三(2-苯并咪唑亚甲基)胺硝酸镍(Ⅱ)配合物的合成及结构

三（２－苯并咪唑亚甲基）胺简称ＮＴＢ与Ｎｉ（Ⅱ）的硝酸盐形成配合物Ｃ２８Ｈ３５Ｎ９Ｏ９Ｓ２Ｎｉ。本文报道其合成，红外光谱及晶体结构。该化合物为三斜晶系，空间Ｐ１↑－，ａ＝９．６５０（３），ｂ＝１２．７１６（２），ｃ＝１４．４３６Ａ，α＝１１．４６（２），β＝９１．６６（３），γ＝９７．５５（２）°，Ｖ＝１７１８（２）Ａ＾３，Ｚ＝２，Ｆ（０００）＝７９３，Ｄｃ＝１．４８ｇ／ｃｍ＾３，Ｍｒ＝７６４．１     

Fe（Ⅲ）－TEA－5－Br－PADAP－H_2O_2体系中催化波的研究及其应

在０．２ｍｏｌ·Ｌ￣（－１）ＮＨ＿４Ｃｌ－ＮＨ＿３·Ｈ＿２Ｏ底液中，（ｐＨ为９．２６），得到一个极为灵敏的Ｆｅ（Ⅲ）－ＴＥＡ－５－Ｂｒ－ＰＡＤＡＰ－Ｈ＿２Ｏ＿２配合吸附催化波，其峰电位为－０．７１Ｖ（ｖｓ．ＳＣＥ）。铁浓度在１．８×１０￣（－１０）～５．４×１０￣（－６）ｍｏｌ·Ｌ￣（－１）范围内与二阶导数波高呈线性关系。对该极谱波的性质进行了研究，证明是一种配合吸附催化波，并成功地应用于各类水样，钒催化剂中微量或痕量铁的测定。     

Simultaneous EQCM and diffuse reflectance UV-visible spectroelectrochemical measurements: poly(aniline-co-o-anthranilic acid) growth and property characterization

Piezoelectric diffuse reflectance spectroelectrochemistry (PDRSEC), a new technique of diffuse reflectance spectroelectrochemistry (DRSEC) in combination with electrochemical quartz crystal microbalance (EQCM), was developed to study the electrochemical copolymerization of aniline and o-anthranilic acid in 1.0 mol l(-1) HClO4 and the properties of these copolymers. The DRSEC using an integral sphere was proven to possess a higher optical sensitivity at the unpolished piezoelectric quartz crystal electrodes used than the mirror reflectance spectroelectrochemistry mode. The copolymers grown from the copolymerization bath of different molar fractions of o-anthranilic acid (F1, relative to the total amount of the two monomers) showed intermediate properties between those of the homopolymers, which varied gradually with F1. The swelling/dissolution behavior of the copolymers vs solution pH was traced via the EQCM frequency and resistance signals, and its large dependence on F1 was found and discussed. In a HAc-NaAc buffer solution at pH 5.6, the amount of adsorbed lysozyme was found to be positively correlated with F1, via an EQCM impedance investigation, demonstrating the feasibility of using poly(aniline-co-o-anthranilic acid) as a load-adjustable immobilization matrix for cationic proteins. The novel PDRSEC method proposed is highly recommended for surface electrochemistry studies at relatively rough electrodes.     

反气相色谱法研究聚丙烯结晶动力学及对熔点和结晶度的测定

<正> 研究聚合物的结晶动力学,过去大多采用膨胀计法和解偏振光法。曾有文献报道采用反气相色谱法测得聚乙烯等温结晶线。通过实验可知,测定聚丙烯结晶度时,试样热历史和测定前陈化温度的选择均影响测定结果。此外在测定聚丙烯试样的熔点时,保留图中出现了两个转折,经反复实验证实:此两转折对应于聚丙烯中不同晶形(α-、β-形)的熔点。     

单分散纳米InVO4(正交相)的低温合成

InVO₄ is a new developed visible light responding photocatalyst for water decomposition, which is obtained by a solid-state reaction at high temperature traditionally. In this paper, pure InVO₄ nano-crystalline powder has been prepared by a hydrothermal process at low temperature and was characterized by TEM, IR, and X-ray diffraction. Many factors such as pH value, reaction time and temperature have been investigated. It is found that the optimal conditions for the preparation is: n_InCl3∶n_NaVO3=1∶2; temperature : 150 ℃; Reaction time: 4～8 h; pH=7.9～8.0. And the experimental result shows that it is a convenient way to get single dispersing InVO₄ nano-crystalline powder by flux in alkyl alcohol.     

