稀土、2,2''''-联吡啶、邻氨基苯基苯甲酸配合物合成、光谱表征及荧光性质

2,2'-联吡啶(bipy)、邻氨基苯基苯甲酸(HL)与稀土离子(RE=Tb,Eu,Sm,Nd)合成了固体稀土配合物.用元素分析、摩尔电导、紫外光谱、红外光谱、差热-热重分析和荧光光谱,对配合物的组成进行了确定和表征,并对TbL3和TbL3·bipy·3H2O的荧光性能进行了测试和讨论.TbL3·bipy·3H2O的荧光强度比TbL3的荧光强度强.     

Self-assembly behaviour of amphiphilic diblock copolymer in selective solvents studied by synchrotron small-angle x-ray scattering

The aggregation behaviour of styrene-vinyl benzoic acid (PSm-b-PVBAn) amphiphilic diblock copolymers in selective solvents with different m and n was investigated by synchrotron small-angle x-ray scattering (SAXS). We have carried out a detailed analysis of scattering intensity, dimension, shape and microstructure of the diblock copolymers of narrow distribution in water, methanol, ethanol and isopropanol selective solvents, respectively. We have found that the aggregation behaviour of the copolymer depends on the nature of the solvent and the micelle forms fiat disc objects with the ratio of radius ω=0.4. The average radius gyration Rg of the copolymer decreases as solvents change from isopropanol to ethanol and to methanol, and increases with increasing pH in aqueous solution, but decreases with the addition of COCl2 in ethanol solvent. The scattering intensity of diblock copolymer micelle follows I(h) ∝ h^-α in different selective solutions, suggesting that the PSm-b-PVBAn coils have self-similar structure behaviour or a fractal structure in the selective solvents. All of these revealed that the aggregation behaviour of the diblock copolymer changes dramatically with experimental condition in the selective solvent. The increase of mass fractal dimension (Dm) from 2.12 to 2.47 indicates that the copolymer chain changes from a swollen coil to a rather compact disc in the course of changing solvents, decreasing surface fractal dimension (Ds) from 2.98 to 2.58 indicates that the copolymer micelle change from a rather rough surface to a smooth form in the course of increasing pH in aqueous solutions, and increasing Dm and Ds from 2.29 to 2.35 and 2.70 to 2.90, respectively, indicates the shrinkage of copolymer micelle to a rather compact and rough disc form by adding COCl2 in ethanol solvents.     

苝二酸酐与嘧啶衍生物的氢键组装

用半经验AM1方法对苝二酸酐与嘧啶衍生物的1:1及1:2氢键复合物进行理论研究,表明随着氢键数目增多,弱相互作用能变大,主体上的供电基和客体上的吸电基有利于氢键相互作用,氢键导致电子从主体流向客体.用INDO/SCI方法计算配合物的电子光谱,表明其长波吸收峰与主体相比发生兰移,各配合物的长波吸收峰位置相差不大,与实验一致.讨论吸收峰兰移的原因并对电子跃迁进行理论指认,同时得到了配合物的双质子转移势能曲线,给出了相对于N-H键的过渡态和活化能.     

Ni（Ⅱ）—MOBTAMB—TritonX—100体系析相光度法测定痕量镍

研究了Triton X-100在浊点条件下,对Ni(Ⅱ)-2-[2′-(6′-甲氧基-苯并噻唑)偶氮]-5-二甲氨基苯甲酸(MOBTAMB)配合物的析相条件。在pH 8.6～9.5的氨-氧化铵缓冲体系中,90℃水浴加热1.5h,析相完全。配合物最大吸收峰位于658nm处,表观摩尔吸光系数为5.5×10~5。镍含量在0～3μg/30ml范围内符合比耳定律。所拟方法用于天然水中的痕量镍测定,结果满意。     

配合物LaL3.H2O的合成及表征

本文以３－甲基苯甲酸为配体，合成了与三价稀土镧离子的固体配合物ＬａＬ３．Ｈ２Ｏ，并对该配合物进行了元素分析，红外光谱，ＵＶ光谱，ＴＧ－ＤＴＡ，ＨＮＭＲ等的测试与表征。该配合物属螯合双齿配位。     

卡尔曼滤波紫外光度法同时测定酱油、食醋中的山梨酸和苯甲酸

在酸性条件下，采用乙酸乙酯萃取、Na2HPO4溶液反萃取分离酱汪、食醋中的山梨酸、苯甲酸，卡尔曼滤波法计算结果，并与比值导数波谱法进行比较。结果表明，卡尔曼滤波法较地数波谱法有较高准确度和精密度，并能监测干扰物质存在与否。用于实际样品分析有更高的可靠性。