Azocalixarenes: Synthesis, Characterization, Complexation, Extraction, Absorption Properties and Thermal Behaviours

Azocalixarenes, which have a conjugated chromophore azo (–N=N–) group in p-positions, are synthesized in “one-pot” procedures in satisfactory yields. Their structures in the solid and solution are elucidated by UV–vis, FT-IR, ¹H and ¹³C NMR spectroscopic methods as well as elemental analysis techniques. Some of them are complexed with metal ions (alkali, alkaline-earth and transition metal ions) under neutral conditions. A wide variety of applications is expected by the functionalization of the side arms. The selective liquid–liquid extraction of various alkali, alkaline-earth and transition metal cations from the aqueous phase to the organic phase is carried out by using azocalixarenes. Furthermore, the synthesized azocalixarenes are utilized for selective extraction of Fe³⁺ cations from the aqueous phase to the organic phase. The effects of varying pH and solvent upon the absorption ability of azocalixarenes substituted with electron-donating and electron-withdrawing groups at their o-, m-, p-positions are examined. The thermal behaviours of azocalixarenes containing upper rim functionalized groups are investigated by means of thermogravimetry (TG), differential thermal analysis (DTA) and differential thermogravimetry (DTG).     

Fast solid-phase extraction-gas chromatography-mass spectrometry procedure for oil fingerprinting. Application to the Prestige oil spill

A rapid and simple fractionation procedure using solid-phase extraction (SPE) cartridges was developed for an accurate determination of aliphatic and polycyclic aromatic hydrocarbons in petroleum residues and further application in chemical fingerprinting of oil spills by gas chromatography-mass spectrometry (GC-MS). Among the adsorbents evaluated, SiO2/C3-CN exhibited the best selectivity, providing, by elution with n-hexane (4 ml) and n-hexane-CH2Cl2 (1:1) (5 ml), two well-resolved aliphatic and aromatic hydrocarbon fractions, with recoveries of 97 +/- 7.2 and 99.7 +/- 13.9%, respectively. The SPE fractionation procedure was compared with the conventional silica-alumina adsorption chromatography showing similar results but practical advantages in terms of reproducibility, analysis time, solvent reduction and cost. Moreover, is particularly suitable for routine analysis with a high sample throughput. The developed methodology was tested in the characterization of fuel-oil samples collected along the Spanish north-west coast, after the Prestige oil spill accident.     

Use of 1-alkyl-3-methylimidazolium hexafluorophosphate room temperature ionic liquids as chelate extraction solvent with 4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedione

Possible use of room temperature ionic liquids (RTILs) as chelate extraction solvent was evaluated by using 1-butyl-3-methylimidazolium hexafluorophosphate ([bmim][PF₆]), 1-hexyl-3-methylimidazolium hexafluorophosphate ([hmim][PF₆]) and 1-octyl-3-methylimidazolium hexafluorophosphate ([omim][PF₆]). These RTILs showed high extraction performance for divalent metal cations with 4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedione (Htta). The extracted metals were back-extracted into 1 mol dm⁻³ nitric acid quantitatively. Furthermore, the extracted species were estimated as neutral hydrated complexes M(tta)₂(H₂O)_n (n= 1 or 2) for M = Ni, Cu and Pb and anionic complexes M(tta)₃⁻ for M = Mn, Co, Zn and Cd.     

Determination of volatile phenols in fino sherry wines

An easy, fast and reliable analytical method is proposed to determine the concentration of volatile phenols (ethyl- and vinylphenols) in fino sherry wines. The technique employed is a single stage sample treatment by solid-phase extraction (SPE) following a simple, fast procedure that enables 12 samples to be extracted simultaneously and requires a small volume sample and little time. Subsequently, the extracts are analyzed by gas chromatography (GC) with flame ionization detection. The method proposed has been applied to the study of fino sherry wines affected by microbial contamination with yeasts of the Brettanomyces genus, and the relationship of these yeasts with the concentrations of volatile phenols present in this wine.     

中厚板轧后快速冷却系统设计与应用

为了完善和丰富钢板的品种和规格,同时提高产品质量和轧制生产效率,针对武钢轧板厂生产线实际情况,设计了一套具有国内领先技术的中厚板轧后快速冷却系统.系统应用工业变频供水、高压水箱水量优化分配及高密度层流等先进技术,同时采用了西门子高性能控制器进行系统综合控制.该系统结构合理,功能完善,控制精度高,已成功投入使用,取得了良好效果.     

水帘极板静电除尘模型的收集性能实验研究

建立了水帘极板电除尘器实验模型,研究了其电晕特性,以及极距、电场风速、水帘流量、供电电压、初始粉尘浓度等参数对除尘效率的影响.结果表明:水帘形成好坏对V-I特性曲线有一定影响,水帘流量影响形成水帘好坏的程度,因而影响除尘效率;极距对除尘效率有较大影响,极距300mm时除尘效率最高;供电电压对除尘效率的影响较为明显,随着电压的升高除尘效率也升高;风速增大除尘效率降低,初始粉尘浓度对除尘效率影响较小.     

白花茵陈茎叶中挥发油化学成分的研究

分别采用水蒸气蒸馏和石油醚萃取法提取白花茵陈中的挥发油,并通过GC-MS对其化学成分进行了分析鉴定.结果表明,2种方法提取的挥发油的主要化学成分基本相似,主要为萜烯类及其含氧衍生物（如百里香酚和香荆芥酚）和脂肪酸及其酯等.     

青藏高原油菜蜂花粉中黄酮类物质的提取与开发的实验设计

本文根据作者从事的青藏高原油菜蜂花粉中黄酮类物质的提取和开发应用的研究，探讨了综合实验的设计，把科学研究引入到实验教学中，将会极大地促进高校的实验教学改革．     

基于选区的彩色图像抽取和融合算法研究

给出了一种利用图像中定义的选择区域（选区），从复杂背景中尽可能保持原样地提取出所关心图像的图像抽取方法；同时还介绍了如何对抽出的图像进行融合设置，进行看似自然的、无缝的融合；另外对算法的应用过程进行了适当的描述，作出算法的实际使用情况说明．     

修饰聚合物液-固亲和体系萃取测定试样中的铜

用亚胺基二乙酸(IDA)修饰聚乙二醇(PEG)8000与吐温80,构建了修饰聚合物-盐-水液-固亲和萃取体系,用于萃取发样、中草药、水样中的铜.在吐温80体积分数5%,(NH4)2SO4浓度1.66 mol/L,PEG-(IDA)2质量浓度0.1%,pH 3.30的萃取条件下 ,Cu(Ⅱ)的萃取率>96.46% .连续变换法测定Cu(Ⅱ)和PEG-(IDA)2的摩尔比是2∶1,由螯合物离解度计算配合物的表观稳定常数lgK= 5.53.该体系的萃取机理是:Cu(Ⅱ)与PEG-(IDA)2形成电中性的螯合物,与非离子型表面活性剂吐温80的羟基实现氢键作用而被萃取.