沉积铁钝化膜的傅立叶变换表面增强拉曼光谱

利用恒电流沉积技术、傅立叶变换表面增强拉曼散射技术现场研究了0 1mol/LNaOH溶液中铁金属电极在不同电位下的表面氧化物的组成。结果表明,在电极预钝化区,表面首先生成的Fe(OH)2可由拉曼谱图中出现的550cm-1表征,证实了以往的研究结果。进入钝化区,表面二价氧化物逐步转化为高价氧化物Fe3O4及α 、δ 和γ FeOOH。在电位回扫的过程中,各氧化产物的还原以及铁表面SERS活性的逐渐消失导致谱峰强度降低。     

开放式微波消解与干灰化法消解测量食品中铅的方法比较

对开放式微波消解法与干灰化法消解测量食品中铅的方法进行了比较，试验表明，前者操作简易，试验周期短，在测量精度和加标回收率方面两种方法无显著性差别。     

The role of variable surface charge and surface complexation in the adsorption of humic acid on magnetite

The ionic strength dependence of humic acid (HA) adsorption on magnetite (Fe₃O₄) was investigated at pH 5, 8 and 9, where variable charged magnetite is positive, neutral and negative, respectively. The adsorption studies revealed that HA has high affinity to magnetite surface especially at lower pH, where interacting partners have opposite charges. However, in spite of electrostatic repulsion at pH 9 notable amounts of humate are adsorbed. Increasing ionic strength enhances HA adsorption at each pH due to charge screening. The dominant interaction is probably a ligand-exchange reaction, nevertheless the Coulombic contribution to the organic matter accumulation on oxide surface is also significant under acidic condition. The results from size exclusion chromatography demonstrate that the smaller size HA fractions enriched with functional groups are adsorbed preferentially on the surface of magnetite at pH 8 in dilute NaCl solution.     

巯基乙酰萘胺极谱行为研究及分析应用 Ⅱ.银(Ⅰ)离子的示波极谱测定

在前文研究的基础上,经试验,证明Ag(Ⅰ)与巯萘剂(TN)反应生成非电活性物质,导致电活性物质DTN电流降低。在最佳条件下,Ag(Ⅰ)浓度在3.7×10~(-8)～4.5×10(-7)mol/L范围内与DTN电流峰高降低值成线性关系,检出限为2.2×10~(-8)mol/L(相当于2.4ng/ml)Ag(Ⅰ)。方法用于纯镍和氢氧化钾中痕最银的测定,结果满意。     

Kinetic features of ethylene polymerization over supported catalysts [2,6‐bis(imino)pyridyl iron dichloride/magnesium dichloride] with AlR3 as an activator

The effects of polymerization temperature, polymerization time, ethylene and hydrogen concentration, and effect of comonomers (hexene‐1, propylene) on the activity of supported catalyst of composition LFeCl₂/MgCl₂‐Al(i‐Bu)₃ (L = 2,6‐bis[1‐(2,6‐dimethylphenylimino)ethyl] pyridyl) and polymer characteristics (molecular weight (MW), molecular‐weight distribution (MWD), molecular structure) have been studied. Effective activation energy of ethylene polymerization over LFeCl₂/MgCl₂‐Al(i‐Bu)₃ has a value typical of supported Ziegler–Natta catalysts (11.9 kcal/mol). The polymerization reaction is of the first order with respect to monomer at the ethylene concentration >0.2 mol/L. Addition of small amounts of hydrogen (9–17%) significantly increases the activity; however, further increase in hydrogen concentration decreases the activity. The IRS and DSC analysis of PE indicates that catalyst LFeCl₂/MgCl₂‐Al(i‐Bu)₃ has a very low copolymerizing ability toward propylene and hexene‐1. MW and MWD of PE produced over these catalysts depend on the polymerization time, ethylene and hexene‐1 concentration. The activation effect of hydrogen and other kinetic features of ethylene polymerization over supported catalysts based on the Fe (II) complexes are discussed. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 5057–5066, 2007     

Protection of iron corrosion by stearic acid and stearic imidazoline self-assembled monolayers

A type of stearic imidazoline (IM) inhibitor was prepared using stearic acid (SA) and diethylenetriamine (DETA) as raw materials. The monolayers of IM and SA were assembled on the iron surface. The electrochemical characterization of stearic acid (SA) and stearic imidazoline (IM) on an oxide free iron surface had been studied. The monolayers of IM inhibitor were characterized by electrochemical impedance spectroscopy (EIS), electrochemical polarization curves, double layer capacitance, X-ray photoelectron spectroscopy (XPS) and molecular simulation. The results of electrochemical studies had illustrated that the inhibition efficiency of IM was higher than SA. XPS showed that the IM molecules adsorbed on the iron surface. The molecular simulation calculations showed that the IM molecules were tilted at an angle on the iron surface.     

Slow positron beam study of corrosion-related defects in pure iron

Corrosion-related defects of pure iron were investigated by measuring Doppler broadening energy spectra (DBES) of positron annihilation and positron annihilation lifetime (PAL). Defect profiles of the S-parameter from DBES as a function of positron incident energy up to 30 keV (i.e. ∼1 μm depth) were analyzed. The DBES data show that S-parameter increases as a function of positron incident energy (mean depth) after corrosion, and the increase in the S-parameter is larger near the surface than in the bulk due to corrosion. Furthermore, information on defect size from PAL data as a function of positron incident energy up to 10 keV (i.e. ∼0.2 μm depth) was analyzed. In the two-state trapping model, the lifetime τ₂ = 500 ps is ascribed to annihilation of positrons in voids with a size of the order of nanometer. τ₁, which decreases with depth from the surface to the bulk, is ascribed to the annihilation of positrons in dislocations and three-dimensional vacancy clusters. The corroded samples show a significant increase in τ₁ and the intensity I₂, and near the surface the corroded iron introduces both voids and large-size three-dimensional vacancy clusters. The size of vacancy clusters decreases with depth.     

火焰原子吸收光谱法测定巨大口蘑子实体中的铁、锌和锰

采用火焰原子吸收光谱法测定了巨大口蘑子实体中的微量元素铁、锌和锰的含量,方法简单,精密度和灵敏度高,相对标准偏差为0.378%-0.842%,回收率95.83%-99.45%.