牛血清白蛋白与Indo-1相互作用的荧光光谱法研究

以牛血清白蛋白(Bovine serum album in,BSA)与荧光探针Indo-1为蛋白质和配体模型,基于Indo-1的荧光强度与BSA的分析浓度间的关系,建立了计算二者相互作用位点数的方法,并利用荧光共振能量转移及各种荧光技术对Indo-1和BSA的相互作用进行了研究.结果表明,Indo-1在BSA中有3个作用位点,这3个作用位点与BSA中的212位色氨酸(Trp 212)间的距离分别为2.93,2.57和2.40 nm;Indo-1通过疏水性作用进入到BSA的3个疏水性空腔.在荧光猝灭实验中,通过M icrolab 500系列进样器和PTI荧光仪的联用实现了荧光强度的自动和实时记录.

Fabrication and luminescent properties of rare earths-doped Gd-2(WO4)(3) thin film phosphors by Pechini sol-gel process

Rare earth ions (Eu3+ and Dy3+)-doped Gd-2(WO4)(3) phosphor films were prepared by a Pechini sol-gel process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), atomic force microscopy (AFM) and photoluminescence (PL) spectra as well as lifetimes were used to characterize the resulting powders and films. The results of XRD indicate that the films begin to crystallize at 600degreesC and the crystallinity increases with the elevation of annealing temperatures. The film is uniform and crack-free, WO(4)(2-)mainly consists of closely packed fine particles with an average grain size of 80 nm. Owing to an energy transfer from 4 groups, the rare earth ions show their characteristic emissions in crystalline Gd-2(WO4)(3) phosphor films, i.e., D-5(J) -F-7(J), (J = 0, 1, 2, 3; J' = 0 1, 2, 3, 4, not in all cases) transitions for Eu3+ and F-4(9/2)-H-6(J) (J = 13/2, 15/2) transitions for D Y3+, with the hypersensitive transitions D-5(0)-F-7(2) (Eu3+) and F-4(9/2) - H-6(13/2) (Dy3+) being the most prominent groups, respectively.

Liquid crystalline and light emitting polyacetylenes: Synthesis and properties of biphenyl-containing poly(1-alkynes) with different functional bridges and spacer lengths

Biphenyl- (Biph-) containing 1-alkynes (3 and 4) and their polymers (1 and 2) with varying bridge groups and spacer lengths were synthesized and the effects of the structural variation on their properties, especially their mesomorphism and photoluminescence behaviors, were studied. The acetylene monomers 3(3) [HCdropC(CH2)(3)O-Biph-OCO(CH2)(10)CH3] and 4(m) [HCdropC(CH2)(m)OCO-Biph-OCO(CH2)(10)-CH3, m = 3, 4] were prepared by sequential etherization and esterification reactions of 1-alkynes. While 3(3) exhibits enantiotropic crystal E and SmB mesophases, its structural cousin 4(3) displays only a monotropic SmB phase. Enantiotropic SmA and SmB mesophases are, however, developed when the spacer length is increased to 4. Polymerizations of the monomers are effected by Mo-, W-, Rh-, and Fe-based catalysts, with the WCl6-Ph4Sn catalyst giving the best results (isolation yield up to 85% and M-w up to 59000). The polymers were characterized by IR, UV, NMR, TGA, DSC, POM, XRD, and PL analyses. Compared to 1(3), 2(3) shows a red-shifted absorption, a higher T-i, and a better packed interdigitated bilayer SmA(d) structure, while the mesophase of 2(4) involves monolayer-packing arrangements of the mesogens. Upon photoexcitation, 1(3) emits almost no light but 2(m) gives a strong ultraviolet emission (lambda(max) similar to 350 nm), whose intensity increases with the spacer length.

