Preparation,Structure, Photoluminescence and Energy Transfer Mechanism of a Novel Holmium Complex

A novel holmium complex [Ho(HIA)_2(H_2O)_4(NO_3)](NO_3)_2(1, HIA = isonicotinic acid) has been synthesized through hydrothermal reactions and characterized by single-crystal X-ray diffraction. Complex 1 crystallizes in the C2/c space group of monoclinic system: a = 14.4797(7), b = 12.4768(2), c = 13.3471(5) ?, β = 118.690(4)°, V = 2115.26(13) ?~3, C_(12)H_(16)HoN_5O_(17), Mr = 667.23, Z = 4, Dc = 2.095 g/cm~3, μ(Mo Kα) = 3.838 mm~(–1) and F(000) = 1304. The crystal structure of 1 is characterized by an isolated structure. Solid-state photoluminescence experiment uncovers that it shows yellow light emission. The emission bands are originated from the characteristic emission of the 4 f electrons intrashell transition of the ~5S_2 → ~5I_8 and ~5F_5 → ~5I_8 of the Ho~(3+) ions. Energy transfer mechanism is explained by the energy level diagram of the Ho3+ ion and the isonicotinic acid ligand. It has remarkable CIE chromaticity coordinates of(0.4929, 0.4632), so it may be a promising color converter for lighting and displays.     

甲基二氯硅烷-甲基乙烯基二氯硅烷二元体系等压汽液平衡

利用新型泵式沸点仪,在１０１．３ｋＰａ下测定了甲基二氯硅烷－甲基乙烯基二氯硅烷二元体系液相平衡数据,同时,对甲基乙烯基二氯硅烷的临界性质进行了估算。分别用Ｍａｒｇｕｌｅｓ,ＶａｎＬａａｒ,Ｗｉｌｓｏｎ和ＮＲＴＬ模型进行了关联,结果令人满意。     

[N-ethyl-4,4'-bipyridinium][ZnX_4](X = Cl or Br) with N-ethyl-4,4'-bipyridinium Generated In Situ:Syntheses,Structures, Fluorescence and TDDFT Calculations

Two new zinc bipyridinium compounds, [N-ethyl-4,4′-bipyridinium][ZnX4](X = Cl(1) or Br(2)) with N-ethyl-4,4′-bipyridinium generated in situ, have been synthesized through solvothermal reactions and structurally characterized by single-crystal X-ray diffraction analyses. Both compounds are isostructural and crystallize in the P21/c space group of monoclinic system. Compound 1: a = 8.4397(5), b = 21.988(1), c = 8.8777(5) , β = 106.490(1)°, V = 1579.7(2) 3, C12H15Cl4N2 Zn, Mr = 394.43, Z = 4, Dc = 1.658 g/cm3, S = 1.068, μ(MoKα) = 2.218 mm-1, F(000) = 796, R = 0.0295 and wR = 0.0766. Compound 2: a = 8.4154(6), b = 22.844(2), c = 9.0308(7) , β = 106.026(1)°, V = 1668.6(2) 3, C12H15Br4N2 Zn, Mr = 572.27, Z = 4, Dc = 2.278 g/cm3, S = 1.033, μ(MoKα) = 11.038 mm-1, F(000) = 1084, R = 0.0427 and wR = 0.1175. Both of them are characteristic of an isolated structure with the zinc atoms locating at a tetrahedral environment. In both compounds, the N-ethyl-4,4′-bipyridinium2+ cations and ZnX42– anions interconnect together via hydrogen bonding interactions to construct a three-dimensional(3-D) supramolecular framework. Fluorescent studies reveal that both compounds exhibit a strong emission in the green region. In combination with the theoretical calculations, we can draw a conclusion that the emissions should result from ligand-toligand charge-transfer(LLCT) transition.     

