果茶中展青霉素含量的高效液相色谱测定

An HPLC procedure is described in this paper for the determination of patulin in nectar. The method con-sists of solvent extraction and chromatographic separation,The conditions of HPLC were column; Zorbax-C_8( 5μm) at 35℃; mobile phase :AcCN/water(5/95,V/V); and detector UV275nm. The detection limit was0. 1μg/mL,the linear range was 0.5～2. 5μg and average recovery was 96.54±2.27%.     

Synthesis,Crystal Structure and Fluorescence of a Bicyclic Product Containing Chromene and Propargylamine Skeleton

The bicyclic product containing a chromene skeleton and a propargylamine skeleton(C_(22)H_(22)N_2O_2) was synthesized from the double sites of terminal alkyne, piperazine derivative and formaldehyde via one-pot procedure. Its structure was characterized by ~1H NMR, ~(13)C NMR, IR and H RMS, and further confirmed by single-crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/n with a = 12.6571(14), b = 11.3249(12), c = 12.6571(14) ?, β = 105.22°,V = 1750.6(3) ?~3, Z = 4, R = 0.0568 and w R = 0.1444. The fluorescence of the product was discussed.     

Bright red electroluminescent devices based on a soluble lanthanide complex Eu(DBM)_3(phen)

Electroluminescent devices with PVK film doped with Eu(DBM)3(phen) and PBD were fabricated. The device structure of glass substrate/indium-tin-oxide/PPV/PVK:Eu(DBM)3-(phen):PBD/Alq3/Al was employed. The emissive layer was formed by spin-casting method. A sharply red electroluminescence with a maximum luminance of 114.4 cd/m2 was achieved at 42 V.     

高效液相色谱法测定家兔血清中盐酸山莨菪碱含量

rapid method for the separation and determination of anisodamine hydrochloride in serum of rabbit has been developed with Nucleosil column of 4. 6× 250mm and CH3OH-H2O-(C2H5)3N (30:70 : 0.125)as mobile phase. Anisodamine hydrochloride was determined by reversed phase HPLC at 214nm.Atropine sulfate was used as an internal standard. The calibration curve was Y= 0.01945X+0. 05623,r= 0. 9998,n= 6.It was rectilinear within the range between 0. 75μg/mL-50.0μg/mL,and the recovery was from 97. 0% to 98. 2%.     

Synthesis of a-SnWO_4 thin-film electrodes by hydrothermal conversion from crystalline WO_3

Thin film electrodes of the orthorhombic form of tin tungstate(a-SnWO4) were prepared using a hydrothermal method to convert thin films of WO3 in aqueous Sn Cl2.The p H dependence of the growth mechanism was identified by scanning electron microscopy(SEM) and X-ray diffraction(XRD).The XRD patterns show complete conversion of WO3(s) to SnWO4(s) at p H 1,4,and 7.SEM images reveal a morphology change from sponge-like platelets to sharp nanowires as the p H increases from 1 to 7.The a-SnWO4 thin films were reddish brown in color,and display an indirect band gap of 1.9 e V by diffuse reflectance UV–vis spectroscopy.a-SnWO4 is therefore solar-responsive,and a chopped light linear sweep voltammogram recorded under 100 m W/cm2AM1.5 simulated solar illumination in a p H 50.1 mol/L KPibuffer show a visible light response for photoelectrochemical water oxidation,producing32 m A/cm2 at 1.23 V vs.RHE.     

液相球化法合成新型正极材料磷酸钒锂

A novel cathode material lithium vanadium phosphate with the microstructure of submicro-particles aggregate was synthesized by liquid-phase sphericizing granulation. XRD pattern showed that the crystal structure of Li3V2(PO4)3 was monoclinic and belonged to P21/n space group. SEM revealed that the diameters of the particle and aggregated particle were in submicron range and about 10 滋m, respectively, with a narrowdistribution. The electrochemical testing showed that the obtained Li3V2(PO4)3 had the maximum discharge capacity of 126.67 mAh·g-1 and initial coulombic efficiency of 95.6%in the range of 3.0-4.3 V (vs Li/Li+), and 170.47mAh·g-1 and 97.5%in the range of 3.0-4.9 V (vs Li/Li+) at a density of 55.6 mA·g-1, respectively. Moreover, the material had a better cycle stability.     

