Atom-probe field ion microscopy

The atom probe field ion microscope (AP-FIM) is a combination of a field ion microscope and a time-of-flight mass spectrometer with a single ion detection sensivity. With the field ion microscope topology of a surface, surface reactions and surface modifications can be studied in atomic detail. By time-of-flight measurements surface layers and interface layers can be chemically analyzed atom by atom and atomic layer by atomic layer. Compositional variations according to surface or interface segregation, precipitations, or surface changes in corrosion or in electrochemical layer formation etc. can be studied quantitatively on a subnanometer scale. Some of our studies on related problems will be decribed briefly.     

氧化镍纳米晶体的制备及其过程分析

为了开发一种新型纳米氧化镍催化剂,能有效地应用于生物质气化过程中去除焦油,本文采用均匀沉淀法成功地制备了纳米氧化镍晶体,并利用TGA、FTIR、XRD、BET、YEM等分析手段对前驱体和产品的性能进行了表征.同时,对前驱体的分解过程进行了全面的分析.分析结果表明前驱体是水合碱式碳酸镍,其分子式为NiCO3·Ni(OH)2·nH2O,它能在360℃下完全分解转化为纳米NiO,同时煅烧条件对合成纳米NiO的晶体粒径影响很大.实验证实所得纳米NiO颗粒呈球形,分散性好,纯度较高,属立方晶系结构,平均粒径约为7.5nm,其BET表面积为187.98m2/g,这显示纳米NiO晶体具有作为高效催化材料的应用可行性.     

Dislocation driven chromium precipitation in Fe-9Cr binary alloy: a positron lifetime study

The influence of initial heat treatment on anomalous Cr precipitation within high temperature solubility region of the Fe–9Cr alloy has been investigated using positron lifetime studies. Air-quenched samples with pre-existing dislocations exhibited a distinct annealing stage in positron lifetime between 800 and 1100?K corresponding to Cr-precipitation. During this stage, Transmission Electron Microscopy showed fine precipitates of average size 4 nm, dispersed throughout the sample and from Energy-dispersive X-ray spectroscopy (EDS) analysis they are found to be Cr-enriched. The presence of dislocations is found to be responsible for Cr precipitation.     

Use of 2, 3-Butanedione Monoxime for Homogeneous Precipitation of Nickel (II)

Abstract

The solid monoxime of 2, 3-butanedione is a more convenient material than liquid dione for the homogenous generation of DMG. 2, 3-butanedione dioxime. Determinations of Ni in steels and in pure Ni(II) solutions have shown the optimum pH and order of adding reagents. Gravimetric and/or an EDTA titrimetric finish are possible for a method of reliability within ± 0.2 mg of Ni in 50–150 mg Ni. The solid has the same character and filterability as that from the 1960 dione method of Salesin and Gordon¹.     

罗丹明B分子印迹聚合物微球的合成及其在固相萃取中的应用

以罗丹明B为模板分子,丙烯酰胺为功能单体,乙二醇二甲基丙烯酸酯为交联剂,采用沉淀聚合法制备了罗丹明B分子印迹聚合物(MIP)微球,并用扫描电子显微镜表征。 采用紫外分光光度法测定了印迹分子罗丹明B与功能单体丙烯酰胺二者之间的结合常数(K=5.303×103 (mol/L)-1)和化学计量比(n=1)。 考察了沉淀剂的种类和用量对聚合物微球的影响。 将分子印迹聚合物微球应用于固相萃取材料自制固相萃取柱,从加标罗丹明B的红椒粉中萃取罗丹明B。 本文优化了固相萃取条件,高效液相色谱检测表明,在一定的萃取条件下,分子印迹聚合物对加标量为0.479 mg/kg的辣椒中罗丹明B的萃取加标回收率可达91.7％～103.5%。     