甲基三氯硅烷——甲基三乙氧基硅烷二元体系等压汽液平衡研究

利用新型泵式沸点仪，在101．3kPa下测定了甲基三氯硅烷－甲基三乙氧基硅烷二元体系汽液平衡数据，对甲基三乙氧基硅烷的临界性质进行了估算，分别用Wilson,NRTL,Margules,Van Laar四种模型对所测数据进行了关联，结果令人满意。     

人工神经网络光致发光法同时测定α-萘乙酸和吲哚-3-乙酸

研究了酸度、有机溶剂、重原子效应和共存物对α-萘乙酸(NAA)及吲哚-3-乙酸(IAA)光致发光性质的影响,建立了人工神经网络不经分离同时测定NAA和IAA的新方法。该法测定NAA和IAA的线性范围分别是0.012~0.24 mg.L-1和0.0034~0.068 mg.L-1(荧光)0、.18~1.8 mg.L-1和0.18~1.8 mg.L-1(燐光),检出限分别为0.0039 mg.L-1和0.0019 mg.L-1(荧光)0、.14 mg.L-1和0.13 mg.L-1(燐光)。方法用于合成样和水样测定,回收率在93%~109%之间,结果满意。     

基于外腔压缩的2μm耗散孤子光纤激光器

研究了2μm掺Tm耗散孤子光纤激光器在大能量下产生的调制不稳定性,通过计算耗散孤子锁模的动力学过程,分析高峰值功率条件下非线性效应对光脉冲特性的影响.通过在环形腔内引入色散补偿光纤和增大模场半径的方式增大腔内净正色散、减小腔内自相位调制效应.针对输出光脉冲线性啁啾较大的特点,采用46.83m的大模场光纤对输出光脉冲进行腔外压缩,最终得到了峰值功率为17.1kW、脉冲宽度为169fs的稳定光脉冲输出.     

乙醇-K2HPO4-KH2PO4双水相萃取固体基质室温燐光法测定色氨酸

提出了一种基于乙醇-电解质-水体系双水相萃取、固体基质室温燐光法(SS-RTP)测定色氨酸的新方法:将适量电解质和乙醇加入试液中,离心后用SS-RTP测定上相中的色氨酸.在最佳萃取体系乙醇-K2HPO4-KH2PO4-H2O中,测定色氨酸的线性范围1.0×10-7～2.0×10-6mol/L、检出限5.4×10-9mol/L(S/N=3).用于大豆、大米、玉米和竹笋中色氨酸的测定,相对标准偏差2.2%～3.3%,与荧光法比较,相对误差-3.3%～3.2%.     

高效液相色谱法同时测定化妆品中7种禁用植物原料标志性成分

建立高效液相色谱法同时测定化妆品的巴豆苷、苦杏仁苷、花椒毒素、狼毒乙素、马兜铃酸、欧前胡素、土木香内酯7种化合物。采用资生堂CAPCELL PAK MG C₁₈柱(250 mm×4.6 mm,5μm),以乙腈-0.05%磷酸为流动相梯度洗脱,流量为1 mL/min,进样体积为10μL,柱温为30℃,采用二极管阵列检测器,在210 nm波长处测定。7种化合物在所测浓度范围内有良好的线性关系,相关系数均大于0.999,平均回收率为90.0%～105.0%,测定结果的相对标准偏差为0.3%～2.8%(n=6),方法检出限为0.02～0.17μg/g。该方法可以高效、准确的检测化妆品中7种禁用植物原料的标志性成分。     

A New 3-D Lanthanide Porphyrin: Synthesis,Structure and Photophysical Properties

A new lanthanide porphyrin, [Sm III(H3TPPSIII)]n·n H2O(1, H6 TPPS = tetra(4-sulfonatophenyl)porphyrin), has been synthesized through a hydrothermal reaction and structurally characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the P4/mcc space group of tetragonal system: a = 15.3683(12), c = 9.895(2) A, V = 2337.0(5) A3, C44H29N4O13S4 Sm, Mr =1100.30, Z = 2, Dc = 1.564 g/cm3, S = 1.063, μ(Mo Kα) = 1.502 mm–1, F(000) = 1102, R = 0.0583 and w R = 0.1666. Compound 1 is characteristic of a three-dimensional(3-D) framework with a slightly distorted square-antiprism eight-coordinated Sm3+ ion. Fluorescent study revealed that compound 1exhibits an emission in the red region. The fluorescence quantum yield and lifetime of 1 were determined to be 3.5% and 9.1 ns, respectively. UV-vis absorption spectra were also investigated.     

甲醇-甲基三甲氧基硅烷二元体系等压汽液平衡

利用新型泵式沸点仪，建立了一套恒压装置，在101．3kPa下测定了甲醇-甲基三甲氧基硅烷二元体系的汽液平衡数据，同时测定了甲基三甲氧基硅烷不同温度下的饱和蒸汽压，回归了它的Antoine常数，并对甲基三甲氧基硅烷的临界性质进行了估算。用Wilson、NRTL、Margules、Van Laar方程分别对所测数据进行了关联，结果良好。