Imidazole Coordinated Sandwich-type Antimony Polyoxotungstates Na9[ {Na（H=O2}3{M（C3H4N2）}3（ Sb W9O33）2]·xH=O（M=Ni^Ⅱ, Co^Ⅱ, Zn^Ⅱ, Mn^Ⅱ）

The imidazole covalently coordinated sandwich-type heteropolymngstates Na9[ {Na（H=O2}3{M（C3H4N2）}3（ Sb W9O33）2]·xH=O（M=Ni^Ⅱ, Co^Ⅱ, Zn^Ⅱ, Mn^Ⅱ） were obtained by the reaction of Na2WO4·2H2O, SbCl3·6H2O, NiCl2·6H2O [MnSO4·H2O, Co（NO3）2·6H2O, ZnSO4·7H2O] and imidazole at pH≈7.5. The structure of Na9[{Na（H2O）2}3{Ni（C3H4N2）}3（SbW9O33）2]·32H2O was determined by single crystal X-ray diffraction. Polyanion [{Na（H2O）2}3{Ni（C3H4N2）}3（SbW9O33）2}3]^9- has approximate C3v symmetry, imidazole coordinated six-nuclear duster [{Na（H2O）2}3{Ni（C3H4N2）}3]^9＋ is encapsulated between two （α-SbW9O33）^9-, the three rings of imidazole in the polyanion are perpendicular to the horizontal plane formed by six metals （Na-Ni-Na-Ni-Na-Ni） in the central belt, and x-stacking interactions exist between imidazoles of neighboring polyanions with dihedral angel of 60%. The compounds were also characterized by IR, UV-Vis spectra, TG and DSC, and the thermal decomposition mechanism of the four compounds was suggested by TG curves.     

A High Sensitivity Detection Method of Singlet Oxygen and Superoxide Anion

This paper, for the first time, reports a method that can be used as a highly sensitive probe for singlet oxygen (^1O2) and superoxide anion (O2^-) in vitro or in vivo. FCLA(3,7-dihydro-6-{4-[2-(N‘-(5-fluoresceinyl)thioureido)ethoxy]phenyl}-2-methylimidazo{1,2-a}pyrazin-3-one sodium salt), a chemiluminescence (CL) analysis reagent, has been reported to sensitively react with ^1O2 and O2^- to emit photons with a spectral peak of 525nm. In this work,when human serum albumin (HSA) was added into FCLA solution to enhance the CL intensity,approximately 20 times, compared to that without HSA. The enhanced CL had the same 525 nm spectral peak, identical to that without HSA. By gradually reducing the molecular oxygen content in the solution, we find that the auto-oxidation of oxygen molecules dissolved in the solution plays an important role in the CL process. Based on these experimental evidences, we propose a novel and highly sensitive detection method of ^1O2 and O2^- which may have a great potential in chemical and medical applications.     

Determination of medecamycin by adsorptive stripping voltammetry with an activated electrode

The adsorptive and electrochemical behaviors of medecamycin were investigated on a glassy carbon electrode (GCE) pretreated by anodic oxidation at +1.8 V for 5 min in 0.025 mol l^–1 NH₃-NH₄Cl (pH 8.6) solution. An adsorptive stripping voltammetric method for the determination of medecamycin at the pretreated glassy carbon electrode has been developed. Medecamycin was accumulated in NH₃-NH₄Cl buffer (pH 9.0) at a potential of –0.7 V (vs. saturated calomel electrode (SCE)) for a certain time, and then determined by second-order differential anodic stripping voltammetry. The second-order differential anodic stripping peak current at +0.72 V was proportional to the concentration of medecamycin in the range 2.0 g ml^–1 to 50.0 g ml^–1. The detection limit (three times the signal-to-noise) was 1.0 g ml^–1 and the relative standard deviation of the results was 3.28% for eight successive determinations of 10.0 g ml^–1 medecamycin. This method has been applied to the direct determination of medecamycin in commercial tablets and spiked urine samples with satisfactory results.     

