Analysis of trace mercury in water by solid phase extraction using dithizone modified nanometer titanium dioxide and cold vapor atomic absorption spectrometry

A new method for analysis of trace mercury in water samples was developed, based on the combination of preconcentration/separation using dithizone-modified nanometer titanium dioxide (TiO2) as a solid phase extractant and determination by cold vapor atomic adsorption spectrometry (CVAAS). Dithizone was dissolved with alcohol and loaded on the surface of nano-sized TiO2 powders by stirring. The static adsorption behavior of Hg2 on the dithizone-modified nanoparticles was investigated in detail. It was found that excellent adsorption ratio for Hg2 could be obtained in the pH range of 7-8 with an oscillation time of 15 min, and a 5 mL of 3.5 mol·L-1 HCl solution could quantitatively elute Hg2 from nanometer TiO2 powder. Common coexisting ions caused no obvious influence on the determination of mercury. The mechanisms for the adsorption and desorption were discussed. The detection limit (3σ) for Hg2 was calculated to be 5 ng·L-1. The proposed method was applied to the determination of Hg2 in a mineral water sample and a Zhujiang River water sample. By the standard addition method, the average recoveries were found to be 94.4%-108.3% with RSD (n = 5) of 2.9%-3.5%.     

飞行时间二次离子质谱--强有力的表面、界面和薄膜分析手段

二次离子质谱（Secondary ion mass spectrometry，简称SIMS）是一种对表面灵敏的质谱技术，建立在表面各种类型带正、负电荷原子或分子发射的基础上。用飞行时间（Time of flight，简称TOF）仪器对这些二次离子进行质量分析，能确保并行质量登录、高质量范围、高流通率下的高分辨和精确质量测定这些优异性能。配合细聚焦扫描一次离子束，可在优于1nm的高深度分辨和优于50nm的横向分辨本领下，实现对表面优于单层ppm(百万分之一）量级的极高检测灵敏度。当今TOF－SIMS已发展为一种成熟且完善的表面分析技术。极高的灵敏度，再加上即使对大分子及不易挥发性分子都独具的敏感性，使它成为很多高技术领域不可缺少的分析手段，这些领域包括微电子学、化学和材料科学以至纳米技术和生命科学等。本文简述了TOF－SIMS的原理、仪器及其多方面的应用和展望。     

大体积砼产生裂缝的原因及防治措施

大体积砼裂缝问题是建筑业普通关心的问题.对砼裂缝进行控制,就必须研究砼结构中裂缝产生的原因以及在实际的设计和施工过程中采取合理的、经济的措施来控制裂缝.本文通过对大体积砼裂缝成因的理论研究,提出了合理的裂缝控制的设计和施工措施.     

调谐质量阻尼器参数设计中的两个问题

本文以单自由度系统安装一个调谐质量阻尼器（简称TMD）为例，对抗风和抗震两类不同激励工况下TMD的参数设计问题进行了理论研究与对比分析。通过给出相对误差系数的概念，定量评价了不同的参数方法对TMD减振性能的影响程度。本文的研究为TMD的参数设计提供了理论指导。     

Uncertainty in Quantitative Electron Probe Microanalysis

Quantitative electron probe analysis is based on models based on the physics or x-ray generation, empirically adjusted to the analyses of specimens of known composition. Their accuracy can be estimated by applying them to a set of specimens of presumably well-known composition.     

