Solvent selection in ultrasonic-assisted emulsification microextraction: Comparison between high- and low-density solvents by means of novel type of extraction vessel

There are numerous published reports about dispersive liquid phase microextraction of the wide range of substances, however, till now no broadly accepted systematic and purpose oriented selection of extraction solvent has been proposed. Most works deal with the optimization of available solvents without adequate pre-consideration of properness. In this study, it is tried to compare the performances of low- and high-density solvents at the same conditions by means of novel type of extraction vessel with head and bottom conical shape. Extraction efficiencies of seven basic pharmaceutical compounds using eighteen common organic solvents were studied in this work. It was much easier to work with high-density solvents and they mostly showed better performances. This work shows that although exact predicting the performance of the solvents is multifaceted case but the pre-consideration of initial selection of solvents with attention to the physiochemical properties of the desired analytes is feasible and promising. Finally, the practicality of the method for extraction from urine and plasma samples was investigated.     

Isotope Zusammensetzung Der Mineralwässer Der Mongolei

Abstract

The isotopic composition (D, ¹⁸O, ⁸⁷Sr, ³He) of thermal and mineral waters of Mongolia is discussed. The Sr-isotope ratio depends on the rock's contact. Near the Chubsugul-lake ³He-/⁴He-values are high. A certain similarity between the waters of Mongolia and those of East Siberia can be derived from the obtained data.     

Deprotection‐free preparation of propargyl ether‐containing phosphinated benzoxazine and the structure–property relationship of the resulting thermosets

Generally, protection and deprotection procedures of amino groups are required in preparing propargyl ether‐containing benzoxazines. In this study, we report a facile, deprotection‐free preparation of a propargyl ether‐containing phosphinated benzoxazine (2) from the nucleophilic substitution of a phenolic OH‐containing phosphinated benzoxazine (1) and propargyl bromide in the catalysis of potassium carbonate. The structure of (2) was characterized and confirmed by a high‐resolution mass spectrum, ¹H, ¹³C, ¹H‐¹H, ¹H‐¹³C nuclear magnetic resonance (NMR) spectra, and X‐ray single crystal diffractogram. infrared (IR) and differential scanning calorimetry were used to monitor the ring‐opening of benzoxazine and crosslinking of propargyl ether. The microstructure and the structure–property relationship of the resulting homopolymers and copolymers are discussed. The T_g of homopolymer of (2) is 208 °C by dynamic mechanical analysis, the coefficient of thermal expansion is 43 ppm/°C, and T_d 5% (N₂) is 393 °C, respectively, which are higher than those of the homopolymer of (1) . Similar trends were observed in the copolymerization system. The results demonstrate the beneficial effect of crosslinking afforded by the propargyl ether group is higher than that by the phenolic OH group. © 2011 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012     

Modelling effects of subgrid-scale mixture fraction variance in LES of a piloted diffusion flame

A posteriori analysis of the statistics of two large-eddy simulation (LES) solutions describing a piloted methane–air (Sandia D) flame is performed on a series of grids with progressively increased resolution reaching about 10.5 million cells. Chemical compositions, density and temperature fields are modelled with a steady flamelet approach and parametrised by the mixture fraction. The difference between the LES solutions arises from a different numerical treatment of the subgrid scale (SGS) mixture fraction variance – an important quantity of interest in non-premixed combustion modelling. In the first case (model I), the variance transport equation is solved directly, while in the second (model II), an equation for the square of the mixture fraction is solved, and the variance is computed from its definition. The comparison of the LES solutions is based on the convergence properties of their statistics with respect to the turbulence resolution length scale. The dependence of the LES statistics is analysed for velocity and the mixture fraction fields, and tested for convergence. For the most part, the statistics converge for the finest grids, but the variance of the mixture fraction shows some residual grid dependence in the high-gradient regions of the jet near field. The SGS variance given by model I exhibits realisability everywhere, whereas in regions of the flame model II is non-realisable, predicting negative variances. Furthermore, the LES statistics of model I exhibit superior convergence behaviour.     

