分子荧光光谱法测定富硒大米中的痕量硒

硒(Ⅳ)与DAN(2,3-二氨基萘)生成具有荧光特性的4,5-苯并苤硒脑,可用分子荧光光谱法测定,优化测定的实验条件,建立了快速准确测定大米中痕量硒的方法.结果表明,其最佳测定条件为:pH=2.0,反应温度为80℃,1.0×10-5 mol/L十六烷基溴化吡啶用作表面活性剂,环己烷萃取条件下,增敏效果明显,在0～0.0...     

高效液相色谱荧光检测法测定福建乌龙茶中痕量硒

本文研究了2,3-二氨基萘(DAN)与Se(Ⅳ)反应,生成4.5-苯并苤硒脑(NSD),利用环已烷萃取反应生成的络合物。将有机相注射入填充有μ一Bondapak C_(18)固定相的色谱柱,以环已烷-四氢呋喃(90:10)为流动相,流速为1.0 mL/min,进行HPLC一荧光检测。测定了福建乌龙茶中的微量硒。方法的精密度和回收度均好。检测限达0.12 ng。     

用气相色谱法研究苯并苤硒脑的光解现象

以硒和2,3-二氨基萘(DAN)相互作用生成苯并苤硒脑(简称硒络物)为基本反应,用光度法、荧光法和气相色谱法测定痕量硒的方法已被广泛采用,而有关硒络物的光解性质,近年来才有一些作者揭示了这一现象。但是对此问题仍然报道不多。     

二溴代苤硒脑极谱吸附波的研究及应用

硒(Ⅳ)与邻芳香二胺类试剂能生成相应的苤硒脑衍生物,利用其电还原性质可用极谱法测定硒^[1,2],二溴代苤硒脑的极谱特性及应用尚未见报道.     

硒杂环化合物(4,5-苯并苤硒脑)在金表面上的自组装

为了寻求新的自组装单分子膜体系,构建新的功能膜,研究了具备平面型的大环共轭硒杂环化合物-- 4,5-苯并苤硒脑(苯并[c]硒二唑,简称苤硒脑)在金表面的自组装单分子膜.通过X射线光电子能谱(XPS)和电化学手段对其进行表征.XPS研究结果表明,自组装形成单分子膜后,苤硒脑分子中Se3d结合能从57.4 eV下降到57.1 eV;表明硒杂环化合物是通过金硒键固定在金表面上的;电化学循环伏安法实验表明,金电极表面上自组装该有机硒后, Fe(CN)63-/4-的氧化还原峰几乎完全消失;以四硼酸钠为底液,测得该化合物自组装在金表面上时,其还原电位在-0.66 V,与在溶液中用裸金电极测得的还原峰电位基本一致.     

土壤中微量硒的荧光测定法

荧光法测定土壤中的微量硒具有选择性好,灵敏度高,简便等特点。方法的基础是硒(Ⅳ)与2,3-二氨基萘(DAN)在酸性介质中生成4,5-苯并苤硒脑,用有机溶剂萃取该络合物以荧光分光光度计测定硒的含量。激发波长为377毫微米,分析荧光波长为522毫微米。方法的检出限为0.002微克硒/毫升,回收率为93.5—102.6％,平均98.9％,变异系数为2.74％。 1.样品消化:称取0.2—0.5克土壤样品(磨至100目)放在300毫升带塞三角烧瓶中,用少量去离子水浸润,加入混合酸消化液(HNO_3):H_2ClO_4=2:1)15—20毫升,在室温下放置30     

紫外分光光度法测定硒氧化过程中二氧化硒

利用5-硝基-2,1,3-苯并苤硒脑对紫外光的吸收特性,用紫外分光光度计测定硒氧化过程中硒(Ⅳ)含量。研究了硒(Ⅳ)与4-硝基邻苯二胺(NPDA)生成5-硝基-2,1,3-苯并苤硒脑的衍生反应条件,验证了测定结果的准确性。结果表明:衍生反应适宜条件为pH2,反应温度60℃,反应时间10 min,NPDA试剂用量为硒(Ⅳ)的168倍。在0.002~0.02 g/L硒(Ⅳ)范围内,硒(Ⅳ)浓度与衍生产物5-硝基-2,1,3-苯并苤硒脑的吸光度线性关系良好。用该法测定硒氧化过程中二氧化硒含量,RSD为0.52%。硒(Ⅳ)的平均加标回收率为98.12%。本文建立的紫外分光光度法为硒含量较大的体系中硒(Ⅳ)定量分析提供了准确、便捷的测定方法,对于其它价态硒(Ⅵ价、Ⅱ价、0价)测定有借鉴作用。     

