二(三苯基膦)水杨酸铜(Ⅰ)乙醇溶剂配合物的晶体结构

0IntroductionThestudyofcopper?complexesisinvestigatedinmanylaboratories.Amongthereasonsforcarryingouttheinvestigationofsuchspeciesaretheirstructuralfeatures犤1犦,theusefulnessofcopper?compoundsinorganicsyntheses犤2犦andthewell-documentedimpor-tanceofcopper?centersattheactivesitesofanumberofprotein犤3犦.Concerningcopper?carboxy-latesafurtherinterestexists,stemmingfromtheiruseinhomogeheouscatalysedhydrogenation犤4犦.Thecopper?bis(triphenylphosphine)cationisasoft,butflexi-bleacceptorionthatcanacc…     

甲胺磷离子选择性电极的研制及其应用

以四苯硼钠与甲胺磷在盐酸介质中生成的离子缔合物为电活性物质,首次研制出一种甲胺磷PVC涂层玻璃电极。并对该电极的响应机理及性能进行了研究。实验表明,该电极的Nernst响应范围为1×10-2~1×10-4(φ),斜率为50.28 mV/pφ。该电极响应迅速,重复性好,用于蔬菜中残留甲胺磷的测定,方法快速、准确,结果满意。     

固相萃取-气相色谱-串联质谱法同时测定人体尿液中4种有机磷农药代谢物

建立了同时测定尿液中4种有机磷类农药代谢物的气相色谱/串联质谱分析方法.尿液样品以WCX固相萃取柱富集提取,乙酸乙酯-乙腈(70∶30,V/V)再萃取,浓缩干燥,甲苯溶解,N-叔丁基二甲基甲硅烷基-N-甲基三氟乙酰胺衍生化.采用HP-5MS色谱柱(30 m×0.25 mm×0.25 μm)程序升温分离,串联质谱多反应检测,内标法定量.通过比较尿样中代谢物在不同萃取溶剂、固相萃取柱及pH值洗脱液等条件下的回收率,优化了前处理方法.在0.2～ 200 μg/L范围内,4种代谢物峰面积与内标峰面积的比值与质量浓度的线性关系良好(R2≥0.992),方法检出限为0.083 ～0.667μg/L,定量限为0.2～2.0 μg/L,平均回收率为54.1％～68.6％,相对标准偏差均小于8.5％(n=6).本方法稳定、可靠,分析时间短,不需要使用大量有机溶剂,可同时处理大批量样品,适用于人群有机磷类农药暴露情况的评估.     

Density Functional Calculations on a Double Hydrogen-bonded Dimer

Density functional theory (DFT) calculations on a double hydrogen-bonded dimer of o-hydroxybenzoic acid were carried out at the B3LYP/6-31G^* level. The optimized geometry of the dimer closely resembles that of the crystal. The calculated results show that the total energy of the dimer is much lower than the sum energies of the two monomers, and the average strength of the double hydrogen bonds is about 38.37 kJ/mol. In order to probe the origin of the interactions in the dimer, natural bond orbital analyses were performed. The thermodynamic properties of the title compound at different temperatures have also been calculated on the basis of vibrational analyses and ΔGT, the change of Gibbs free energy for the aggregation from monomer to the dimmer, is 26.47 kJ/mol at 298.15 K and 0.1MPa, implying the spontaneous process of forming the dimer. The correlation graphics of Sm^0 Hm^0 and temperatures is depicted.     

钛硅沸石分子筛TiMCM-41的微波合成与表征

ＭＣＭ４１分子筛是一类以表面活性剂季铵碱或季铵盐为模板剂,液晶模板机理合成,孔道六方有序排列,孔径大小可在１６～１０ｎｍ范围内调节的新颖中孔硅铝分子筛材料．在多相催化、离子交换、吸附分离以及高等无机材料等领域具有较高的工程应用与学术研究价值［１］...     

傅立叶变换离子回旋共振质谱进展

综述了傅立叶变换离子回旋共振质谱（ＦＴＩＣＲＭＳ）仪器特点和各种新技术。主要对紫外光解离技术、红外多光子解离技术、表面诱导解离、黑体红外辐射离、电子捕获解离等离子解离新方法进行了介绍。此外,应用多次激发碰撞活化技术、超低能量激发技术、持续偏共振激发、存储波形逆傅立叶变换技术等离子再测量技术能提高源内离子碰撞诱导解离效率,更好的实现ＭＳ＾n的产技术。文章最后阐述了ＦＴＭＳ在生物分析及气相分子离子反应     

聚苯胺纳米纤维的共溶剂界面聚合及储能性能研究

本文采用以盐酸溶液为水相、四氯化碳为有机相的界面聚合法,通过向水相中分别引入具有非对称结构的甲醇和乙醇,以及具有对称结构的异丙醇和丙三醇作为共溶剂,成功制备出聚苯胺纳米纤维.采用场发射扫描电镜、紫外可见光谱和傅里叶红外光谱对其形貌和结构进行了表征分析,并通过循环伏安测试、恒流充放电测试和交流阻抗测试着重研究了不同共溶剂...     

一维链状配位聚合物[Cd(N-MeIM)2(SCN)2]n的结构表征和电化学性能研究(英)

A novel cadmium(Ⅱ) isothiocyanate complex [Cd(N-MeIM)₂(SCN)₂]_n(N-MeIM=N-methylimidazole) has been prepared and characterized by spectroscopic analysis and crystallographic method. The title compound crystallize in the Triclinic system, space group P1, with lattice parameters a=0.589 50(12) nm, b=0.785 70(16) nm, c=0.882 00(18) nm, α=110.98(3)°, β=106.49(3)°, γ=95.08(3)°, and Z=1. The title compound exhibits an infinite chain structure in which each pair of Cd atoms is bridged by two η-1,3-SCN^- groups. The unique Cd atom lies on an inversion centre and the coordination sphere is completed by two N-MeIM N atoms to form a CdS₂N₄ octahedron. The polymeric chains are further extended into three-dimensional network via π…π stackings interactions between the imidazole rings. The cyclic voltammetry behaviors of the compound on glass carbon electrode showed a typical irreversible process. CCDC: 265283.     

[1-芳基甲羰基-2-(1,2,4-三唑-1-基)]乙基-N,N-二烷基二硫代氨基甲酸酯衍生物的合成、结构表征及生物活性研究

以芳香基三唑类杀菌剂三唑酮为先导物设计并合成了5个含N,N-二烷基二硫代氨基甲酸酯的芳香三唑类化合物, 通过元素分析、红外光谱、核磁共振氢谱和质谱对其结构进行了表征. 用X射线单晶衍射测定了[α-(4-甲氧基苯甲酰基)-2-(1,2,4-三唑-1-基)]乙基-N,N-二甲基二硫代氨基甲酸酯的晶体结构, 晶体属于三斜晶系, 空间群, 晶胞参数为: a＝0.73482(15) nm, b＝1.1051(2) nm, c＝1.1209(2) nm, α＝90.32(3)°, β＝101.97(3)°, γ＝105.13(3)°, V＝0.8578(3) nm³, Z＝2, D_c＝1.357 g/cm³, F(000)＝368, µ＝0.324 mm^－1. 生物测试结果显示这5种有机化合物都具有杀菌性和植物生长调节活性