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41.
Summary A porous polymer resin loaded with hydrous zirconium oxide (Zr-gel) was evaluated as a stationary phase for the liquid chromatographic separation of disubstituted aromatic compounds. The prepared Zr-gel was used to separate disubstituted phenols andortho-substituted benzoic acid derivatives in reversed-phase mode. The retention time of catechol was greater than those of other disubstituted phenols; this implies that the Zr-gel has specificity for the phenolic hydroxyl group. The retention behavior ofortho-substituted benzoic acid derivatives on the Zr-gel was also evaluated in reversedphase mode using buffer. Phthalic acid was specifically retained in the vicinity of pH 6.0, which has been regarded as the equal adsorbic point. Similar behavior was also observed for salicylic acid, although the retention time of salicylic acid was less than that of phthalic acid. It seems that the specific retention behavior of hydrous zirconium oxide is a result of complexation with ligands such as hydroxyl and carboxyl groups. The results of this study have revealed that the retention mechanism of hydrous zirconium oxide is a combination of ion exchange and interaction based on complexation with ligands. 相似文献
42.
trans-RhCl(CO)(TPPTS)2 (TPPTS=tris(m-sulfonatophenyl)phosphine) has been intercalated into Zn-Al layered double hydroxides (LDHs) by the method of ion exchange. The structure, composition and thermal stability of the composite material have been characterized by powder X-ray diffraction, Fourier transform infrared and 31P solid-state magic-angle spinning nuclear magnetic resonance spectroscopy, elemental analysis, thermogravimetry, and differential thermal analysis. The geometry of trans-RhCl(CO)(TPPTS)2 was fully optimized using the PM3 semiempirical molecular orbital method, and a schematic model for the intercalated species has been proposed. The thermal stability of trans-RhCl(CO)(TPPTS)2 is significantly enhanced by intercalation, which suggests that such materials may have prospective application as the basis of a supported catalyst system for the hydroformylation of higher olefins. 相似文献
43.
Determination of trace elements in biological materials using tetramethylammonium hydroxide for sample preparation 总被引:1,自引:0,他引:1
Patrícia Martins Dirce Pozebon Valderi L. Dressler Gisele A. Kemieciki 《Analytica chimica acta》2002,470(2):62-204
A method to prepare milk powder, bovine liver and bovine muscle samples for analysis by electrothermal atomic absorption spectrometry (ETAAS) is proposed. Samples are mixed with a small amount of tetramethylammonium hydroxide (TMAH) and a stable and homogeneous slurry is produced in ca. 2 h with heating at 60–70 °C. After such sample preparation and dilution with water, trace elements are determined in certified reference materials. Pyrolysis and atomisation temperatures are optimised for each element, and several modifiers are investigated. External calibration is used for every analyte. Limits of detection (LODs), precision and accuracy are reported for Cd, Pb, Ni, Cr, Cu and Ag and compared with those obtained after conventional acid digestion. The main advantages of the proposed method are the simplicity of sample preparation and the longer lifetime of the graphite tube. 相似文献
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BaCe1—xRExO3—0.5x的溶胶—凝胶法合成及离子导电性 总被引:3,自引:0,他引:3
用溶胶-凝胶法合成了系列钙钛矿结构的BaCe1-xRExO3-0.5x(RE=La,Nd,Sm,Eu,Gd,Dy,Ho,Er和Y)复合氧化物,通过XRD和热分析对样品结构及生成过程进行了研究.测定了不同温度下样品的交流阻抗谱,讨论了稀土离子掺杂对BaCeO3电性质的影响.溶胶-凝胶法比固相反应法合成温度降低了600~800℃,稀土掺杂使BaCeO3离子导电率提高了10~40倍. 相似文献
46.
Effects of polystyrene-encapsulated magnesium hydroxide on rheological and flame-retarding properties of HIPS composites 总被引:1,自引:0,他引:1
In this study, polystyrene (PS)-encapsulated magnesium hydroxide (Mg(OH)2) was successfully prepared by in situ polymerization of styrene on the surface of Mg(OH)2 in a high-speed mixer. A large amount of PS chemically bonded on Mg(OH)2 surface was confirmed by means of FT-IR, TGA and SEM. A series of composites of high impact polystyrene (HIPS) were prepared by melt blending in a co-rotating twin-screw extruder. The effects of PS-encapsulated filler on the properties of HIPS composites were studied by SEM, rheology and combustion tests (horizontal burning tests and cone calorimetry). The dispersion and adhesion patterns of PS-encapsulated Mg(OH)2 in HIPS matrix were investigated through FT-IR and SEM. The experimental results demonstrated that comparing to the composites containing untreated filler, the rheological and flame retardant properties of those containing PS-encapsulated filler were found to be significantly improved. This improvement is mostly attributed to a better dispersion of the encapsulated filler and a strong adhesion between the filler and matrix. 相似文献
47.
48.
The unseeded non-hydrolytic sol-gel synthesis of ZrW2O8 and ZrMo2O8 produces trigonal ZrM2O8 (M = W, Mo) at 740 and 300–400°C, respectively. Cubic ZrW2O8 can be prepared using non-hydrolytic sol-gel methods by seeding with small amounts of preprepared cubic material, and the formation of the trigonal polymorph can be suppressed completely. Seeds with a small particle size are necessary for the preparation of cubic ZrW2O8. In contrast, seeding of ZrMo2O8 gels with either cubic ZrMo2O8 or cubic ZrW2O8 only lowers the temperature at which the trigonal phase crystallizes. 相似文献
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50.
Igor Djerdj Georg Garnweitner Markus Niederberger 《Journal of solid state chemistry》2007,180(7):2154-2165
The preparation of lanthanum hydroxide and manganese oxide nanoparticles is presented, based on a nonaqueous sol-gel process involving the reaction of La(OiPr)3 and KMnO4 with organic solvents such as benzyl alcohol, 2-butanone and a 1:1 vol. mixture thereof. The lanthanum manganese oxide system is highly complex and surprising results with respect to product composition and morphology were obtained. In dependence of the reaction parameters, the La(OH)3 nanoparticles undergo a shape transformation from short nanorods with an average aspect ratio of 2.1 to micron-sized nanofibers (average aspect ratio is more than 59.5). Although not directly involved, KMnO4 plays a crucial role in determining the particle morphology of La(OH)3. The reason lies in the fact that KMnO4 is able to oxidize the benzyl alcohol to benzoic acid, which presumably induces the anisotropic particle growth in [0 0 1] direction upon preferential coordination to the ±(1 0 0), ±(0 1 0) and ±(−110) crystal facets. By adjusting the molar La(OiPr)3-to-KMnO4 ratio as well as by using the appropriate solvent mixture it is possible to tailor the morphology, phase purity and microstructure of the La(OH)3 nanoparticles. Postsynthetic thermal treatment of the sample containing La(OH)3 nanofibers and β-MnOOH nanoparticles at the temperature of 800 °C for 8 h yielded polyhedral LaMnO3 and worm-like La2O3 nanoparticles as final products. 相似文献