Mass spectrometric analysis of ceramic components for solid oxide fuel cells

For the determination of trace impurities in ceramic components of solid oxide fuel cells (SOFCs), some mass spectrometric methods have been applied such as spark source mass spectrometry (SSMS), laser ionization mass spectrometry (LIMS), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and inductively coupled plasma mass spectrometry (ICP-MS). Due to a lack of suitable standard reference materials for quantifying of analytical results on La _x Sr _y MnO₃ cathode material a matrix-matched synthetic standard-high purity initial compounds doped with trace elements-was prepared in order to determine the relative sensitivity coefficients in SSMS and LA-ICP-MS. Radiofrequency glow discharge mass spectrometry (rf-GDMS) was developed for trace analysis and depth profiling of thick non-conducting layers. Surface analytical techniques, such as secondary ion mass spectrometry (SIMS) and sputtered neutral mass spectrometry (SNMS), were used to determine the element distribution on surfaces (homogeneity) and the surface contaminants of SOFC ceramic layers.Dedicated to Professor Dr. rer. nat. Hubertus Nickel on the occasion of his 65th birthday     

Far infrared spectra of solid molecular nitrogen

This paper reports the observation of the far infrared absorption spectrum of a single crystal of N₂, measured over absorption paths of 4 cm (lengthwise) and 2 cm (across the crystal). The crystal chamber, with quartz windows, was immersed in a flow of cold helium gas. The spectrum from 20 to 120 cm^–1 was recorded in the liquid phase, the-phase, and over the full temperature range of the-phase (35.6–2.0 K) with a Fourier transform spectrometer. The spectral resolution, which was not instrument-limited, and the large path allowed the observation of more detailed multiphonon-transition structure in the spectrum of the-phase than has previously been observed.     

CeO2—LnO1.5固溶体的表征及其甲烷催化燃烧性能

向CeO2中引入Ln3 离子后形成的CeO2－LnO1.5（Ln=La，Nd，Sm，Gd）固溶体（n（Ce）：n（Ln）=1：1）是一种无贵金属的新型高效甲烷燃烧催化剂．比表面、XRD、Raman、TEM等分析证实，这类固溶体具有部分畸变的萤石结构，Ln3 进入晶格后诱发的结构变化使得团溶体的表面和本体能同时参与氧化还原反应．实验表明，该固态溶液体系是甲烷催化燃烧的良好催化剂．     

Solid Phase Extraction and Flame Atomic Absorption Spectrometric Determination of Trace Amounts of Zinc and Cobalt Ions in Water Samples

A simple and rapid method for the preconcentration of Co²⁺ and Zn²⁺ as their 2-guanidino-benzimidazole chelates is proposed using an octadecyl silica cartridge. The retained analytes were recovered with a mixture of 5mL of 0.01M HNO₃ and 5mL of methanol. The metal ions in the effluent were determined by flame atomic absorption spectrometry. The effect of different parameters, such as sample matrix, amount of ligand, type of eluent for elution of ions from cartridge, flow rates of sample solution and eluent, breakthrough volume, and limit of detection, were evaluated. The effects of various cationic and anionic interferences on the percent recovery of Co²⁺ and Zn²⁺ were also studied. Quantitative extraction efficiencies were obtained by elution of the cartridge with a minimal amount of solvent. Hence, with a typical preconcentration factor of 50, the limits of detections of the proposed method are 0.26 and 1.62ngmL^–1 for Zn²⁺ and Co²⁺, respectively. The method was applied to the determination of zinc and cobalt ions in different water samples.     

Single-crystal 2H NMR of deuterated 1,10-decanedicarboxylic acid included in hydrogenated urea channels

The intergrowth of 1,10-decanedicarboxylic acid and urea give infinite hydrogen-bonded chains of the guest included in the hexagonal urea host. A deuterium high-resolution solid-state NMR study of the selectively deuterated intergrowth compound 1,10-decanedicarboxylic acid/hydrogenated urea at variable temperature in the range 90 < or = T < or = 300 K was performed on a single crystal. The analysis of the second moment as a function of temperature is shown to be compatible with the known phase transition occurring near T(c) = 203 K. Moreover, the spectra indicate that the orientational disorder is strong, and is compared to an axial uniform disorder. For this purpose, the general equation for the second moment of a system with uniform two-dimensional axial orientational disorder is given, and a method to take into account the non-uniform excitation of the pulse sequence is proposed.     

