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The progress made in recent years in the area of micro total analysis system (μ-TAS) has allowed the development of analytical tools for determination and measurement of elements and compounds that previously required bench laboratory equipment for such purposes. μ-TAS provides a high degree of sensitivity and they are simple and affordable. This work details a process by which classical colorimetric methodologies used in analysis have been adapted from discontinuous to continuous flow systems, for determination of cobalt in aqueous solutions in real time. The purpose of this adaptation is the subsequent system miniaturization using low temperature co-fired ceramics (LTCC). The adapted methodology for the colorimetric determination of cobalt uses 3-Hydroxy-4-nitroso-2,7-naphtalene disulfonic acid disodium salt or nitroso-R salt (NRS) as the main reagent, in an environment of acetate and sodium citrate which favors the reaction. The carrier solution is prepared with sulfuric acid. The system encompasses a microfluidic structure in LTCC, a peristaltic pump to maintain the continuous flow, a six-way valve for sample injection, and an issuer of light of 540 nm based on a multiled. Using the integrated circuit TCS3414, the signal is sent to the computer wirelessly through zigbee protocol, and at the end a LabVIEW-based application shows the absorbance for a range of concentrations between 0.5 and 10 mg/L.

An optical microfluidic system based on the use of modified gold nanoparticles for monitoring Hg(II) is presented. The system is based on the specific recognition of the heavy metal by a new synthesized ionophore based on a modified thiourea, which is attached to the gold nanoparticles. This interaction generates a change on the gold Surface Plasmon Resonance (SPR) band. The sensitivity and selectivity of the procedure is firstly studied in batch. The obtained results demonstrate the mercury selective response over the different tested ions that can be found in environmental water samples. Due to the remarkable unusual rapid signal change observed during the interaction of the metal and the modified gold nanoparticles, the reaction can be easily performed in a microfluidic system. Results obtained by using the microfluidic system revealed improved analytical features compared to batch experiments such as a lower detection limit (11 ppb), higher sensitivity and faster analysis time, all this with an easy and automated procedure. Therefore, the approach has shown great potential for designing low cost instrumentation for automatic in-field discrete or continuous measurements of Hg(II).

This work describes the development of a fully integrated Low Temperature Co-fired Ceramic (LTCC) microreactor for the synthesis of carbon dots (CDots). The microreactor integrates fluidics, a heating resistor and an optical window for fluorescence imaging of the reaction progress in a monolithic, all ceramic device, ensuring homogeneous surface chemistry and physical properties. A pool of different CDots was synthesized at high temperature and pressure using a hydrothermal method, demonstrating the robustness of the microreactor. The synthesis was monitored by following the photoluminescence of the produced CDots, and the reaction conditions were optimized according to their Quantum Yield (QY) and the flow pattern inside the microchannel. The obtained CDots exhibited blue photoluminescence upon irradiation with UV light with QYs of up to 0.77. The CDots were screened as metal nanoprobes and bioimaging contrast agents.

A novel fluorescence dip-probe POF (Polymer Optical Fiber) sensor that allows performing in situ chemical determinations has been fabricated. The dip-probe sensor design has been optimized by simulations in order to improve the fluorescence collection. To demonstrate its possibilities, it has been chemically activated with a lead-selective plasticized PVC (polyvinylchloride) membrane containing a new synthesized suitable fluoroionophore and a commercial lead ionophore. The analytical response of the dip-probe sensor has been characterized and it shows a fully reversible response with a sensitivity of −35.10 mV/dec C and a Pb2+ detection limit of 7 × 10−6 M, which can be appropriate for monitoring contamination episodes. No significant interferences with other metal ions have been found. The device has been finally tested to determine the lead content in contaminated natural samples with promising results.

A miniaturized and robust optical fluorosensor, designed as a portable instrumentation for the in situ analysis of ions in water samples by using optodes has been constructed with low cost discrete optical components. The chemical recognition element of the device consists of a plasticized PVC-based fluorescent optode, which includes a new hexamethine–hemicyanine dye as a fluorophore. The signal can be attributed to a certain analyte depending on the ionophore employed. In this work, a commercial potassium ionophore (valinomycin) has been used to formulate a model membrane selective to potassium. The sensor has been fully characterized using a simple flow injection analysis (FIA) system and analytical parameters such as sensitivity (0.71 mV dec −1 ), limit of detection (2.2 × 10 −5 M K + ), repeatability (R.S.D. = 4.2%), reproducibility, lifetime and ionic interferences have been determined. The developed miniaturized system has been applied to the potassium concentration determination in spiked tap water samples. The obtained results have been compared to those acquired by the ICP-OES reference method and the suitability of the experimental setup for the determination of ions in water samples by the miniaturized fluorescence proposal has been demonstrated.

