Hydrogen analysis in solid samples by utilizing He metastable atoms induced by TEA CO2 laser plasma in He gas at 1 atm

A TEA CO₂ laser (350 mJ–1.5 J, 10.6 μm, 200 ns, 10 Hz) was focused onto a metal sub-target under He as host gas at 1 atmospheric pressure with a small amount of impurity gas, such as water and ethanol vapors. It was found that the TEA CO₂ laser with the help of the metal sub-target is favorable for generating a strong, large volume helium gas breakdown plasma at 1 atmospheric pressure, in which the helium metastable-excited state was then produced overwhelmingly. While the metal sub-target itself was never ablated. The helium metastable-excited state produced after the strong helium gas breakdown plasma was considered to play an important role in exciting the atoms. This was confirmed by the specific characteristics of the detected H emission, namely the strong intensity with low background, narrow spectral width, and the long lifetime. This technique can be used for gas and solid samples analysis. For nonmetal solid analysis, a metal mesh was introduced in front of the nonmetal sample surface to help initiation of the helium gas breakdown plasma. For metal sample, analysis can be carried out by combining the TEA CO₂ laser and an Nd–YAG laser where the Nd–YAG laser is used to ablate the metal sample. The ablated atoms from the metal sample are then sent into the region of helium gas breakdown plasma induced by the TEA CO₂ laser to be excited through the helium metastable-excited state. This technique can be extended to the analysis of other elements, not limited only to hydrogen, such as halogens.     

低温加氢催化剂的设计: 理论与实践

简要总结了我们在C=C及C=O双键低温加氢双金属催化剂方面的最新研究成果. 首先, 我们以环己烯加氢为探针反应, 证明了平行使用多种研究手段的重要性, 包括单晶表面的基础研究与DFT计算, 多晶表面的合成与表征, 负载型催化剂的制备与性能测试等. 其次, 总结了双金属催化剂在其他加氢反应, 如丙烯醛C=O双键的选择性加氢, 苯的低温加氢, 以及乙炔的选择性加氢等反应中的应用. 最后, 讨论了利用金属碳化物代替贵金属Pt以减少双金属催化剂中Pt用量的可能性.     

Analytical procedures for quantification of peptides in pharmaceutical research by liquid chromatography–mass spectrometry

Peptide quantification by liquid chromatography–mass spectrometry (LC–MS) combines the high resolving power of reversed-phase (RP) chromatography with the excellent selectivity and sensitivity of mass spectrometric detection. On the basis of comprehensive practical experience in the analysis of small molecules, pharmaceutical research is developing technologies for analysis of a growing number of peptidic drug candidates. This article is a detailed review of procedures based on LC–MS techniques for quantitative determination of peptides. With the focus on pharmaceutical applications several technologies for sample preparation, various aspects of peptide chromatography, important characteristics of ESI–MS, selectivity of MS-detection modes, the large variability of internal standards, and modern instrumentation are discussed. The demand for reliable, robust, sensitive, and accurate methods is discussed using numerous examples from the literature, complemented by experiments and results from our laboratory.     

The characterization of silica microparticles by electrophoretic mobility measurements

Summary Electrophoretic mobility measurements in the pH 2‐10 range are described for several commercial HPLC silica microparticles and a laboratory-produced product. The content of metal impurities for the silicas was also determined by AAS. An acidic/hydrothermal treatment was used to generate a more homogenous surface for some of the silicas. The zero points of charge (zpc) for both a native and a treated silica plus several commercial HPLC silicas were compared. The electrophoretic mobility method may be useful in predicting the utility of certain types of silica supports for chromatographic separations.     

金属基上以YSZ为过渡层的YBCO薄膜的微观结构

采用透射电子显微术（ＴＥＭ），研究了用磁控溅射技术在柔性金属基体上制备的、钇稳定的ＺｒＯ２（ＹＳＺ）为过镀层的ＹＢａ２Ｃｕ３Ｏ７－ｙ（ＹＢＣＯ）薄膜的横断面结构。所得ＹＢＣＯ膜的超导临界转变温度Ｔｃ为９１Ｋ，临界电流密度Ｊｃ＝２×１０３Ａ／ｃｍ２（７７Ｋ，０Ｔ）。基体为Ｎｉ基合金（ＨａｓｔｅｌｏｙＣ）。ＹＳＺ层为致密、均匀的细晶组织，约１２μｍ厚，具有织构取向，并与基体紧密连接。ＹＢＣＯ层的厚度不均匀，约５００ｎｍ；ＹＢＣＯ／ＹＳＺ界面有时连接较差，在该界面上有杂质出现，杂质有可能引发裂纹。     

