大尺寸NaI（T1）晶体的热锻及封装

本文在讨论了NaI(T1)晶体热锻及封装机理和工艺的基础上，对大尺寸NaI(T1)晶体的热锻及封装的工艺作了详细地研究，并成功地制备了各项性能指标的大尺寸NaI(T1)晶体闪烁探测器。     

一维链状钴配位聚合物{[CO(4,4'-bipy)(C9H8O3N)2](H2O)4}n的溶剂热合成、晶体结构及热稳定性

芳香羧酸与金属离子构筑的配合物在材料、药物、分子电化学、生物化学、生物制药等许多领域中表现出了潜在的应用价值,芳香羧酸配合物的合成与结构研究一直是人们关注的热点课题之一[1-3].     

温度对Zn(II)-TiO2体系吸附可逆性的影响

用延展X射线吸收精细结构光谱(EXAFS)研究了不同温度对Zn(II)-锐钛矿型TiO2吸附产物微观构型和吸附可逆性的影响机制. 宏观的吸附-解吸实验表明, 不同温度下的吸附等温线可以用Langmuir 模型进行较好的描述(R2≥0.990). 随温度升高, 吸附等温线显著升高, Zn(II)在TiO2表面的饱和吸附量由5 ℃时的0.125 mmol·g-1增至40 ℃时的0.446 mmol·g-1; 而体系的不可逆性明显减弱, 解吸滞后角θ由32.85°减至8.64°. 求得体系反应的热力学参数⊿H、⊿S分别为24.55 kJ·mol-1 和159.13 J·mol-1·K-1. EXAFS结果表明, Zn(II)主要是通过共用水合Zn(II)离子及TiO2表面上的O原子结合到TiO2表面上,其平均Zn-O原子间距为RZn-O=(0.199±0.001) nm. 第二配位层(Zn-Ti 层)的EXAFS图谱分析结果表明, 存在两个典型的Zn-Ti 原子间距, 即R1=(0.325±0.001) nm (边-边结合的强吸附)和R2=(0.369±0.001) nm(角-角结合的弱吸附). 随温度升高, 强吸附比例(CN1)基本不变而弱吸附比例(CN2)增加, 两者比值(CN1/CN2)逐渐减小. 该比值的变化从微观角度解释了宏观实验中温度升高, 不可逆性减弱的吸附现象.     

2D氢键网络镍配合物｛[Ni(4,4′-bipy)(H_2O)_4]·(α-furacrylic acid)_2·(H_2O)｝_n的水热合成、晶体结构及电化学性质

配位聚合物由于在催化材料、磁性材料和光学材料等领域中具有广泛的应用价值,近年来已引起人们的极大关注。含氮、含氧桥联配体是合成具有     

配合物[Cu(PTA)(phen)2]·(PTA)·(H2O)4的合成、晶体结构及电化学性质

The title complex has been synthesized by using terephthalic acid (PTA), 1,10-phenanthroline (phen) and copper monohydrate. It crystallizes in monoclinic space group C2/c with a=2.959 0(2) nm, b=1.466 4(10) nm, c=1.764 3(12) nm, β=105.593(11)°, V=7.372(9) nm³, Dc=1.489 g·cm^-3, Z=8, F(000)=3 416, R₁=0.043 6, wR₂= 0.151 9. The crystal structure shows that the copper atom is coordinated with four nitrogen atoms from two phens and one oxygen atom from one terephthalic acid, forming a distorted square-pyramid coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 277047.     