Structural Description of Polyaromatic Nucleus in Residue

The proton nuclear magnetic resonance spectroscopy （1H-NMR）, the synchronous fluorescence spectrometry （SFS） and the ruthenium ions catalyzed oxidation （RICO） method were used to determine the chemical structure of polyaromatic nucleus in Oman residue fractions. The results of 1H-NMR analyses showed that the average numbers of aromatic rings in the aromatics, resins and asphaltenes units were 3.2, 5.6 and 8.2, respectively. SFS was used to investigate the distribution of aromatic rings in residue fractions, the main distribution range of aromatic rings in aromatics, resins and asphaltenes were 3 4 rings, 3--5 rings and more than 5 rings, respectively. The aromatic network in residue fractions was oxidized to produce numerous carboxylic acids. The types and content of benzenepolycarboxylic acids, such as phthalic acid, benzenetricarboxylic acids, benzenetetracarboxylic acids, benzenepentacarboxylic acid and benzenehexacarboxylic acid disclosed the condensed types of aromatic nuclei in the core. The biphenyl fraction （BIPH）, the cata-condensed fraction （CATA）, the peri-condensed fraction （PERI） and the condensed index （BCI） were calculated based on the benzenepolycarboxylic acids formed. The results implied that there was less biphenyl type structures in all residue fractions. The aromatics fraction was almost composed of the cata-condensed type system, and the asphaltenes fraction was wholly composed of the peri-condensed type system, while in the resins fraction co-existed the two types, herein the peri-con- densed type was predominant over the cata-condensed type. Based on the analytical results obtained in the study, the components --aromatics, resins and asphaltenes -- were given the likely structural models.     

新型涂料增稠剂的化学成分鉴定

本文用红外光谱法对一种新型涂料增稠剂进行了化学成分鉴定,其主要成分为羟丙基甲基纤维素与蒙脱土。     

Temperature effects on the mass flow rate in the SBI and similar heat‐release rate test equipment

In various medium‐to‐large‐scale fire test equipments like the ISO room corner test (RC), and more recently, the single burning item test (SBI) the mass flow rate measurement of the combustion gases plays a key role in the determination of the heat‐release rate and smoke‐production rate. With the knowledge of the velocity profile and the temperature of the flow, the mass flow rate is obtained by measuring the velocity on the axis of the duct. This is done by means of a bi‐directional probe based on the pitot principle. However, due to the variation of the mean temperature and the temperature gradient in any cross section of the duct, introduced by ever changing combustion gas temperatures, the velocity nor the density profile are constant in time. This paper examines the resulting uncertainty on the mass flow rate. Copyright © 2006 John Wiley & Sons, Ltd.     

Mass transfer kinetics of neodymium(III) extraction by calix[4]arene carboxylic acid using a constant interfacial area cell with laminar flow

BACKGROUND: Thermodynamics and kinetics data are both important to explain the extraction property. In order to develop a novel separation technology superior to current extraction systems, many promising extractants have been developed including calixarene carboxylic acids. The extraction thermodynamics behavior of calix[4]arene carboxylic acids has been reported extensively. In this study, the mass transfer kinetics of neodymium(III) and the interfacial behavior of calix[4]arene carboxylic acid were investigated. RESULTS: The rate constant (K_ao) becomes constant when the stirring speed was controlled between 250 rpm and 400 rpm. The activation energy (E_a) was calculated to be 21·41 kJ mol^?1 or 88·17 kJ mol^?1 (dependent on temperature) from the slope of log K_ao against 1000/T. The linear relationship between the specific area and the extraction rate is the characteristic of an interfacial reaction control. The minimum bulk concentration of the extractant necessary to saturate the interface (C_min) is lower than 4·19 × 10^?4 mol L^?1. CONCLUSION: The effect of stirring speed, temperature, and species concentration on the extraction rate demonstrates that the extraction regime depends on the extraction conditions. The chemical reaction control governs the extraction regime at temperatures below 303 K and a mixed control regime occurs when the temperature is between 303 K and 318 K. The probable locale for the chemical reaction is at the liquid–liquid interface and the rate equation is deduced to be: ? d[Nd³⁺]_(a)/dt = k_f[Nd³⁺]_(a)[H₄A]_(o)^0·727[H⁺]_(a)^?0·978. The rate‐controlling step was suggested by the analysis of the experimental results. Copyright © 2008 Society of Chemical Industry     

Secondary ion emission from Ti and Si targets induced by medium energy Ar ion bombardment - Experiment and computer simulation

The paper presents experimental results of secondary ion energy distributions obtained for Ti and Si targets bombarded by 20-30 keV monoisotope Ar⁺ ion beam. The influence of the extraction voltages between target and a slit of the electrostatic energy analyzer entrance on the energy distributions of secondary ions was investigated. After optimization of the secondary ion extraction system, the mass spectra of secondary ions were also measured. The investigations were done using recently built experimental system. Experimental data are compared with the computer simulation results obtained using TRQR and SATVAL codes.