In situ optical spectroelectrochemistry of single-walled carbon nanotube thin films

A detailed study is presented on the optical absorption of thin films of single-walled carbon nanotubes (SWNT) under electrochemical conditions. The procedure for the preparation of free-standing semitransparent films of SWNT is used for the fabrication of a working electrode for transmission optical spectroelectrochemistry. The analysis of the potential dependent spectroscopic response of the SWNT film benefits from the widest possible electrochemical window, in which the charging of SWNT can safely be investigated. This electrochemical window is not limited by parasitic electrochemistry and/or galvanic breakdown reactions occurring at supporting electrode materials such as indium–tin oxide conducting glass or semitransparent Pt film, which were employed in earlier studies. Electrochemical doping of SWNT is observable at the optical absorptions, which are assigned to allowed electronic transitions between van Hove singularities in the density of states of SWNT. Furthermore, the spectral response of counterions, balancing the charging of the nanotube skeleton, is traceable at certain conditions. The latter effect is monitored here through the overtones of C–H stretching vibrations from tetrabutylammonium cations.     

Electrochemical formation of anodic oxide films on Nb surfaces: ellipsometric and Raman spectroscopical studies

Electrochemical formation of anodic oxide films on niobium (Nb) surfaces in 1 M H₂SO₄ solutions was studied using ellipsometry and Raman spectroscopy. By in situ ellipsometric measurements, the coefficient of film thickness growth and the complex index of refraction of anodic oxide films in the voltage range between 0 and 100 V were determined. The Raman spectra reveal that the thin passive films are amorphous. In the beginning of crystallization, the anodic oxide films consist of mixtures of NbO₂ and Nb₂O₅, while NbO₂ is completely transformed to Nb₂O₅ for thicker and well-crystallized films.     

Electrochemically induced transformations of heteropolyanions: new electroactive metal oxide films studied by the electrochemical quartz crystal microbalance

New oxide films have been electrodeposited from [P₂Mo₁₈O₆₂]⁶⁻ by potential cycling in mildly acidic aqueous media. To obtain an adherent and persistent film, it is necessary that more than six electrons/molecule be fixed on the framework of the heteropolyanion. The film is then studied in pure supporting electrolyte. In this medium, a remarkable current increase is observed during the potential cycling. Whether the film is deposited on a glassy carbon electrode or on the gold electrode of an electrochemical quartz crystal microbalance (EQCM), exactly the same steady current increase up to a maximum is obtained in cyclic voltammetric measurements. The EQCM reveals a steady mass increase during the continuous cycling of the film in the supporting electrolyte. This behaviour is interpreted as featuring an irreversible water and electrolyte intake into the film, up to a maximum, after which the phenomena observed during reduction and oxidation processes are taken as featuring intercalation/deintercalation, respectively. This behaviour is much the same as described in the literature for WO₃ and MoO₃ bronzes, except that the present films seem very stable and have shown no tendency to dissolve or deactivate. Received: 2 December 1998 / Accepted: 26 January 1999     

Voltammetry and electrochemical impedance spectroscopy of gold electrodes modified with CdTe quantum dots and their conjugates with nickel tetraamino phthalocyanine

This work reports on the synthesis of conjugates of cadmium telluride quantum dots (CdTe-QDs) caped with thioglycolic acid and peripherally substituted nickel tetraamino phthalocyanine (NiTAPc) complex. The conjugates are characterized using cyclic (CV) and differential pulse (DPV) voltammetries, electrochemical impedance spectroscopy, X-ray powder diffraction, infrared spectroscopy, Raman spectroscopy, atomic force microscopy and time correlated single photon counting. CV and DPV show that NiTAPc stabilizes the CdTe QDs against oxidation to metallic products.     

Effect of the modification of mercuric oxide on the properties of mercury films at HgO-modified carbon paste electrodes

The influence of modifications of the mercuric oxide on the voltammetric properties of mercury film carbon paste electrodes was studied. The mercury film was formed electrochemically from the bulk red or yellow mercuric oxide-modified carbon paste electrodes. Differential pulse anodic stripping voltammetry and optical microscopy in polarised light were used to characterise the properties of the mercury films. The results were compared with those obtained using the conventional preparation of mercury-plated carbon paste electrodes when the mercury film is deposited on the surface of the electrode by reduction of Hg(II) ions in solution utilising a sufficient negative potential. It was shown that the mercury film formed from the yellow modification of the mercuric oxide provides better voltammetric characteristics than the red one owing to the high distribution of its small particles, i.e. the mercury droplets after electrochemical treatment. Such a mercury film has similar properties to those of a mercury film generated from solution. Received: 06 December 1999 / Accepted: 16 March 2000     

Nanocomposite thin film structures based on polyarylenephthalide with SWCNT and graphene oxide fillers

Investigations of nanocomposite thin films based on polyarylene- phthalide, single-walled carbon nanotubes and graphene oxide have been carried out. Using these films as a transport layer, field-effect transistors were assembled and their output and transfer characteristics were measured. The mobility of charge carriers was estimated and the obtained values are as follows: μ_PAP/GO = 0.020 cm² V^?1 s^?1 and μ_PAP/SWCNT = 0.071 cm² V^?1 s^?1.     

