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At least 253 records · Page 14Linked to original sources
PubMed2003

Determination of the antibiotic drug pefloxacin in bulk form, tablets and human serum using square wave cathodic adsorptive stripping voltammetry.

A simple, rapid, reliable and fully validated square wave cathodic adsorptive stripping voltammetric procedure has been developed for the determination of the antibiotic pefloxacin drug in bulk form, tablets and human serum, based on its electrochemical reduction at a hanging mercury drop electrode. The Britton-Robinson buffer of pH 7.0 was found to be reasonable as a supporting electrolyte for assay of the drug. Pefloxacin drug, at the optimized conditions, showed a single 2-electron well-defined peak at -1.07 V (versus Ag/AgCl/KCl(s)) using an accumulation potential of -0.40 V. This peak may be attributed to the reduction of the C=O group. A mean recovery of 99.54%+/-0.23 and a detection limit of 1.65 x 10(-10) M pefloxacin were achieved. After being validated, the proposed procedure was successfully applied for the determination of the drug in tablets and human serum with mean recoveries of 99.57+/-0.48 and 98.55+/-0.78%, respectively. A detection limit of 4.50 x 10(-10) M was achieved for the determination of the drug in human serum. Results of the proposed procedure were comparable with those obtained by reported methods.

4-Quinolones↗
PubMed1998

Trace iron determination in aminoisophthalic acid using differential-pulse cathodic stripping voltammetry at carbon paste electrodes.

Application of differential-pulse cathodic stripping voltammetry using a carbon paste electrode (consisting of carbon powder and liquid paraffin) have been investigated for trace determination of iron in 5-aminoisophthalic acid (AIPA). Samples were dissolved in 1 M HC1, pH was adjusted to 4-5 after addition of EDTA. Voltammetric measurements were performed after filtration. No sample decomposition (mineralization) was necessary. The method showed a good linearity between current and concentration from 3 x 10(-7) to 5 x 10(-5) mol dm-3 of iron, with a detection limit of 3 x 10(-7) mol dm-3 (resp. 1 ppm in solid AIPA). The results agreed well to those obtained by atomic absorption spectrometry (AAS) using electrothermic atomisation. For AAS measurement, however, microwave digestion of samples was necessary.

Carbon↗
PubMed1998

Chromium determination in osteoblast-like cell culture medium by catalytic cathodic stripping voltammetry with a mercury microelectrode.

A catalytic cathodic stripping voltammetric procedure for the determination of total chromium in osteoblast-like cell culture medium using a mercury film microelectrode (MFM) was optimised. The method is based on the pre-concentration of the Cr(III)-diethylenetriaminepentaacetic acid (DTPA) complex by adsorption at the potential of-1.00 V (vs. Ag/AgC1) in the presence of 10 x 10(-3) mol/L DTPA, 0.70 mol/L sodium nitrate, 0.04 mol/L sodium acetate and 1.0 x 10(-3) mol/L potassium permanganate at pH 5.9-6.0. The limit of detection obtained for a 40 s collection time was 2.80 x 10(-10) mol/L of chromium. The results achieved by stripping voltammetry using the MFM were compared to those obtained by atomic absorption spectrometry (AAS) to ensure the reliability of the electrochemical method. This procedure proved to be an alternative to AAS and valuable in biocompatibility studies performed in vitro using osteoblast-like cells.

Acetates↗
PubMed2002

Electroreduction of O(2) to water at 0.6 V (SHE) at pH 7 on the "wired" Pleurotus ostreatus laccase cathode.

