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…

Atomic fluorescence determination of inorganic arsenic in soils after microwave-assisted distillation

Abstract An inexpensive microwave-assisted distillation procedure has been developed for quantitative determination of inorganic arsenic in soils by atomic fluorescence spectrometry (AFS). After reduction of As(V) to its trivalent state with potassium iodide, inorganic arsenic was distilled as AsCl 3 that was finally determined by atomic fluorescence after hydride generation with NaBH 4 in HCl medium. The different parameters that control the distillation: concentration and volume of HCl, time of distillation, sample weight, and oven load, were studied. The methodology developed has a detection limit of 0.015 μg l −1 , which corresponds to a concentration of 0.006 μg of As per gram of soil,…

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…

Spectrophotometric determination of carbaryl by on-line elution after its preconcentration onto polyurethane foam.

Abstract An analytical methodology has been developed for the UV-spectrophotometric determination of carbaryl in waters after its preconcentration onto a polyether type polyurethane foam followed by on-line elution. The aforementioned strategy offers an easy way for in-field sampling and to improve the analytical sensitivity. Several chemical and flow variables (mass of sorbent, sample flow rate, sample volume and carrier flow rate) were studied to ensure the best performance of the system. Recovery studies, carried out on natural water samples spiked with known amounts of carbaryl at concentration levels between 250 and 500 μg l−1, provided recovery percentages between 94 and 105%. A detec…

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…

Geographical variation of land mineral composition