New norcyanine dyes were characterised for their use as long wavelength chromoionophores in optodes. Different membrane compositions were formulated for pH determination in water and their response in terms of sensitivity, linear range, response time and reversibility was examined with the aim to apply them in planar optochemical sensors. Their absorbance maxima are located in the NIR region (785–830 nm), which is very appropriate for applications using common low cost telecommunication components. The characterised optodes showed good analytical features. Hence, fully reversible, reproducible, fast, and sensitive bulk optodes were obtained. The photostability of dyes in the plasticised matrices and their tendency to leach from the membrane phase were also evaluated at different conditions.

Some new symmetrical and unsymmetrical near-infrared absorbing acidochromic dyes are synthesised by a simple one-step reaction. Such indicators belong to the ketocyanine dyes type and as well as their full characterisation as the relationship between their structure and optical properties are discussed. They are mainly tested for their future application as pH or solvent polarity sensors. The absorption maxima of the long-wavelength absorbing acidic form span the region from 715 to 750 nm, nearly matching the emission wavelength of the 780 nm laser diode. p K a values in ethanol cover the range between 1.7 and 4.3, and reversible absorption spectra are observed while pH is changed forth and back. As merocyanine dyes, the synthesised ketocyanine dyes show a positive solvatochromism. Since one of the requirements for a solvatochromic molecule to be useful to establish a solvent polarity scale is its stability, the photostability of the dyes is tested in ethanolic solution as well.

Twenty ketocyanine dyes are evaluated as potential pH fluoroionophores to be used in the development of new integrated waveguide fluorescence optodes (IWFOs). Its fluorescence characterization, as well as the pH response is first undertaken in ethanolic solution and then in plasticized PVC membranes with a conventional spectrofluorimeter. Analytical parameters such as basicity, reversibility, leaching and calibration curves are determined in both media and finally, photostability is also measured. Besides, some photophysical fluorescent parameters, such as the emission wavelength, are evaluated for both species, the acidic and the basic form, and quantum yields are calculated in ethanolic solution. Ketocyanine dyes have demonstrated their suitability for being used as acidochromic fluoroionophores in bulk optodes for the development of new IWFOs. They exhibit high fluorescence intensities in the far-visible region, an adequate photostability and an optimum pH response.

The continuous monitoring of processes in the food industry, and in particular in wine production, holds great interest as it can help to increase the quality of the goods produced and also the efficiency of the production process. One process that is feasible to control is the stabilisation of wine by means of ion-exchange resins. The use of this technique is of great promise since it allows continuous wine treatment and also on-line monitoring systems can be applied to determine the saturation of the resin in addition to the fraction of wine requiring stabilisation. The development of a pH, calcium and potassium analyser for on-line monitoring of wine in a continuous flow system is reported here. The potentiometric sensors used are ion-selective field-effect transistors (ISFETs). The stability of these sensors in hydro-alcoholic media was studied obtaining a sensitivity of 56 mV per decade for the pH ISFET and sensitivities of −26 mV per decade and −50 mV per decade for calcium and potassium sensors, respectively. The long-term stability of pH-ISFETs was 7 and 4 months for cation sensors. Results obtained in the continuous flow system with wine samples demonstrated that the proposed system is capable to detect the saturation point of the ion-exchange resin in wine stabilisation process and also to determine the ratio of wine required to stabilise it.

The present report describes the development of a thick-film sensor with intended applications for soil analysis. A probe incorporates three sensors, each at a different depth and featuring a copper plate as the reference electrode. In addition, the probe also contains all necessary instrumentation required for processing the sensor signal and to transmit it via radio. The developed sensors were calibrated in situ using two different soil compositions by adding standard solutions. Results show a quasi-Nernstian response in soil, in response to the addition of fertilisers. Extracts of soil samples analysed by the Kjeldahl method were compared with results from the probe. This comparison confirms that the sensors are capable or measuring chemical parameters in situ in an automated fashion.

A new approach for developing absorbance optochemical sensors is presented in this paper. It is based on a planar microoptic circuit where an optochemically active membrane, which responds selectively to a compound, is deposited in the device, yielding a part of the guiding planar structure. Light is propagated through the membrane, which changes its spectral absorption properties and controls the selectivity of the measurements by means of several immobilised compounds. This way, high sensitivity of the device can be easily obtained due to relatively long light paths through the membrane, and low response times can be achieved as the analyte diffusion occurs perpendicularly to the light path and through a thin membrane. Experimental results on measurements of the concentration of a specific ion in solution using the fabricated sensors are also presented.

Ion-selective electrodes with poly(vinyl chloride) membranes cast directly on conductive composite substrates are easy to build and have shown their usefulness both in quiescent and flow analysis applications. Matching PVC-composite technology to that of ion-sensitive field-effect transistors (ISFETs) has produced a new type of hybrid chemical sensor. In this novel configuration, a graphite-loaded araldite layer is used to cover the gate opening of encapsulated ISFETs. A poly(vinyl chloride) membrane featuring a plasticiser and an ionophore is cast on top of the conductive composite, rendering the device sensitive to the ion of choice. The resulting hybrid devices show similar electrochemical features when compared to traditional sensors (ISFET + PVC membrane). They also display increased longevity and reduced optical sensitivity when compared with ISFETs featuring transparent PVC membranes.