A Comparative Electrochemical Behaviour Study and Analytical Detection of the p-Nitrophenol Using Silver Solid Amalgam, Mercury, and Silver Electrodes

This work reports a comparative electrochemical behaviour study and p-nitrophenol analytical detection using silver solid amalgam, hanging dropping mercury, and silver electrodes. For this, square wave voltammetry was employed, where the analytical responses and the redox mechanisms could be compared for reduction processes of 4-nitrophenol by analysis of the voltammetric responses. The analytical performance of the electrode was evaluated and detection and quantification limits, recovery percentages, repeatability, and reproducibility for the silver solid amalgam and hanging dropping mercury electrodes presented similar values; the results presented for the silver electrode indicated worse analytical parameters than the other electrodes. The results indicate that the silver solid amalgam electrode can be considered a suitable tool and an interesting alternative for the analytical determination of 4-nitrophenol, as well as for the determination of other biological and environmentally interesting compounds that present analytical responses on mercury surfaces

Indirect determination of sulfite using a polyphenol oxidase biosensor based on a glassy carbon electrode modified with multi-walled carbon nanotubes and gold nanoparticles within a poly(allylamine hydrochloride) film

AbstractThe modification of a glassy carbon electrode with multi-walled carbon nanotubes and gold nanoparticles within a poly(allylamine hydrochloride) film for the development of a biosensor is proposed. This approach provides an efficient method used to immobilize polyphenol oxidase (PPO) obtained from the crude extract of sweet potato (Ipomoea batatas (L.) Lam.). The principle of the analytical method is based on the inhibitory effect of sulfite on the activity of PPO, in the reduction reaction of o-quinone to catechol and/or the reaction of o-quinone with sulfite. Under the optimum experimental conditions using the differential pulse voltammetry technique, the analytical curve obtained was linear in the concentration of sulfite in the range from 0.5 to 22μmolL−1 with a detection limit of 0.4μmolL−1. The biosensor was applied for the determination of sulfite in white and red wine samples with results in close agreement with those results obtained using a reference iodometric method (at a 95% confidence level)

Correction: Exploring the origins of the apparent "electrocatalytic" oxidation of kojic acid at graphene modified electrodes (Analyst (2013) 138 (4436-4442))

The text that appears on page 4437 under the heading ‘Experimental section’ that reads: ESI Fig. S1A† depicts a typical Transmission Electron Microscope (TEM) image of the commercially purchased graphene and ESI Fig. S1B† shows a high resolution TEM image where a hexagonal arrangement of carbon atoms, which is characteristic of graphene, is clearly evident. should be changed to: ESI Fig. S1A† depicts a typical TEM image of a graphene sheet that has been fabricated using the same method as our commercially sourced graphene and Fig. S1B† shows a high-resolution TEM image (from the same source) where a hexagonal arrangement of carbon atoms, which is characteristic of graphene, is clearly evident. Independent TEM and Raman analysis of the commercially sourced graphene (as received from the supplier and consequently as used throughout this work) is presented in Fig. S3 and S4† respectively. The Royal Society of Chemistry apologises for these errors and any consequent inconvenience to authors and readers

Exploring the origins of the apparent "electrocatalytic" oxidation of kojic acid at graphene modified electrodes

We explore the recent reports that the use of graphene modified electrodes gives rise to the electrocatalytic oxidation of kojic acid. It is demonstrated that large quantifiable voltammetric signatures are observed on bare/unmodified graphitic electrodes, which are shown to be analytically useful and superior to those observed at graphene modified alternatives. This work is of importance as it shows that control experiments are critical and must be undertaken before "electrocatalysis" is conferred when investigating graphene in electrochemistry. In terms of the electroanalytical response of graphene modified electrodes, a bare edge plane pyrolytic graphite electrode is shown to give rise to an improved linear range and limit of detection, questioning the need to modify electrodes with graphene. © 2013 The Royal Society of Chemistry

Imparting improvements in electrochemical sensors: evaluation of different carbon blacks that give rise to significant improvement in the performance of electroanalytical sensing platforms

Three different carbon black materials have been evaluated as a potential modifier, however, only one demonstrated an improvement in the electrochemical properties. The carbon black structures were characterised with SEM, XPS and Raman spectroscopy and found to be very similar to that of amorphous graphitic materials. The modifications utilised were constructed by three different strategies (using ultrapure water, chitosan and dihexadecylphosphate). The fabricated sensors are electrochemically characterised using N,N,N',N'-tetramethyl-para-phenylenediamine and both inner-sphere and outer-sphere redox probes, namely potassium ferrocyanide(II) and hexaammineruthenium(III) chloride, in addition to the biologically relevant and electroactive analytes, dopamine (DA) and acetaminophen (AP). Comparisons are made with an edge-plane pyrolytic graphite and glassy-carbon electrode and the benefits of carbon black implemented as a modifier for sensors within electrochemistry are explored, as well as the characterisation of their electroanalytical performances. We reveal significant improvements in the electrochemical performance (excellent sensitivity, faster heterogeneous electron transfer rate (HET)) over that of a bare glassy-carbon and edge-plane pyrolytic graphite electrode and thus suggest that there are substantial advantages of using carbon black as modifier in the fabrication of electrochemical based sensors. Such work is highly important and informative for those working in the field of electroanalysis where electrochemistry can provide portable, rapid, reliable and accurate sensing protocols (bringing the laboratory into the field), with particular relevance to those searching for new electrode materials.The authors acknowledge financial support from the following Brazilian funding agencies: FAPESP (Proc. 2013/16770-0,2014/04284-6 and 2010/20754-1), CNPq and CAPES

Flow injection turbidimetric determination of acetylcysteine in pharmaceutical formulations using silver nitrate as precipitant reagent

A simple, accurate and precise flow-injection turbidimetric procedure is reported for the determination of acetylcysteine in pharmaceutical formulations. The procedure is based on the precipitation of acetylcysteine with silver nitrate solution in acid medium and the insoluble salt produced was monitored at 410 nm. The analytical curve for acetylcysteine was linear in the concentration range from 1.0 × 10-4 to 1.0 × 10-3 mol L-1 with a detection limit of 5.0 × 10-5 mol L-1. The sampling rate was 60 h-1 and the relative standard deviations (RSDs) were less than 2.0% for 1.0 × 10-4 and 5.0 × 10-4 mol L-1 acetylcysteine solutions (n=10). The recovery of this analyte in four samples ranged from 97.6 to 103 %. A paired t-test showed that all results obtained for acetylcysteine in pharmaceutical products using the proposed flow-injection procedure and the official procedure agreed at the 95% confidence level