Preparation and characterization of imprinted microspheres for clopyralid

In this work, the molecularly imprinted polymers (MIPs) and non-imprinted polymers (NIPs) for clopyralid (3,6-DCP) were successfully synthesized via precipitation polymerization using methacrylic acid (MAA) as functional monomer, ethylene glycol dimethacrylate (EGDMA) as crosslinker and a mixture of butanone (MEK) and n-heptane as porogen under the existence of azobisisobutyronitrile (AIBN). The morphologies, particle sizes, structures, adsorption properties and selective recognitions of polymers were investigated systematically. The average particle sizes of MIP3 and NIP3 were 2.76 μm and 2.15 μm. The apparent maximum binding amount (Q_max) of MIP3 and NIP3 were 67.50 mg·g^?1 and 65.02 mg·g^?1 in Scatchard analysis. Langmuir isotherm displayed that the Langmuir constant (K_l) of MIP3 and NIP3 were 0.015 L·mg^?1 and 0.0065 L·mg^?1, the saturation adsorption capacity (Q_max) of MIP3 and NIP3 were 63.23 mg·g^?1 and 58.17 mg·g^?1. Lagergren pseudo-second-order kinetic plot described that the adsorption process of MIP3 was visualized as chemical absorption. Selectivity analysis revealed that MIP3 possessed highly specific recognition for 3,6-DCP.     

Targeted deposition of Au aerosol nanoparticles on vertical nanowires for the creation of nanotrees

Complex tree-like nanostructures with controlled morphology are becoming increasingly important for the development of nanoscale devices. The position of branches on III–V semiconductor nanotrees is determined by the distribution of Au seed particles. Here we report the dependence of the distribution of Au aerosol nanoparticles on nanowires on parameters including distance between wires, particle size, wire length, wire diameter, III–V material and particle charge. It was observed that different wire lengths and separation distances as well as different particle polarities have a significant effect on the resulting particle distribution while different wire diameters, particle diameters, materials and deposition voltages do not.     

Improved Method for the Determination of Polychlorinated Dibenzo-p-dioxins and Dibenzofurans (PCDD/Fs) in Sanitary Napkins

Abstract

An improved method was developed for determining highly toxic 2,3,7,8-substituted polychlorinated dibenzo-p-dioxins and polychlorinated dibenzo-p-furans (PCDD/Fs) in sanitary napkins. Samples were extracted by Soxhlet (50% dichloromethane/hexane) and sonication (hexane), and a multi-layer silica column was used for clean-up after acetone precipitation to separate the superabsorbent polymers. Improved separation efficiency of PCDD/Fs from sanitary napkins with a high level of superabsorbent polymers was achieved using the acetone precipitation method. Hexane was then applied as an alternative solvent to remove residual interfering substances including sticky components contained on sanitary napkins via alumina column chromatography in the second clean-up step. Recoveries approached 100% with an average relative standard deviation of less than 15%, and recoveries of internal standards were from 70.5 to 114.8% and 0.6 to 13.6% for the two extraction methods. The mean method detection limit was 0.075–0.968?pg/g for Soxhlet extraction and 0.0032–0.091?pg/g for sonication extraction. The established method meets the quality criteria for the screening of dioxins stated in EU Regulations 589/2014 and 709/2014, and therefore provides a suitable alternative for the determination of dioxins in sanitary napkins containing superabsorbent polymers.     

Supercritical fluid chromatography tandem mass spectrometry employed with evaporation-free liquid–liquid extraction for the rapid analysis of cinnarizine in rat plasma

Cinnarizine is a weak base, which can produce supersaturation and precipitation during gastrointestinal transit, affecting its absorption in vivo. Therefore, it is necessary to investigate whether the oral bioavailability of cinnarizine can be improved after co-administration with precipitation inhibitors or not. In order to evaluate the pharmacokinetic behavior of cinnarizine in rats, a simple, rapid, sensitive, and environmentally friendly supercritical fluid chromatography-tandem mass spectrometric method was established and validated. In this method, flunarizine, a structural analogue of cinnarizine, was selected as the internal standard, and cinnarizine was extracted from rat plasma using evaporation-free liquid–liquid extraction method. The analytes were separated on a Torus 1-AA column (3.0 mm × 100 mm, 1.7 μm) within 2.0 min, using a gradient elution procedure. The transitions of cinnarizine and flunarizine were m/z 369.1 → 167.1 and m/z 405.1 → 203.1, respectively. Cinnarizine showed good linear correlation in the range of 1–500 ng/ml with a lower limit of quantification of 1 ng/ml. The intra- and interday precision and accuracy of all quality control samples were within ±15%. This high-throughput, accurate, sensitive, and reproducible method has been successfully applied to study the effects of the precipitation inhibitor cinnarizine on the pharmacokinetics in rats.