Electrochemical Characterization of and Stripping Voltammetry at Screen Printed Electrodes Modified with Different Brands of Multiwall Carbon Nanotubes and Bismuth Films

A screen-printed electrode sensor has been fabricated by modifying the carbon ink surface with different brands of multiwall carbon nanotubes (MWCNTs) and bismuth film (BiF) for the determination of traces of lead, cadmium and zinc ions by square wave anodic stripping voltammetry. The MWCNTs, from three different sources, were functionalized and dispersed in Nafion (MWCNT-Nafion) solution and placed on screen printed electrodes (MWCNT-Nafion/SPE); bismuth films were then prepared by ex-situ plating of bismuth onto the MWCNT-Nafion/SPE electrodes. The electrochemical characteristics of BiF/MWCNT-Nafion/SPE/ were examined by electrochemical impedance spectroscopy and showed differences; the charge transfer resistance tends to decrease with negative applied potentials. After optimizing the experimental conditions, the square-wave peak current signal is linear in the nmol L^?1 range. The lowest limit of detection found for the separate determination of lead, cadmium and zinc were 0.7 nmol L^?1, 1.5 nmol L^?1, and 11.1 nmol L^?1, respectively, with a 120 s deposition time.     

Flame spray pyrolysis for the one-step fabrication of transition metal oxide films: Recent progress in electrochemical and photoelectrochemical water splitting

Developing large scale deposition techniques to fabricate thin porous films with suitable opto-electro nic properties for water catalysis is a necessity to mitigate climate change and have a sustainable environment.In this review,flame spray pyrolysis(FSP)technique,a rapid and scalable methodology to synthesize nanostructured transitional metal oxide films with designed functionalities,is firstly introduced.Furthermore,applications in electrochemical(EC)and photoelectrochemical(PEC)water splitting for the production of hydrogen fuel is also presented.The high combustion temperature and the aggregation of flame aerosol ensure that the FSP-made films possess high crystallinity,tunable porosity and high surface areas,making this method suitable either as catalysts for EC water splitting or as efficient semiconductor materials for PEC water splitting.Finally,a perspective on the next generation FSP engineered films with potential applications in energy storage and conversion is described.     

Solid polymers doped with rare earth metal salts. II. Thermal behavior and morphology of the neodymium acetate–poly(ethylene oxide) system

Samples of poly(ethylene oxide), PEO, doped with neodymium acetate, Nd (Act)₃, were prepared and found to be microphase separated. At an EO/Nd (Act)₃ molar ratio no less than 4, wide-angle x-ray diffraction (WAXD) patterns and small-angle x-ray scattering (SAXS) data suggest that bulk Nd (Act)₃ and ionic clusters are both absent. It is inferred from differential scanning calorimetry (DSC) thermograms that in the presence of PEO, Nd (Act)₃ forms an amorphous phase which is different from the amorphous phase formed by Nd (Act)₃ alone. The tighter binding of CH₃COO^- to Nd³⁺, in comparison to Cl^-, appears to be responsible for the lack of true dissolution of Nd (Act)₃ in PEO, a behavior clearly distinct from a number of polymer-metal salt complexes reported in the literature. © 1993 John Wiley & Sons, Inc.     

Speciation and detection of arsenic in aqueous samples: A review of recent progress in non-atomic spectrometric methods

Inorganic arsenic (As) displays extreme toxicity and is a class A human carcinogen. It is of interest to both analytical chemists and environmental scientists. Facile and sensitive determination of As and knowledge of the speciation of forms of As in aqueous samples are vitally important. Nearly every nation has relevant official regulations on permissible limits of drinking water As content. The size of the literature on As is therefore formidable. The heart of this review consists of two tables: one is a compilation of principal official documents and major review articles, including the toxicology and chemistry of As. This includes comprehensive official compendia on As speciation, sample treatment, recommended procedures for the determination of As in specific sample matrices with specific analytical instrument(s), procedures for multi-element (including As) speciation and analysis, and prior comprehensive reviews on arsenic analysis. The second table focuses on the recent literature (2005–2013, the coverage for 2013 is incomplete) on As measurement in aqueous matrices. Recent As speciation and analysis methods based on spectrometric and electrochemical methods, inductively coupled plasma-mass spectrometry, neutron activation analysis and biosensors are summarized. We have deliberately excluded atomic optical spectrometric techniques (atomic absorption, atomic fluorescence, inductively coupled plasma-optical emission spectrometry) not because they are not important (in fact the majority of arsenic determinations are possibly carried out by one of these techniques) but because these methods are sufficiently mature and little meaningful innovation has been made beyond what is in the officially prescribed compendia (which are included) and recent reviews are available.     

Biosensors and rapid diagnostic tests on the frontier between analytical and clinical chemistry for biomolecular diagnosis of dengue disease: a review

The past decades have witnessed enormous technological improvements towards the development of simple, cost-effective and accurate rapid diagnostic tests for detection and identification of infectious pathogens. Among them is dengue virus, the etiologic agent of the mosquito-borne dengue disease, one of the most important emerging infectious pathologies of nowadays. Dengue fever may cause potentially deadly hemorrhagic symptoms and is endemic in the tropical and sub-tropical world, being also a serious threat to temperate countries in the developed world. Effective diagnostics for dengue should be able to discriminate among the four antigenically related dengue serotypes and fulfill the requirements for successful decentralized (point-of-care) testing in the harsh environmental conditions found in most tropical regions. The accurate identification of circulating serotypes is crucial for the successful implementation of vector control programs based on reliable epidemiological predictions. This paper briefly summarizes the limitations of the main conventional techniques for biomolecular diagnosis of dengue disease and critically reviews some of the most relevant biosensors and rapid diagnostic tests developed, implemented and reported so far for point-of-care testing of dengue infections. The invaluable contributions of microfluidics and nanotechnology encompass the whole paper, while evaluation concerns of rapid diagnostic tests and foreseen technological improvements in this field are also overviewed for the diagnosis of dengue and other infectious and tropical diseases as well.