Indirect automatic atomic absorption determination of sulphate based on its precipitation with barium

A continuous precipitation flame atomization atomic absorption spectrometric method for the indirect determination of sulphate is proposed. By using a reversed flow-injection configuration for precipitation as barium sulphate, this anion was determined in the range 10–150 g/ml, with a relative standard deviation of 2.6%. The sensitivity was increased by a factor of seven by using a nitrous oxide-acetylene flame to measure barium.     

Multiphoton-Ionization-Mass Spectrometry (MUPI-MS) [New Analytical Methods (34)]

Mass spectrometry is one of the most important analytical tools in chemistry, biology, medicine and related areas. During the past 30 years, methods have been developed, both for the qualitative as well as the quantitative analysis of a wide variety of substances. The introduction of lasers into chemistry has also profited mass spectrometry, since its nonlinear properties and its tunability open up fundamentally new frontiers. Multiphoton ionization mass spectrometry combines UV-spectroscopy and mass spectrometry, thus providing a two-dimensional method that enables substance-specific and even state-specific analyses. This progress report presents the fundamentals and possibilities of MUPI mass spectrometry and discusses investigations on amino acids, peptides, chlorophylls and sugars. For each substance, multiphoton ionization can be tuned in such a way that only the molecular ion is formed. An increase of laser intensity induces substance-specific fragmentations of the molecule, thus contributing to a quick and easy identification of the substance.     

亲和标记-基质辅助激光解吸电离飞行时间质谱用于蛋白质相对定量方法的研究

将亲和标记技术和基质辅助激光解吸电离飞行时间串联质谱联用,建立了蛋白质相对定量方法,以牛血清白蛋白为实验对象,考察了该方法的准确度、重现性等指标;又以数种标准蛋白混合物为研究对象,考察了该方法的动态范围及相应的标准偏差,为实际生物样品中差异蛋白质分析奠定了基础。     

Thermal Stability Of Folic Acid in the solid-state

This study attempts to identify the degradative process which folic acid undergoes in the solid-state under thermal stress. In order to facilitate the process, the various pieces of the chemical structure, namely, p-amino benzoic acid, pterin and glutamic acid as both its d- and l-isomers were investigated as separate entities. These structured solid-state pieces were then compared to the composite solid state folic acid degradative curves in order to identify the peaks seen and provide direction for the interpolation of the degradative mechanism. It was observed that none of the structural pieces could be superimposed as assumed earlier and hence an attempt was made to identify the decomposition products using various analytical techniques such as infrared spectroscopy, mass spectroscopy and X-ray diffraction which suggested that the glutamic acid fragment is lost first as evidenced by acid loss and amide enhancement in the IR spectra. The vitamin was ultimately degrading to carbon fragments and that further identification was not necessary. This revised version was published online in August 2006 with corrections to the Cover Date.     

含吩噻嗪金属配合物的合成及非线性光学性质研究

本文报道了一种新的配体:10-乙基-3-甲酰吩噻嗪缩肼基二硫代甲酸甲酯(HL)及其金属配合物的合成。采用了元素分析、质谱、核磁共振、红外光谱对配体及其金属配合物进行了表征。此外,并应用紫外、荧光和Z-扫描技术,测定了配体及其金属配合物的荧光最佳发射波长(λ_max^em)、荧光量子产率(Φ_f)、寿命(τ)和非线性光学性质。结果表明它们在DMF溶液中都能发射出较强的橄榄色荧光,配体及其金属配合物都有双光子吸收,并且金属配合物的非线性光学效应比配体明显增强。用半经验量子化学方法(RHF/PM3)计算结果与实验值较为吻合。     

LC-MS/MS method for the confirmatory determination of aromatic amines and its application in textile analysis

A confirmation method for the determination of 18 aromatic amines originating from azo dyes after reductive cleavage was developed. The method is based on the use of high-performance liquid chromatography/tandem mass spectrometry with atmospheric-pressure chemical ionization. For the identification of the analytes one precursor ion and two daughter ions (multi-reaction monitoring, MRM) were selected and the LC-MS/MS parameters optimized to obtain high sensitivity and selectivity. The linear ranges varied from 0.1–1 to 30–50 g mL^–1 with correlation coefficients of 0.99 or better. The applicability of the method to determine o-tolidine (3,3-dimethylbenzidine) and 3,3-dimethoxybenzidine in textiles following reductive cleavage of acid red 114, trypan blue, and Chicago sky blue 6B was demonstrated.     

天花粉蛋白的化学——Ⅴ.粉末状结晶天花粉蛋白的拉曼光谱

本文报道粉末状结晶天花粉蛋白的拉曼光谱。酰胺Ⅰ和酰胺Ⅲ的振动谱带在1680和1250 cm~(-1)。骨架C_α—C—N的振动谱带在965 cm~(-1)。苯丙氨酸残基的特征谱带在1010和1620 cm~(-1)。酪氨酸残基的特征谱带在845和862 cm~(-1)。色氨酸残基的特征谱带在765 cm~(-1)。酰胺Ⅰ和Ⅲ的谱带中,B折叠和无序结构的特征较为明显。表征无序结构的965 cm~(-1)谱带很弱。     

成像X射线光电子能谱定量分析研究

探索了直接用实验测得的XPS图像强度来做元素或化学态相对定量分析的可能性。以AgCl和Na2S2O3样品为例，实验结果表明：XPS图像强度与成像时间有良好的线性关系，根据图像强度对两种元素或化学态进行相对定量是可能的。     

衬钽管石墨炉原子吸收法测定痕量镓时基体改进剂的研究及应用

提出用钒和铜混合基体改进剂衬钽管石墨炉原子吸收测定镓的方法。衬钽管使镓的灵敏度提高6倍左右,钒和铜混合基体改进剂不仅能进一步提高灵敏度,而且能提高灰化温度,降低原子化温度,增强抗干扰能力。测定 GSD 标准样品中的镓时,不需对样品进行预分离即可直接进行测定,结果与参考值相符。     

XPS,AFM, ATR and TPD evidence for terraced,dihydrogen terminated, 1×1 (100) silicon

Heating (100) silicon at high temperature (say, higher than 850 °C) in H₂, cooling to 670–700 °C in the same ambient, and quenching to room temperature in N₂ results in environmentally robust, terraced 1 × 1 (100) SiH₂. Evidence for this conclusion is based on angle‐resolved x‐ray photoelectron spectroscopy, atomic force microscopy, infrared absorption spectroscopy in the attenuated total reflection mode, thermal programmed desorption, and reflection high‐energy electron diffraction. Copyright © 2005 John Wiley & Sons, Ltd.