Phase separation of poly(γ-benzyl L-glutamate) to liquid crystal and isotropic solution in various helicogenic solvents

Solvent effects on the phase separation of poly(-benzyl L-glutamate) to liquid crystal and isotropic solution have been observed in various helicogenic solvents. The temperature-composition phase diagrams have been determined for each solution. The critical concentrations, ₂ ^* , at which the phase separation occours have been compared in various solvents. In dimethylformamide in which the polymer is molecularly dispersed, the observed ₂ ^* value has agreed with that calculated by Flory's theory. In some solvents in which the polymer aggregates in a head-to-tail mode such as chloroform, the observed ₂ ^* values have been considerably small. It is assumed that the polymer aggregates behave as longer particles than the original particles. In dioxane in which the polymer aggregates highly both in a head-to-tail and a side-by-side modes, the ₂ ^* value has been a little larger than that in chloroform. In this case the relationship between the aggregation and the liquid crystal formation is so complicated that further investigation is necessary. In aromatic solvents such asm-cresol that dissolves the polymer almost molecularly, the ₂ ^* is smaller than that in dimethylformamide. Therefore, the intermolecular interactions between the phenyl groups in the side groups of the polymer and those in solvent molecules must be considered.The author is grateful to Mr. K. Sano and Mr. M. Watanabe for their observation of the liquid crystal formation.     

低温加氢催化剂的设计: 理论与实践

简要总结了我们在C=C及C=O双键低温加氢双金属催化剂方面的最新研究成果. 首先, 我们以环己烯加氢为探针反应, 证明了平行使用多种研究手段的重要性, 包括单晶表面的基础研究与DFT计算, 多晶表面的合成与表征, 负载型催化剂的制备与性能测试等. 其次, 总结了双金属催化剂在其他加氢反应, 如丙烯醛C=O双键的选择性加氢, 苯的低温加氢, 以及乙炔的选择性加氢等反应中的应用. 最后, 讨论了利用金属碳化物代替贵金属Pt以减少双金属催化剂中Pt用量的可能性.     

Identification of radicals spin-trapped in autoxidized linoleic acids: A high performance liquid chromatography and electron spin resonance study

Radicals generated in linoleic acid and deuterated linoleic acid have been trapped by the spin trap 2-methyl-2-nitroso-propane (MNP) and identified by electron spin resonance (ESR) and ENDOR spectroscopy. The formation of two distinct secondary alkyl radical adducts (one conjugated, the other non-conjugated, as shown by their UV absorption spectra) was demonstrated by 11, 11-dideuterio-9-cis-12-cis-linoleic acid using HPLC and ESR spectroscopy.     

三元无规芳—脂族聚酯酰胺的热致液晶行为

采用低湿溶液缩聚的方法合成了对苯二甲酰氯，二甲基联苯胺和己二醇为单体的芳酯族液晶聚酯酰胺。用ＤＳＣ，Ｘ光衍射分析和偏光显微镜等手段研究了该系列聚酯酰胺的热致液晶行为，确认了二甲基联苯胺单体用量在２０％（ｍｏｌ）的情况下，所得聚酯酰胺仍为向列型液晶聚合物。由于聚酯酰胺分子间聚酰胺链段之间的氢键作用，随着二甲基联苯胺用量增加至６０ｍｏｌ％时，所得的聚酯酰胺己无液晶转变温度，其液晶区间即从熔融温度直至分     

Infrared dichroism measurements on the alkyl chain packing of an ionic detergent intercalated between silicate layers

 Microcrystals of the metal silicate hydrate ilerite orient macroscopically on the surface of a ATR-crystals and thus, are accessible for infrared linear dichroism measurements. We present first results which indicate that the alkyl chain packing and the orientation of the polar group of dodecyltrimethylammoniumbromide (DTAB) intercalated between silicate layers can be determined in terms of infrared order parameters. The properties of DTAB can be modulated by the relative humidity of the surrounding atmosphere and by temperature. Upon heating DTAB undergoes a phase transition from a paraffin-like solid to a fluid phase. The former is characterized by the orthorhombic perpendicular packing of the frozen alkyl chains with tilted long axes. The interactions between the ionic groups of the surfactant and that of the host matrix stabilize the lamellar arrangement of DTAB in the crystalline and in the fluid phases. Received: 14 January 1998 Accepted: 27 July 1998