97 resultados para In-tube SPME

em Chinese Academy of Sciences Institutional Repositories Grid Portal


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A simple, rapid and sensitive on-line method for simultaneous determination of four endocrine disruptors (17 beta-estradiol, estriol, bisphenol A and 17 alpha-ethinylestradiol) in environmental waters was developed by coupling in-tube solid-phase microextraction (SPME) to high-performance liquid chromatography (HPLC) with fluorescence detection (FLD). A poly(acrylamide-vinylpyridine-NAP-methylene bisacrylamide) monolith, synthesized inside a polyether ether ketone (PEEK) tube, was selected as the extraction medium. To achieve optimum extraction performance, several parameters were investigated, including extraction flow-rate, extraction time, and pH value, inorganic salt and organic solvent content of the sample matrix. By simply filtered with nylon membrane filter and adjusting the pH of samples to 6.0 with phosphoric acid, the sample solution then could be directly injected into the device for extraction. Low detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method were achieved in the range of 0.006-0.10 ng/mL and 0.02-0.35 ng/mL from spiked lake waters, respectively. The calibration curves of four endocrine disruptors showed good linearity ranging from quantification limits to 50 ng/mL with a linear coefficient R-2 value above 0.9913. Good method reproducibility was also found by intra- and inter-day precisions, yielding the RSDs less than 12 and 9.8%, respectively. Finally, the proposed method was successfully applied to the determination of these compounds in several environmental waters. (c) 2006 Elsevier B.V. All rights reserved.

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An erbium-doped phosphate glass fibre has been drawn by the rod-in-tube technique in our laboratory. The gain for the Er3+-doped phosphate glass fibre with different pump powers and with different input signal wavelengths is investigated. The 2.2-cm-long fibre, pumped by a single-mode 980-nm fibre-pigtailed laser diode, can provide a net gain per unit length greater than 1.8dB/cm. The pump threshold is about 50 mW at the wavelength of 1534 nm, and below 70 mW at 1550 nm. The gain linewidth of the Er3+-doped phosphate glass fibre is greater than 34 nm and can cover the C band in optical communication networks.

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An oligonucleotide ligation assay-based DNA chip has been developed to detect single nucleotide polymorphism. Synthesized nonamers, complementary to the flanking sequences of the mutation sites in target DNA, were immobilized onto glass slides through disulfide bonds on their 5' terminus. Allele-specific pentamers annealed adjacent to the nonamers on the complementary target DNA, containing 5'-phosphate groups and biotin labeled 3'-ends, were mixed with the target DNA in tube. Ligation reactions between nonamers and pentamers were carried out on chips in the presence of T4 DNA ligase. Ligation products were directly visualized on chips through enzyme-linked assay. The effect of G:T mismatch at different positions of pentamers on the ligation were evaluated. The results showed that any mismatch between pentamer and the target DNA could lead to the decrease of ligation, which can be detected easily. The established approach was further used for multiplex detection of mutations in rpoB gene of rifampin-resistant Mycobacterium tuberculosis clinical isolates. (C) 2003 Elsevier B.V. All rights reserved.

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In this study we report on surface crystallization phenomena and propose a solution for the fabrication of long and robust tellurite glass fibers. The bulk tellurite glasses of interest were prepared by melting and quenching techniques. Tellurite glass preforms and fibers were fabricated by suction casting and rod-in-tube drawing methods, respectively. The surfaces of the tellurite bulk glass samples and of the drawn fibers prepared under different controlled atmospheres were examined by X-ray diffraction. When the tellurite glass fibers were drawn in ambient air containing water vapor, four primary kinds of small crystals were found to appear on the fiber surface, alpha-TeO(2), gamma-TeO(2), Zn(2)Te(3)O(8) and Na(2)Zn(3)(CO(3))(4)center dot 3H(2)O. A mechanism for this surface crystallization is proposed and a solution described, using an ultra-dry oxygen gas atmosphere to effectively prevent surface crystallization during fiber drawing. (C) 2010 Elsevier B.V. All rights reserved.

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By controlling the surface effects during droplet evaporation of imogolite solutions, imogolite nanotubes were dispersed individually and directly observed by transmission electron microscopy (TEM), and the structure evolution of imogolite nanotubes in the synthetic process was investigated. It was found that the number of imogolite nanotubes continuously increased with time in the whole reaction. The average length grew slowly over time after a remarkable increase in the initial 24 h, and the length distribution experienced a similar variation with the polydispersity index always below 2. No appreciable changes in tube diameters were detected under TEM observation.

