The preparation of thick-film glass capillary columns

A detailed method for the routine preparation of glass capillary columns is presented. The method consists of coating a glass tube with quartz powder prior to pulling the tube into a capillary. The inner surface of the capillary consists of an even distribution of quartz particles fused to the walls. This surface has been found readily deactivated by standard procedures and ideal for the preparation of thick-film glass capillary columns. The method has been thoroughly tested in two independent laboratories to ensure that the procedures described are reproducible.     

Formation of a disordered layer lattice during the intercalation of water into anhydrous vanadyl phosphate

The course of intercalation of water into ₁-VOPO₄ has been studied by thermomechanical analysis and X-ray diffraction. Neither formation of vanadyl phosphate monohydrate nor staging were observed during the intercalation. The broadening and the shift of the positions of the lines in the diffractograms have been explained by the random stacking of intercalated and nonintercalated layers in the sample.     

治疗小儿厌食症中药强壮灵冲剂微量元素测定及其与疗效关系探讨

已证明小儿厌食症除与缺乏微量元素锌关系密切外,还与其他多种微量元素和宏量元素的缺乏或低下也有关。本院以自行研制的中药强壮灵冲剂治疗小儿厌食症疗效显著。其于浸膏粉经２０余种微量元素测定表明含有锌、铁、钴、铜、镍、锰、铬、锗、锶、铝、钡、硒、硅、钛等多种人体必需且品种齐全,含量适度的微量元素。上述元素又恰是患儿体内所缺乏和低下的品种,无疑对患儿全面适度的补充大有裨益．中药强壮灵与西药硫酸锌临床对比研究表明,无论比发锌回升数值以及从厌食等全面疗效统计,中药组均明显优于西药组,并且发现疗效与药物的补锌量不成正相关。说明中药的调理脾胃功能及综合整体治疗作用是其突出优点,值得推广．     

Electron microprobe analysis of micro amount powder samples: A case study on high purity coal

For the major, minor and trace element analysis of the inorganic compounds of a Ruhr-Saar coal different preparation techniques are investigated with X-ray fluorescence analysis, electron microprobe and classical wet chemical methods minimizing sample weight at standard preparation times and analytical accuracies. Considering accuracy as well as preparation efforts, determinations by electron microprobe on small sample amounts (<50 mg) proved to be superior to the other methods.Abbreviations AAS atomic absorbtion spectrometry - EMA electron microprobe analysis - IC ion chromatography - ISE ion sensitive electrode - PHOT photometry - WCA wet chemical analysis - XRF X-ray fluorescence analysis - LTA low temperature plasma ashing - HTA high temperature ashing - l.o.i. loss on ignition     

SYNTHESIS OF SODALITE BY DRY POWDER METHOD

用新颖的干粉方法合成系列沸石的研究已从五元环沸石延伸到具有四元环和六元环的方钠石。本研究运用干粉方法在Ｎａ２Ｏ－ＳｉＯ２－Ａｌ２Ｏ３混合物中分别以乙醇胺和乙二胺－氟化物为模板，合成出了方钠石。有机模板剂以吸附态模板方式进入体系。用ＸＲＤ数据、扫描电镜图及红外光谱测试结果对实验产品做了表征。结果表明，干粉体系制备的方钠石的晶胞参数小于水热体系和非水体系合成的方钠石的相应值。而以乙醇胺为模板制备的方钠石与以乙二胺－氟化物为模板的样品比较，后者具有较快的晶化速度、较小的晶胞体积和晶粒     

Synthesis and characterization of hollandite-type material intended for the specific containment of radioactive cesium

The hollandite Ba₁Cs_0.28Fe_0.82Al_1.46Ti_5.72O₁₆, which has been proposed for the cesium-specific conditioning, can be synthesized either by an alcoxyde or a dry route. In both cases, a two-step protocol is applied, i.e., a calcination at 1000 °C followed by a sintering at 1200 °C. After sintering, both synthetic processes lead to a tetragonal form. According to the X-ray diffraction (XRD) patterns collected at the barium and the cesium K absorption edges, the different positions of these two elements have been evidenced with a more centered position in the oxygen cubic site of the tunnel for Ba than for Cs. On the contrary, after calcination, the two synthetic routes yield different products. The alcoxyde route gives rise to a mixture of the aforementioned Cs- and Ba-containing tetragonal I4/m hollandite, a Cs-only-containing monoclinic I2/m hollandite and an unidentified phase with a weak coherence length containing only Ba. The dry route yields a single tetragonal hollandite material containing Ba and Cs slightly different in composition from the targeted compound.     

Thermal and mechanical-induced phase transformations during YAG and alumina–YAG syntheses

The preparation of pure Y₃Al₅O₁₂ (YAG) and 50 vol% Al₂O₃–YAG composite powders by a wet chemical route is presented. The role of the synthesis temperature during reverse-strike precipitation has been investigated, showing its relevant effect on the purity and homogeneity of YAG powder. The composite material was prepared by comparing two different synthesis routes. A composite powder was synthesized via reverse-strike temperature-controlled co-precipitation. In the latter case, a pure-alumina precursor was firstly reverse-strike precipitated and then doped with an yttrium salt solution. For both syntheses, the role of thermal and mechanical pre-treatments on the phase development was demonstrated.     

超细粉Pb0.75Ca0.25[(Ni1/3Nb2/3)0.08Ti0.912Mn0.008]O3的制备与表征

报道了用化学共沉淀法制备掺杂Ca、Ni、Nb、Mn钛酸铅超细陶瓷粉末的方法。制得的粉料化学式为:Pb_0.75Ca_0.25[(Ni_1/3Nb_2/3)_0.08Ti_0.912Mn_0.008]O₃,粒径小于0.1μm,所有的掺杂元素均能定量掺入。     

Al3Ti1B1RE细化剂对罐用铝材的细化效果及稀土的作用

采用XRD，OM，SEM，EDAX等探讨了一种新型Al3Ti1B1RE中间合金细化剂对罐用铝材的细化效果及RE的作用。结果表明，该细化剂对罐用铝材的细化效果优于进口和国产Al3Ti1B，且具有长效性，达6h后仍未见明显衰退，明显提高了该材料的强度和塑性；其细化效果及稳定性好的主要原因是：RE可降低铝液的表面能，增加铝液对细化核心(如TiAl3，TiB2)的润湿性，既充分发挥了异质形核作用，又防止了TiB2聚集沉淀倾向；RE也极易在结晶前沿富集造成成分过冷，阻碍了α-Al晶粒生长，并促进其在细化核心上形核；此外RE还兼有一定的净化、细化和变质作用，尤其是净化作用提高了该细化剂的冶金质量。