Hydrogen peroxide monitoring in Fenton reaction by using a ruthenium oxide hexacyanoferrate/multiwalled carbon nanotubes modified electrode

A novel amperometric sensor based on the incorporation of ruthenium oxide hexacyanoferrate (RuOHCF) into multiwalled carbon nanotubes (MWCNTs) immobilized on a glassy carbon electrode is described. Cyclic voltammetry experiments indicated that the cathodic reduction of hydrogen peroxide at the RuOHCF/MWCNTs100/GC modified electrode is facilitated, occurring at 0.0 V vs. Ag/AgCl/KCl(sat). Following the optimization of the experimental conditions, the proposed sensor presented excellent analytical properties for hydrogen peroxide determination, with a low limit of detection (4.7 mu mol L-1), a large dynamic concentration range (0.1-10 mmol L-1) and a sensitivity of 1280 mu A mmol(-1) L cm(-2). The usefulness of the RuOHCF/MWCNTs100/GC electrochemical sensor was confirmed by monitoring the consumption of hydrogen peroxide during the degradation of phenol by the Fenton reaction. (C) 2012 Elsevier B.V. All rights reserved.

Amperometric urea biosensors based on the entrapment of urease in polypyrrole films

Urease (Urs) was immobilized in electrochemically prepared polypyrrole (PPy) and the resulting films were characterized by cyclic voltammetry, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and ultraviolet visible spectroscopy (UV-VIS). The enzymatic activity of Urs entrapped in the PPy matrix was confirmed by the catalytic conversion of urea into carbon dioxide and ammonia, when urea was detected amperometrically at different concentrations in standard samples and commercial fertilizers. The PPy/Urs biosensors exhibited selectivity, a relatively high efficiency at urea concentrations below 3.0 mmol L-1, and a sensitivity to urea of 2.41 mu A cm(-2) mmol(-1) L (C) 2011 Elsevier Ltd. All rights reserved.

An electrochemical gas sensor based on paper supported room temperature ionic liquids

A sensitive and fast-responding membrane-free amperometric gas sensor is described, consisting of a small filter paper foil soaked with a room temperature ionic liquid (RTIL), upon which three electrodes are screen printed with carbon ink, using a suitable mask. It takes advantage of the high electrical conductivity and negligible vapour pressure of RTILs as well as their easy immobilization into a porous and inexpensive supporting material such as paper. Moreover, thanks to a careful control of the preparation procedure, a very close contact between the RTIL and electrode material can be achieved so as to allow gaseous analytes to undergo charge transfer just as soon as they reach the three-phase sites where the electrode material, paper supported RTIL and gas phase meet. Thus, the adverse effect on recorded currents of slow steps such as analyte diffusion and dissolution in a solvent is avoided. To evaluate the performance of this device, it was used as a wall-jet amperometric detector for flow injection analysis of 1-butanethiol vapours, adopted as the model gaseous analyte, present in headspace samples in equilibrium with aqueous solutions at controlled concentrations. With this purpose, the RTIL soaked paper electrochemical detector (RTIL-PED) was assembled by using 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl) imide as the wicking RTIL and printing the working electrode with carbon ink doped with cobalt(II) phthalocyanine, to profit from its ability to electrocatalyze thiol oxidation. The results obtained were quite satisfactory (detection limit: 0.5 mu M; dynamic range: 2-200 mu M, both referring to solution concentrations; correlation coefficient: 0.998; repeatability: +/- 7% RSD; long-term stability: 9%), thus suggesting the possible use of this device for manifold applications.

MEH-PPV Thin Films for Radiation Sensor Applications

This work deals with MEH-PPV thin films to be used as gamma radiation sensors. The polymer thin films with two different thicknesses (30 and 100 nm) were irradiated at room temperature with different gamma radiation doses (up to 25 kGy). Optical properties of the material were investigated with FTIR and UV-Vis absorption spectroscopy. Results show that gamma radiation does not degrade substantially the thin-film material, suggesting that a crosslink effect may be occurring. The characteristic absorption peak of MEH-PPV, around 500 nm is shifted to shorter wavelengths with the increase of gamma radiation doses for both thicknesses samples. The 30-nm-thick samples showed a larger variation absorbance at a specific wavelength and a larger peak shift. These results indicate their potential for use in monitoring the radiation doses used on the sterilization of health care products.

