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991.
Silica nanoparticles for separation of biologically active amines by capillary electrophoresis with laser-induced native fluorescence detection 总被引:1,自引:0,他引:1
This paper describes the analysis of biologically active amines by capillary electrophoresis (CE) in conjunction with laser-induced native fluorescence detection. In order to simultaneously analyze amines and acids as well as to achieve high sensitivity, 10 mM formic acid solutions (pH < 4.0) containing silica nanoparticles (SiNPs) were chosen as the background electrolytes. With increasing SiNP concentration, the migration times for seven analytes decrease as a result of increase in electroosmotic flow (EOF) and decrease in their electrophoretic mobilities against EOF. A small EOF generated at pH 3.0 reveals adsorption of SiNPs on the deactivated capillary wall. The decreases in electrophoretic mobilities with increasing SiNP concentration up to 0.3x indicate the interactions between the analytes and the SiNPs. Having a great sensitivity (the limits of detection at a signal-to-noise ratio (S/N) = 3 of 0.09 nM for tryptamine (TA)), high efficiency, and excellent reproducibility (less than 2.4% of the migration times), this developed method has been applied to the analysis of urinal samples with the concentrations of 0.50 +/- 0.02 microM, 0.49 +/- 0.04 microM, and 74 +/- 2 microM for TA, 5-hydroxytryptamine, and tryptophan, respectively. The successful examples demonstrated in this study open up a possibility of using functional nanoparticles for the separation of different analytes by CE. 相似文献
992.
MgF2 protective and antireflective coatings have been conventionally produced by sputtering or chemical vapour deposition CVD [1, 2], but here sol-gel routes to MgF2 are explored. MgF2(M) and MgF2(E) were prepared using an alkoxide:HF:ROH mole ratio of 1:2:200 with methanol and ethanol respectively. All sols were stable for over a year. X-ray diffraction confirmed the presence of MgF2 in samples (but also traces of MgO), and X-ray photoelectron spectroscopy suggested some F deficiency in the surface. Nevertheless, the MgF2 xerogels had surface areas and porosities that were very high and this may be used to advantage in coatings or sensors. 相似文献
993.
Mojumdar S. C. Kozánková J. Chocholoušek J. Majling J. Fábryová D. 《Journal of Thermal Analysis and Calorimetry》2004,78(1):73-82
Fluoroapatite containing glass-ceramics were prepared from Li2O-CaO-CaF2-P2O5-SiO2 system. The glass was melted at 1480°C for 1 h. The object of observation was the preparing crystal phase of fluoroapatite
in amorphous glass matrix. The morphology of lithium disilicate glass-ceramics was studied by SEM. The crystal growth and
thermal properties of fluoroapatite were studied by X-ray diffraction and DTA. The more the content of P2O5, the more the presence of fluoroapatite particles. SEM investigation clearly indicated the phase separation and formation
of a primary crystalline phase of fluoroapatite in the studied glass-ceramics. DTA curves of the fluoroapatite samples exhibit
exothermic effects in the temperature range 337-694°C depending on the composition of the materials. The position of exothermic peak for lithium disilicate on DTA curves moves with increasing specific surfacetowards lower temperatures which points on its preferential surface crystallization. As far as physical qualities are concerned,
mainly color and gloss, the best qualities of all observed materials belong to glass-ceramics with 10% P2O5.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
994.
Dr. Meaghan M. Deegan Dr. Kareem I. Hannoun Prof. Dr. Jonas C. Peters 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2020,132(50):22820-22826
The prototypical reactivity profiles of transition metal dihydrogen complexes (M-H2) are well-characterized with respect to oxidative addition (to afford dihydrides, M(H)2) and as acids, heterolytically delivering H+ to a base and H− to the metal. In the course of this study we explored plausible alternative pathways for H2 activation, namely direct activation through H-atom or hydride transfer from the σ-H2 adducts. To this end, we describe herein the reactivity of an isostructural pair of a neutral S= and an anionic S=0 Co-H2 adduct, both supported by a trisphosphine borane ligand (P3B). The thermally stable metalloradical, (P3B)Co(H2), serves as a competent precursor for hydrogen atom transfer to tBu3ArO⋅. What is more, its anionic derivative, the dihydrogen complex [(P3B)Co(H2)]1−, is a competent precursor for hydride transfer to BEt3, establishing its remarkable hydricity. The latter finding is essentially without precedent among the vast number of M-H2 complexes known. 相似文献
995.
PbO2阳极在硫酸溶液中的析氧失活行为 总被引:1,自引:0,他引:1
采用热分解鄄电镀法制备了以Sb 掺杂SnO2(Sb-SnO2)为底层的Ti 基PbO2阳极(Ti/PbO2). 采用加速电解寿命测试、电化学阻抗谱、XRD、SEM-EDX 等技术, 研究了Ti/PbO2阳极在硫酸溶液中的电解失效行为和机制.结果表明,在新制备的PbO2镀层中, 由于氧空位的存在, PbO2镀层的内应力表现为拉应力, 随着电解的进行, 阳极表面生成的活性氧原子在向基底扩散的过程中, 将Pb3+态氧化为Pb4+态, 逐渐占据镀层内作为自由电子施主的氧空位, 这不仅导致镀层的导电性能下降, 同时使镀层的应力逐渐由拉应力转变为压应力, 镀层性质逐渐劣化. 这一过程基本结束时,活性氧原子才大量扩散至Ti基底导致基底的钝化, 在Ti 基底和镀层界面出现显著的界面应力, 在界面应力和镀层内压应力的共同作用下, 阳极出现鼓泡、脱落, 迅速进入失活阶段. 相似文献
996.
