The solid state structure of triphenyltelluronium cyanate-chloroform( )

Three-dimensional X-ray crystal structure analysis shows that the organotelluronium salt, triphenyltelluronium cyanate-chloroform( ), exists as a tetramer in the solid state with both end-to-end and terminally bridging NCO groups. The oligomer is predominantly ionic with tellurium—nitrogen and tellurium—oxygen distances significantly shorter than respective van der Waals distances. Refinement of the structure, based on 3817 reflections collected by automatic diffractometry, converged to a conventional R factor of 4.9% and a weighted R factor of 4.2%. Crystal data for Ph₃Te(NCO) · CHCl₃ are as follows: a = 12.083(6)Å, b = 12.900(12)Å, c = 13.878(10)Å, α = 95.83(7)°, β = 103.47(7)°γ = 98.87(6)°, V = 1901ų (temperature = 23°C) and Z = 4.     

Asymmetric synthesis of quaternary alpha-amino phosphonates using sulfinimines

The addition of lithium diethylphosphonate to enantiopure ketosulfinimines is highly diastereoselective (>95%), affording the first examples of quaternary alpha-alkyl alpha-amino (arylmethyl)phosphonates.     

Thermal decomposition,kinetic study and evolved gas analysis of 1,3,5-triazine-2,4,6-triamine

The thermo-physical properties for four rock types (granite, granodiorite, gabbro, and garnet amphibolite) from room temperature to 1,173 K were investigated. Thermal diffusivity and specific heat capacity were measured using the laser-flash technique and heat flux differential scanning calorimetry, respectively. Combined with the density data, rock thermal conductivities were calculated. Rock thermal diffusivity and conductivity decrease as the temperature increases and approach a constant value at high temperatures. At room temperature, the measured thermal conductivity is consistently near or lower than the calculated conductivity using the mineral series model, which suggests that real thermal conduction is more complicated than is depicted in the model. Therefore, in situ measurement remains the best method for accurately obtaining thermal conductivity for rocks.     

Thermal degradation of B-group vitamins: B1, B2 and B6

The thermal behaviour of vitamins B₁, B₂ and B₆ under non-isothermal conditions and dynamic air atmosphere was studied. According to our study, it was determined that the most stable compound is vitamin B₂. A kinetic analysis of the thermodegradation process using four different data processing methods (Friedman, Flynn–Wall–Ozawa, Kissinger–Akahira–Sunose and modified NPK) was performed. The NPK was the only method that made it possible to evaluate the contribution to the reaction rate of the temperature and conversion, respectively. The results obtained from kinetic analysis were corroborated with the molecular architecture of the studied compounds.     

Pre-concentration of trace elements in short chain alcohols using different commercial cation exchange resins prior to inductively coupled plasma-optical emission spectrometric detection

Chelex-100, Dowex 50W-x8 and Dowex MAC-3 exchange resins were investigated for separation and pre-concentration of trace amounts of Cd, Cr, Cu, Fe, Mn, Pb, Ti and Zn in alcohols with respect to retention and desorption characteristics. Dowex 50W-x8 was found to be the best sorbent with percentages recoveries >95%. In addition, Chelex-100 appeared to be suitable for the pre-concentration of Cu, Fe and Zn, whereas Dowex MAC-3 was selective for Cu and Fe. Therefore, Dowex 50W-x8 was used for further investigations. The relative standard deviations <4% (n = 20), limits of detection and quantification were 0.1–1.2 μg L⁻¹ and 0.3–1.5 μg L⁻¹, respectively. The SPE method was validated against a certified reference material and the results were in agreement with certified values. The accuracy of the optimized method was verified by the recovery test in the spiked alcohol samples. The accuracy and spike recovery test for different metal ions were in the range 98–102% and 95–105%, respectively. The optimized method was applied to the separation and pre-concentration of metal ions in different commercial alcohol samples.     

Association patterns in (HF)(m)(H2O)(n) (m + n = 2-8) clusters

In an attempt to understand the phase behavior of aqueous hydrogen fluoride, the clustering in the mixture is investigated at the molecular level. The study is performed at the mPW1B95/6-31+G(d,p) level of theory. Several previous studies attempted to describe the dissociation of HF in water, but in this investigation, the focus is only on the association patterns that are present in this binary mixture. A total of 214 optimized geometries of (HF)n(H2O)m clusters, with m + n as high as 8, were investigated. For each cluster combination, several different conformations are investigated, and the preferred conformations are presented. Using multiple linear regressions, the average strengths of the four possible H-bonding interactions are obtained. The strongest H-bond interaction is reported to be the H2O...H-F interaction. The most probable distributions of mixed clusters as a function of composition are also deduced. It is found that the larger (HF)n(H2O)m clusters are favored both energetically and entropically compared to the ones that are of size m + n < or = 3. Also, the clusters with equimolar contributions of HF and H2O are found to have the strongest interactions.