{[Co(4，4′-bipy)(H2O)4]·(α-Furacrylic acid)2·(H2O)}n的水热合成、晶体结构及电化学分析

A complex {[Co(4,4′-bipy)(H₂O)₄]·(α-Furacrylic acid)₂·(H₂O)}_n with α-furacrylic acid, 4,4′-bipy and cobaltous chloride hexahydrate has been synthesized by means of hydrothermal way and characterized. Crystal data for this complex: monoclinic, space group P2₁/c, a=1.147 0(2) nm, b=1.099 9(2) nm, c=1.111 1(2) nm, β=97.829(3)°, V=1.388 7(5) nm³, D_c=1.429 g·cm^-3, Z=2, μ(Mo Kα)=0.682 mm^-1, F(000)=622, S=1.025, R₁=0.035 8, wR₂=0.086 1. The crystal structure shows that the cobalt(Ⅱ) ion is coordinated with two nitrogen atoms of two 4,4′-bipy molecules and four oxygen atoms from four water molecules, respectively, giving a distorted octahedral coordination geometry. Adjacent cobalt(Ⅱ) ions are bridged by 4,4′-bipy groups, resulting in a 1D chain structure. The adjacent Co(Ⅱ)-Co(Ⅱ) distance is 1.147 0 nm. The cobalt(Ⅱ) ion isn′ t coordinated with α-Furacrylic acid. The complex molecules form 2D structure through hydrogen bonds. The cyclic voltametric behavior of the complex was also investigated. CCDC: 648243.     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Mn2（phen）2（p-CBA）4（H2O）

One novel complex Mn2(phen)2(p-CBA)4(H2O) has been hydrothermally syn- thesized from p-chlorobenzoic acid (p-CBA), 1,10-phenanthroline (phen) and anhydrous man- ganese(Ⅱ) sulfate and then characterized. Crystal data for this complex: monoclinic, space group C2/c, with a = 2.3416(3), b = 1.5604(2), c =1.5605(2) nm, β = 121.048(2)o, V = 4.8849(12) nm3, Dc = 1.510 g/cm3, Mr = 555.26, Z = 8, μ = 0.798 mm-1, F(000) = 2256, GOOF = 1.032, the final R = 0.0393 and wR = 0.0816. The crystal structure shows that two neighboring manganese(Ⅱ ) ions are linked together by two bridge-chelating p-chlorobenzoic groups and one bridging water molecule, forming a cage structure with the Mn–Mn bond distance of 0.3512 nm. Each manganese(Ⅱ ) ion is coordinated by two nitrogen atoms of one 1,10-phenanthroline molecule and four oxygen atoms from three p-chlorobenzoic acid anions and one water molecule, giving a distorted octahedral coordination geometry. The cyclic voltammetric behavior of the complex was also investigated.     

Solvothermal Synthesis,Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)_2(2,2′-bipy)(H_2O)]·(H_2O)

One novel complex [Co(p-MBA)2(2,2′-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2′-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic,space group P1 with a=0.70479(14),b=1.1211(2),c=1.6718(3) nm,α=103.806(3),β=90.795(3),γ=104.207(3)o,V=1.2399(4) nm3,Mr=512.41,Dc=1.373 g/cm3,Z=2,F(000)=532,μ=0.733 mm-1,R= 0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2′-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

一维链状锰配位聚合物[Mn(3,5-Me2PhCO2)2(phen)]n的合成与晶体结构

A manganese coordination polymer [Mn(3,5-Me₂PhCO₂)₂(phen)]_n(phen=1,10-phenanthroline) has been synthesized by hydrothermal methods. The crystal structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with a=0.770 3(4) nm, b=1.145 2(6) nm, c=1.537 0(9) nm, α=78.182(9)°, β=77.170(9)°, γ=89.784(9)°, V=1.292 8(12) nm³, Z=2, M_r=533.47, D_c=1.370 g·cm^-3, μ=0.549 mm^-1, F(000)=554, R_int=0.043 4, R=0.060 8 ,wR=0.148 4. In the crystal the manganese atom is six-coordinated by two nitrogen atoms from phen and four oxygen atoms from four 3,5-dimethylbenzolate molecules, completing an octahedral geometry. And the title complex forms one-dimensional chain structure through bridging 3,5-dimethylbenzolate molecules. CCDC: 642920.     

梨果及土壤中亚胺唑及其代谢物的气相色谱分析

介绍了杀菌剂亚胺唑及其代谢物ＩＢＣ－０１在梨果实及土壤样品内的提取、净化方法以及气相色谱的分析测定方法。保留时间：亚胺唑为３８．３６ｍｉｎ，ＩＢＣ－０１为１７．０１ｍｉｎ。变异系数：亚胺唑为０．４５％～１５．５３％，ＩＢＣ－０１为３．０３％～９．５２％。回收率：亚胺唑为８８．２８％～９８．５％，ＩＢＣ－０１为８４．９８％～９８．１３％。