Lead migration from toys by anodic stripping voltammetry using a bismuth film electrode.

Metals may be released from toys via saliva during mouthing, via sweat during dermal contact, or via gastric and intestinal fluids after partial or whole ingestion. In this study, we determined the lead migration from toys bought on the Portuguese market for children below 3 years of age. The lead migration was performed according to the European Committee for Standardization EN 71-3, which proposes a 2-hour migration test that simulates human gastric conditions. The voltammetric determination of migrated lead was performed by anodic stripping voltammetry (ASV) at a bismuth film electrode (BiFE). For all the analyzed toys, the values of migrated lead did not exceed the limits imposed by the European Committee for Standardization EN 71-3 (90 mg kg-1) and by the EU Directive 2009/48/EC (13.5 mg kg-1) on the safety of toys.

Ofloxacin determination in urine, serum and pharmaceuticals using an automatic flow potentiometric system.

An automatic system was developed to determine ofloxacin in biological fluids and pharmaceutical formulations. Drug detection was carried out by a potentiometric membrane sensor based on [bis(trifluoromethyl)phenyl]borate as molecular-recognition material. The tubular shaped detector system was solidly attached to the manifold, creating a high-throughput stable setup (50 samples per hour) appropriate for routine antibiotic assessment. Under the optimized flow conditions, the sensor displayed a mean detection limit of 1 × 10(-5) M, a linear response over the concentrations of 2 × 10(-5) to 5 × 10(-3) M (slope of 57.4 mV decade(-1)) and a wide working pH range (2.1 - 6.6). The procedure was successfully applied to ofloxacin analysis in pharmaceuticals (relative deviation lower than 6%) and biological fluids at levels usually found after drug administration of clinical doses (recoveries between 91 and 106%). No significant interference from common excipients found in commercial formulations and inorganic ions usually present in biological fluids was noticed.

Sequential injection kinetic flow assay for monitoring glycerol in a sugar fermentation process by Saccharomyces cerevisiae.

A sequential injection system to monitor glycerol in a Saccharomyces cerevisiae fermentation process was developed. The method relies on the rate of formation of nicotinamide adenine dinucleotide in its reduced form (NADH, measured spectrophotometrically at 340 nm) from the reaction of glycerol with NAD(+) cofactor, catalysed by the enzyme glycerol dehydrogenase present in solution. This procedure enables the determination of glycerol between 0.046 and 0.46 g/l, (corresponding to yeast fermentation samples with concentrations up to 50 g/l) with good repeatability (relative standard deviation for n = 10 lower than 2.2% for three different samples) at a sampling frequency of 25/h. The detection and quantification limits using a miniaturised spectrophotometer were 0.13 and 0.44 mM, respectively. Reagent consumption was of 0.45 mumol NAD(+) and 1.8 microg enzyme per assay, and the waste production was 2.8 ml per determination. Results obtained for samples were in agreement with those obtained with a high-performance liquid chromatography method.

A double-line sequential injection system for the spectrophotometric determination of copper, iron, manganese, and zinc in waters.

A double-line sequential injection system was developed for the spectrophotometric determination of several metal ions in waters. The proposed double-line configuration was used to enable adding sample and chromogenic reagents as merging zones. The methodology was applied to the spectrophotometric determination of copper, iron, manganese, and zinc in samples of diverse origins at the range of 0.15-5.00, 0.10-10.0, 0.48-4.00, and 0.11-5.00 mg/L, respectively. Different chromogenic reagents and detection wavelengths were used. The chromogenic reagents for iron and manganese were 1,10-phenanthroline and formaldoxime, respectively. Copper and zinc were both determined using the analytical reagent zincon. Analytical characteristics of the methodology, such as manifold parameters, buffer pH, and reagent concentrations were optimized, and interference of some of the metal ions commonly present in water sample was assessed. Results of the analysis were in agreement with those obtained by atomic absorption spectrometry. Repeatability, expressed as the relative standard deviation for 10 consecutive injections of water samples, was lower than 6%. The determination rate was approximately 36/h.

Use of a single air segment to minimise dispersion and improve mixing in sequential injection: turbidimetric determination of sulphate in waters.

In this work, we propose the use of an air segment in a sequential injection system to simultaneously improve the overlapping of the stacked zones and minimise dispersion. This strategy was developed for the determination of sulphate in natural and wastewaters. Barium chloride was used as a precipitating agent and the turbidity of the suspension formed was measured at 420 nm. Analysis was performed without sample pre-treatment and the system was able to monitor sulphate concentration at a rate of at least 20 determinations per hour. Slightly different analytical sequences were developed for natural and wastewaters in order to minimise specific interferences. Direct determination of sulphate was possible within a concentration range of 10-100 and 16-100 mg SO(4)(2-) L(-1) for natural and wastewaters, respectively. Results obtained were comparable with those of the reference method with relative deviations lower than 5%. Relative standard deviations between 1.6% and 3.3% were found.