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Identification of sulfur interferences during organotin determination in harbour sediment samples by sodium tetraethyl borate ethylation and gas chromatography-pulsed flame photometric detection.

Because of the high toxicity of organotin compounds and the current regulation about their applications, analytical method usable in routine analysis is required. A speciation procedure based on NaBEt4 ethylation and GC-PFPD analysis has shown to be suitable for the organotin determination. Unfortunately, some matrix effects were observed during the analysis of harbour sediments from Chile. These effects were identified as the alkylation of elemental sulfur and the coelution between the organotin compounds and some dialkylsulfides. The re-optimization of GC parameters and application of solid phase microextraction (SPME) were proposed to solve these analytical problems. Certified reference materials and different harbour sediment samples were analysed in order to evaluate the suitability of the methods for organotin control in complex environment samples.

Borates↗

Effect of TiO2 on electron paramagnetic resonance, optical transmission and dc conductivity of vanadyl doped sodium borate glasses.

Glass systems with composition xTiO2.(30 - x)Na2O.70B2O3 (series I) and xTiO2.(70 - x)B2O3.30Na2O (series II) containing 2 mol% V2O5 have been prepared (0 < or = x < or = 7, mol%) by normal melt-quenching. The electron paramagnetic resonance (EPR) spectra of VO2+ ions have been recorded in the X-band (approximately 9.13 GHz) at room temperature. Spin Hamiltonian parameters, gparallel, gperpendicular, Aparallel, Aperpendicular, the dipolar hyperfine coupling parameter (P) and the Fermi contact interaction parameter (K) have been calculated. The increase in Deltagparallel/Deltagperpendicular with increase in TiO2 content in series I shows that the octahedral symmetry of V4+O6 complex is reduced, whereas in series II the octahedral symmetry is improved with increase in x. The decrease in P, in both the series, indicates that the 3dxy orbit expands with increase in mol% of TiO2. The molecular orbital coefficients, alpha2 and gamma2 have been calculated by recording the optical transmission spectra in the range 500-850 nm. alpha2 and gamma2 increase with increase in x in both the series, which indicates that, the covalency of the vanadium oxygen bonds decreases. The dc conductivity sigma, decreases and activation energy, W increases with increase in TiO2:Na2O ratio whereas with increase in TiO2:B2O3 ratio the variation in sigma and W is within experimental error.

Borates↗

The effect of modifiers on the fluorescence and life-time of Gd3+ ions doped in borate glasses.

The effect of glass modifiers on the fluorescence and life time of the 6P(7/2) energy state of the Gd3+ ion has been investigated. A shift in the energy of maximum of the fluorescence has been observed. The results are explained on the basis of the relative cation and anion field strengths due to modifiers. A variation in the life-time of the 6P7.2 energy state of the Gd3 ion has also been noted.

Borates↗