O(2) was electroreduced to water at 0.6 V (SHE) near neutral pH on the "wired" Pleurotus ostreatus laccase cathode. We previously reported high-current density (5 mA cm(-2)), four-electron electroreduction of O(2) to water on a "wired" Coriolus hirsutus laccase electrode at +0.7 V (SHE) in pH 5 in citrate buffer. Since the enzyme was inhibited by chloride and because its activity declined steeply when the pH was raised to neutral, the rate of O(2) electroreduction in a physiological buffer solution was only approximately 1% of that at pH 5 in absence of chloride. Here we show that substitution of the C. hirsutus laccase by laccase from P. ostreatus allows the upward extension of the pH range of O(2) electroreduction. The current density of the electrode made with laccase from P. ostreatus in pH 7 citrate buffer was approximately 100 microA cm(-2) and at pH 7 and in phosphate buffered NaCl (PBS, 20 mM phosphate, 0.1 M NaCl) it still retained 6% of its maximal (1 mA cm(-2)) current density at pH 5 in citrate buffer. The electrocatalyst consisted of the crosslinked P. ostreatus laccase and the electron conducting redox polymer PVI-Os(dmebpy)(tpy)(2+/3+) [PVI=poly(N-vinyl imidazole) with about 1/5th of the rings complexed with (Os-dmebpy-tpy)(2+/3+); dmebpy=4,4'-dimethyl-2,2'-bipyridine; tpy=2,2',6',2"-terpyridine].

Bioelectric Energy Sources↗
PubMed2000

Ultrasonically enhanced leaching: removal and destruction of cyanide and other ions from used carbon cathodes.

The used carbon cathodes ('Spent Pot Lining', SPL) from aluminium smelting are typically contaminated with F-, CN- and Na+ which must be removed before disposal to produce material which satisfies environmental guidelines in respect of maximum rates of ion release. Leaching of powdered and crushed carbon samples in aqueous solution were studied in the presence and absence of ultrasound. First, it was demonstrated that the total leaching of F-, CN- and Na+ from the carbon powder could be accomplished after approximately 20 min of sonication using ultrasound. Second, carbon particles (< 5 mm) showed leaching characteristics under ultrasound which were in good quantitative agreement with the National River Authority (NRA) test under silent conditions; the former being a much more rapid (approximately 1 h compared to 24 h for the NRA test) but equivalent method to the latter standard test. Third, the removed CN- ions were found to be destroyed in the presence of ultrasound, possibly via the oxidative action of hydrogen peroxide generated by the sonication of water.

Journal Article↗
PubMed1991

Determination of trace iodine in food and biological samples by cathodic stripping voltammetry.

This paper describes a sensitive and selective method for the determination of iodine in food and biological samples. The method involves treatment of samples by combustion in an oxygen flask and determination of iodide by cathodic stripping voltammetry of the solid phase formed with the quaternary ammonium salt Zephiramine as the ionic associating agent; Br- is used as the complexing agent in the preconcentration process. We have studied the effect of concentration of Zephiramine, Br-, I-, and some other elements presented, deposition potential, preelectrolysis time, and scan rate, on the stripping curve shape and maximum stripping current. Determinations of trace iodine in table salt, laver, and eggs were demonstrated as practical examples.

Eggs↗
PubMed2001

Determination of picomolar levels of iron in seawater using catalytic cathodic stripping voltammetry.

A new procedure for the direct determination of picomolar levels of iron in seawater is presented. Cathodic stripping voltammetry (CSV) is preceded by adsorptive accumulation of the iron(III)-2,3-dihydroxynaphthalene (DHN) complex from seawater, containing 20 microM DHN at pH 8.0, onto a static mercury drop electrode, followed by reduction of the adsorbed species. The reduction current is catalytically enhanced by the presence of 20 mM bromate. Optimized conditions include a 60-s adsorption period at -0.1 V and a voltammetric scan using sampled dc modulation at 10 Hz. In these conditions, a detection limit of 13 pM iron in seawater was achieved which can be lowered further by extending the adsorption time to 300 s. The new catalytic CSV method is approximately 5 times more sensitive than existing CSV methods and was tested on samples from the Atlantic Ocean.

Journal Article↗
PubMed2006

Chemical speciation of iron in seawater by cathodic stripping voltammetry with dihydroxynaphthalene.

