12-钼磷酸四丁基铵杂多蓝的光化学合成表征与晶体结构

用450W高压汞灯照射H3PMo12O40·5H2O和（Bu4N）Br（TBA）的DMF（N,N-二甲基甲酰胺）溶液,合成了12-钼磷酸四丁基铵杂多蓝（Bu4N）4[PMo12O40]·2DMF·H2O,用元素分析,IR,固体漫反射电子光谱,ESR,XPS和CV等进行了表征。晶体结构分析表明,标题化合物属单斜晶系,空间群P21/c,晶胞参数a=14.124（3）,b=17.481（4）,c=22.744（5）A,β=101.66（3）°,V=5500（2）A3,C70H160Mo12N6O43P,Mr=2956.29,Z=2,Dc=1.785g/cm3,F（000）=2970,μ（MoKα）=1.412mm-1,R=0.0638,wR=0.1975。标题化合物是由4个四丁基铵阳离子、1个12-钼磷混合价杂多阴离子[PMo12O40]4-、2个DMF分子和1个水分子构成。

Laser-time-resolved fluorescence spectroscopy in immunoassays

This paper described a laser-excited time-resolved fluoroimmunoassay set. It made lanthanide ion to couple the anhydrde of diethylenetriaminepentaacetic acid (DTPAA) for labeling antibodies. The experiment used polystyrene tap coated with HCV antigen as the solid phase and a chelate of the rare earth metal europium as fluorescent label. A nitrogen laser beam was used to excite the Eu3+ chelates and after 60 ys delay time,the emission fluorescence was measured. Background fluorescence of short lifetimes caused by serum components and Raman scattering can be eliminated by set the delay rime. In the system condition, fluorescent spectra and fluorescent lifetimes of Eu3+ beta-naphthoyltrifluroacetone (NTA) chelates were measured. The fluorescent lifetime value is 650 mu s. The maximum emssion wavelength is 613 nm. The linear range of europium ion concentration is 1 x 10(-7)- 1 x 10(-11) g.mL(-1) and the detection limit is 1 x 10(-13) g.mL(-1). The relative standard deviation of determination ( n = 12) for samples at 0.01 ng.mL(-1) magnitude is 6.4%. Laser-TRFIA was also found to be suitable for diagnosis of HCV. The sensitvity and specificity were comparable to enzyme immunoassay. The result was obtained with laser-TRFIA for 29 human correlated well with enzyme immunoassay.

Study of the effect of hydrogen bonding on the phase behaviour of p-nitro azobenzene derivatives with hydrophilic tails

The infrared spect ra of N-n-(4-nitrophenyl)azophenyloxyalkyldiethanolamines (Cn) are examined in the range of 4000-400 cm(-1) at different temperatures and the assignment of the fundamental vibrations given. Based on (1) the localization of the broad absorption band at 3456 cm(-1), and (2) attribution of the associated OH bands centred at 1410-1390, 1100, and 650-634 cm(-1) to, respectively delta OH deformation, nu C-O stretching and gamma OH out-of-plane bending, intermolecular hydrogen bonding between OH groups in the crystalline, liquid crystalline and isotropic states is proposed. By considering the results of FTIR, WAXD and DSC measurements, the molecular arrangement of C10 in its smectic A phase as consisting of hydrogen bonding and strong interaction between dipolar groups (NO,) is proposed. This may explain the high stability and high orientational ordering property of Cn compounds in the liquid crystalline state compared with that of n-bromo-1-[4-(4-nitrophenyl)azophenyl]oxyalkanes (Bn).

Crystal Structure of [PrAl(CF3COO)(2)(CF3CHOO)(C2H5)(2)(C4H8O)(2)](2)

[PrAl (CF3COO)(2) (CF3CHOO) (C2H5)(2) (C4H8O)(2)](2) M-r = 1420. 56, monoclinic, P2(1)/n, a = 10. 651 (6) , b = 24. 276(9), c = 11. 110(5) Angstrom, beta = 107. 650 (4)degrees , V = 2737. 4(1) Angstrom (3) , Z = 2, D-c = 3. 45 g/cm(3) , F(000) = 2816 , T = 233K, MoK alpha radiation (lambda= 0. 71069 Angstrom), mu(MoK alpha) = 38. 017 cm(-1) , R = 0. 048 for 2847 observed reflections (I greater than or equal to 3 sigma(I)). It is isostructural with [LnAl (CF3COO)(2) (CF3CHOO) -R-2 (C4H8O)(2)](2) (Ln = Ho, R = Et; Ln = Ndt Y, R = Bu-1). Pr3+ is coordinated by eight oxygen atoms from five bridging ligands and two THF forming a distorted bicap-prism.

The application of the MPB4 theory to the interface between between two immiscible electrolyte solutions .4. The differential capacitance of the water/nitrobenzene interface in the presence of 2:2 electrolyte

We have developed a new theoretical model based on the MPB4 theory to calculate the differential capacitance of the interface of 0.05mol/L MgSO4 in water and 0.1mol/L TBATPB in nitrobenzene. Our results coincide with the experimental values very well. It indicates that our model may describe well the structure of ITIES not only in the presence of 1:1 electrolyte but also in the presence of 2:2 electrolyte.

Preparation of Pb-Ca-Na master alloy using molten chloride salt electrolysis

An electrolysis technique for co-deposition of Ca2+ and Na+ at the liquid lead cathode was put forward. The experiment was carried out at an electrolysis temperature below 650 degrees C and had a current efficiency of 98%, which are respectively 100 similar to 300 degrees C lower and 15% similar to 30% higher than those reported both at home and abroad.

