2A12-T6铝合金表面双-(γ-三乙氧基硅丙基)四硫化物薄膜的特性

采用傅立叶变换红外光谱分析了2A12-T6铝合金表面自组装双-(!-三乙氧基硅丙基)四硫化物硅烷偶联剂(SCA)薄膜结构特征,并采用电化学极化曲线评价了薄膜的耐蚀性能.结果表明,铝材表面自然晾干,SCA薄膜分子之间主要通过氢键连接,腐蚀电流密度减小1个数量级以上.120℃的加热处理促进铝板表面通过SiOSi链接而形成SCA网状薄膜结构,并通过在界面上形成SiOAl界面相结构而与铝板表面牢固连接,腐蚀电流密度降低2个数量级以上.SCA乙醇溶液浸泡处理10min比浸泡2s～1min的铝板表面SCA薄膜内氢键缔合羟基要多.     

VOCl_3/Et_3Al_2Cl_3/CCl_4溶剂体系催化乙烯丙烯共聚

本文以VOCl_3/Et_3Al_2Cl_3为催化剂,在CCl_4溶剂中进行乙烯共聚反应。在聚合过程中,发生一异常的颜色突变现象。颜色突变后,体系催化聚合生成分子量很低的产物。从聚合物的结构表征及机理探讨表明:颜色突变后,体系产生了新的活性中心,催化机理发生了转变——由配位机理转变为阳离子机理。     

A downsized flow set up based on multicommutation for the sequential photometric determination of iron(II)/iron(III) and nitrite/nitrate in surface water

In this work, a downsized flow set up designed based on multicommutation concept for photometric determination of iron(II)/iron(III) and nitrite/nitrate is surface water is described. The flow system network comprised a set of three-way solenoid valves, reaction coil and a double-channel flow cell, which were nested in order to obtain a compact and small-size instrument. To accomplish the downsizing requirement light source (LED) and radiation detection (phototransistor) were coupled to the flow cell. In order to demonstrated the effectiveness of the system, the photometer methods based on Griess reaction and 1-10-phenantroline for nitrite and iron(II) determination, respectively, were selected. Under computer control the set up provided facilities to handle four reagent solutions employing a single pumping channel, thus permitting also the determination of nitrate and iron(III) after its reduction to nitrite and to iron(II), respectively. The overall system performance was demonstrated working several days running standard solution, no significant variation of base line, linear response range and slop (less than 1%) were observed. The usefulness of the downsized system was ascertained by analyzing a set of surface water. Aiming to access the accuracy sample were also analyzed employing reference procedures and no significant difference at 95% confidence level were observed for the four analytes. Other profitable features such as analytical throughput of 40 determination per hour; relative standard deviation of 1%; linear response range between 50 and 300 μg l⁻¹ for nitrite and nitrate, 0.5-6.0 mg l⁻¹ iron(II) and iron(III); low reagent consumption 75 μg for nitrate/nitrite and 0.6 mg for iron(II)/iron(III) per determination; and 2.4 ml waste generation per determination were also achieved.     

气相色谱质谱法快速测定人血浆中克仑特罗

血浆样品经0.01mol·L-1盐酸和无水乙醇浸取,在碱性条件下用氯仿萃取,GG-MS-选择离子测量法测定,外标法定量。在选定的色谱条件下,盐酸克仑特罗的检出限为0.05ng,线性范围为0.1-100ng,方法的平均回收率为95.6％,RSD小于6.82％(n=6)。该法毋需衍生化,基质无干扰,简便可靠,适用于生物材料中克仑特罗的快速分析。     

混合稀土对共晶Al-2%Fe合金组织形态的影响

研究了富La混合稀土对共晶Al-2?合金组织形态的影响. 当混合稀土加入量较少时, 合金中的α-Al相为明显的胞状枝晶;随着混合稀土加入量的增加, α-Al枝晶优先形核生长得到抑制, 共晶Al3Fe相得到细化;当稀土加入量增至0.6% (质量分数)共晶Al3Fe相尺寸逐渐增大. 并对混合稀土对共晶Al-2?合金组织形态的影响机制进行了探讨.     

