Separation of alkylbenzyl quaternary ammonium compounds by capillary zone electrophoresis with sample stacking injection

Summary A systematic investigation of operational buffer systems, sample preparation and instrument parameters for achieving the best possible performance for determinating an homologous series of N-benzyl-N-alkyl-N,N-dimethylammonium chloride compounds by capillary zone electrophoresis with direct UV detection. The most effective separation was achieved within 3.5 min with the addition of acetonitrile (40%) in a phosphate buffer (20 mM pH 5.2) using a 40 cm fused-silica capillary operating at 25 KV and 20°C. Degassing of all electrolyte solutions and samples was very important. The linearity and repeatability for each compounds were satisfactory. To improve detection limits, on-column sample preconcentration, sample stacking, was investigated achieving a tenfold enrichment factor and quantitation limits about 10⁻⁷M.     

NMR analysis of multiple samples using parallel coils: improved performance using reference deconvolution and multidimensional methods

Improvements in the Multiplex Sample NMR method are investigated to explore its capabilities of analyzing multiple samples simultaneously. Issues of quantitation and resolution in the multiple-coil probe are examined in one- and two-dimensional experiments. Improvements in quantitation are shown to result from the use of reference deconvolution for one-dimensional experiments, while the use of two-dimensional methods has much improved resolution and shows the potential for significantly increased parallelism. A multiplicative scheme is shown to be an easily implemented, effective method for generating individual sub-spectra from individual samples.     

Stationary-phase focusing in capillary gas-liquid chromatography: Enhancement of the maximum permissible sample size

Equations have been derived to predict the extent to which the sample size may be increased, without decreasing the column performance, by stationary-phase focusing at sub-ambient temperatures. Under favorable circumstances the sample size may be enhanced several hundredfold.     

Scattering experiments on the structure of concentrated dispersions

 In this work the Couette cell is compared with a more recently constructed disk shear cell. There are distinct advantages of the disk over the Couette cell, in particular, when it comes to the determination of the intensity along certain Bragg rods. Received: 12 December 2000 Accepted: 31 January 2001     

New SPE loading material for affinity‐based separation of cyclodextrins from drug:CD complexes in order to overcome Beer's law deviations

Molecular inclusion of guest molecules within CDs is known to alter guest molecule spectrophotometric absorptivity, making their determination, based on spectrophotometric data, inaccurate. Therefore specific analytical methods capable of quantifying the drugs as free molecules must be developed and validated. SPE was selected to simplify sample and avoid more time‐consuming alternatives. A new solid phase was synthesized and characterized by infrared spectrometry, differential scanning calorimetry and elemental analysis. The competitive complexation of adamantane groups immobilized on the silica substrate facilitates drug:CD complex dissociation and elimination of CD from samples. The drug molecules, now free from CD, can be easily analysed by an already available HPLC method. This new SPE loading material was employed in the determination of ketoprofen in its CD complex as a representative example of the utility of this novel material. The calculated analytical errors were reduced from a maximum of 20.79% (without SPE) to a minimum of 3.99%.     

Porosity, mechanical properties, residual stresses of supersonic plasma-sprayed Ni-based alloy coatings prepared at different powder feed rates

The aim of this paper was to investigate the effect of powder feed rate (PFR) on the microstructure and mechanical properties of the supersonic plasma-sprayed Ni-Cr-B-Si-C coatings. The microstructure, porosity and mechanical properties of the coatings and the residual stresses at the coating surfaces were experimentally determined. Results showed that the variations of porosity, elastic moduli and micro-hardness of the coatings followed Weibull distribution. From the statistical trend, the porosity of the coating increased with increasing PFR. However, the elastic modulus and the micro-hardness of the coating decreased and reached local minima and then increased with increasing PFR. Elastic modulus could be generally considered to be an increasing function of micro-hardness. The mean value of the elastic modulus of the coating calculated from Weibull plot was almost proportional to the square root of the mean value of the micro-hardness of the coating. Moreover, with increasing PFR, the residual stress at the coating surface, which was mainly governed by the elastic modulus of the coating, decreased to a local minimum and then increased.     

Synthesis of silicated hydroxyapatite Ca10(PO4)6−x(SiO4)x(OH)2−x

The preparation of silicated hydroxyapatite Ca₁₀(PO₄)_6−x(SiO₄)_x(OH)_2−x (SiHA) with 0?x?2 was investigated using a wet precipitation method followed by a heat treatment. X-ray diffraction and Rietveld refinement, Fourier transformed IR (FTIR) spectroscopy, elemental analyses, transmission electron microscopy and thermal analyses were used to characterize the samples. The raw materials were composed of a partially silicated and carbonated apatite and a secondary minor phase containing the excess silicon. Single phase silicated hydroxyapatites, with 0?x?1, could be synthesized after a thermal treatment of the raw powders above 700 °C. The presence of carbonate groups in the raw apatite played an important role in the incorporation of silicates during heating. From the different results, the mechanisms of formation of SiHA are discussed.     

On the influence of the solute sample size on temperature-programmed retention indices

The effect of the solute sample size on the measurement of temperature-programmed retention indices (I_TP) has been studied on glass capillary columns with different stationary phases, film thicknesses, and temperature programs. The sample capacity of a solute is little affected by the parameters of temperature program, i. e. initial temperature and heating rate. However, it has been found that in a temperature programmed run, allowable sample sizes for high I_TP values are lower than for low I_TP values. About 10 ng of each compound is recommended as the sample size for accurate measurement of I_TP values on commonly used capillary columns.     

Sample average approximation of expected value constrained stochastic programs

We propose a sample average approximation (SAA) method for stochastic programming problems with expected value constraints. Such problems arise, for example, in portfolio selection with constraints on conditional value-at-risk (CVaR). We provide a convergence analysis and a statistical validation scheme for the proposed method.     

沿海软粘土取土质量的对比分析

本文在简要介绍固定活塞式薄壁取土器取土技术基础上，详尽分析了在连云港、赤湾港和广深路所进行的软粘土取土技术对比试验结果。试验结果表明，土样扰动对于室内所测定的力学性指标影响极大，但对物理性指标影响不大。研究结果还有力地证明，只要操作正确，采用薄壁取土器能取得高质量土样，而采用敞口式厚壁取土器取出的土样扰动较大。