Y_2O_3∶Eu~(3+)发光薄膜的溶胶凝胶法制备、表征及图案化

采用Pechini溶胶 凝胶法制备了纳米级Y2O3∶Eu3+发光薄膜,同时,通过软石印技术得到了条纹宽度为5～60μm的Y2O3∶Eu3+图案化发光薄膜。通过X射线衍射(XRD)、付里叶变换 红外光谱(FT IR)、原子力显微镜(AFM),光致发光(PL)光谱及寿命等方法对得到的发光薄膜进行了表征。XRD结果表明500℃时薄膜开始结晶,900℃已结晶完全,得到了立方相的产物。图案化的条纹在烧结的过程中发生了明显的收缩(50%)。Y2O3基质向掺杂的稀土离子Eu3+发生了有效的能量传递,使得Eu3+显示出5D0 7FJ(J=0,1,2,3,4)特征发射。寿命和光致发光光谱的研究表明,发光强度随着温度的升高而增强。

Networks with hexagonal circuits in co-ordination polymers of metal ions (Zn-II, Cd-II) with 1,1 '-(1,4-butanediyl)bis(imidazole)

Three new compounds, [ZnL1.5(H2O)(SO4)]. 6H(2)O 1, [ZnL1.5(H2O)(2)][NO3](2). 2H(2)O 2 and [CdL1.5(H2O)(2)(SO4)]. 4H(2)O 3 were obtained from self-assembly of the corresponding metal salts with 1,1'-(1,4-butanediyl)bis(imidazole) (L). In both 1 and 2 zinc ion is five-co-ordinated, showing a less-common trigonal bipyramidal co-ordination polyhedron, while cadmium ion of 3 is six-co-ordinated with a common octahedral arrangement. The sulfate ions of 1 and 3 are co-ordinated, however the nitrate ions of 2 are not. Each of the three compounds is composed of a (6, 3) network with the hexagonal smallest circuit containing six metal ions and six L; each L is co-ordinated to two metal ions, acting as a bridging ligand. In 1 the 2-D sheet of (6, 3) networks is interpenetrated in an inclined mode by symmetry related, identical sheets to give an interlocked 3-D structure, while the (6, 3) networks of both 2 and 3 stack in a parallel fashion to construct frameworks having channels.

Ce_(1-x)Sm_xO_(2-x/2)的溶胶-凝胶法的合成及氧空位的研究

本文利用溶胶-凝胶法合成了Ce_(1-x)Sm_xO_(2-x/2)(x=0-0.4)系列固体电解质,并且系统地研究了其晶体结构随Sm含量的变化关系。XRD表明:该体系从160℃开始即形成了立方萤石结构,且在所研究的组成范围内全部形成了单相固溶体。此温度远低于传统的高温固相合成法所需的温度,同时也较水热合成法的温度低。高温X-ray衍射研究表明直到800℃Ce_(1-x)Sm_xO_(2-x/2)未出现结构相转变,其晶格常数和晶胞体积随温度升高而增大。EPR测试证实了由于Sm~(3+)部分置换Ce~(4+)固溶体中所存在的单电荷缺陷(Sm_(Ce’),V_o~(oo))结构。在固溶体的Raman谱中观察到:纯CeO_2在465cm~(-1)仅有一个Raman振动模式,随着掺杂量的增大,此振动模式向低频方向移动,而且Raman线变宽且在570cm~(-1)附近出现一新的峰,这些变化都是由Sm~(3+)取代Ce~(4+)所产生的氧空位引起的。

~(57)Fe,~(119)Sn掺杂Bi_2Sr_2Ca_(n-1)Cu_nO_(2n+4)的化学键性质和Mssbauer谱位移研究

利用电介质的平均能带模型计算了Bi2 Sr2 Can- 1CunO2n +4 (n =1,2 ,3)的化学键参数 .应用由共价性和极化率定义的化学环境因子计算了57Fe和119Sn在Bi2 Sr2 Can - 1CunO2n +4 中的M ssbauer同质异能位移 ,确定了57Fe和119Sn在Bi2 Sr2 Can- 1CunO2n +4 中的价态和占位情况 .

