双波长双指示剂催化光度法测定铜的研究

研究了在pH 4.0的HAc～NaAc缓冲介质中,利用痕量铜(Ⅱ)催化过氧化氢氧化罗丹明B和亚甲基蓝褪色的指示反应,通过测量540 nm和660 nm下,催化体系和非催化体系吸光度的变化,建立了双波长双指示剂催化动力学光度法测定痕量铜的新方法.方法的线性范围为0.00080～0.048μg/mL,检出限为4.0×10~(-11) g/mL.方法可用于水中铜的测定.     

双波长双指示剂催化光度法同时测定Fe和Cu

研究了在Na2SO4介质中,痕量Fe(Ⅲ)和Cu(Ⅱ)催化H2O2氧化次甲基蓝和甲基橙褪色的指示反应,通过测量440和664 nm波长下,催化反应体系和非催化反应体系的吸光度,建立了双波长、双指示剂催化动力学光度法同时测定痕量Fe(Ⅲ)和Cu(Ⅱ)的新方法.同时测定Fe(Ⅲ)和Cu(Ⅱ)的线性范围分别为0.0050～0.50 μg/25 mL和0.0025～0.75 μg/25 mL,检出限分别为6.9×10-8 g/L和8.7×10-8 g/L.用于水样中痕量Fe(Ⅲ)和Cu(Ⅱ)的测定.     

亚甲基蓝-高碘酸钾催化动力学光度法测定痕量钌(Ⅲ)

在稀H_2SO_4介质中及加热85℃的条件下,钌(Ⅲ)对KIO_4氧化亚甲基蓝的褪色反应具有显著的催化作用,建立了一个催化动力学光度法测定痕量钌(Ⅲ)的新分析方法.探讨了该催化反应的最佳实验条件.非催化反应吸光度A_0与催化反应吸光度A之间的差值△A与钌(Ⅲ)质量浓度ρ在0～0.06μg/mL范围内呈良好的线性关系,检出限为2.37×10~(-10)g/mL.测定了动力学参数,反应为准一级反应,表观速率常数为3.63×10~(-4)/s,表观活化能为58.13 kJ/mol.对1.0μg Ru(Ⅲ)测定的相对标准偏差RSD为1.7%(n=11).方法用于分子筛样品中痕量钌(Ⅲ)的测定,回收率98.3%.     

溴酚蓝和亚甲蓝双显色体系萃取光度法测定铜

向三元络合物[Cu(phen)_3)BPB的二氯乙烷萃取液中,加入KCN水溶液,形成的[Cu(CN)_2)~-和溴酚蓝离子(BPB)进入水相,向其中加入与BPB颜色相近的亚甲蓝(MB)再进行萃取光度测定。因萃取液中[MB_2BPB)和[Cu(CN)_2)MB两者的吸光作用,使本方法具有很高的灵敏度,ε=1.77×10~5L·mol~(-1)·cm~(-1)。铜含量在0～5μg/25ml遵从比耳定律,对含铜量为10~(-8)g/ml的水样测定5次,相对标准偏差为2％。     

Synthesis,characterization and antimicrobial screening of quinoline based quinazolinone-4-thiazolidinone heterocycles

In an attempt to find new pharmacologically active molecules, we report here the synthesis and in vitro antimicrobial activity of various 2-(2-chloro-6-methyl(3-quinolyl))-3-[2-(4-chlorophenyl)-4-oxo(3-hydroquinazolin-3-yl)]-5-[(aryl)methylene]-1,3-thiazolidin-4-ones. In vitro antimicrobial activity of the title compounds are screened against two Gram positive bacteria (Staphylococcus aureus, Streptococcus pyogenes), two Gram negative bacteria (Escherichia coli, Pseudomonas aeruginosa) and three strains of fungi (Candida albicans, Aspergillus niger, Aspergillus clavatus) using broth micro dilution method. Some derivatives bearing chloro or hydroxy group exhibited very good antimicrobial activity.     

依来络兰黑R褪色光度法测定痕量铜

在氨水介质中,微量铜可催化亚硝酸钠氧化依来络兰黑R褪色,由此建立了一种高灵敏度光度法测定微量铜的方法。间接摩尔吸光系数ε530＝2．5×106L·mol-1·cm-1,线性范围为0～8μg／25ml,线性回归方程△A＝0．0123C+0．0076,r＝0．9994,方法用于环境废水中微量铜的测定,选择性好,灵敏度高,结果满意。     

Cu_3B_2O_6/CuB_2O_4单晶的制备及其可见光催化降解亚甲基蓝

以醋酸铜/硝酸铜和硼酸为原料,柠檬酸作发泡剂,采用溶胶-凝胶法制得了高纯度的单晶结构硼酸铜(Cu3B2O6/CuB2O4).利用X射线衍射(XRD)、扫描电镜(SEM)、高分辨率透射电镜(HRTEM)、热重-差热分析(TGDTA)等对样品进行了表征,并考察了Cu3B2O6/CuB2O4在可见光(400 nmλ1100 nm)下对亚甲基蓝(MB)溶液的催化降解性能.结果表明,两种结构的硼酸铜都具有良好的光催化性能.当亚甲基蓝的初始浓度为50 mg·L-1,催化剂用量为1 g·L-1,光照6 h后,CuB2O4对亚甲基蓝的光催化降解率为63.36%,Cu3B2O6对亚甲基蓝的光催化降解率为99.52%.紫外-可见漫反射光谱(UV-Vis DRS)结果表明,Cu3B2O6的中间能态宽度为1.78 eV,小于CuB2O4的中间能态宽度(1.95 eV),且Cu3B2O6的禁带宽度较窄(Eg=2.34 eV),不仅可以发生价带顶与中间能态的电子跃迁,同时可以发生禁带间的电子跃迁,所以Cu3B2O6比CuB2O4具有更高的可见光催化性能.     