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针对氢/空气混合物,通过实验研究了其预混火焰在半开口管道中的火焰传播加速现象,结果表明,火焰传播状态随着氢气当量比的变化而发生改变。当氢/空气混合物被点燃后,由于障碍物的扰动,火焰在管道中不断加速传播,并最终到达一准稳态传播。在氢气当量比0.31附近时,火焰速度发生跃变。当氢气当量比足够大时,火焰传播由爆燃态转变为爆轰态。在本实验条件下,爆燃转准爆轰的临界条件是d/Lambda>=2.6(d是圆环形障碍物内径,人是爆轰格胞尺度)。障碍物阻塞比的变化对最大火焰速度和压力提升的影响不明显。

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An experimental study and a numerical simulation were conducted to investigate the mechanical and thermodynamic processes involved in the interaction between shock waves and low density foam. The experiment was done in a stainless shock tube (80mm in inner diameter, 10mm in wall thickness and 5360mm in length). The velocities of the incident and reflected compression waves in the foam were measured by using piezo-ceramic pressure sensors. The end-wall peak pressure behind the reflected wave in the foam was measured by using a crystal piezoelectric sensor. It is suggested that the high end-wall pressure may be caused by a rapid contact between the foam and the end-wall surface. Both open-cell and closed-cell foams with different length and density were tested. Through comparing the numerical and experimental end-wall pressure, the permeability coefficients a and 0 are quantitatively determined.

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在一端封闭、一端开口的火焰传播管中均匀布置障碍物,研究了障碍物结构对管道中预混火焰传播的影 响。结果表明,由于障碍物的扰动,火焰不断加速,在阻塞比相同的条件下,最终的火焰稳态速度与障碍物的形状 和间距基本无关,其中障碍物间距仅仅影响火焰的加速速率,在障碍物间距约等于火焰传播管内径( W/ D≈1. 0) 时,平均火焰速度达到最大值,火焰到达稳态传播的距离最短。同时,本文用一维简化模型模拟了火焰在障碍物管 道中的加速过程,计算结果与实验测试结果在定性上比较吻合,说明在管内火焰速度较低的情况下,用一维可压缩 流动近似处理能初步揭示管内火焰的加速机制。

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The high-speed combustible gas ignited by a hot gas jet, which is induced by shock focusing, was experimentally investigated. By use of the separation mode of shock tube, the test section of a single shock tube is split into two parts, which provide the high-speed flow of combustible gas and pilot flame of hot gas jet, respectively. In the interface of two parts of test sections the flame of jet was formed and spread to the high-speed combustible gas. Two kinds of the ignitions, 3-D “line-flame ignition” and 2-D “plane-flame ignition”, were investigated. In the condition of 3-D “lineflame ignition” of combustion, thicker hot gas jet than pure air jet, was observed in schlieren photos. In the condition of 2-D “plane-flame ignition” of combustion, the delay time of ignition and the angle of flame front in schlieren photos were measured, from which the velocity of flame propagation in the high-speed combustible gas is estimated in the range of 30–90 m/s and the delay time of ignition is estimated in the range of 0.12–0.29 ms.

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在单脉冲激波管上,研究了1,2-二氯乙烷的热裂解.实验的激波条件为:温度区间1020 K<T<1190 K, 压力: P=0.12 MPa,实验时间τ=0.5 ms;实验气体为1,2-二氯乙烷稀释于Ar气中(3.95 mmol/L).以4-甲基-1-环己烯作为对比速率法实验的内标物,用4-甲基-1-环己烯开环反应的速率常数k=1015.3exp(-33400/T) s-1,以及从其产物的浓度推定出实验温度.经激波加热后的实验气体的终产物用气相色谱分析出主要成分为C2H3Cl,指示出主要反应通道为β消去反应.如把所有产物C2H3Cl都归于β消去反应,则可推定出表观之反应速率常数k1a=5.0×1013exp(-30000/T) s-1.对于由C-Cl键断键反应引发的链反应的可能影响做了分析研究.用了一种简便分析可推知在实验的温度范围内的低端(1020 K)链反应的影响可以忽略,而在其高端(1190 K)链反应将给出10%的终产物C2H3Cl的附加浓度,获得真实的β消去反应速率常数则必须把这部分予以扣除.经过这样的校正之后,最后得到CH2ClCH2Clβ消去反应速率常数为k1c=2.3×1013exp(-29200/T) s-1.