The chemical speciation of iron in seawater is determined by cathodic stripping voltammetry using 2,3-dihydroxynaphthalene (DHN) as adsorptive and competing ligand. The optimized conditions include a DHN concentration of 0.5-1 microM, seawater at its original pH of 8, and equilibration overnight. The alpha-coefficient for DHN (=[FeDHN]/[Fe']) was calibrated against EDTA giving values of 166 for 0.5 microM DHN and 366 at 1 microM DHN and a value of 8.51 +/- 0.07 for log K'(Fe'DHN). The dissociation of the natural iron species FeL was found to have a characteristic reaction time of 50 min, indicating that titrations should be equilibrated overnight rather than the shorter periods sometimes used onboard ship. The method was applied to samples from the Pacific giving ligand concentrations of 1.1 and 1.6 nM for deep and surface waters, respectively, with an average value for log K'(FeL) of 11.9 +/- 0.3 compared to a value of 11.5 for the siderophore deferoxamine. The results are similar to those obtained previously for similar samples, but the new method has much greater sensitivity for iron than previous methods, leading to lower limits of detection and shorter analysis time.

Journal Article↗
PubMed2006

Cathodic detection of H2O2 using iodide-modified gold electrode in alkaline media.

Oxidative chemisorption and cathodic stripping reductive desorption of iodide have been studied at a smooth polycrystalline gold (Au (poly)) electrode. Potential-dependent surface coverage of iodide has been controlled on the basis of its reductive desoprtion in 0.1 M KOH alkaline media and its quantitative oxidation to aqueous iodates in acidic media. The Au (poly) electrode surface catalyzes the decomposition of H2O2 to O2. Specific adsorption of iodide on the Au electrode inhibits fully the catalytic decomposition and electrochemical oxidation of H2O2 as well as the adsorption of unknown impurities and the oxidative degradation of the electrode surface by H2O2. A quantitative characterization/detection of H2O2 at the iodide-modified Au (poly) electrode in the alkaline media has, thus, been achieved. Performance of the electrode toward the detection of H2O2 with respect to response time and sensitivity as well as operational stability has been evaluated. It has a sensitivity of 0.272 mA cm(-2) mM(-1) in amperometric measurements with a detection limit of 1.0 x 10(-5) M H2O2, and the response time to achieve 95% of the steady-state current is <20 s. The effect of O2 in the air-saturated solution can be minimized by subtracting the additional current for the O2 reduction. Experimental measurements were based upon cyclic voltametric and amperometric techniques.

Journal Article↗
PubMed2000

Field-emission cold-cathode el source for a microscale ion trap mass spectrometer

A cold-cathode electron impact ionization source based on field emission from an array of diamond-coated silicon whiskers is described. The source is coupled to a microscale ion trap mass spectrometer (r0 = 0.50 mm, z0 = 0.50 mm). An electron beam of 250 nA could be obtained through the 0.45-mm diameter opening in the end cap electrode.

Journal Article↗
PubMed2001

A kinetic study of nickel complexation in model systems by adsorptive cathodic stripping voltammetry.

Adsorptive cathodic stripping voltammetry (AdCSV) in conjunction with the competing ligand-exchange method (CLEM) was investigated as a tool for measuring dissociation rate coefficients of nickel complexes in model systems. Dimethylglyoxime (DMG) was used as the competing ligand. Citric acid (CA) and a well-characterized fulvic acid (FA) were used as model ligands. The rate coefficients were calculated, and the consistency of equilibrium and kinetic data was discussed. The contributions of the disjunctive pathway (proceeding by the dissociation of the initial complex) and the adjunctive pathway (proceeding by the formation of an intermediate complex as a result of direct attack of the competing ligand on the initial complex) on the overall reactions were investigated. The reactions of Ni-CA or Ni-FA complexes with DMG were demonstrated to proceed by both disjunctive and adjunctive pathways. The predominant pathway for the overall reaction depends on the nickel-to-initial ligand and the DMG-to-initial ligand ratios. The reactions follow predominantly the disjunctive pathway for [DMG] > or = 3 mM and Ni-to-dissolved organic carbon (DOC) ratios greater than 10 nM Ni 2+/g of DOC. Since free nickel ion in freshwaters is reported to be toxic, its rate and pathway of formation are of environmental concern.

Benzopyrans↗
PubMed2002

Recycling of scrap cathode ray tubes.