An Alternative Method for the Simultaneous Determination of Copper and Lead for Quality Control of Sugar Cane Spirit using a Nanotube-Based Sensor

The development of an electroanalytical method for simultaneous determination of copper and lead ions in sugar cane spirit (cachaca) using carbon paste electrode modified with ascorbic acid and carbon nanotubes (CPE-AaCNT) is described. Squarewave voltammetry (SWV) with anodic stripping was employed, and this technique was optimized with respect to the following parameters: frequency (50 Hz), amplitude (100 mV) and scan increment (9 mV). The analytical curves were linear in the range from 0.0900 to 7.00 mg L-1 for lead and copper. The limits of detection were 48.5 and 23.9 mu g L-1 for lead and copper, respectively. The developed method was applied to the simultaneous determination of copper and lead in five commercial samples of sugar cane spirit. The results were in good agreement with those obtained by F AAS/GF AAS (flame atomic absorption spectrometry/graphite furnace atomic absorption spectrometry) and showed that CPE-AaCNT can be successfully employed in the simultaneous determination of these metals in real sugar cane spirit samples.

Quantification of terbinafine in pharmaceutical tablets using capillary electrophoresis with contactless conductivity detection and batch injection analysis with amperometric detection

Terbinafine hydrochloride (TerbHCl) is an allylamine derivative with fungicidal action, especially against dermatophytes. Different analytical methods have been reported for quantifying TerbHCl in different samples. These procedures require time-consuming sample preparation or expensive instrumentation. In this paper, electrochemical methods involving capillary electrophoresis with contactless conductivity detection, and amperometry associated with batch injection analysis, are described for the determination of TerbHCl in pharmaceutical products. In the capillary electrophoresis experiments, terbinafine was protonated and analyzed in the cationic form in less than 1 min. A linear range from 1.46 to 36.4 mu g mL(-1) in acetate buffer solution and a detection limit of 0.11 mu g mL(-1) were achieved. In the amperometric studies, terbinafine was oxidized at +0.85 V with high throughput (225 injection h(-1)) and good linear range (10-100 mu mol L-1). It was also possible to determine the antifungal agent using simultaneous conductometric and potentiometric titrations in the presence of 5% ethanol. The electrochemical methods were applied to the quantification of TerbHCl in different tablet samples; the results were comparable with values indicated by the manufacturer and those found using titrimetry according to the Pharmacopoeia. The electrochemical methods are simple, rapid and an appropriate alternative for quantifying this drug in real samples. (C) 2012 Elsevier B.V. All rights reserved.

Immbolization of uricase enzyme in Langmuir and Langmuir-Blodgett films of fatty acids: Possible use as a uric acid sensor

Preserving the enzyme structure in solid films is key for producing various bioelectronic devices, including biosensors, which has normally been performed with nanostructured films that allow for control of molecular architectures. In this paper, we investigate the adsorption of uricase onto Langmuir monolayers of stearic acid (SA), and their transfer to solid supports as Langmuir Blodgett (LB) films. Structuring of the enzyme in beta-sheets was preserved in the form of 1-layer LB film, which was corroborated with a higher catalytic activity than for other uricase-containing LB film architectures where the beta-sheets structuring was not preserved. The optimized architecture was also used to detect uric acid within a range covering typical concentrations in the human blood. The approach presented here not only allows for an optimized catalytic activity toward uric acid but also permits one to explain why some film architectures exhibit a superior performance. (C) 2011 Elsevier Inc. All rights reserved.

