). To evaluate the device under more challenging working conditions, a homogenized mice kidney sample containing the drug candidate that was administered in life condition was cleaned and enriched with the extraction and evaporation modules and characterized by high-performance liquid chromatography, yielding an overall analysis time of 15-20 min per sample only. The system has the potential to be operated in a continuous fashion, making it appealing to be implemented in screening or high-throughput applications.

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