A New Hydroxo‐bridged Chromium(III) Dimer [Cr(saltn)OH]2·4H2O: Synthesis,Crystal Structure and Magnetic Properties

A new hydroxo‐bridged dimeric Cr(III) complex [Cr(saltn)OH]₂·4H₂O [H₂saltn=N,N′‐bis(salicylidene)trimethylenediamine] has been synthesized and its structural and magnetic properties have been investigated. The complex crystallizes in the triclinic space group P‐1 with one dimeric formula unit in a cell of dimensions a=0.95828(19) nm, b=0.95926(19) nm, c=1.0437(2) nm, α=86.77(3)°, β=82.48(3)°, and γ=64.93(3)°. The geometry around each chromium(III) center is six‐coordinate, distorted‐octahedral. The bridging Cr₂O₂ unit is strictly planar, as required by the crystallographic symmetry. The Cr? O? Cr′ bridging angle is 99.94(16)°, and the distance between Cr…Cr′ is 0.3019 nm. The magnetic susceptibility of the complex has been examined in the range of 2‐300 K. By using the spin‐spin coupled model for an S₁=S₂=3/2 dimeric system , the magnetic data were fitted to give the parameters of g=2.01(1), J=‐0.85(2) cm^‐1, and zJ' =0.18(3)cm^‐1, indicating the presence of a weak antiferromagnetic spin‐exchange interaction between the Cr(III) ions in the binuclear complex.     

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     

BaF2/La2O3催化剂上甲烷氧化偶联反应活性氧物种的原位红外光谱

用原位红外光谱研究了BaF2/La2O3催化剂上甲烷氧化偶联反应的活性氧物种.结果表明,催化剂经O2预吸附后,在1 108~1 118 cm-1处出现超氧物种O2-的O-O键伸缩振动峰.经18O2同位素交换实验后,原1 108~1 118 cm-1处谱峰的强度减弱,同时在1 086和1 051 cm-1处出现(O18O)-物种和18O2-物种的吸收峰.同位素交换实验进一步确证了1 108~1 118cm-1处谱峰确为O2-物种的吸收峰.在700℃下,O2-物种能够活化CH4生成C2H4,而且O2-物种的消耗量和C2H4的生成量呈很好的消长对应关系.超氧物种O2-是BaF2/La2O3催化剂上甲烷氧化偶联反应的活性氧物种.     

Elastic scattering cross sections for 160<Superscript>°</Superscript> and 170<Superscript>°</Superscript>backscattering of 1.40-2.64 MeV protons from natural vanadium

Summary The elastic scattering cross sections of natural vanadium for protons have been measured for beam energies below 2.64 MeV in steps of 10 keV and in the angular 160° and 170°. The overall standard error (Δσ_Exp/σ_Exp) in the measured cross sections is estimated to be better than ±3% at all the beam energies and angles. The results are presented in graphical and tabular forms that should be useful for those who wish to use the cross sections for material analysis.     

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.     

Ir（Ⅳ）—KBrO3—DBS—偶氮氯膦催化分光光度法测定微量铱的研究

ＫＢｒＯ３－ＤＢＳ偶氮氯膦在０．８ｍｌ．Ｌ＾－１的Ｈ２ＳＯ４介质中长时间加热亦无明显褪色现象，但在有微量铱存在时，褪色反应在３ｍｉｎ内完成，且与Ｉｒ（Ⅳ）的浓度有良好的线性关系，据此建立了微量铱的催化褪色分光光度分析法，其检出限为０．０１μｇ．１０ｍＬ＾－１铱的含量在０．０１－０．２０μｇ．１０ｍＬ＾－１范围内符合比尔定律。     

Analysis of effective molecular diffusion rates for verteporfin in subcutaneous versus orthotopic Dunning prostate tumors

Photosensitizer biodistribution change inside tissue is one of the dominant factors in photodynamic therapy efficacy. In this study, the pharmacokinetics of a benzoporphyrin derivative (BPD), delivered in verteporfin for injection formulation, have been quantified in the rat Dunning prostate tumor MAT-LyLu model, using both subcutaneous and orthotopic sites. Blood plasma sampling indicated that BPD had a bi-exponential metabolic lifetime in vivo, with the two lifetimes being 9.6 min and 8.3 h. The spatial distributions in the tumor were quantified as a function of distance from the perfused blood vessels, using fluorescence histologic images of the tumor. A fluorescent vascular marker was used to obtain locations and shapes of perfused capillaries at a wavelength of emission different from that of BPD and to allow colocalized images to be acquired of vessel and BPD locations. Using the BPD fluorescence images obtained 15 min after intravenous administration, a forward finite-element solution to the diffusion equation was used to predict the drug distribution by matching the fluorescence intensity images observed microscopically. An inverse solver was used to minimize the root mean square error between the image of simulated diffusion and the experimental image, resulting in estimation of the diffusion coefficient of BPD in the tumor models. Effective diffusion coefficients were 0.88 and 1.59 microm2/s for the subcutaneous and orthotopically grown tumors, respectively, indicating that orthotopic tumors have significantly higher vascular extravasation rates as compared with subcutaneous tumors. This analysis supports the hypothesis that leakage rates of the photosensitizer vary considerably. Thus, although varying the time between injection and optical irradiation may be used to vary the targeting between vascular and less vascular areas, the precise time of treatment will depend on the nature of the permeability of the vasculature in the tissue being treated.     

二维卷积在动力学分析中的应用

本文用计算机模拟和二维卷积研究了稀土与间乙酰基偶氮氯膦的显色反应，选择不同的模型参数可描述这类反应的细节，二维卷积则增强对叠合二维谱的分辨。