环境样品中硒的形态分析方法研究

基于2,3-二氨基萘(DAN)试剂对四价硒的选择性测定,同时选择了4N盐酸作为还原剂将溶液样品中的六价硒定量还原到四价,用硝酸-高氯酸体系将以负二价形式存在的有机硒氧化到四价后分别测定,用差减法获得样品中不同形态硒的含量,并讨论了最佳实验条件。实验部分测定方法:待测溶液调整到PH1.5左右,再加入5ml 0.1％DAN的0.1N盐酸溶液,混合物在50℃下恒温避光反应20分钟后取出冷却到室温。加入5ml环己烷回旋萃取5分钟,分离     

碘-二甲基亚砜促进新型四环噻唑并[3',2':2,3]吡啶并[4,5-d]吡啶并[1,2-a]嘧啶酮类衍生物的合成（英文）

介绍了在碘-二甲基亚砜(I_2-DMSO)促进作用下,通过Pictet-Spengler反应合成噻唑并[3',2':2,3]吡啶并[4,5-d]吡啶并[1,2-a]嘧啶酮(5)衍生物的合成方法.该反应的关键中间体2-(3-氨基-5-苯氨基噻唑-2-基)-4H-吡啶[1,2-a]嘧啶-4-酮(3),由2-氯甲基-4H-吡啶[1,2-a]嘧啶-4-酮(1)与N-苯基-N'-氰基-咪唑硫代碳酸钾(2)通过Thorpe-Ziegler异构化反应制得.该合成方法反应条件温和,操作简单,收率高.     

Cp2TiCl2/BuiMgBr/THF体系还原二芳基二硒醚

有机硒化合物具有生物活性[14],将硒基团引入到有机分子的一般方法是使亲核性的硒金属盐与亲电试剂反应 .二芳基二硒醚是制备有机硒化合物的重要中间体 .当它被还原时转化为硒负离子 ,被卤素等氧化时转化为亲电的硒试剂 .还原二硒醚通常使用ＮａＢＨ4[5 ],最近报道一些新的方法 ,如使用水合肼 /甲醇钠体系[6 ],Ｓｍ/ＨｇＣｌ2 体系[7].本文报道Ｃｐ2 ＴｉＣｌ2 /ＢｕｉＭｇＢｒ/ＴＨＦ体系还原二芳基二硒醚 .1　结果与讨论Ｃｐ2 ＴｉＣｌ2 与ＢｕｉＭｇＢｒ反应产生的钛氢化物是一种强的还原剂[8].在室温下 ,钛氢化物很容易与二硒醚反应生成…     

国产硅藻土吸附尿激酶机理的研究

在常温下, 尿激酶在浙江土和吉林土表面的吸附等温线分别为V型和II型; 焙烧后两者皆转为III型。吸附等温线类型与硅藻土表面结构、孔结构、表面ζ电位有关。在400℃焙烧的硅藻土等电点值最低, 吸附量最大; 改性后, 吸附量也发生改变。本文还测定了尿激酶在硅藻土表面的吸附形态, 其吸附等温线方程符合0/(1-0)=(Kc)^1/β, 并讨论了平衡常数K和尿激酶吸附功能链段数β随温度的变化。     

DFT Study on the Effect of Hydrogen-bond Formation on the Adsorption of Aminotriazines on Graphene

DFT calculations have been performed to explore the aminotriazine adsorption on graphene surfaces.Relative energies,equilibrium geometries and electronic structures of monomer and dimer of aminotriazine molecules adsorbed at the surface were investigated and analyzed in details.It was found that the hydrogen atoms in the NH2 group of aminotriazine molecules are directed toward the graphene surface,and the adsorption energy increases as the NH2 group is added.The adsorbed aminotriazine molecules facilely form a dimer through the hydrogen bonding interactions,and the two aromatic rings of optimized structure of 2-amino-1,3,5-triazine(B) dimmer(denoted by B2) and melamine(D) dimmer(denoted by D2) are parallel to the graphene sheet.The large deviation of the averaged adsorption energy of B2 and D2 compared to monor adsorption may reflect the increase of π-π repulsion and the effect of hydrogen bond formation.The electronic structure analyses reveal that the formation of hydrogen bonds in melamine dimer has great influence on the adsorption mode at the graphene surface.     

