0000000000335892
AUTHOR
Ricardo J. Cassella
Flow injection-FTIR determination of dithiocarbamate pesticides
A flow injection Fourier transform infrared spectrometric procedure has been developed for the determination the dithiocarbamate pesticides Ziram and Thiram in solid samples. All the operations involved, such as extraction, filtration and measurement, were integrated in the experimental set-up in order to avoid excessive manipulation of samples and standards. Ultrasonic assisted and mechanical extraction were evaluated for the solubilization of the analytes and, additionally, the effect of carrier flow rate, sample loop volume and the ratio between sample mass and volume of solvent employed were studied. Quantitative extractions with chloroform were obtained for both Ziram and Thiram, after…
Novel approach for the determination of azithromycin in pharmaceutical formulations by Fourier transform infrared spectroscopy in film-through transmission mode
Abstract This work reports the development of a new method for the determination of azithromycin in pharmaceutical formulations employing Fourier transform infrared (FTIR) technique. The measurements were performed using a novel approach based on a film-through transmission mode. Several variables that could influence the analytical performance of the method were evaluated (solvent, nominal resolution, number of scans, mode of measurement and spectral region selected for measurement). Acetonitrile was the best solvent for the determination of azithromycin, employing the absorption band of the C O group at 1729 cm− 1. The extraction of azithromycin from the formulations was made by mechanica…
Retention of carbaryl by polyether type polyurethane foam: a critical study
This paper reports the retention of carbaryl by polyether type polyurethane foam in a dynamic mode. Several parameters that can influence the extraction of carbaryl from water samples were investigated such as concentration of carbaryl, mass of sorbent in the column, sample pH, saline concentration, solvent washing and sample flow rate. Results show that it is possible to achieve quantitative extractions when the sample flow rate is maintained up to 2.4 mL min−1, a mass of foam of 300 mg and a sample volume of 30 mL in 0.5 NaCl are employed. They also indicate that there is an ether-like solvent extraction mechanism controlling the sorption of the substance by the foam. Some recovery tests …
Determination of sulfide in waters by flow-injection solid phase spectrophotometry
A highly sensitive flow injection solid-phase spectrophotometric method was developed for the determination of sulfide in waters. The method is based on the formation of Methylene Blue (MB) by reaction between sulfide and N,N-dimethyl-p-phenylenediamine chloride in presence of Fe(III) in acidic medium. The MB formed was adsorbed on C18 bonded silica, located inside a laboratory-made flow cell, which was placed in the optical path of the spectrophotometer. Analyte retention and detection at 666 nm were performed simultaneously, followed by elution with a mixture of methanol and hydrochloric acid. Several variables of the system, such as amine concentration, acidity of the reaction medium, re…
Study of passive sampling of polycyclic aromatic hydrocarbons in gas phase using Amberlite XAD resins as filling materials of semipermeable membranes
Abstract In this work, a study was performed to evaluate the use of Amberlite XAD resins (XAD-2, XAD-4 and XAD-16), for the first time, as filling materials for low-density polyethylene membranes, which will be inserted as passive samplers for polycyclic aromatic hydrocarbons (PAHs) in gas phase. The use of samplers deployed for 48 h evidenced a relative capability to retain the compounds under study. A detailed study was performed to evaluate the recovery of analytes from the sampler through microwave-assisted extraction by using acetonitrile. A clean-up step using alumina-C18 cartridges was necessary before determination of the PAHs by high performance liquid chromatography with fluoresce…
Rapid on-line sample dissolution assisted by focused microwave radiation for silicate analysis employing flame atomic absorption spectrometry: iron determination.
An on-line automated flow injection system with microwave-assisted sample digestion was used to perform silicate rock dissolution in acid medium for iron determination. For this purpose, a continuous flow system was built up by using an automatic flow injection analysis (FIA) system coupled to a flame atomic absorption spectrometer (FAAS), including a focused microwave oven unit. Inside the microwave cavity was inserted a polytetrafluoroethylene (PTFE) reactor coil (300cm length and 0.8mm i.d.) where the dissolution takes place. Chemical and flow variables as well as iron determination parameters were studied. In the flow system, a slurry of the rock sample (50mg in 200ml of acid mixture HF…
Estuarine sediment quality assessment by Fourier-transform infrared spectroscopy
Partial least squares Fourier-transform infrared (PLS-FTIR) models were developed for the quality assessment of estuarine sediments through the evaluation of several physico-chemical parameters. Models were based on the chemometric treatment of attenuated total reflection (ATR) spectra directly obtained from samples previously lyophilized and sieved through a lower than 63 μm grid. Spectra were scanned from 3997 to 523 cm-1, averaging 36 scans per spectrum with a nominal resolution of 8 cm-1. Models were built using reference data obtained for sediment samples collected from Ria de Arousa estuary. Hierarchical cluster classification of sediment ATR spectra was employed for the establishment…