(NH4)(3)[PMo12O40]center dot 21H(2)O

The determination of the crystal structure of the title compound, triammonium hexatriacontaoxo(tetraoxophosphato)dodecamolybdate(3-) henicosahydrate, shows that the polyanion has a pseudo-Keggin structure with m (3) over bar m symmetry. The central PO4 group is disordered with P-O distances of 1.55 (3) Angstrom. The Mo-O distances range from 1.617 (14) to 2.414 (14) Angstrom.

Synthesis and structure of 1:1 complex of ethylphenyltin dichloride with N-4-methoxyphenyl-2-hydroxynaphthylideneimine

A novel organotin complex, EtPhSnCl(2) . 2HOC(10)H(6)CH = NC6H1OCH3 was synthesized, and its crystal structure was determined by X-ray diffraction method. The crystal is triclinic, belonging to space group, with unit cell parameters a = 1.150 8(5) nm, b = 1. 153 1(5) gm, c = 1. 004 6 (3) nm, alpha = 94. 15 (3)degrees, beta = 115.47 (3)degrees, r = 85. 94 (4)degrees, V = 1199 7(1) nm(3), Z=2, D-c=1.68 g/cm(3), mu=13. 20 cm(-1), F(000)=618 for 4 131 reflections tions. R=0. 047, R(w)=0. 047. The ligand coordinates to tin atom via phenolic oxygen atom. The complex has a distored trigonal bipyramidal structure, the phenolic oxygen atom of the ligand and one of two chlorine atoms occupy the axial position. The distance between noncoodinated nitrogen atom with phenolic oxygen atom is 0. 257 4 nm, which indicates that the intramolecular hydrogen bond of Schiff base ligand is retained in the complex.

双1:11镝的硅钼杂多酸的液/液界面电化学研究

用循环线性电流扫描计时电位法和循环伏安法研究了双1∶11镝的硅钼杂多酸阴离子在水／硝基苯界面的转移。在pH＝1．1～5．3时，转移离子为H9Dy（SiMo11O39）24－．根据循环伏安结果计算得转移离子的标准电位差和Gibbs转移自由能分别为0．102V和－39．5kJ·ml-1，并由循环线性电流扫描计时电位法计算了转移离子的有关动力学参数，H9Dy（SiMo11O39）24-在水／硝基苯界面的转移属准可逆转移.

A STUDY OF CATALYTIC PROPERTIES OF PEROVSKITE-TYPE OXIDES LAMNYCO1-YO3 .1. THE RELATIONSHIP BETWEEN THE TYPE OF OXYGEN SPECIES AND THE CATALYTIC PROPERTY IN AMMONIA OXIDATION

The type of oxygen species in perovskite-type oxides LaMnyCo1-yO3 (y = 0.0, 0.1, 0.3, 0.5, 0.7, 0.9, 1.0) has been studied by means of XRD, XPS and TPD. The catalytic activity in ammonia oxidation was also investigated. It was found that there were three desorption peaks in TPD curve corresponding to three types of oxygen species (alpha, beta, beta'). The desorption temperatures were 293 K less-than-or-equal-to T(alpha) less-than-or-equal-to 773 K, 773 K less-than-or-equal-to T(beta) less-than-or-equal-to K and T(beta') greater-than-or-equal-to 1073 K respectively. The relationship among the composition, structure and the catalytic property of.the catalyst was correlated and could be explainned with a model based on solid defect reaction and the interaction between Co and Mn ions. The adsorption strength and quantity of a oxygen are proportional to the catalytic activity. The, result indicates that the synergetic effect between B-site ions seems to the benefit of the ammonis oxidation reaction.

聚[1-(三甲硅基)1-丙炔]——一种有希望的气体分离膜材料

聚[1-(三甲硅基)]-丙炔(PTMSP)膜的气体透过速率高于目前已知的,不管在室温是玻璃态还是橡胶态的任何聚合物.PTMSP在室温是玻璃态.PTMSP的高透气性主要来源于极高的对气体溶解度及高扩散系数,而这是因为在这种玻璃态聚合物中,有大量处于非松弛区域的自由体积.PTMSP的最大问题是它的高透气性随着时间的过去和热历史而衰减.近来,为解决这一问题进行了大量的努力,如加入低挥发材料,氟化、溴化,与其它单体共聚,与其它聚合物共混等.