氧缺位铁酸盐的制备及结构与还原行为的研究

在３５８Ｋ下用２００ｍｌ／ｍｉｎ的空气氧化碱性悬浮液合成了ＭＦｅ_２Ｏ_（４＋δ）（δ≥０，Ｍ＝Ｆｅ、Ｃｏ、Ｎｉ、Ｍｎ），并在５７３Ｋ下用４０ｍｌ／ｍｉｎ的Ｈ_２还原ＭＦｅ_２Ｏ_（４＋δ）制备了氧缺位铁酸盐ＭＦｅ_２Ｏ_（４－δ）（δ＞０）。用ＸＲＤ、Ｍｓｓｂａｕｅｒ谱等测试方法对铁酸盐的结构进行了表征，考察了铁酸盐的组成及第二金属组分（Ｃｏ、Ｎｉ、Ｍｎ）对铁酸盐还原性能的影响。在Ｈ_２还原３ｈ内，铁酸盐氧缺位程度随还原时间增加而增大，晶格常数也相应增大；５ｈ以上，铁酸盐将被还原为ＭＯ－ＦｅＯ或α－Ｆｅ，晶格常数几乎不变。按Ｆｅ、Ｃｏ、Ｎｉ、Ｍｎ顺序，ＭＯ与ＦｅＯ的相互作用能力、ＭＯ－ＦｅＯ固溶体的稳定性及铁酸盐还原为ＭＯ－ＦｅＯ的能力均增强，ＭＯ－ＦｅＯ进一步还原为α－Ｆｅ的能力却减弱。     

Raman spectra of olivine solid solutions (FexMg1−x )2SiO4 and spin-vibration interaction

Room temperature Raman spectra of synthesized powder (Fe_xMg_1?x )₂SiO₄ solid solutions are obtained. Frequency trend of all modes versus composition shows clearly the existence of a step at x = 0.3. A step-like behavior of vibration frequencies at the given composition that coincides with the percolation threshold for the olivine lattice is related to the appearance of magnetic excitations in the disordered magnetic medium owing to the spin-vibration interaction.     

固相微萃取参数选择及其对有机锡分析的影响

固相微萃取是一种新型的、不断发展和完善的样品前处理方法，它与其它技术联用可对多种样品基体中挥发、半挥发性有机化合物进行测定。目前，该技术在毒性金属有机化合物中的应用很少。本文分析参数选择对固相微萃取的影响的同时，还对其在有机锡化合物分析中的应用作了综述。     

固体电解质La2-xCaxMo1.7W0.3O9-δ(0≤x≤0.2)的合成、表征及电性能

在氧离子导体La₂Mo_1.7W_0.3O₉的基础上，采用固相法合成了La位掺杂的Ca系列新型氧化物La_2-xCa_xMo_1.7W_0.3O_9-δ(0≤x≤0.2)。通过XRD、Raman和XPS等手段对化合物结构进行表征，交流阻抗谱测试其电性能。结果表明：掺杂离子Ca²⁺的半径小于基质离子La³⁺的半径导致晶格收缩；Ca的掺杂在La₂Mo_1.7W_0.3O₉自身内置氧空位的基础上增加了额外的氧空位，提高了氧离子导体的电导率，550 ℃电导率由0.79 × 10^-4 S·cm^-1 (x=0.0)增加到1.5 × 10^-4 S·cm^-1 (x=0.16，0.2)，电导率增加89.9%。     

室温固相反应一步合成N-亚水杨基-4-氨基安替比林

4-氨基安替比林与水杨酬醛通过室温固相反应合成N-亚水杨基-4-氨基安替比 林，反应无溶剂，15 min即可完成，产率达95%，用元素分析，IR，~1H NMR，X射 线粉末衍射和X射线单晶衍射对产物进行了表征。