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首页> 外文学位 >Direct analysis of liquid and solid microsamples using a capacitively coupled microwave plasma atomic emission spectrometer.
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Direct analysis of liquid and solid microsamples using a capacitively coupled microwave plasma atomic emission spectrometer.

机译：使用电容耦合微波等离子体原子发射光谱仪直接分析液体和固体微量样品。

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摘要

The ultimate goal of the research is the trace multielement determination of microsamples. This is accomplished using a capacitively coupled microwave plasma atomic emission spectrometer. The plasma is used as an atomization source, and the resulting emission is analyzed with an echelle spectrometer with a charge injection device for detection. A sample cup is built into the electrode on which the plasma is generated which holds the discrete amount of the microsample to be analyzed. These amounts are generally five microliters for liquids or one-half milligram of solid material.;The system has been evaluated by a series of optimization studies for such parameters as applied power, plasma gas flow rates, and electrode design. Following system optimization, a series of aqueous calibration standards were run for single elements to evaluate the performance of the system. Detection limits are generally in the low part-per-billion range with precision of less than 10 percent. In addition, samples such as sweat and some certified reference materials have been analyzed to determine the applicability of the technique to real samples. Preliminary results for real samples were promising, although the accuracy of the method worsens near the detection limits. Preliminary work in the area of direct solids analysis is also promising, with linear calibration and detection limits in the low parts-per-million range. However, emission signal reproducibility is a problem with the solid samples, and some of the more refractory elements in both solids and liquids can not be analyzed using this system.;This technique is unique because of its ability to perform simultaneous multielement analysis on solid or liquid discrete microsamples without the need to change the system or alter the conditions in any way. For liquid samples, the technique has detection limits similar to or, slightly higher than similar atomic emission techniques. For solids analysis, few techniques at present have attempted analyzing microsamples without the need for sample preparation, with the additional capability of multielement analysis. The capacitively coupled microwave plasma atomic emission spectrometer is a promising tool in the analysis of real microsamples.
机译：研究的最终目标是微量样品中痕量多元素的测定。这是使用电容耦合微波等离子体原子发射光谱仪完成的。等离子体用作雾化源，并使用带有电荷注入装置的echelle光谱仪分析产生的发射以进行检测。样品杯内置在电极上，在该电极上产生等离子体，该等离子体保持离散量的待分析微量样品。对于液体或半毫克固体材料，这些量通常为5微升。;已通过一系列优化研究对系统进行了评估，这些研究包括施加功率，等离子气体流速和电极设计等参数。系统优化之后，针对单个元素运行了一系列含水校准标准液，以评估系统的性能。检测极限通常在十亿分之几的低范围内，精度不到10％。此外，还分析了汗液和一些经认证的参考物质等样品，以确定该技术对实际样品的适用性。真实样品的初步结果令人鼓舞，尽管该方法的准确性在检测极限附近变差。直接固体分析领域的前期工作也很有希望，线性校准和检测极限在百万分之几的范围内。但是，发射信号的重现性是固体样品的问题，使用该系统无法分析固体和液体中的某些难熔元素。该技术之所以独特是因为它能够同时对固体或固体进行多元素分析。液体离散微量样品，而无需以任何方式改变系统或改变条件。对于液体样品，该技术的检测极限类似于或略高于类似的原子发射技术。对于固体分析，目前很少有技术在不需要样品制备的情况下尝试分析微量样品，并具有多元素分析的附加功能。电容耦合微波等离子体原子发射光谱仪是分析实际微量样品的有前途的工具。

著录项

  • 作者

    Croslyn, Andrea Elizabeth.;

  • 作者单位

    University of Florida.;

  • 授予单位 University of Florida.;
  • 学科 Analytical chemistry.
  • 学位 Ph.D.
  • 年度 1998
  • 页码 129 p.
  • 总页数 129
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

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