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Design and evaluation of a gas chromatographic detector based on the measurement of the power reflected from a microwave plasma.

机译:基于对微波等离子体反射功率的测量,对气相色谱检测器进行设计和评估。

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摘要

The operation of the microwave induced plasma, gas chromatographic detector is based on the measurement of the change in reflected power arising from the interaction of the analyte with an atmospheric pressure argon plasma sustained in the highly efficient TM{dollar}sb{lcub}010{rcub}{dollar} resonant cavity. Microwave forward power and tangential gas flow are optimized for n-pentane. Using the same sample, the analytical performance of the detector is evaluated by obtaining a calibration curve. The results showed that this detection method yields a quadratic calibration curve. The effect of plasma torch design on the analytical performance (sensitivity and detection limits) of the detector is evaluated using a tangential flow torch and a water-cooled capillary plasma torch. The sensitivity with the water-cooled capillary torch was found be to higher by a factor of 7500 and the limit of detection superior by 4 orders of magnitude over the tangential flow torch. Noise analysis of the reflected power signal revealed that the major noise types in the frequency window considered (0-200 Hz) are white noise, low frequency 1/f noise and high frequency discrete noise. The overall magnitude of the noise spectra exhibited a marked dependence on the degree of coupling of power to the microwave cavity and, to a lesser extent, on the flow rate of the plasma gas. The noise did not change consistently as plasma tube cooling water flow rate was changed. The detector's responses to several alkanes, alcohols, and the permanent gases, hydrogen, oxygen, and carbon dioxide are compared with those exhibited by the flame ionization detector. To describe the reflected power signal production mechanism, a simple mathematical model is proposed and evaluated. The model assumes that the major process generating the signal is atomic ionization.
机译:微波感应等离子体气相色谱检测器的运行基于对分析物与高效TM {dollar} sb {lcub} 010 {中所维持的大气压氩等离子体的相互作用”产生的反射功率变化的测量。 rcub} {dollar}谐振腔。微波正向功率和切向气流针对正戊烷进行了优化。使用相同的样品,通过获得校准曲线来评估检测器的分析性能。结果表明,该检测方法可产生二次校准曲线。使用切向流割炬和水冷毛细管等离子体割炬,评估等离子体割炬设计对检测器的分析性能(灵敏度和检测极限)的影响。发现水冷毛细管割炬的灵敏度比切向割炬高7500倍,检出限比切线割炬高4个数量级。对反射功率信号的噪声分析表明,在考虑的频率窗口(0-200 Hz)中,主要噪声类型为白噪声,低频1 / f噪声和高频离散噪声。噪声频谱的总体幅度显示出与功率与微波腔的耦合程度的显着相关性,并且在较小程度上取决于等离子气体的流速。随着等离子管冷却水流速的变化,噪声并没有始终如一地变化。将检测器对几种烷烃,醇以及永久气体,氢气,氧气和二氧化碳的响应与火焰离子化检测器的响应进行比较。为了描述反射功率信号的产生机理,提出并评估了一个简单的数学模型。该模型假定产生信号的主要过程是原子电离。

著录项

  • 作者单位

    North Carolina State University.;

  • 授予单位 North Carolina State University.;
  • 学科 Chemistry Analytical.
  • 学位 Ph.D.
  • 年度 1992
  • 页码 126 p.
  • 总页数 126
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 化学;
  • 关键词

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