It is estimated that approximately 50% of the weight of a computer monitor is composed of cathode ray tube (CRT) glass. Thus, the successful recycling of scrap CRT glass can greatly relieve the disposal problem created by scrap monitors. CRT glass may be considered a hazardous waste due to its high lead concentration. A CRT can be divided into panel (front) glass and funnel (back) glass. Several coatings have been applied to the surface of the CRT panel and funnel glass. These coatings may present an adverse effectto the environment by obstructing the recycling and reuse of the CRT glass. To recycle CRT glass, a series of tests has been conducted to remove the coatings from scrap CRT glass. In this study, the CRT panel and funnel glass obtained from scrap computer monitors was cleaned by wet-scrubbing and ultrasonic cleaning methods. This cleaned CRT glass is intended to be recycled and reused by CRT manufacturers. This study shows that the wet-scrubbing method has a better coating removal performance and no associated pollution problem (i.e., no additional chemical additives). Thus, the wet-scrubbing method is recommended for use as a CRT coating removal method. The results of these tests are presented in this paper.

Beta Particles↗
PubMed2003

Leaching of lead from computer printed wire boards and cathode ray tubes by municipal solid waste landfill leachates.

The proper management of discarded electronic devices (E-waste) is an important issue for solid waste professionals because of the magnitude of the waste stream and because these devices often contain a variety of toxic metals (e.g., lead). While recycling of E-waste is developing, much of this waste stream is disposed in landfills. Leaching tests are frequently used to characterize the potential of a solid waste to leach when disposed in a landfill. In the United States, the Toxicity Characteristic Leaching Procedure (TCLP) is used to determine whether a solid waste is a hazardous waste by the toxicity characteristic. The TCLP is designed to simulate worse-case leaching in a landfill environment where the waste is co-disposed with municipal solid waste (MSW). While the TCLP is a required analysis from a regulatory perspective, the leachate concentrations measured may not accurately reflect the concentrations observed under typical landfill conditions. Another method that can be performed to assess the degree a pollutant might leach from a waste in a landfill is to use actual landfill leachate as the leaching solution. In this study, two lead-containing components found in electronic devices (printed wire boards from computers and cathode ray tubes from computers and televisions) were leached using the TCLP and leachates from 11 Florida landfills. California's Waste Extraction Test (WET) and the Synthetic Precipitation Leaching Procedure were also performed. The results indicated that the extractions using MSW landfill leachates resulted in lower lead concentrations than those by the TCLP. The pH of the leaching solution and the ability of the organic acids in the TCLP and WET to complex with the lead are factors that regulate the amount of lead leached.

Electronics↗
PubMed1999

Design of Ligands That Stabilize Cu(I) and Shift the Reduction Potential of the Cu(II/I) Couple Cathodically in Aqueous Solutions.

The ligands R(2)NCH(2)CH(2)N(R)CH(2)CH(2)N(R)CH(2)CH=CH(2), where R = H, CH(3), were synthesized. The stability constants of their complexes with Cu(II) and Cu(I) in aqueous solutions were determined. Both ligands stabilize Cu(I) in aqueous solutions, though the reduction potentials of both (CuL(i)())(2+/+) couples are shifted cathodically in comparison to the Cu(2+/+)(aq) couple. These properties indicate that these complexes should be good catalysts for a variety of processes that are catalyzed by Cu(I).

Journal Article↗
PubMed2004

High-efficiency, environment-friendly electroluminescent polymers with stable high work function metal as a cathode: green- and yellow-emitting conjugated polyfluorene polyelectrolytes and their neutral precursors.

A series of aminoalkyl-substituted polyfluorene copolymers with benzothiadiazole (BTDZ) of different content were synthesized by Suzuki coupling reaction, and their quaternized ammonium polyelectrolyte derivatives were obtained through a postpolymerization treatment on the terminal amino groups. Copolymers are soluble in environmentally friendlier solvents, such as alcohols. It was found that the efficient energy transfer occurs by exciton trapping on the narrow band gap BTDZ site under UV illumination. Only 1% of BTDZ content is needed to completely quench a fluorene emission for both the neutral and the quaternized copolymers in the neat film. Absolute PL efficiencies of copolymer films were greatly enhanced as a result of the suppression of excimer formation. Light-emitting devices fabricated from these copolymers show high external quantum efficiencies over 3% and 1% for the neutral precursor and the quaternized copolymers, respectively, with high work function metals such as Al as a cathode. To the best of our knowledge, this is the first report on an electroluminescent polymer which bears the high EL efficiency, the electron-injection ability from high work function metals, and the solubility in environment-friendly solvents at the same time. These features make them a promising candidate for the next generation of light-emitting copolymers in PLED flat panel display application.