Cu3B2O6/CuB2O4单晶的制备及其可见光催化降解亚甲基蓝

以醋酸铜/硝酸铜和硼酸为原料,柠檬酸作发泡剂,采用溶胶-凝胶法制得了高纯度的单晶结构硼酸铜（Cu₃B₂O₆/CuB₂O₄）. 利用X射线衍射（XRD）、扫描电镜（SEM）、高分辨率透射电镜（HRTEM）、热重-差热分析（TGDTA）等对样品进行了表征,并考察了Cu₃B₂O₆/CuB₂O₄在可见光（400 nm<λ<1100 nm）下对亚甲基蓝（MB）溶液的催化降解性能. 结果表明,两种结构的硼酸铜都具有良好的光催化性能. 当亚甲基蓝的初始浓度为50 mg·L^-1,催化剂用量为1 g·L^-1,光照6 h后,CuB₂O₄对亚甲基蓝的光催化降解率为63.36%,Cu₃B₂O₆对亚甲基蓝的光催化降解率为99.52%. 紫外-可见漫反射光谱（UV-Vis DRS）结果表明,Cu₃B₂O₆的中间能态宽度为1.78 eV,小于CuB₂O₄的中间能态宽度（1.95 eV）,且Cu₃B₂O₆的禁带宽度较窄（E_g=2.34 eV）,不仅可以发生价带顶与中间能态的电子跃迁,同时可以发生禁带间的电子跃迁,所以Cu₃B₂O₆比CuB₂O₄具有更高的可见光催化性能.     

铜催化抗坏血酸还原酸性铬深蓝动力学光度法测定痕量铜

在乙酸-乙酸钠介质中,以邻菲罗啉为活化剂,铜对抗坏血酸还原酸性铬深蓝具有强烈的催化作用,测定了反应的表观活化能,探讨了反应机理,建立了测定痕量铜的催化动力学新方法,测定的线性范围为2.5～60ng·ml~(-1),直接用于食品及人发中铜的测定。结果满意。     

Synthesis and characterization of stannacyclododecane-yl-dithiocarbamates

Thirteen new stannacyclododecane dithiocarbamate complexes have been prepared by reacting 12-chloro-12-n-butyl-1,11-dioxa-4,8-dithia-12-stannacyclododecane (1) and 12-chloro-12-n-butyl-1,4,8,11-tetrathia-12-stannacyclododecane (2) with pyrrolidine-, morpholine-, thiomorpholine-, piperidine-, piperazinebis-, and 3-pyrroline-carbodithioates, respectively, as well as with diethyl-dithiocarbamate. All complexes were characterized by elemental analyses, IR, EI-MS, and NMR (¹H, ¹³C, and ¹¹⁹Sn) studies. The spectroscopic data suggest the replacement of the chlorides by the corresponding dithiocarbamates with monodentate coordination, leading to six-coordinate tin atoms in all the cases.     

含混合配体多酸超分子化合物的水热合成、晶体结构及催化活性

在水热条件下合成了四个含混合配体4,4’-bipy和2,2’-bipy/phen的多酸配位聚合物[Cu(4,4’-bipy)(2,2’-bipy)2]2[SiW12O40]?4H2O (1),[Ag4(4,4’-bipy)3(2,2’-bipy)2][SiW12O40]?2H2O (2),[Cu(4,4’-bipy)(phen)]2[H3O]2[SiW12O40]?8H2O (3)和[Cu(4,4’-bipy-Cl)(phen)]2[H3O][PW12O40]?H2O (4) (bipy = 联吡啶,phen = 邻菲罗啉),通过红外光谱、热重、元素分析、X-单晶衍射对聚合物进行了表征,在苯乙烯催化环氧化反应中,3和4显示了较高的催化活性,这与结构中存在配位不饱和金属中心有关.     

Chiral Coordination Polymers with Amino Acids: $\rm ^{2}_{\infty}[Cu_{2}(\mu-L-tryptophanato)_{2}(\mu-4,4\prime-bipyridine)(H_{2}O)_{2}](NO_{3})_{2}$

The two‐dimensional mixed‐ligand network catena‐[(μ‐4,4′‐bipyridine)‐bis(μ‐L‐tryptophanato‐κ³N,O,O′)‐diaqua‐dicopper(II) dinitrate] is constructed through the bridging action of both the tridentate amino carboxylato and the bidentate 4,4′‐bipyridine ligand. The enantiomeric L‐tryptophanato ligand acts as an N,O chelate towards one copper atom and bridges through the second carboxylate oxygen atom to the adjacent copper ion. Stacking of the corrugated nets creates channels which are occupied by the hydrogen‐bonded and very weakly Cu‐coordinating nitrate ions.     

Synthesis and spectroscopic studies of diorganotin(IV) adducts based on cyclotriphosphazene scaffolds with exocyclic pyrazolyl substituents

Functionalized cyclotriphosphazenes with four pyrazolyl substituents have been employed for the synthesis of two new organotin complexes. These new compounds have been characterized by elemental analysis and IR, ¹H, ³¹P and ¹¹⁹Sn NMR spectroscopy. On the basis of these data, pyrazolylcyclotriphosphazene is bis-bidentate neutral ligand coordinating to two SnMe₂Cl₂ molecules in the resulting adducts. Coordination occurs only via the pyrazolyl nitrogens; cyclotriphosphazene ring nitrogens are not involved in coordination. The ¹¹⁹Sn NMR data are consistent with increasing of coordination number of tin(IV) in solution.