Synthetic receptors based on calix[4]arene functionalized at the lower rim in molecular recognition of dicarboxylic, α-hydroxycarboxylic,and α-amino acids

New calix[4]arenes, di- and tetrasubstituted at the lower rim, with different functional groups were synthesized. They were studied as carriers of a series of dicarboxylic and -hydroxycarboxylic acids through a liquid impregnated membrane. The calix[4]arenes under study are capable of molecular recognition of oxalic acid in the series of structurally similar dicarboxylic and -hydroxycarboxylic acids. The regularities found make it possible to change purposefully the receptor ability of 1,3-disubstituted calix[4]arenes by variation of the nature of substituents.     

A High Sensitivity Fluorescent Chemo-sensory System Based on β-Cyclodextrin Dimer Modified with Dansyl Moieties

-Cyclodextrin dimer linked with ethylenediamine at the upper rim of the cyclodextrin has been synthesized and then modified with two dansyl moieties inthe presence of N,N'-dicyclohexylcarbodiimide. The sensing ability and bindingproperty of the title compound were investigated for steroids and terpenoids. Thefluorescence intensity of this dimer was decreased when a host–guest complex was formed. The value I/I⁰, where I⁰ and I are fluorescence intensitiesin the absence and presence of a guest and I is I⁰- I, was used as a parameter of sensitivity. This host exhibited a much higher sensitivity and selective molecular recognition ability for bile acids such as ursodeoxycholic acid andchenodeoxycholic acid and terpenoids such as (-)-borneol than the dansyl-modifiedcyclodextrins reported previously including -cyclodextrin dimer. The behaviors of the appended moieties of the host during the formation of host–guest complexes were studied using induced circular dichroism (ICD) and fluorescence spectra. The ICD intensityof this dimer was decreased on accommodation of a guest and this spectral pattern of the title dimer was opposite to that of bis dansyl-modified -cyclodextrin monomer. Theguest-induced variations in the fluorescence and ICD intensities suggest that this dimer formed a 1 : 1 host–guest complex and the appended moieties act as a hydrophobic cap.     

Can the new ISO Guide 25/EN 45001 create better confidence in laboratory operations?

 Confidence in laboratory operations is discussed based on the ongoing revision of the ISO/IEC Guide 25. Confidence is a subjective attribute, which also depends on whose interest is considered. New and better-defined quality systems and technical elements will be included, and these are beneficial to the transparency of laboratory operations, as well as to the accreditation process. The ultimate aim is, of course, to satisfy customers. The testing laboratories' industrial customers are, however, generally unfamiliar with the ISO/IEC Guide 25 and accreditation. The main reason for improved confidence in testing and calibration laboratories is foreseen to come from closer interaction between laboratories and their customers.     

粉末化学镀法制备的NiB／TiO2非晶态合金催化剂对环丁烯砜加氢反应的催化性能

 采用诱导沉积法及粉末化学镀法分别制备了纯态NiB及负载型NiB／TiO2非晶态合金催化剂．用XRD，ICP，SEM，TEM和DSC等手段对催化剂的物性及TiO2载体与NiB非晶态合金之间的相互作用进行了表征，考察了非晶态合金的结构、组成、形貌和热稳定性，并将其用于环丁烯砜加氢反应中．结果表明，相对于NiB而言，NiB／TiO2催化剂具有优良的热稳定性和催化活性，这缘于NiB和TiO2载体之间的相互作用及载体的分散作用．     

氢化物发生石墨炉原位富集直接测定高温镍基合金中碲

通过选择碲的氢化物发生条件，克服了高含量镍对碲的干扰，把氢化物富集在涂钯石墨管里，然后再原子化，成功地测定了高温镍基合金中碲。