Journal Article↗
PubMed2006

Demonstrating oxygen loss and associated structural reorganization in the lithium battery cathode Li[Ni0.2Li0.2Mn0.6]O2.

The cathode in rechargeable lithium-ion batteries operates by conventional intercalation; Li+ is extracted from LiCoO2 on charging accompanied by oxidation of Co3+ to Co4+; the process is reversed on discharge. In contrast, Li+ may be extracted from Mn4+-based solids, e.g., Li2MnO3, without oxidation of Mn4+. A mechanism involving simultaneous Li and O removal is often proposed. Here, we demonstrate directly, by in situ differential electrochemical mass spectrometry (DEMS), that O2 is evolved from such Mn4+ -containing compounds, Li[Ni(0.2)Li(0.2)Mn(0.6)]O2, on charging and using powder neutron diffraction show that O loss from the surface is accompanied by diffusion of transition metal ions from surface to bulk where they occupy vacancies created by Li removal. The composition of the compound moves toward MO(2). Understanding such unconventional Li extraction is important because Li-Mn-Ni-O compounds, irrespective of whether they contain Co, can, after O loss, store 200 mAhg(-1) of charge compared with 140 mAhg(-1) for LiCoO(2).

Journal Article↗
PubMed2003

Determination of selenium in nuts by cathodic stripping potentiometry (CSP).

The aim of this work was to determine the selenium content in nut samples by cathodic stripping potentiometry. Dry-powdered nuts were digested by HNO(3) and dissolved with concentrated hydrochloric acid. To avoid the interference of natural oxygen, the potentiometric determination of selenium was carried out in an electrolyte solution consisting of 2 M CaCl(2) and 4 M HCl. The analysis was executed applying an electrolysis potential of -150 mV for 60 s and a constant current of -30 microA. Under these conditions, detection limits lower than 1.0 ng g(-)(1) were obtained for selenium analysis in nuts. The relative standard deviation of these measurements (expressed as rsd %) ranged from 0.44 to 0.88% while recoveries ranged from 90.2 to 95.3%. The results obtained with the proposed method were compared with those obtained via hydride vapor generation atomic absorption spectroscopy, a common method for determining selenium. The results of the two methods agreed within 5% for almond, hazelnut, and pistachio samples. The mean concentrations of selenium determined in Sicilian samples of almond, hazelnut, and pistachio were 531 +/- 1, 865 +/- 1, and 893 +/- 4 microg/kg, respectively.

Corylus↗
PubMed2003

Determination of selenium content in different types of seed oils by cathodic stripping potentiometry (CSP).

Seed oils are consumed worldwide; moreover, they are used in the alimentary, cosmetic, pharmaceutical, and chemical industries. Due to their diffusion, it is interesting to investigate the presence of important micronutrients such as selenium in seed oils. The aim of this work was to develop a rapid, precise, and sensitive cathodic stripping potentiometry (CSP) method to determine the concentration of selenium in different types of seed oils. Selenium was extracted from the oily matrix by concentrated hydrochloric acid treatment at 90 degrees C. The analysis was executed by applying an electrolysis potential of -150 mV for 60 s and a constant current of -30 microA. Under these conditions, detection limits of <0.5 ng g(-1) were obtained. The method reproducibility (expressed as total RSD %) spanned from 0.2 to 0.8%. Recoveries ranged from 92.1 to 97.5%, providing evidence that selenium quantification remained unaffected by the extraction procedure described. The results obtained with the proposed method were compared with those obtained via graphite furnace atomic absorption spectroscopy (GFAAS), a common method for determining selenium. The results of the two methods agreed within 93.5-107.7%. The mean amounts of selenium found were 313.0 +/- 2.0, 458.3 +/- 1.3, 224.6 +/- 0.9, 99.5 +/- 0.8, 332.2 +/- 0.5, 144.0 +/- 0.7, and 295.5 +/- 1.2 ng g(-1), respectively, in peanut, soybean, sunflower, rice, corn, grapestone, and seed oils.

Plant Oils↗