重油催化裂化汽油中含氮化合物的分析

利用酸萃取技术浓缩分离重油催化裂化（RFCC）汽油中的氮化物，比较了两种萃取剂和两种油剂比对分离效果的影响，结果发现选用10％（体积分数）HCl作萃取剂，油剂比为10：1（体积比）时，碱性氮化物的提取率较高；浓缩分离出的氮化物用色谱－质谱联用方法对其进行了检测，结果表明RFCC汽油中的氮化物主要是C0－C2苯胺及少量吡啶类、喹啉类碱性氮化物。     

氨基酚异构体的离子对反相液相色谱分析的研究

本文研究了离子对反相液相色谱分析氨基酚异构体的可能性、影响因素和色谱条件，发现以含４×１０－８ｍｏｌ／Ｌ四丁基碘化铵、０．１８４ｍｏｌ／Ｌ醋酸钠的甲醇水溶液（２３：７７）作为流动相，ＯＤＳ为固定相时可以实现氨基酚异构体的良好分离。     

烯丙基碘和锡与醛的选择加成反应

含活性基团的醛可与烯丙碘和锡粉直接进行亲核加成反应，得到高烯丙基的醇，水的存在不利于此反应的进行，与烯丙基溴相比，烯丙基碘反应活性更强，可在短时间内得较高的产率。     

Binding of wogonin to human serum albumin: a common binding site of wogonin in subdomain IIA

The binding of wogonin to human serum albumin (HSA) has been studied by spectroscopic method including circular dichroism (CD), infrared spectra (IR) and fluorescence spectra. The fluorescence properties of HSA were examined in presence of wogonin and the fluorescence intensity of HSA was significantly decreased in the presence of wogonin. The binding parameters of wogonin were studied from the fluorescence decreasing of HSA by the fluoremetric titrations. The Stern-Volmer plots indicated that the binding of wogonin to HSA at 296, 303, 310 K is characterized by one binding site with the binding constant K(S-V) at 1.872 x 10(5), 1.561 x 10(5), 1.392 x 10(5), respectively, which are good agreement with the results from the Scatchard plots. The binding process was exothermic, enthalpy driven and spontaneous, as indicated by the thermodynamic analyses, and the major part of the binding energy is hydrophobic interaction, which were consistent with the result of molecule modelling study, and there are also a numbers of hydrogen bonds between wogonin and HSA. Furthermore, the displacement experiments indicate that wogonin can bind to the subdomain IIA, that is, the site I of HSA, which is also good agreement with the result of molecule modelling study.     

Highly efficient visible-light photocatalytic ethane oxidation into ethyl hydroperoxide as a radical reservoir

Photocatalytic ethane conversion into value-added chemicals is a great challenge especially under visible light irradiation. The production of ethyl hydroperoxide (CH₃CH₂OOH), which is a promising radical reservoir for regulating the oxidative stress in cells, is even more challenging due to its facile decomposition. Here, we demonstrated a design of a highly efficient visible-light-responsive photocatalyst, Au/WO₃, for ethane oxidation into CH₃CH₂OOH, achieving an impressive yield of 1887 μmol g_cat⁻¹ in two hours under visible light irradiation at room temperature for the first time. Furthermore, thermal energy was introduced into the photocatalytic system to increase the driving force for ethane oxidation, enhancing CH₃CH₂OOH production by six times to 11 233 μmol g_cat⁻¹ at 100 °C and achieving a significant apparent quantum efficiency of 17.9% at 450 nm. In addition, trapping active species and isotope-labeling reactants revealed the reaction pathway. These findings pave the way for scalable ethane conversion into CH₃CH₂OOH as a potential anticancer drug.

Highly efficient visible-light driven photocatalytic oxidation of ethane into ethyl hydroperoxide was realized for the first time over Au/WO₃.