MCM-41表面氧化铜的分散研究

金属离子修饰的M41S介孔分子筛催化剂体系是当前多相催化剂研究的热点.虽然有关介孔分子筛金属离子修饰的方法有多种[1],但均存在着负载的金属粒子在载体表面负载量低或分散不均匀等缺点;采用本课题组的有机官能团化法[2]可以得到高分散度和高负载量的介孔分子筛负载金属氧化物     

Simulation Analysis on the Profiles of Droplets Wetting on the Substrates

To study the structural characteristics and physical properties of droplets sitting on the inclined substrates and cylindrical surfaces, wetting experiments are conducted in different cases. The profile curves of the droplets are recorded and extracted by a CCD camera and image processing, respectively. Contact angles are figured out by fitting the profile curves and taking the derivative at the front and rear triple points. Based on the experimental results, a Surface Evolver is employed to simulate the morphological changes by minimizing the total energy of the system. Furthermore, theoretical shapes and feature parameters, including the heights and the spreading distances of the droplets, which are hard to obtain by normal experimental measurements are provided. The contact-angle hysteresis when the heavy droplet sitting on the inclined substrate is discussed. Meanwhile, the evolutions of the contour of the three-phase contact line are predicted when heavy droplets spread on the convex and concave cylindrical surfaces, respectively. This study provides a finite-element analysis method to describe the surface properties of molten droplets on different substrates, and the simulation results agree well with the experimental results.     

Quantum calculations on the adsorption of halide ions on the noble metals

The interaction of halide ions with the three noble metals has been investigated using the B3LYP density functional method and the cluster model approximation. The results of calculations for the M—X⁻ and M₁₂—X⁻ (M = Cu, Ag, Au; X = F, Cl, Br, I) systems are presented. At the (100) surface, modeled in the present work by the M₁₂ cluster, all halide ions have been found to adsorb preferentially at the hollow site, followed by the bridge and by the top positions. The adsorption energy has been found to decrease when going from fluoride to iodide in both atom—ion and cluster—ion cases. The opposite trend is observed for the estimates of the charge transfer from the ions to the surface. When different metals are compared, the M₁₂—X⁻ interaction energies decrease in the order Au > Ag > Cu, but for the smaller ions some deviations from this line do appear. The relative values of the calculated harmonic vibrational frequencies do agree with those found experimentally, but their magnitude is much smaller as a result of the effect of the lower surface coverage.     

Microcalorimetric investigations on the influence of propolis on the bacterium micrococcus luteus

Propolis or bee-glue is the third important product of honey bees after honey and wax. Known for thousands of years for its curative effects it is finding evermore attention in alternative and classical therapy in recent times against, e.g. infections, inflammations, dermatologic diseases and in wound healing.

Microcalorimetric experiments were performed on the influence of several propolis samples from Germany, Uruguay, Ethiopia and of a commercial propolis tincture on growth and metabolism of the recommended gram-positive bacterium Micrococcus luteus. Propolis extracts were prepared following established recipies for the water-soluble and insoluble components and the precipitate.

Addition of these extracts to a growing M. luteus culture in different growth phases resulted in a strong decline of the heat production rate, a prolongation of the lag phase or an introduction of a new, second lag phase, while the form of the calorimetric power-time curve remained unchanged. The calorimetric response showed a linear dependence on the propolis concentration. Although the quantitative gain of the extracts from the different propolis samples was nearly constant, the effects varied considerably between the specimens used.

The calorimetric investigations were supplemented by polarographic oxygen monitoring and by the standard agar well technique to determine the growth inhibition factor of the propolis extracts.     

关于变价态奎宁电极的研制与Ph对电极斜率影响的探讨

本文研究在两种质子化状态存在时奎宁的电极行为与特点,证明在不同pH溶液中变价态奎宁电极电位不能直接用能斯脱公式或Nicolsky-eisenman公式表出,提出了变价态电极的S-σ经验或,并依据此式,用奎宁选择性电极测出20℃下I=0.5McIlvaine缓冲液双质子化奎宁,辛可宁、硫胺的Ka1分别为(8.37±0.96)x10[-5],(8.00±0.92)x10[-5].(8.37±0.96)x10[-6].指出:同系列溶剂介电常数增大,液膜电极斜率增大,存在S-1/ε线性关系,电极可用于奎宁的电位滴定法或直接电位法测定。     

Processes on aluminium on the negative side of the open-circuit potential

Cathodic current—time transients were recorded on high-purity aluminium immersed into a neutral 2 M NaCl solution, when subjected to a potential pulse from a potential around the open-circuit potential, to different negative values. Hydration of the oxide layer occurs at potentials more negative than −1700 mV vs. SCE, whereupon hydrogen is evolved at the metal—hydrated oxide interface. A linear Tafel function is obtained for the maximum current attained in that potential region with a slope of 110 mV dec⁻¹ indicating that the Volmer reaction is the rate-determining step, and the exchange current density for hydrogen evolution at aluminium is estimated at 5 × 10⁻¹¹ A cm⁻². Anodic current responses to the return of the potential to the rest values were also recorded at three different time scales. The presence of some substances, formed at the more negative potentials, other than gaseous hydrogen, was detected and their dependence on potential and cathodic pulse duration is discussed.