固相微萃取与高效液相色谱联用技术的进展

 较全面地评述了固相微萃取与高效液相色谱联用技术的发展与应用 ,包括该技术的原理、接口装置、涂层材料等。     

Preparation and Characterization of Zirconia-Magnesia Support Modified by Alkylphosphonic Acid for Liquid Chromatography

Interest in zirconia as a chromatography support has increased considerably recently because of its chemical inertness and its promise as a useful support. We have reported the preparation of spherical zirconia and characterization of its chromatographic behavior. However, the zirconia was found unsatisfactory for its chromatographic efficiency, probably owing to the poor pore structure of it. In this paper, we for the first time report the preparation of alkylphosphonic acid modified zirconia-magnesia stationary phase, and characterization of its structure and chromatographic behavior.     

A new proposal for the discretization of the Griffin—Wheeler—Hartree—Fock equations

A polynomial expansion is proposed as a new way to discretize the Griffin-Wheeler-Hartree-Fock equations of the Generator Coordinate Hartree-Fock method. The implementation of the polynomial expansion in the Generator Coordinate Hartree-Fock method discretizes the Griffin-Wheeler-Hartree-Fock equations through a numerical mesh which is not equally spaced. This procedure makes the optimization of Gaussian exponents in the Generator Coordinate Hartree-Fock method more flexible and more efficient. The results obtained with the polynomial expansion for atomic Hartree-Fock energies show this technique is very powerful when employed in the design of compact and high accurate Gaussian basis sets used in ab initio non-relativistic (Hartree-Fock) and relativistic (Dirac-Fock) calculations.     

Highly Catalytic Enantioselective Addition of Diethyl Zinc to Aldehydes and Chalcone in the Presence of Chiral Ligands

Catalytic asymmetric carbon-carbon bond formation is one of the most important reactions and have attracted much attention to develop more efficient enantioselective C-C formation methods in organic synthesis. In this field, asymmetric addition of diethylzinc to aldehydes[1] and conjugate addition to enones[2] have drawn special interests and have been greatly developed. Regardless of it, much spaces in these areas still exist, so it needs more extensive and intensive researches for the purpose of as follows: (1) attaching ligands to a polymer for the easy separation of the catalysts so as to be able to allow very efficient recovery and reuse of the catalysts, and the possibility of carrying out the desired transfomation in continuous mode in a flow reactor, etc., (2) searching for novel chiral catalysts with such features as more suitable for more extensive substrates varieties, and more convenient and economical as well as possessing applicable prospect, and so on. Here we report some works in these areas done in our laboratory.     

基于MEMS姿态传感器的声矢量传感器设计

针对声矢量传感器姿态变化难以准确测量导致目标测向精度低的现状,设计一种微型MEMS姿态传感器,并将其封装在声矢量传感器内部,实现基于MEMS姿态传感器的声矢量传感器设计。首先根据声矢量传感器姿态测量与校正原理,采用四元数姿态解算方法及扩展卡尔曼滤波器设计MEMS姿态传感器,并对其进行姿态精度测试;然后基于MEMS姿态传感器进行声矢量传感器样机设计、制作、参数测试;最后对样机进行了海上实验,结果表明,通过姿态校正后声矢量传感器目标方位估计精度与GPS推算方位精度一致,验证了利用MEMS姿态传感器设计声矢量传感器的可行性。     

Photoemission of spinpolarized electrons from strained GaAsP

Strained layer GaAs_.95P_.05 photo cathodes are presented, which emit electron beams spinpolarized to a degree of P = 75% typically. Quantum yields around QE = 0.4% are observed routinely. The figure of merit P² × QE = 2.3 × 10^–3 is comparable to that of the best strained layer cathodes reported in literature. The optimum wavelength of irradiating light around 830 nm is in convenient reach of Ti:sapphire lasers or diode lasers respectively. The cathodes are produced using MOCVD-techniques. A GaAs_.55P_.45-GaAs_.85P_.15 superlattice structure prevents the migration of dislocations from the substrate and bottom layers to the strained overlayer. The surface is protected by an arsenic layer so that no chemical cleaning is necessary before installation into vacuum. The source of polarized electrons attached to the Mainz race track microtron MAMI works with such cathodes now. More than 1000 hours beamtime have been performed successfully.     

Fluorocarbon- containing hydrophobically modified poly(N-isopropylacrylamide)

A fluorocarbon-modified poly(N-isopropylacrylamide) has been synthesized by copolymerization of N-isopropyl acrylamide with a small amount of acrylate or methacrylate containing a perfluoroalkyl group. It was found that the hydrophilicity of macromolecular backbone is an important factor to the solution properties of the copolymers and that hydrophobic association between fluorocarbon groups is stronger than that between the corresponding hydrocarbon analogies. The viscosity of some of the copolymer solutions was very sensitive to temperature. It was dilatant at higher fluorocarbon comonomer content ( > 0.20-1.0 mol%) and was Newtonian at very low fluorocarbon comonomer content (0.03-0.2 mol% ) . Evidence for hydrophobic association of the fluorocarbon groups was obtained from the effects of adding Nad and surfactants on the solution viscosity. The LC-ST properties of these copolymers were studied by DSC method and this was also found to be consistent with hydrophobic association between the fluorocarbo     

碱基在十二胺-N,N-二亚甲基膦酸改性氧化锆固定相上色谱行为的研究

研究了碱基在十二胺-N,N-二亚甲基膦酸(DDPA)改性氧化锆固定相（DPZ）上的色谱保留行为,考察了流动相中甲醇含量、流动相pH值、缓冲溶液中离子类型和离子强度对碱基保留的影响,对DDPA在氧化锆表面的吸附方式进行了研究。研究结果表明,DDPA仅以一个膦酸基与氧化锆结合,因而DPZ固定相表面上除了有长链的疏水烷基外,还有酸性的膦酸基和碱性的氨基。碱基分子中也存在氨基和酰胺基等极性基团,因此碱基在DPZ固定相上除了有疏水作用外,还具有电荷排斥作用、离子交换作用等多种保留机理。由于多种保留机理的存在,使得碱基在DPZ固定相上具有较好的分离选择性,在酸性条件下对碱基混合样品的分离取得了满意的结果。