Solid support flame synthesis of 1-D and 3-D tungsten-oxide nanostructures

In this paper we report the growth of 1-D and 3-D tungsten-oxide nanostructures on tungsten wire probes inserted in an opposed-flow oxy-fuel flame. The probe diameter and oxygen content in the oxidizer were varied to study their influence on the growth of tungsten-oxide nanostructures. The introduction of a 1-mm diameter W probe into the flame environment with an oxidizer composition of 50%O₂ + 50%N₂, resulted in the formation of 1-D nanorods on the upper surface of the probe. The formation of triangular, rectangular, square, and cylindrical 3-D channels with completely hollow or semi-hollow morphology was achieved by reducing the probe diameter to 0.5 mm. Whereas, the increase of the O₂ content to 100% and the employment of a 1-mm probe resulted in the growth of ribbon-like micron-sized structures. The lattice spacing of ∼0.38 nm measured for the 1-D W-oxides closely matches a monoclinic WO₃ structure. X-ray photoelectron spectroscopy analysis revealed that the larger 3-D structures also consist of WO₃ confirming that the chemical composition of the structures remains the same while varying the probe and flame parameters. The proposed growth mechanism states that the 3-D WO₃ structures are formed through the lateral coalescence of 1-D W-oxide nanorods.     

Improving the Flame Retardancy of Polybenzoxazines with a Reactive Phosphorus-Containing Compound

A novel flame retardant resin was prepared by modifying benzoxazines with a reactive phosphorus-containing compound, 2-(6-Oxido-6H-dibenzo[c,e][1,2]oxa-phosphorin-6-yl) 1,4-benzenediol (ODOPB). The curing reactions of the benzoxazines containing ODOPB (ODOPB-BOZ) and a type of bifunctional benzoxazine (B-BOZ) were investigated via differential scanning calorimetry. The ODOPB-BOZ precursors exhibited lower curing temperature in comparison with the B-BOZ. Through dynamic mechanical analysis tests, it was found that the glass transition temperature and storage modulus of the cured ODOPB-BOZ were lower than those of the cured B-BOZ. Moreover, the tensile and flexural properties of the cured ODOPB-BOZ were also lower than those of the cured B-BOZ. The TGA tests proved that, owing to the presence of ODOPB, the char yield of the polybenzoxazines were remarkably raised while the decomposition rates at higher temperature were reduced. It was found that the flame retardancy of cured ODOPB-BOZ attained V-0 grade upon the UL-94 tests while that of cured B-BOZ was V-1 grade. SEM images showed that more compact char layers were formed in the cured ODOPB-BOZ after combustion, resulting in the improvement of flame retardance.     

Flamelet structure in turbulent premixed swirling oxy-combustion of methane

Two key flame macrostructures in swirling flows have been observed in experiments of oxy-combustion (as well as air-combustion); as the equivalence ratio is raised, the flame moves from being stabilized on just the inner shear layer (Flame III) to getting stabilized on both the inner and outer shear layers (Flame IV). We report results of an LES investigation of two different inlet oxy-fuel mixtures, in a turbulent swirling flow at $\text{Re}=20,000,$ that capture these two macrostructures. Previous work on the effects of heat loss have mostly focused on its impact on macro-scale observations. In this paper, we examine how heat loss impacts the flame microstructures as well for these two macrostructures. For both flames, the flamelet structure, as represented by a scatter plot of the normalized fuel concentration against the normalized temperature, depends on whether the combustor walls are adiabatic or non-adiabatic. For the adiabatic case, the flamelets of both macrostructures behave like strained flames. When wall heat transfer is included, Flame III microstructure is more bimodal. Since this flame extends farther downstream and part of it propagates along the walls, heat transfer has a greater impact on it’s microstructure. These results show that heat loss impacts not just the macro properties of the flame such as its shape or interactions with the wall, but also fundamentally changes its internal structure. Scatter plots of the turbulent flames are constructed and compared to different 1D laminar flame profiles (e.g., strained or with heat loss), and comparisons suggest the important role of the wall thermal boundary conditions in the accurate simulations of combustion dynamics and interpretations of experimental data, including data reduction and scaling.