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Critical statements have appeared recently in the literature concerning the need for classical dry ashing in trace element analysis of biological materials. In contrast, respected institutions (AOAC, Nordic Committee on Food Analysis, etc.) as well as numerous other laboratories have developed, verified, and/or successfully used classical dry ashing in practical analyses of a number of materials...
Batch-injection analysis exhibits the advantages of rapid and simple electroanalysis of microlitre samples. Nafion-coated mercury thin film electrodes have been evaluated for use in batch-injection analysis with anodic stripping voltammetry (BIA-ASV). The advantages of Nafion-coated electrodes in reducing electrode contamination by components of complex matrices are combined with the analysis of...
The designs and applications of non-flow microcells in voltammetry and stripping voltammetry for samples with volumes from sub-microliters to 5 ml are reviewed. The analysis of microcell designs was carried out on the basis of their classification: (i) microcells with a static sample, including thin-layer microcells with a static sample; (ii) microcells with forced convection of the sample; and...
Reactive Violet 5 and its hydrolysis product, which is produced as a side product in the dyeing process, can be determined in an admixture at sub-ppb levels by cathodic stripping voltammetry because the potentials of their azo reduction peaks are separated sufficiently. For both dyes, at intermediate pH values the azo peak is preceded by a complexed -copper reduction peak at a less negative potential,...
Cathodic stripping voltammetry was used to determine 5-fluorouracil (5-FU) in the presence of traces of Cu(II). It was found that the addition of 5 10 -9 mol dm -3 Cu(II) to the measurement cell greatly enhanced the peak current of the adsorbed molecule. Different parameters were tested to optimize the conditions for the determination of 5-FU. The adsorbed form is reduced...
The electroanalytical behaviour of the herbicide Nitralin has been studied by means of different voltammetric techniques. Nitralin is adsorbed on the mercury electrode and gives 2 reduction waves at -0.6 and -0.7 V versus Ag/AgCl reference electrode, for pH values > 10. The electrochemical process is irreversible and strongly influenced by pH solution. A systematic study of the several instrumental...
With the aim of carrying out a calibration transfer for routine analysis, partial least squares (PLS) regression was successfully applied to simultaneously determine thallium and lead by stripping voltammetry when an interfering background current is present. The presence of a significant blank signal that overlaps the thallium peak, together with the overlapping thallium and lead signals were both...
Two different standardization procedures have been applied in order to minimize the experimental effort necessary to determine copper in presence of iron by differential pulse anodic stripping voltammetry. The significant matrix interference caused by iron in the voltammetric determination of copper has been successfully solved by using partial least squares (PLS) regression. The use of this multivariate...
A Tosflex-mercury film electrode (TMFE) was prepared by spin-coating a solution of the perfluorinated anion exchange polymer Tosflex onto a glassy carbon electrode surface followed by electrodeposition of mercury film on this electrode. This electrode was used for the determination of trace bismuth(III) which was preconcentrated onto the TMFE as anionic bismuth(III) complexes with chloride in a chloride...
A method for the simultaneous voltammetric determination of free sulfide and volatile alkythiols (methanethiol/ethanethiol) existing as contaminant in parenteral nutrition (PN) solutions was developed. The volatile sulfides (dihydrogensulfide and alkylthiols) formed in the formulations were distilled over 45 min at 47 o C in a purpose-made Conway cell. The analytes were quantified by differential...
A study into the sonoelectroanalysis of silver at a highly boron-doped diamond electrode is presented, exploring the benefits of the introduction of power ultrasound and new electrode materials into classical electrochemical techniques. Both cathodic and anodic stripping voltammetry have been investigated in terms of their analytical suitability towards silver detection. Cathodic stripping voltammetry,...
An electrochemical stripping procedure for ultra-trace measurements of adenine is described based on the adsorption of the adenine-copper complex on a static mercury drop electrode. Cyclic voltammetry was used to characterize the interfacial and redox behavior. Optimum experimental conditions were found when using a 0.005 M NaOH solution containing 0.4 ppm of copper, an accumulation potential of -0...
The electrochemical response of metal ions in different samples of coloured ceramic tin-lead glazes attached to graphite/polyester composite electrodes is described. In addition to the ubiquous signals for lead, reductive dissolution processes are followed by anodic stripping peaks for Co, Cu, Sb, Mn, Sn and Fe, enabling the direct identification of such elements in microsamples proceeding from archaeological...
The adsorption behavior of levofloxacin on a glassy carbon electrode was explored by cyclic and square-wave voltammetry. The drug was accumulated on a glassy carbon electrode and a well-defined oxidation peak was obtained in acetate buffer pH 5.0. Using square-wave anodic stripping voltammetry and accumulation at +0.4 V versus Ag/AgCl (saturated KCl) for 300 s, linear calibration graph was obtained...
The cathodic adsorptive electrochemical behavior of guanine in the presence of some metal ions at the static mercury drop electrode was investigated. A 1.0x10 -3 mol l -1 NaOH or a 2.0x10 -2 mol l -1 Hepes buffer at pH 8.0 solutions were used as supporting electrolytes. The reduction peak potential for guanine was found to be around -0.15 V, which...
The voltammetric behaviour of Sildenafil citrate (SC) and its main metabolite UK-103,320 (UK) was studied by square wave techniques, leading to two methods for its total determination in biological samples (urine and human serum). The application of the square wave (SW), without the adsorptive accumulation, shows a maximum response at -0.950V. The effect of experimental parameters that affect this...
A highly selective and sensitive anodic stripping differential pulse polarographic method has been developed for the determination of trace amount of bismuth in various samples after adsorption of its 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex on amberlite XAD-2 resin in the pH range of 2.0-3.0. The retained analyte on the resin recovered with 10.0ml of 2M hydrochloric acid and bismuth...
A procedure for the determination of chromium is described based on synergistic pre-concentration of the chromate anion at a carbon paste electrode modified in situ with quarternary ammonium salts such as 1-ethoxycarbonylpentadecyltrimethylammonium bromide (Septonex ( R)), cetyltrimethylammonium bromide (CTAB) or cetylpyridinium bromide (CPB). The proper electrochemical detection utilises...
Multicriteria optimization, widely used in engineering, does not much used in the optimization of analytical signals. The aim of this paper is to show the usefulness of the desirability function to optimize instrumental responses obtained in instrumental analysis. The simultaneous optimization of a signal and of its variability is a generic question of interest to any chemical analyst. It is clear...
A reliable and very sensitive procedure for the determination of ultra trace of molybdenum is proposed. Molybdenum was determined by cathodic stripping differential pulse voltammetry based on the adsorption collection of the Mo(VI)–Tiron complex on a hanging mercury drop electrode (HMDE). The variation of peak current with pH, concentration of Tiron and chlorate, plus several instrumental parameters...
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