RESUMO
The use of silicone for detection of aromatic hydrocarbons in water using near-infrared spectroscopy is proposed. A sensing phase of poly(dimethylsiloxane) (PDMS) was prepared, and a rod of this material was adapted to a transflectance probe for measurements from 850 to 1800 nm. Deionized water samples contaminated separately with known amounts of benzene, toluene, ethylbenzene, and m-xylene were used for evaluation of the PDMS sensing phase, and measurements were made in a closed reactor with constant stirring. Equilibrium states were obtained after 90, 180, 360, and 405 min for benzene, toluene, ethylbenzene, and m-xylene, respectively. The PDMS sensing phase showed a reversible response, presenting linear response ranges up to 360, 290, 100, and 80 mg L(-1), with detection limits of 8.0, 7.0, 2.6, and 3.0 mg L(-1) for benzene, toluene, ethylbenzene, and m-xylene, respectively. Reference spectra obtained with different rods showed a relative standard deviation of 0.5%, indicating repeatability in the sensing phase preparation. A relative standard deviation of 6.7% was obtained for measurements performed with six different rods, using a 52 mg L(-1) toluene aqueous solution. The sensing phase was evaluated for identification of sources of contamination of water in simulated studies, employing Brazilian gasoline type A (without ethanol), gasoline type C (with 25% of anhydrous ethanol), and diesel fuel. Principal component analysis was able to classify the water in distinct groups, contaminated by gasoline A, gasoline C, or diesel fuel.
RESUMO
This work describes an FIA potentiometric procedure for the quantification of dipyrone in pharmaceutical products. For the detector, a tubular electrode comprising a polymeric membrane containing tetraoctylammonium as an electroactive material (5% w/w), dibutylphtalate as a mediator solvent (65% w/w) and PVC (30% w/w) directly applied above a graphite conductor support was used. This unit was incorporated into a monochannel FI-system with a 0.1 mol/L phosphate buffer solution (pH = 5.2) as the carrier solution. The electrode showed a linear response from 8.0 x 10(-4) to 10(-1) mol/L dipyrone, a slope of 62.1 +/- 0.2 mV/dec in pH 5.2 units, an injection volume of 500 microL and a carrier flow-rate of 6 mL/min. This procedure was applied to the analysis of pharmaceutical formulations (oral and injectable) containing dipyrone; the obtained results gave a relative error of less than 3.9% and coefficients of variation less than 1% and 5%, respectively, for the FIA and classical iodometric methods.