Ab-initio calculations for a realistic sensor: A study of CO sensors based on nitrogen-rich carbon nanotubes

The use of nanoscale low-dimensional systems could boost the sensitivity of gas sensors. In this work we simulate a nanoscopic sensor based on carbon nanotubes with a large number of binding sites using ab initio density functional electronic structure calculations coupled to the Non-Equilibrium Green's Function formalism. We present a recipe where the adsorption process is studied followed by conductance calculations of a single defect system and of more realistic disordered system considering different coverages of molecules as one would expect experimentally. We found that the sensitivity of the disordered system is enhanced by a factor of 5 when compared to the single defect one. Finally, our results from the atomistic electronic transport are used as input to a simple model that connects them to experimental parameters such as temperature and partial gas pressure, providing a procedure for simulating a realistic nanoscopic gas sensor. Using this methodology we show that nitrogen-rich carbon nanotubes could work at room temperature with extremely high sensitivity. Copyright 2012 Author(s). This article is distributed under a Creative Commons Attribution 3.0 Unported License. [http://dx.doi.org/10.1063/1.4739280]

Active crop sensor to detect variability of nitrogen supply and biomass on sugarcane fields

Nitrogen management has been intensively studied on several crops and recently associated with variable rate on-the-go application based on crop sensors. Such studies are scarce for sugarcane and as a biofuel crop the energy input matters, seeking high positive energy balance production and low carbon emission on the whole production system. This article presents the procedure and shows the first results obtained using a nitrogen and biomass sensor (N-Sensor (TM) ALS, Yara International ASA) to indicate the nitrogen application demands of commercial sugarcane fields. Eight commercial fields from one sugar mill in the state of Sao Paulo, Brazil, varying from 15 to 25 ha in size, were monitored. Conditions varied from sandy to heavy soils and the previous harvesting occurred in May and October 2009, including first, second, and third ratoon stages. Each field was scanned with the sensor three times during the season (at 0.2, 0.4, and 0.6 m stem height), followed by tissue sampling for biomass and nitrogen uptake at ten spots inside the area, guided by the different values shown by the sensor. The results showed a high correlation between sensor values and sugarcane biomass and nitrogen uptake, thereby supporting the potential use of this technology to develop algorithms to manage variable rate application of nitrogen for sugarcane.

Flow injection analysis of free glycerol in biodiesel using a copper electrode as an amperometric detector

The main goal of this work was to develop a simple analytical method for quantification of glycerol based on the electrocatalytic oxidation of glycerol on the copper surface adapted in a flow injection system. Under optimal experimental conditions, the peak current response increases linearly with glycerol concentration over the range 60-3200 mg kg(-1) (equivalent to 3-160 mg L(-1) in solution). The repeatability of the electrode response in the flow injection analysis (FIA) configuration was evaluated as 5% (n = 10), and the detection limit of the method was estimated to be 5 mg kg(-1) in biodiesel (equivalent to 250 mu g L(-1) in solution) (S/N = 3). The sample throughput under optimised conditions was estimated to be 90 h(-1). Different types of biodiesel samples (B100), as in the types of vegetable oils or animal fats used to produce the fuels, were analysed (seven samples). The only sample pre-treatment used was an extraction of glycerol from the biodiesel sample containing a ratio of 5 mL of water to 250 mg of biodiesel. The proposed method improves the analytical parameters obtained by other electroanalytical methods for quantification of glycerol in biodiesel samples, and its accuracy was evaluated using a spike-and-recovery assay, where all the biodiesel samples used obtained admissible values according to the Association of Official Analytical Chemists. Crown Copyright (C) 2011 Published by Elsevier Ltd. All rights reserved.

Ultrasonic sensor for the presence of oily contaminants in water

The determination of the complex reflection coefficient of ultrasonic shear-waves at the solid-liquid interface is a technique employed for the measurement of the viscoelastic properties of liquids. An interesting property of the measurement technique is the very small penetration depth of the shear-waves into the liquid sample, which permits measurements with liquid films of some micrometers thick. This property, along with the adhesion of oily substances to surfaces, can be used for the detection of oily contaminants in water. In this work, the employment of the ultrasonic shear-wave reflection technique to the detection of oily contaminants in water is proposed and the theoretical and experimental concepts involved are discussed. Preliminary experimental results show the measurement technique can detect SAE 40 automotive oil in water in volume proportions less than 0.5%.