Density of supercritical CO_2-tetrahydrofuran binary mixture and the partial molar volume of the cosolvent

The densities of supercritical CO2-tetrahydrofuran (cosolvent) binary mixture weremeasured at temperatures in range of 308.15 to 323.15 K and at pressure up to 16.5 MPa.The concentrations of tetrahydrofuran were from 0 to 0.57 mol/L.The partial molar volume of tetrahydrofuran was calculated based on the relationship between the density of the mixture and the concentration of the cosolvent.It is observed that the partial molar volume of the cosolvent is negative and the absolute value decreases with increasing pressure and the concentration of the cosolvent.     

中药配方颗粒红外光谱法的快速鉴别

采用红外光谱法对中药配方颗粒及其辅料进行了鉴别研究。结果表明：不同生产厂商的配方颗粒中所添加的辅料类型及用量有较大差别；不同种的配方颗粒在辅料含量较低的情况下有较明显的指纹性，而辅料含量较高时，采用差谱技术可以提高谱图的指纹性，达到中药配方颗粒--鉴别的目的。该法简便、快速、可靠，是中药配方颗粒宏观质控的一个强有力的手段。     

A Minor New Flavone from Scutellaria baicalensis Georgi

A new flavone,6,2′-dihydroxy-5,7,8,6′-tetramethoxyflavone,was isolated from the roots of Scutellaria baicalensis. Its structure was established on the basis of spectral evidences.     

盐类和温度对非离子型表面活性剂溶液粘度的影响

研究在各种盐类存在下,温度对非离子表面活性剂(OP类)溶液粘度的影响,发现相对粘度的对数值与1/T呈线性关系,从直线的斜率可得活化自由能ΔG′。由热力学关系式可计算粘性流体的活化焓ΔII′和活化熵ΔS′。用所得热力学函数对胶束型态的转化进行了讨论。     

Determination of trace scandium by ion-exchanger phase spectrophotometry withp-nitrochlorophosphonazo

Ion-exchanger phase Spectrophotometry withp-nitrochlorophosphonazo (CPApN) has been developed for the determination of scandium. The linear range is 1–8 g of scandium in 50 ml of solution, using 0.8 g of resin, with an apparent molar absorptivity of 2.76 × 10⁵ 1 mol^–1 cm^–1. Aluminum and rare earth elements in reasonable amounts do not interfere. The method has been applied successfully to the determination of scandium in alloys, with relative standard deviations of 2–4%.     

PREPARATION AND CHARACTERIZATION OF SHISH-KEBAB TYPE LIQUID CRYSTALLINE POLY（p-PHENYLENEVINYLENE）

Novel shish-kebab type liquid crystalline poly（p-phenylenevinylene） derivatives were synthesized by Stille coupling reaction from 2,5-bis[（4-n-alkoxyl）benzoyloxy]1,4-dibromobenzene （monomer l） and 1,2-bis（tributylstannyl） ethylene （monomer 2）. The polymers with alkoxy groups are soluble in common organic solvents and exhibit blue fluorescence. Both the cast film and the annealed film have large red-shifts in fluorescence spectra and show yellow fluorescence. The polymers with CN and NO2 groups show poor solubility and green fluorescence. All the polymers possess liquid crystalline smectic phases. The melting point （Tm） of the polymers decreases when the length of the alkoxy tails of the mesogenic units increases. The polymers are easily aligned under a magnetic field of 10 Tesla. It is found that the conjugated backbone and LC side chain are aligned perpendicular and parallel to the magnetic field, respectively. The polymers show optical dichroism in fluorescence spectra, suggesting that they are available for advance materials with linear optical polarization.     

Knoevenagel condensation catalysed by poly（vinyl chloride） supported tetraethylenepentamine （PVC-TEPA）

Poly(vinyl chloride) supported tetraethylenepentamine (PVC-TEPA) has been found to be an efficient catalyst for the Knoevenagel condensation. A wide range of aromatic aldehydes easily undergo condensations with ethyl cyanoacetate and malononitrile in the commercial 95% ethanol in refluxing using PVC-TEPA as catalyst to afford the desired products of good purity in moderate to excellent yields. A recycling study confirmed that the catalyst could be reused, the yield of the desired condensation product were not reduced. The merits of this protocol are environmentally benign, simple operation, convenient work-up and good yields. Furthermore, the catalyst can easily be recovered and reused at five times with comparable yields.