Synthesis,Structure and Thermal Property of a Cobalt Supramolecular Complex Containing N-[（4-Carboxyphenyl）-sulfonyl]glycine

Utilizing N-[(4-carboxyphenyl)-sulfonyl]glycine (abbreviated as cbsglyH3),a new cobalt complex [Co(cbsglyH)(bipy)2]3H2O (bipy = 2,2'-bipyridine) has been synthesized under mild conditions and characterized by IR,elemental analysis,thermogravimetric analysis and X-ray diffraction analysis. It crystallizes in the monoclinic system,space group C2/c with a = 34.978(3),b = 12.0437(11),c = 20.0041(19) ,β = 122.2990(10)°,V = 7123.0(11) 3,Z = 8,C29H28CoN5O9S,Mr = 681.55,μ = 0.593 mm-1,Dc = 1.271 Kg/m3,F(000) = 2816,the final R = 0.0434 and wR = 0.1351. The title complex is a monomeric compound which is further assembled by intermolecular hydrogen bonds into a 3-D supramolecular network. Thermogravimetric analysis illustrates that this complex begins decomposing at 100 ℃ and decompounding completely at 560 ℃.     

A New Supramolecular Compound Based on Cd（II）-Schiff-base and Keggin-type [PMo_（12）O_（40）]~3

A new supramolecular compound, {[Cd(L)2]2[PMo12O40NO3]·CH3CN·2H2O}n 1 (L is 1,4-bis(4-imidazolyl)-2,3-diaza-1,3-butadiene), based on Cd(II)-Schiff-base and Keggin- type [PMo12O40]3- was synthesized via self-assembly and structurally characterized by elemental analysis, infrared spectroscopy, and single-crystal X-ray diffraction analysis. The crystal is of triclinic, space group P1 with a = 12.0128(11), b = 13.6196(13), c = 13.9995(13) , α = 103.868(2), β = 95.225(2), γ = 101.024(2)°, V = 2160.0(3) 3, Z = 1, C34H39N26O45Cd2Mo12P, Mr = 2938.96, Dc = 2.259 g/cm3, μ = 2.276 mm-1, F(000) = 1400, the final R = 0.0565 and wR = 0.1613 for 4973 observed reflections with I 2σ(I). The crystal structure can be described by the packing of Keggin anionic and Metal-Schiff-base cationic layers.     

计算受体和配体结合自由能的新方法

利用ABEEMσπ浮动电荷力场与连续介质模型相结合的方法,计算了受体和配体的结合自由能.将结合自由能分解为真空中的力场作用项、溶剂化能量以及熵效应.由于ABEEMσπ/MM方法充分考虑了外界环境发生变化引起的体系中各个位点之间的电荷极化,因而极大地提高了结合自由能的计算精度.利用该方法计算的2个复合物的结合自由能与实验值的偏差均小于0.5kJ/mol.     

应用手持式XRF分析仪快速测定白铜中的Cu、Ni、Co含量

采用国产手持式XRF分析仪快速分析了白铜合金主元素的含量,探讨了白铜合金基体效应对测量结果的影响,采用经验系数法中多元回归分析建立数学模型,较好地校正基体效应,分析白铜合金中铜、镍、钴的平均相对误差分别为0.39%、1.83%、1.59%。     

钽内标X射线荧光光谱法测定钨精矿中WO_3

提出了以钽为内标波长色散X射线荧光光谱法测定钨精矿中WO3的新方法。以Na2B4O7和Li2B4O7(质量比65:35)的混合物作为熔剂,Ta2O5为内标,同时加入LiNO3为氧化剂,在1200℃下进行熔融制样,最后将本方法应用于实际样品的分析,结果表明,以钽作为内标测定WO3,不仅可以在很大程度上降低实验操作和仪器测量带来的偏差,也可以消除基体效应的影响。方法用于测定白钨精矿和黑钨精矿中WO3,其准确度和精密度优于重量分析法。     

静电位阻模型在纳滤膜跨膜电位解析中的应用

采用静电位阻模型对纳滤膜的跨膜电位进行了理论解析, 考察了溶液体积通量密度、原料液浓度、阴阳离子扩散系数比、膜孔半径和膜体积电荷密度对KCl(1-1型电解质)和MgCl2(2-1型电解质)中的纳滤膜跨膜电位的影响. 研究结果表明, 随着通量密度的增大, KCl和MgCl₂的跨膜电位线性程度增强; 两种电解质的跨膜电位均随着原料液浓度和膜孔半径的增大而下降; 在不同的考察范围内, 阴阳离子扩散系数比对1-1型和2-1型电解质的跨膜电位的影响差别较大; KCl的跨膜电位随着膜体积电荷密度的变化关于零点呈现出对称性, 而MgCl₂的跨膜电位零点则出现在膜体积电荷密度为负的条件下.     

