Synthesis and luminescent properties of ternary complex Eu(UVA)3Phen in nano-TiO2

By introducing 2-hydroxy-4-methoxy-benzophenone(UVA) and 1,10-phenanthroline(Phen) as the ligands, the ternary rare earth complex of Eu(UVA)3Phen is synthesized, and it is characterized by elemental analysis, mass spectra(MS) and infrared(IR) and ultraviolet(UV) spectroscopy. Results show that the Eu(III) in complex emits strong red luminescence when it is excited by UV light, and it has higher sensitized luminescent efficiency and longer lifetime. The organic-inorganic thin film of complex Eu(UVA)3Phen doped with nano-Ti O2 is prepared, and the nano-Ti O2 is used in the luminescence layer to change the luminescence property of Eu(UVA)3Phen. It is found that there is an efficient energy transfer process between ligands and metal ions. Moreover, in an indium tin oxide(ITO)/poly(N-vinylcar-bazole)(PVK)/Eu(UVA)3Phen/Al device, Eu3+ can be excited by intramolecular ligand-to-metal energy transfer process. The main peak of emission at 613 nm is attributed to 5D0→7F2 transition of the Eu3+, and this process results in the enhanced red emission.     

Two-dimensional Lanthanide Coordination Polymers Constructed from Ce3＋/pr3＋ Cation, Imidazole-4,5- dicarboxylate and in situ Generated Oxalate Anions

Two new lanthanide coordination polymers [Ln(C 5 H 2 N 2 O 4)(H 2 O) 2 (C 2 O 4) 0.5 ] n nH 2 O (Ln=Ce III (1) or Pr III (2);C 5 H 2 N 2 O 4=imidazole-4,5-dicarboxylate anion;C 2 O 4=oxalate anion) have been synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses and IR spectrum.Both compounds crystallize in monoclinic,space group P2 1 /c with a=7.5225(3),b=17.2416(6),c=8.6089(3),β=110.9610(10)°,V=1042.68(7)3,Z=4,C 6 H 8 N 2 O 9 Ce,M r=392.26,D c=2.499 g/cm 3,μ(MoKα)=4.414 mm 1,F(000)=752,the final R=0.0167 and wR=0.0412 for 1;a=7.4973(3),b=17.2113(8),c=8.5729(4),β=110.9440(10)°,V=1033.14(8)3,Z=4,C 6 H 8 N 2 O 9 Pr,M r=393.05,D c=2.527 g/cm 3,μ(MoKα)=4.764 mm 1,F(000)=756,the final R=0.0192 and wR=0.0455 for 2.X-ray diffraction analyses reveal that the lanthanide cations in compound 1 or 2 are linked by imidazole-4,5-dicarboxylate and in situ generated oxalate anions via Ln-O and Ln-N covalent bonds to form two-dimensional layered networks.The successful synthesis of compound 1 or 2 also indicates a crystallographic confirmation for the decomposition of curcumin to form oxalate anion under solvothermal conditions.     

尿素-水混合溶剂中硫酸热力学性质的研究

本文应用电动势法测定下面无液接电池在278．15-318．15K温度范围内的电动势。     

气相色谱法测定1-(5-溴-1H-吲唑-1-基)乙酮

建立了测定1-(5-溴-1H-吲唑-1-基)乙酮纯度的气相色谱法。采用DB–5型色谱柱,程序升温,火焰光度检测器,外标法定量,1-(5-溴-1H-吲唑-1-基)乙酮在100~1 000 mg/L范围内内线性关系良好,检出限为0.01mg/L。测定结果的相对标准偏差为1.67%~1.89%(n=5),样品加标回收率为98.1%~107.9%。用该方法测定了自制的1-(5-溴-1H-吲唑-1-基)乙酮样品的纯度。该测定方法准确度高、专属性较强且灵敏度较高,适用于1-(5-溴-1H-吲唑-1-基)乙酮的质量控制。     

吸收光谱法同时检测食品中的苯甲酸钠与山梨酸钾

利用苯甲酸钠和山梨酸钾的紫外吸收光谱特性,设计了正交试验,结合偏最小二乘变量筛选法,获得变量数少、相关系数高、预报准确性好、能同时对苯甲酸钠和山梨酸钾进行浓度预报的模型,并应用于饮料、蜜饯、糕点和调色酒样品中苯甲酸钠和山梨酸钾的检测。样品平行测定结果的相对标准偏差均小于10%,方法的加标回收率为82%～107%,苯甲酸钠和山梨酸钾的检测范围分别为0.1～16.0 mg.L-1和0.1～6.0 mg.L-1,检出限分别为0.05 mg.L-1和0.01 mg.L-1。样品的检测结果与国标法的检测结果相吻合。     

托特罗定氢溴酸盐的合成

以对甲酚和肉桂酸为起始原料，经脱水、环合、水解、还原、酯化及胺化等反应合成托特罗定氢溴酸盐，结构经^1H NMR和EI-MS进行确证．总收率为63％，此方法成本低廉，工艺安全简便，利于工业化生产．