Magnetic Poly(Amidoamine) Dendrimer for the Dispersive Solid Phase Extraction of Nitrophenols from Environmental Water Samples.

A fast and simple dispersive solid phase extraction method is described for nitrophenols determination in water samples by using gas chromatography-nitrogen phosphorous detector. Firstly, the Poly(amidoamine) grafted Fe3O4 magnetic nanoparticles were synthesized in different generations by successive addition of butyl acrylate and ethylenediamine. After characterization, the prepared dendrimer was utilized as an adsorbent for magnetic solid phase extraction of 2-nitrophenol, 3-nitrophenol, and 4-nitrophenol to benefit large number of surface amine interaction sites. The effects of the different parameters influencing the sample preparation efficiency were investigated. The proposed method showed linearity in the ranges of 0.04-700 and 0.05-700 µg/dm3 for nitrophenols. The obtained limits of detection and quantification under optimized conditions were 0.01-0.02 and 0.04-0.05 µg/dm3, respectively. The relative standard deviations (n = 5) were less than 3.8% (at 10 µg/dm3). Moreover, the calculated enrichment factors were above 200. In addition, the relative recoveries for a spiked river water sample were satisfactory.

Adsorption and sequential thermal release of F2 , Cl2 , and Br2 molecules by a porous organic cage material (CC3-R): Molecular dynamics and grand-canonical Monte Carlo simulations.

The adsorption-desorption behavior of fluorine, chlorine, and bromine molecules onto a crystalline porous organic cage, namely CC3-R was calculated at different temperatures using molecular dynamics (MD) and grand-canonical Monte Carlo (GCMC) simulations. Self-diffusion coefficients, radial distribution functions (RDF), and adsorption isotherms were calculated for this purpose. The results show that CC3-R has varied capacities to capture these halogens at ambient and high temperatures, so that the thermal release of fluorine is completed with increasing temperature up to around 70°C and chlorine molecules remain at the CC3-R surface up to 100°C and all bromine molecules are removed from the CC3-R surface at 200°C. We found that bromine self-diffusion was almost independent of temperature between 0 and 100°C in contrast to fluorine and chlorine. Among different diffusion regimes, Knudsen diffusion appears to have an important role in the adsorption of heavy halogens at higher temperatures.

Polytetrafluoroethylene physisorption-assisted emulsification microextraction as a cleanup and preconcentration step in the gas chromatography determination of aliphatic hydrocarbons in marine sediment samples.

For the first time, the application of polytetrafluoroethylene powder as an extractant phase collector or holder in liquid-phase microextraction has been developed. For this purpose, the analytical performances of two different ways of applying polytetrafluoroethylene powder in microextraction methods including polytetrafluoroethylene physisorption-assisted emulsification microextraction and dispersive liquid-phase microextraction via polytetrafluoroethylene extractant phase holders have been compared for analysis of aliphatic hydrocarbons in aqueous phases. Under the same conditions, the former showed better extraction efficiencies over the latter and as a result, it was applied as preconcentration and cleanup step in the analysis of aliphatic hydrocarbons in sediment samples followed by gas chromatography analysis. The linearity of the polytetrafluoroethylene physisorption-assisted emulsification microextraction method was obtained over a range of 3.7 and 2000 ng/g (R2 > 0.993). The relative standard deviations were less than 6.5% (n = 3). The limits of detection and quantification obtained by this method were 1.1-9.0 and 3.7-30 ng/g, respectively, indicating that satisfactory results were achieved by the procedure.

Selective separation and determination of isoproterenol on thin layers of bismuth silicate ion-exchanger.

A simple and sensitive method for the separation and determination of isoproterenol from other doping drugs has been developed on thin layers of bismuth silicate, a synthetic inorganic ion exchanger as adsorbent in thin layer chromatography (TLC). A mixture of methanol and 0.1 mol/L formic acid (3:7, v/v) was employed as the mobile phase. The development time was 32 min. The quantitative measurement were performed with a Camag TLC Scanner-3 at wavelength (λ) of 410 nm. The isoproterenol recovery in this procedure was 98.9%. The linear correlation coefficient was greater than 0. 987 1 and the relative standard deviation (RSD) was less than 0.94. The limit of detection (LOD) and limit of quantification ( LOQ) were 7.7 x 10(-7) mol/L and 3.85 x 10(-6) mol/L, respectively. This method has been applied in the determination of isoproterenol in dosage forms and in biological fluids.

Dissolved carbon dioxide flotation: an effective way for phase separation in emulsification microextraction method.

Dissolved carbon dioxide flotation after emulsification microextraction (DCF-EME) technique coupled with gas chromatography-electron capture detection (GC-ECD) was introduced for preconcentration and determination of six organochlorine pesticides (OCPs) in seawater samples. DCF-EME method is based on the rapid and simple phase separation of low density organic solvent from the aqueous phase via introducing of a saturated NaHCO3 solution (9.6% w/v) into the acidified sample solution (0.1M of HCl) containing analytes. Thanks to the in situ generation of carbon dioxide (CO2) bobbles intensified by ultrasound radiation, the dispersed extraction solvent was collected to the surface of the aqueous sample and then was narrowed to the capillary part of a special home-made extraction cell for facile retrieving. Under the optimal conditions, the limits of detection were at the range of 2.6-9.2 ng L(-1) and preconcentration factors were varied between 271 and 307 for different OCPs. The applicability of the developed method was evaluated by the extraction and determination of the target analytes from Caspian seawater samples.

Chromatographic separation of inorganic ions on thin layers of titanium phosphate ion-exchanger.

The chromatographic behavior of 30 inorganic cations has been studied on thin layers of titanium phosphate ion-exchanger using several aqueous, organic and mixed mobile phases. The separation of one ion from several other ions and also ternary and binary separations have been developed. Some important analytical separations are reported. The effect of pH of the mobile phase on retention factor (Rf) values of the cations in the presence of complex-forming anion along with the separation power of the ion-exchanger were studied. This ion-exchanger exhibits high sorption capacity and varying selectivity towards metal ions and makes it a suitable stationaiy phase in thin layer chromatography.