混合模式硅胶基质毛细管电色谱整体柱的制备及其电色谱性能研究

采用温和条件下的溶胶-凝胶技术,成功制备了阴离子交换-反相混合模式硅胶基质毛细管电色谱整体柱.通过调整反应液中不同前体的比例,优化了整体柱的制备条件.通过扫瞄电镜,对柱床进行了表征和分析.实验发现,所制备的整体柱电渗流的方向和大小可随流动相pH值的改变而改变,在酸性和中性条件下,具有从阴极流向阳极的电渗流;当流动相pH值升至约7.5时,电渗流方向发生了反转(由阳极流向阴极).在优化的实验条件下,用所制备的整体柱对所考察的酸性(中性)化合物实现了快速分离,并获得了高达160,000 N/m的柱效.     

Aqueous Knoevenagel Condensation Catalyzed by Aminopropyl-functionalized MCM-41

Since much more attention has been paid to the sustainable development, many researchers try to improve conventional chemical process and find new and more, environmentally friendly routes1. Aqueous-phase reactions are of interest as environ- mentally ben…     

A New Asterosaponin from the Starfish Culcita novaeguineae

A new asterosaponin named novaeguinoside A, along with a known saponin, asteronyl pentaglycoside sulfate, was isolated from the starfish Culcita novaeguineae. The new compound was identitied to be sodium 6α-O-{β-D-fucopyranosyl-(1→2)-β-D-fucopyranosyl-(1→4)-[β-D-quinovopyranosyl-(1→2)]-β-D-xylopyranosyl-(1→3)-[β-D-quinovopyranosyl}-5α-pregn-9(11)-en-20-one-3β-yl-sulfate by extensive spectral analysis and chemical evidence.     

Determination of Gossypol in Trace Level by Flow Injection Analysis with Chemiluminescence Detection

Gossypol, [1, 1′, 6, 6′, 7,7′-hexahydroxyl-5,5′-diisopropyl-3,3′-dimethyl-(2,2′-binaphtha- lene)-8,8′-dicarboxaldehyde] is a polyphenolic yellow compound naturally occurring in various parts of cotton plants1. The compound has been associated with     

Comparative X-ray photoelectron spectroscopic study on the desulfurization of thiophene by Raney nickel and rapidly quenched skeletal nickel

The desulfurization of thiophene on Raney Ni and rapidly quenched skeletal Ni (RQ Ni) has been studied in ultrahigh vacuum (UHV) by X-ray photoelectron spectroscopy (XPS). The Raney Ni or RQ Ni can be approximated as a hydrogen-preadsorbed polycrystalline Ni-alumina composite. It is found that thiophene molecularly adsorbs on Raney Ni or RQ Ni at 103 K. At 173 K, thiophene on alumina is desorbed, while thiophene in direct contact with the metallic Ni in Raney Ni undergoes C-S bond scission, leading to carbonaceous species most probably in the metallocycle-like configuration and atomic sulfur. On RQ Ni, the temperature for thiophene dissociation is about 100 K higher than that on Raney Ni. The lower reactivity of RQ Ni toward thiophene is tentatively attributed to lattice expansion of Ni crystallites in RQ Ni due to rapid quenching. The existence of alumina and hydrogen may block the further cracking of the metallocycle-like species on Raney Ni and RQ Ni at higher temperatures, which has been the dominant reaction pathway on Ni single crystals. By 473 K, the C 1s peak has disappeared, leaving nickel sulfide on the surface.     

In-channel indirect amperometric detection of nonelectroactive anions for electrophoresis on a poly(dimethylsiloxane) microchip

In the present paper, we describe a microfluidics-based sensing system for nonelectroactive anions under negative separation electric field by mounting a single carbon fiber disk working electrode (WE) in the end part of a poly(dimethylsiloxane) microchannel. In contrast to work in a positive separation electric field described in our previous paper (Anal. Chem. 2004, 76, 6902-6907), here the electrochemical reduction reaction at the WE is not coupled with the separation high-voltage (HV) system, whereas the electrochemical oxidation reaction at the WE is coupled with the separation HV system. The electroactive indicator is the carbon fiber WE itself but not dissolved oxygen. This provides a convenient and sensitive means for the determination of nonelectroactive anions by amperometry. The influences of separation voltage, detection potential, and the distance between the WE and the separation channel outlet on the response of the detector have been investigated. The present detection mode is successfully used to electrochemically detect F-, Cl-, SO4(2-), CH3COO-, H2PO4-. Based on the preliminary results, a detection limit of 2 microM and a dynamic range up to three orders of magnitude for Cl- could be achieved.     

A new piezoelectric response model for population growth of bacteria

A piezoelectric response model on the population growth of microorganism is proposed. This model is based on a novel population growth model, which has a more obvious ecological meaning and the fact that the series piezoelectric quartz crystal (SPQC) sensor responses to conductivity changes of the medium during the growth of the microorganism. From the response model four parameters can be obtained including the maximum specific growth rate mu(m), saturated population size N(m), and two constants C and K(1). The influence of the parameters on the response curve is discussed in which the influences of mu(m) and N(m) are more obvious. With the proposed model the quantitative determination of bacteria may be more accurate than the frequency detection time (FDT) method. Then the growth of Escherichia coliform (E. coli) monitored with a SPQC sensor is compared with the simulated growth curve obtained by the proposed model and a good agreement is obtained.     

Gap exponents for percolation processes with triangle condition

A study is made of the gap exponents for percolation processes with the triangle condition in the subcritical region. It is show that the gaps are given by _t =2 fort=2, 3,. Scaling theory predicts thatP _p (¦C ₀¦S(p))–(p _c –p) andE _p (1/¦C ₀¦; ¦C ₀¦S(p))–(p _c –p)³, whereS(p) is the typical cluster size. It is found that (p _c –p)P _p (|C ₀S(p) ^1–)(p _c –p)^1–2 and (p _c –p)³E _p (1/|C ₀|;|C ₀|S(p) ^1–))(p _c –p)^3–4.     

The determination of calcium in yttrium oxide by alpha-particle activation analysis

The determination of calcium in yttrium oxide through the⁴⁰Ca(α, p)⁴³Sc reaction was studied, using a post-irradiation radiochemical separation procedure. The half-life of⁴³Sc was determined to be 3.87 hr. The chemical recovery was about 70%. The detection limit was about 10 ppb, for a 30 min irradiation at an alpha-particle beam current of 1 μA (E_α=13.4 MeV) and γ−γ coincidence counting (background counts being<1, cpm), with counting starting at 4 hours after the end of irradiation. Four samples of a batch of yttrium oxide (A.R.) were analyzed, and found to contain 13.9±1.0 ppm of calcium.