醋酸乙烯酯乳液聚合数学模型(Ⅰ) 阶段Ⅰ模型

研究了较大亲水性单体醋酸乙烯酯(VAc)乳液聚合的乳胶粒生成和生长过程,提出了VAc乳液聚合阶段Ⅰ数学模型.该模型既考虑到胶束成核机理,又考虑到水相中低聚物沉淀成核机理.研究了自由基解吸与吸附在单体珠滴上的乳化剂对VAc乳液聚合阶段Ⅰ动力学的影响,并对模型预计结果与实验数据进行了比较和讨论.

聚丁二烯红外目标因素分析

前文报道了聚丁二烯微观结构的分析方法,在目标因素分析中测摩尔消光系数对标定聚丁二烯含量要作校正,少量杂质还会影响准确定量,如在1000～650 cm~(-1)谱区的结果不是很满意的。本文按文献的谱线趋向,去掉谱区内的杂质吸收部分,以此修正摩尔消光系数作为目标向量,从而进行目标因素分析定量计算,所得结果较满意。

聚苯胺及聚邻甲基苯胺的直接裂解质谱研究

本文用直接裂解质谱和裂解色谱/质谱研究了不同氧化程度聚苯胺(PAn)和聚邻甲基苯胺(POT)的裂解过程及链结构,并用碰撞诱导解离(CID)和联合扫描(B/E)等技术探讨了链的断裂机理。结果表明,聚苯胺及其衍生物在650℃下裂解时产生5个单元的线状齐聚物,PAn及POT中苯二胺和醌亚胺两种结构单元共存。并提出了PAn和POT的自由基过渡态热解机理。

STRUCTURE OF 1,10-DIAMINODECANE TETRACHLOROZINCATE

[NH3(CH2)10NH3][ZnCl4], M(r) = 381.51, triclinic, P1BAR, a = 7.296 (1), b = 10.110 (3), c = 12.814 (4) angstrom, alpha = 90.84 (2), beta = 101.17 (2), gamma = 92.52 (2)-degrees, V = 926.13 angstrom 3, Z = 2, D(x) = 1.37 Mg m-3, lambda(Mo K-alpha) = 0.71073 angstrom, mu = 1.925 mm-1, F(000) = 396, T = 298 K, final R = 0.070 for 1237 unique reflections [I > 3-sigma(I)]. The structure is characterized by layers of inorganic ions sandwiched between layers formed by the paraffinic chains.

水蒸汽条件下草酸钇的热分解

用TG方法研究了十水草酸钇在水蒸汽条件下的热分解。结果表明,十水草酸钇首先分步失去八个水分子形成较稳定的二水盐,继续升温到420℃以较快的速率分解,经过不稳定的非晶态Y_2O_2CO_3,到650℃生成粒径为0.01～0.03μm、立方结构的氧化钇。为水蒸汽下制备氧化钇超微粉新工艺提供了理论依据。

钴卟啉修饰碳纤维微葡萄糖酶传感器的研究

本文成功地制备了四苯基钴卟啉修饰碳纤维微柱电极并讨论了其对氧的催化行为。继以四苯基钴卟啉化学修饰碳纤维微柱电极为基底电极,偶合葡萄糖氧化酶制成微葡萄糖酶电极。这种微酶电极的检测上限为2.0 mmol/L,响应时间小于4s,抗干扰能力强。是一种很有发展前途的微电化学感感器。

衬钽管石墨炉原子吸收光谱测定锡时基体改进剂和保护气氛的研究

本文提出用Ar-5%H_2作保护气氛和铜作基体改进剂的衬钽管石墨炉原子吸收光谱测定锡的方法。衬钽管的测定灵敏度是热解涂层石墨管的六倍左右。本法抗干扰能力强,测定精度(R.S.D.)小于2%。H_2保护了衬钽管,测定重现性好,衬钽管使用寿命可达650次左右。本法不经预分离直接测定蕃茄、蘑菇罐头及河流底泥样品中的锡,结果与其它方法相吻合。

A potent anti-oxidant property: fluorescent recombinant alpha-phycocyanin of Spirulina

To express and product a fluorescent antioxidant holo-alpha-phycocyanin (PC) of Spirulina platensis (Sp) with His-tag (rHHPC; recombinant holo-alpha-phycocyaninof Spirulina platensis with His-tag) in 5-l bench scale. A vector harbouring two cassettes was constructed: cpcA along with cpcE-cpcF in one cassette; ho1-pcyA in the other cassette. Lyases CpcE/F of Synechocystis sp. PCC6803 (S6) could catalyse the 82 site Cys in apo-alpha-PC of Sp linking with bilin chromophores, and rHHPC was biosynthesized in Escherichia coli BL21. The constant feeding mode was adopted, and transformant reached the biomass of rHHPC up to 0.55 g l(-1) broth in 5-litre bench scale. rHHPC was purified by Ni2+ affinity column conveniently. The absorbance and the fluorescence emission spectra of rHHPC had lambda(max) at 621 and 650 nm, respectively. The IC50 values of rHHPC were 277.5 +/- 25.8 mu g ml(-1) against hydroxyl radicals and 20.8 +/- 2.2 mu g ml(-1) against peroxyl radicals. Combinational biosynthesis of rHHPC was feasible, and the constant feeding mode was adopted to produce good yields of rHHPC. Fluorescent rHHPC with several unique qualitative and quantitative features was effective on scavenging hydroxyl and peroxyl radicals. A potent antioxidant rHHPC was co-expressed, produced and characterized for nutritional and pharmacological values, which would help to develop phycobiliproteins' applications in their fluorescent and biological activities.