CRYSTAL-STRUCTURE OF 1, 10-DECANEDIAMMONIUM TETRACHLOROZINCATE

The crystal structure of the title compound has been determined from single crystal X-ray diffraction. The complex crystallizes in the triclinic space group P1 with Z=2. Lattice parameters are: a = 0.7296(1), b = 1.0110(3), c = 1.2814(4) nm; alpha = 90.84(2), beta = 101.17(2), gamma = 92.52(2)-degrees. Intensity data were collected on a Nicolet R3M/E four-circle diffractometer using MoK alpha (lambda = 0.071073 nm) radiation. The structure was solved by Patterson and Fourier techniques and refined by least-squares techniques to R = 0.065. The structure of the complex consists of tetrahedral ZnCl42- anions which form a two-dimensional sheets. Tetrahedral ZnCl42- anions are sandwiched between two hydrocarbon layers which consist of [NH3(CH2)10NH3]2+ cations. Each [NH3(CH2)10NH3]2+ group is in a gauche bond between C atoms near NH3 polar heads.

SYNTHESIS AND CRYSTAL-STRUCTURE OF NEODYMIUM COMPLEX OF 1-METHYL-1, 4, 7, 10-TETRAAZACYCLODODECANE

The complex [Nd(L)(CH3CN)(CF3SO3)3] has been synthesized. Where L = 1-methyl-1, 4, 7, 10-tetraazacycldodecane. The crystal structure of the complex has been determined by a four-circle X-ray diffractometer to a final deviation factor B value of 0.0370 and R(w) value of 0.0385 respectively. The crystal is triclinic system, space group P1BAR with a = 0.8738(2), b = 1.2870(3), c = 1.2900(3) nm, alpha = 85.63(2), beta = 87.25(2), gamma = 78.30(2)-degrees, V = 1.41571 (60) nm3, Z = 2, D(c) = 1.92 g/cm3. The neodymium ion is eight-coordinated to forming a distorted square antiprism.

SYNTHESES OF METHYLCYCLOPENTADIENYL DERIVATIVES OF LANTHANIDES (LN = LA-ND) AND CRYSTAL-STRUCTURES OF [(THF)2LI(MU-CL)2]2[MECPND(THF)] AND [LI(DME)3][MECPLA(NPH2)3]

The reaction of LnCl3.2LiCl with 1 equiv of MeCpNa in THF gives the complexes [(THF)2Li(mu-Cl)2]2[MeCpLn(THF)] (Ln = Nd (1), La (2)) in good yield. These precursors react further with 2 equiv of LiNPh2 to produce the new complexes [Li(DME)3][MeCpLn(NPh2)3] (Ln = La (3), Pr (4), Nd (5)). They have been characterized by elemental analyses and IR and NMR spectra, as well as by structural analyses of 1 and 3. The chloride 1 crystallizes in the monoclinic space group P2(1)/n (No. 14) with a = 12.130 (5) angstrom, b = 17.343 (5) angstrom, c = 17.016 (5) angstrom, beta = 108.54 (3)-degrees, V = 3393.87 angstrom3, Z = 4, and D(c) = 1.45 g/cm3. Least-squares refinement led to a final R value of 0.051 (I greater-than-or-equal-to 3-sigma(I(o))) for 2004 independent reflections. Complex 3 crystallizes in the monoclinic space group P2(1)/c (No. 14) with a = 18.335 (6) angstrom, b = 16.576 (5) angstrom, c = 17.461 (6) angstrom, beta = 96.04 (3)-degrees, V = 5277.17 angstrom3, D(c) = 1.26 g/cm3, Z = 4, and R = 0.057 (I greater-than-or-equal-to 2.5-sigma(I(o))) for 3378 reflections. The structure of 3 consists of discrete ion pairs [Li(DME)3]+ and [MeCpLa(NPh2)3]- with average La-N and La-C(ring) distances of 2.459 (8) and 2.84 (1) angstrom, respectively.