Determination of acetone, 2-butanone, diethyl ketone and BTX using HSCC-UV-IMS

A combination of a custom-designed ion mobility spectrometer (IMS) with a UV ionization source and a high speed capillary column (HSCC) has been developed as an analytical device for the sensitive detection of volatile organic compounds (VOCs), e.g. 2-propanone (acetone), 2-butanone and 3-pentanone (diethyl ketone) in the gas phase. A fast separation of the three selected substances and benzene, toluene and m-xylene (BTX) - all of which occur in human breath - has been achieved within less than four minutes at a carrier gas flow rate of 4.5 mL x min(-1). Multi-dimensional correlations presented support the interpretation of the acquired spectra of mixtures. Method detection limits were 2.7 microg x L(-1) for acetone and 2-butanone and 3.0 microg x L(-1) for diethyl ketone in nitrogen, respectively. The assay linear dynamic range is 4-320 microg x L(-1).     

Chromatographic evaluation of perphenylcarbamoylated β-cyclodextrin bonded stationary phase for micro-high performance liquid chromatography and pressurized capillary electrochromatography

Application of mono (6^A-N-ethylenediamine-6^A-deoxy) perphenylcarbamoylated β-cyclodextrin (β-CD) bonded stationary phase (CSP) in micro-high performance liquid chromatography (micro-HPLC) and pressurized capillary electrochromatography (p-CEC) was firstly presented. A series of racemic α-amidophosphonates were resolved in reversed- and normal-phase modes on this CSP. The investigated chromatographic parameters include retention factor (k′), separation factor (α) and resolution (Rs) of solutes. In addition, the structural variation of the solutes and the experimental factors affecting chiral separations have been examined, including the percentage of alcohol modifier, the linear velocity (u) of the mobile phase, electrical field strength, etc. Baseline separation was achieved for most of the entities. Hydrophobic interaction, steric effect and π-π interaction contribute to the possible mechanism. Comparative results indicate that higher Rs value up to 3.1 was found in micro-HPLC, higher efficiency up to 29,970 in p-CEC.     

C–H· π Interaction and N·H–O Hydrogen Bonding in the Chair-like p-tert-Butylcalix[8]arene Complex Including Four Pyridine Molecules

Crystal structure analysis shows that the p-tert-butylcalix[8]arene host and its four pyridine guests sit around an inversion center in the P2₁/c crystal lattice. The monoclinic cell parameters and its volume are: a = 19.617(4), b = 9.912(2), c = 25.178(5) , = 101.03(3)°, V =4805.27(17) ³. For Z = 2 and Mw = 1614.18, the calculated density Dcalc = 1.116 g/cm³. A host calixarene molecule includes four pyridine guests in two different ways: by hydrogen bonding and by possible C–H· interaction between the molecules. The hydrogen bonding drives the host macrocycle into a chair-like conformation.     

Ba-K-Bi-O和Ba-K-Pb-O氧化物的碘量滴定

本文提出了碘量法滴定Ba－K－Bi-O和Ba－K－Pb－O氧化物中Ba和Pb的名义价态，然后据此计算这些氧化物中K和Ba含量的方法。该法适用于正常条件下合成的具有ABO3型钙钛矿结构的Ba－K－Bi-O和Ba－K－Pb－O晶体。用本法的滴定结果表明，Tc为31K的Ba－K－Bi-O超导体的K含量为0．4，当K含量减少时，Tc随之下降。     

SYNTHESIS AND CHARACTERIZATION OF A NEW POLYSILOXANE CONTAINING N,N’-BIS(DIPHENYLSILYL)TETRAPHENYLCYCLODISILAZANE

A new kind of polysiloxane containing N,N'-bis(diphenylsilyl)tetraphenylcyclodisilazane was prepared by anionicnon-equilibrium polymerization with a "seed solution" as initiator. The monomer, N,N'-bis(hydroxydiphenylsilyl)-tetraphenyl-cyclodisilazane (BHPTPC), was synthesized via the hydrolysis of N,N'-bis(chlorodiphenylsilyl)tetraphenyl-cyclodisilazane (BCPTPC). A new method for the preparation of BCPTPC is also reported here with high yield and simplermanipulation. The synthesized polysiloxane containing N,N'-bis(diphenylsilyl)tetraphenylcyclodisilazane was characterized by ~1H-NMR, ~(29)Si-NMR, gel permeation chromatography (GPC) and intrinsic viscosity.     

复合固体超强酸催化剂SO_4~(2-)_4-WO_3-ZrO_2的结构研究

已报导，经适当处理的SO42-ZrO2和WO3－ZrO2具有超强酸性［1］．在此基础上将SO42-和WO3同时负载于ZrO2表面，发现其表面酸性有明显增强，得到的固体超强酸504－W0s－Zro。在很宽的焙烧温度范围内（700七00“C）都具有HO三一16．04的酸强度，吸附毗院的红外光谱研究表明，其表面同时具有强的L酸性和B酸性问，140“C时，对正乙烷裂解及异构化的催化活性比SO4－－ZrO。和WO3－ZI02都高，表现出相当的协同效应同．本文用XRD，DTA－TG，比表面测定等技术研究催化剂的组成、结构形态及其随焙烧温度的变化．并与504－Zro：和WO。…     

A novel approach to carbon hollow spheres and vessels from CCl4 at low temperatures

Carbon hollow spheres (400-600 nm) and vessels (400 nm x 3000 nm) have been synthesized from sp3-CCl4 at 190 and 230 degrees C, respectively. The HRTEM images and Raman spectra reveal the sp2 nature of the as-obtained products, indicating that the transformation from carbon sp3 to sp2 occurs in the reactions. The possible mechanism has also been proposed.     

土壤环境中铅的化学

论述了环境中铅的背景值、来源、污染、质量标准、化学循环以及环境中铅的烷基化，为铅污染治理提供理论依据。     

水杨酸与烟草铜锌超氧化物歧化酶的相互作用

利用邻苯三酚自氧化法监测了磷酸盐缓冲体系中水杨酸（SA）对超氧化物歧化酶（SOD）活力的影响。通过荧光光谱法研究了水杨酸与超氧化物歧化酶的相互作用机制，求得两者结合的形成常数和配位数，使用Forster非辐射能量转移技术求出了两者的结合位置距色氨酸残基间的距离为2.60nm。