Layer Zirconogermanate——(H_2DETA)[ZrGe_3O_8F_2] Showing Odd 3MR and 7MR

A layered zirconogermanate,(H2DETA)[ZrGe3O8F2](1),was hydro(solvo)thermally synthesized with diethylenetriamine(DETA) as template,and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallized in the monoclinic space group P21/c with data of unit cell:a=0.7644(2) nm,b=1.1235(2) nm,c=1.6860(3) nm,V=1.4479(5) nm3,μ(Mo Kα)=6.931 mm-1,Z=4,R1=0.0402 for 3236 reflections with Fo>2σ(Fo). The structure of compound 1 was formed by alternatively packing the inorganic layer of ZrGe3O8F2 and H...     

斯蒂芬酸氢铷的制备，晶体结构和热分解机理

A new compound,[RbHTNR]_∞[HTNR:C_6H(NO_2)_3(OH)O],was synthesized by the reaction of rubidium ni-trate and styphnic acid.The molecular structure was characterized using X-ray diffraction analysis,elementalanalysis and FTIR spectroscopy.The crystalline is monoclinic with space group P2_1/n and the empirical formulaC_6H_2N_3O_8Rb.The unit cell parameters are:a=0.4525 nm,b=1.0777 nm,c=1.9834 nm,β=90.47(2)°,V=0.96725 nm~3,Z=4,D_c=2.263 g/cm~3,Mr=329.58,F(000)=640,μ(Mo Kα)=5.165 mm~(-1).The thermal decompo-sition mechanism of the complex was studied by differential scanning calorimetry(DSC),thermogravimetry-derivative thermogravimetry(TG-DTG)and FTIR techniques.At the linear rate of 10 ℃/min,the thermaldecomposition of the complex showed three mass reducing processes between 60 and 500 ℃,and finally evolvedRbCN and some gaseous products.     

超细CaCO_3的粒子尺寸对PP结晶行为的影响

The effects of CaCO3 on the crystallization behavior of polypropylene (PP) were studied by means of DSC and WAXD.The average sizes of the CaCO3 powders used were 0.1μm (UC) and 0.5μm (GC),respectively.The PP/CaCO3 composites at compositions of 1phr and 10 phr were investigated.The results showed that the addition of CaCO3 reduced the supercooling,the rate of nucleation and the overall rate of crystallization (except for the 10phr UC/PP sample).The crystallinity of PP was increased and the size distribution of the crystallites of α-PP was broadened.On the other hand,the crystallization rate of 10phr UC/PP is 1.5 times higher than that of neat PP.It has an overall rate of crystallization 2 times as much as that of the neat PP and has the maximum crystallinity.The sizes of crystallites and the unit cell parameters of α-PP were varied by the addition of CaCO3.β-PP was formed by addition of GC and was not detected by addition of UC.The differences of crystallization behaviors of PP might be attributed to the combined effects of the content and size of CaCO3 filled.     

Study of CO2 Hydrogenation to Methanol over Cu-V/γ-Al2O3 Catalyst

The effect of vanadium addition to CU/γ-Al2O3 catalyst used in the hydrogenation of CO2 to produce methanol was studied. It was found that the catalytic performance of the Cu-based catalyst improved after V addition. The influence of reaction temperature, space velocity and the molar ratio of H2 to CO2 on the performance of 12%Cu-6%V/γ-Al2O3 catalyst were also studied. The results indicated that the best conditions for reaction were as follows: 240℃, 3600 h-1 and a molar ratio of H2 to CO2 of 3:1. The results of XRD and TPR characterization demonstrated that the addition of V enhanced the dispersion of the supported CuO species, which resulted in the enhanced catalytic performance of CU-V/γ-Al2O3 binary catalyst.