付里叶变换红外光谱仪的操作参数对光谱的影响

本文以二苯基甲酮的ＫＢｒ压片为标样，在Ｂｒｕｋｅｒ ＩＦＳ １２０ＨＲ付里叶变换红外光谱仪上系统考察了该仪器折一些重要操作参数（光源光栏、切趾函数、扫描速度）对光谱质量（信噪比，分辨率）的影响。从而获得了测样时的优化操作条件。     

镍 钴 钯 铁2—（二苯基膦基）吡啶配合物的合成及其催化羰基化反应

众所周知,铑催化剂是醇类羰基化的有效催化剂,但是铑价格昂贵且对设备有腐蚀性,因此,寻找出对醇类羰基化催化活性好的非贵金属催化剂,对醇类羰化的工业化有十分重要的意义。 本文在温和条件下,合成了四种含有相同配体(Ph_2PPy)不同金属的有机配合物(金属基分别为Ni、Co、Pd、Fe),并探索了它们对乙醇羰基化反应的催化活性。     

Absorption and Capture of Methane into Ionic Liquid

A reversible storage-release process switched by a temperature difference of 10℃around room temperature can be realized. This fast, recyclable, energy efficient, low cost and green system within a wide range of temperature and pressure is reported here for the first time. The system is believed to open up a new route for the storage and homogeneous utilization of methane.     

硅胶担载四核羰基钴催化剂的EXAFS和IR研究

本文以透射法EXAFS和IR等手段研究了四核羰基钴金属簇Co_4(CO)_(10)(PPh)_2担载在SiO_2上以后及用于烯烃醛化反应前后的变化,确定了相应的结构参数并探讨了催化活性与结构的关系。     

A novel hyperbranched polyester acrylate used for microfabrications

A novel hyperbranched polyester acrylate (HPEA) was synthesized based upon ethylenediamine tetraacetic acid as a “core” molecule, 5‐hydroxyisophthalic acid as an AB₂ monomer, and 2‐hydroxyethyl acrylate as an endcapping reagent. The obtained oligomer has an unsaturation concentration of 4.10 mmol_C?C g^?1 measured by nuclear magnetic resonance and a wide molecular weight distribution of 1.64 measured by gel permeation chromatography. The two‐photon absorption (TPA) photopolymerization of HPEA under the exposure of a Ti : sapphire femtosecond laser with a wavelength of 800 nm was investigated through laser exposure dose‐dependant spatial resolutions of its resins. The TPA photopolymerization thresholds at the range 1.6–4.3 × 10⁷ mJ cm^?2, and exposure dose windows at the range 3.4–4.3 for three formulations were determined. A spatial resolution of 0.85 μm was obtained through the TPA photopolymerization of the formulation containing 1 wt% photoinitiator and 0.3 wt% photoinhibitor. A diffraction grating and real three‐dimensional coupled gear wheel created by TPA photopolymerization were described to demonstrate the unique capability of HPEA in microfabrications. Copyright © 2004 John Wiley & Sons, Ltd.     

Reversed phase and normal phase liquid chromatography on poly(1-vinyl-2-pyrrolidone) or poly(1-vinylimidazole) bonded silica using γ-methacryloxypropyltrimethoxysilane as coupling agent. Stationary phases 23

Summary A method for preparing selective phases for reversed phase and normal phase liquid chromatography is described. Two different polymeric modified silica gel phases were prepared by simultaneously bonding with -methacryloxypropyltrimethoxysilane as coupling agent. Modification of these polymer phases was achieved by treatment with poly(1-vinyl-2-pyrrolidone) or poly(1-vinylimidazole). By eluting a number of standard mixtures containing polyaromatics and haloaromatics, the selectivity of each phase was evaluated. In reversed phase mode, the partition of sample components between mobile phase and stationary phase was found to be similar for polymer phases and -methacryloxypropylsilyl phase. In normal phase mode, only the poly(1-vinyl-2-pyrrolidone) phase or the poly(1-vinylimidazole) phase could interact electronically with aromatic nuclei.Part 22: see [1]     

Electrochemical detector with a 20 nl volume for micro-columns liquid chromatography

Summary A flow-through two electrode wall-jet cell with a platinum measuring electrode and a cell volume of 20 nl has been designed and evaluated. It has been used to detect phenols by reversed phase liquid chromatography using short micro bore columns. The linear dynamic range between the measured current and the concentration is greater than 10³ (1.5×10^–7–5×10^–4 mol/l) and the minimum analyzable amount was found to be 10 pg for pyrocatechol. A negligible broadening in the detector permits the use of micro columns down to 0.5 mm internal diameter, packed with 5 m particles, without any substantial distortion of eluted zones.Presented at the 14th International Symposium on Chromatography London, September, 1982     

Tetra(μ3-hydroxo)hexa(μ2-carboxylato-O,O′)-bridged tetranuclear terbium(III) cubane complex

A novel tetranuclear terbium(III) complex [Tb₄(OH)₄(pybet)₆(H₂O)₈][Tb₄(OH)₄(pybet)₆(H₂O)₇ (NO₃)](ClO₄)₁₄·6H₂O has been synthesized and shown by X-ray crystallography to have a cubane-like Tb₄(μ₃-OH)₄(μ₂-carboxylato-O,O′)₆ core. The ligand pybet is pyridinoacetate, C₅H₅⁺N-CH₂CO₂⁻. Magnetic susceptibility data were measured for this Tb₄ complex in the range of 2.0–320 K and in fields of 1.0 G to 50.0 kG. It is concluded that either there is very weak antiferromagnetic exchange interaction (J = −0.015 cm⁻¹) or there is a small crystal-field splitting of the ⁷F₆ Tb^III ground state.     

Dehydrogenative coupling of phenanthroline under hydrothermal conditions: crystal structure of a novel layered vanadate complex constructed of 4,8,10-net sheets: [(2,2'-biphen)Co]V3O8.5

2,2'-Biphenanthroline (2,2'-biphen) formed from 1,10-phenanthroline when a new two-dimensional layered vanadium oxide metal coordination complex, [(2,2'-biphen)Co]V3O8.5, which contains novel 4,8,10-net sheets, was hydrothermally synthesized.     

可逆反应的热静力学研究法

化学反应的焓变△H和平衡常数K的测定是热静力学研究的重要任务。通常用量热法可以此较准确地测定△H,但要从量热数据直接得到K则是在六十年代初才开始有所探索。在达方面,Drago和Christensen的工作是值得借鉴的。本文建立了一种中性配位体与一价金属离子络合反应体系的热静力学研究法,并用这种方法研究了二苯并18-冠-6与Na~+的络合反应,同时得到了反应的△H和平衡常数K。实验值与文献值符合。