Physical and Electrochemical Characterization of Hydrothermal Prepared α'-NaV_2O_5 Crystals

α'-NaV2O5 was prepared by a simple hydrothermal process.X-ray diffraction confirmed the orthorhombic structure of α'-NaV2O5,with preferential growth along the (001) direction.Scanning electron microscopy showed α'-NaV2O5 was composed of flake-shaped crystals.X-ray photoelectron spectroscopy confirmed the co-existence of V4+ and V5+ in α'-NaV2O5,which results in an average V4.5+ oxidation state of α'-NaV2O5.The observed Raman bands are ascribed to different V―O vibrations.α'-NaV2O5 shows a reversible specific capacity of about 100 mA·h·g-1 between 3.5 and 1.0 V,with a good capacity retention.The good electrochemical stability of the material is attributed to its structural stability during Li+ intercalation.     

Hydrothermal Synthesis and Crystal Structure of a Manganese Complex

The title compound [Mn(Phen)(p-MBA)2]n(1) was synthesized via the hydro-thermal reaction of KMnO4 and NaOH with phen and p-methybenzoic acid(p-MBA) in water.The title compound was characterized by elemental analysis and infrared spectra.The crystal of 1 crystallizes in orthorhombic,space group Pbcn with a = 24.132(1),b = 10.404(0),c = 9.386(0) ,V = 2356.65(13) 3,Z = 4,C28H22MnN2O4,Mr = 505.42,Dc = 1.424 g/cm3,F(000) = 1044 and μ(MoKα) = 0.598 mm-1.The final R = 0.0781 and wR = 0.1363 for 1972 observed reflections with Ⅰ 2σ(Ⅰ) and R = 0.0897 and wR = 0.1420 for all data.X-ray diffraction reveals that the Phen and p-methy benzoic acid ligand link the Mn atoms into a single one-dimensional coordination polymer,and extensive intermolecular π-π interactions lead these 1D chains to form a two-dimensional supramolecular architecture.     

水蒸气重整生物质裂解油及其模型分子制氢

随着能源枯竭和环境日益恶化,利用可再生的生物质裂解油或其模型分子重整制氢逐渐引起人们重视。本文结合国内外重整制氢的研究进展,从催化剂、反应过程和反应机理三个方面对生物质裂解油及其模型分子(乙醇、乙酸、乙二醇、丙三醇、葡萄糖和苯酚等)水蒸气重整制氢研究现状进行了回顾。在重整催化剂方面主要对贵金属和过渡金属催化剂的研究进展进行了总结,对一些新的重整过程如液相重整等也进行了介绍。在反应机理方面主要是对乙醇、乙酸、乙二醇和葡萄糖在重整反应中的反应路径进行了归纳。此外,对水蒸气重整反应中遇到的问题如积碳和副产物的产生等也进行了详细的分析,并对生物质制氢未来发展的方向进行了展望。     

平行因子分析在赤潮藻滤液三维荧光光谱特征提取中的应用

在实验室条件下培养我国沿海常见的10种赤潮藻,测定了赤潮藻生长过程中藻滤液的三维荧光光谱.用平行因子分析对光谱进行分解,获得每种赤潮藻滤液荧光峰的个数及类型,即每种赤潮藻的特征光谱.在此基础上比较每种藻特征光谱的相似性和差异性,并分析了赤潮藻生长过程中滤液的荧光峰强度和生长阶段的关系,为基于赤潮藻滤液三维荧光光谱的赤潮藻种类识别测定技术提供依据.结果表明:不同赤潮藻的特征光谱之间存在差异.在指数生长期,类蛋白和类腐殖质荧光峰强度与藻密度呈正相关,说明两类有机物在水体中不断积累;在稳定期和衰亡期,两类有机物的荧光强度迅速增大,这可能是衰老和死亡细胞的破碎释放,以及细菌降解作用所致.平行因子分析可以有效提取赤潮藻的荧光特征,考察了赤潮藻荧光峰强度和生长阶段的关系.