On the Sodium Tetrahydroxoaluminate Chloride Na2[Al(OH)4]Cl The hitherto unknown compound Na2[Al(OH)4]Cl was prepared by crystallisation from a NaCl containing sodium aluminate solution. According to the X-ray single crystal investigation (tetragonal, space group P4/nmm, a = 7.541 Å, c = 5.059 Å, Z = 2) the compound represents the first example of a crystalline hydroxoaluminate with monomeric [Al(OH)4]? anions. Cl? shows a quadratic anti prismatic coordination to 4 Na+ and over hydrogen bonds to 4 O2? while Na+ is octahedrally coordinated by 4 O2? and 2 Cl? (axial). The results of the crystal structure analysis are confirmed by 27Al and 23Na MAS NMR investigations. Na2[Al(OH)4]Cl decomposes at about 200°C without intermediates under formation of β-NaAlO2 and NaCl. 相似文献
997.
Migration behavior and enantioseparation of racemic hydrobenzoin and structurally related compounds, including benzoin and benzoin methyl ether, in CZE with a dual CD system consisting of heptakis-(2,3-dihydroxy-6-O-sulfo)-beta-CD (SI-S-beta-CD) and beta-CD as chiral selectors in the presence and absence of borate complexation at pH 9.0 were investigated. The results indicate that enantioseparation of hydrobenzoin is mainly governed by CD complexation of hydrobenzoin-borate complexes with SI-S-beta-CD when SI-S-beta-CD concentration is relatively high. Whereas CD complexation of hydrobenzoin-borate complexes with beta-CD plays a significant role in enantioseparation when SI-S-beta-CD concentration is comparatively low. The (S,S)-enantiomer of the hydrobenzoin-borate complex was found to interact more strongly than the corresponding (R,R)-enantiomer with both SI-S-beta-CD and beta-CD. These two types of CD show the same chiral recognition pattern, but they exhibit opposite effects on the mobility of the enantiomers of hydrobenzoin-borate complexes. Enantiomer migration reversal of hydrobenzoin occurred in the presence of borate complexation when varying the concentration of beta-CD, while keeping SI-S-beta-CD at a relatively low concentration. Binding constants of the enantiomers of benzoin-related compounds to beta-CD and those of hydrobenzoin-borate complexes to SI-beta-CD were evaluated; the mobility contributions of all complex species to the effective mobility of the enantiomers of hydrobenzoin as a function of beta-CD concentration in a borate buffer were analyzed. In addition, comparative studies on the enantioseparation of benzoin-related compounds with SI-S-beta-CD and with randomly sulfate-substituted beta-CD were made. 相似文献
998.
The halohydrin reaction of chiral N-enoyl-2-oxazolidinones 1 by halogen (Br2/I2) and water were efficiently carried out in aqueous organic solvent promoted by silver(I) with high anti- and regioselectivity and moderate to good diastereoselectivities. The alkenoyl, cinnamoyl and electron-deficient cinnamoyl substrates smoothly underwent bromohydrin reaction in aqueous acetone but no iodohydrin reaction, where as electron-rich cinnamoyl substrates preferred to undergo iodohydrin reaction in aqueous acetone with moderate diastereoselectivity and enhanced diastereoselectivity was observed in aqueous THF. 相似文献
999.
Varughese M. Alexander 《Tetrahedron letters》2005,46(40):6957-6959
Bismuth(III) nitrate pentahydrate is found to be an efficient catalyst for the Pechmann condensation reaction of phenols and β-ketoesters under solvent-free conditions. The reaction protocol is simple and is followed by aqueous work-up leading to the formation of the corresponding coumarin derivatives in good yield and high purity. 相似文献
1000.
Xuchu Ma Xuebing Li Yi Du Fen Xu Yitai Qian 《Journal of solid state chemistry》2004,177(10):3824-3829
The micro-sized Sb2O3 octahedra can be synthesized on a large scale via a simple PEG-1000 polymer-assisted hydrothermal route (PAHR) in the temperature range of 160-180 °C for 10-14 h. The structures, compositions, and morphologies of the as-synthesized products are derived from X-ray power diffraction pattern, X-ray photoelectron spectra, and field emission scanning electronic microscope. Meanwhile, the optical properties of the micro-sized Sb2O3 octahedra are studied by their photoluminescene spectroscopy and Raman spectrum. Furthermore, the possible growth mechanism of the micro-metered Sb2O3 octahedra is discussed on the basis of a series of supplementary experiments. And it has been found that PEG-1000, sodium tartrate, the reaction temperature, and the reaction time have considerable effects on the final morphology of Sb2O3, while the pH value has an influence on the formation of the Sb2O3 crystals. 相似文献