Vanadium and Titanium Mixed Oxide Films: Synthesis, Characterization and Application as Ion Sensor

Vanadium/titanium mixed oxide films were produced using the sol-gel route. The structural investigation revealed that increased TiO2 molar ratio in the mixed oxide disturbs the V2O5 crystalline structure and makes it amorphous. This blocks the TiO2 phase transformation, so TiO2 stabilizes in the anatase phase. In addition the surface of the sample always presents larger amounts of TiO2 than expected, revealing a concentration gradient along the growth direction. For increased TiO2 molar ratios the roughness of the surface is reduced. Ion sensors were fabricated using the extended gate field effect transistor configuration. The obtained sensitivities varied in the range of 58 mV/pH down to 15 mV/pH according to the composition and morphology of the surface of the samples. Low TiO2 amounts presented better sensing properties that might be related to the cracked and inhomogeneous surfaces. Rising the TiO2 quantity in the films produces homogeneous surfaces but diminishes their sensitivities. Thus, the present paper reveals that the compositional and structural aspects change the surface morphology and electrical properties accounting for the final ion sensing properties of the V2O5/TiO2 films. (C) 2012 The Electrochemical Society. [DOI: 10.1149/2.053206jes] All rights reserved.

USE OF THE LINEAR LIGHT SENSOR ILX554 IN OPTICAL SPECTROSCOPY

USE OF THE LINEAR LIGHT SENSOR ILX554 IN OPTICAL SPECTROSCOPY. This technical note describes the construction of a low-cost optical detector. This device is composed by a high-sensitive linear light sensor (model ILX554) and a microcontroller. The performance or the detector was demonstrated by the detection of emission and Raman spectra of the several atomic systems and the results reproduce those found in the literature.

STRATEGIES FOR PREPARATION OF MOLECULARLY IMPRINTED POLYMERS MODIFIED ELECTRODES AND THEIR APPLICATION IN ELECTROANALYSIS: A REVIEW

Molecularly imprinted polymers (MIP's) have been applied in several areas of analytical chemistry, including the modification of electrodes. The main purpose of such modification is improving selectivity; however, a gain in sensitivity was also observed in many cases. The most frequent approaches for these modifications are the electrodeposition of polymer films and sol gel deposits, spin and drop coating and self-assembling of films on metal nanoparticles. The preparation of bulk (body) modified composites as carbon pastes and polymer agglutinated graphite have also been investigated. In all cases several analytes including pharmaceuticals, pesticides, and inorganic species, as well as molecules with biological relevance have been successfully used as templates and analyzed with such devices in electroanalytical procedures. Herein, 65 references are presented concerning the general characteristics and some details related to the preparation of MIP's including a description of electrodes modified with MIP's by different approaches. The results using voltammetric and amperometric detection are described.

Static postural balance study in patients with vestibular disorders using a three dimensional eletromagnetic sensor system

The vestibular-ocular reflex assessment is important, but not enough. Tridimensional electromagnetic sensor systems represent a new method to assess posturography. Aim: To assess body sway in healthy subjects who had positive Dix Hallpike and Epley maneuvers and with other vestibular dysfunctions by means of a three-dimensional system. Study design: Prospective. Materials and Methods: We had 23 healthy women, 15 with peripheral vestibular dysfunction found upon caloric test and 10 with positive Epley and Dix Hallpike maneuvers. All tests performed in the following positions: open and closed eyes on stable and unstable surfaces. Results: With the Eyes Open and on a stable surface, p < 0.01 between the control group and the one with peripheral vestibular dysfunction in all variables, except the a-p maximum, full speed and mediolateral trajectory velocity, which had a p < 0.01 between the group with vestibular dysfunction and controls in all positions. The group with positive Epley and Dix Hallpike maneuvers had p < 0.01 at full speed and in its components in the x and y in positions with open and eyes closed on an unstable surface. Conclusion: The tridimensional electromagnetic sensors system was able to generate reliable information about body sway in the study volunteers.