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Solution nebulization device (ultrasonic nebulizer) for inductively coupled plasma spectrometry and alternate plasma source (low-pressure inductively coupled plasma) for mass spectrometry.

机译:溶液雾化设备(超声波雾化器)用于电感耦合等离子体光谱法,备用等离子体源(低压电感耦合等离子体)用于质谱法。

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摘要

Ultrasonic nebulizers (USNs) are useful analytical tools for liquid sample analysis in plasma spectrometry. It provides better sensitivity and detection limits as a result of its high nebulization efficiency. This work deals with the design and construction of ultrasonic nebulizers for sample introduction into the inductively coupled plasma (ICP). A direct air-cooled USN has been developed and evaluated for use in inductively coupled plasma atomic emission spectrometry (ICP-AES) using multielement solutions in 2% nitric acid. Pertinent figures of merit such as signal-to-background, sensitivity detection limit and linear dynamic range has been obtained for the USN and compared to those of the pneumatic and glass frit nebulizers. Response times were also compared and stability & reproducibility tests were conducted. In addition, the performance of the USN was evaluated for solutions with high salt content (i.e. synthetic ocean water). Another USN employing an indirect water-cooling method for the transducer was designed and evaluated for analysis of non-aqueous solutions by inductively coupled plasma mass spectrometry (ICP-MS).;A low pressure inductively coupled plasma (LP-ICP) has been developed and characterized as an alternate ion source for mass spectrometry. The advantages provided by the LP-ICP include (1) low gas consumption which makes the use of high purity gases more affordable, (2) low power requirements, (3) easy ignition, (4) elimination of interferences due to atmospheric entrainment, (5) plasma gas flexibility, and (6) adaptability to existing instrumentation. Of particular importance is the generation of a low pressure He ICP. Helium plasmas are better ionization sources due to He's high ionization energy. However, the generation of a stable He-plasma at atmospheric pressure is not an easy task. By generating the He ICP under low pressure conditions, a stable plasma can be obtained. The performance of the LP-He ICP-MS has been evaluated for the analysis of gaseous samples in the form of gas chromatographic (GC) eluates which resulted in detection limits in the low pg range for the halogenated (bromine and chlorine) test compounds. In addition, a low pressure air ICP has also been used for the detection of halogen (iodine)-containing GC eluates. Detection of supercritical fluid chromatography products (ferrocene and ferrocene derivatives) using the LP-He ICP-MS has been attempted. An investigation on the feasibility of liquid sample analysis via solution nebulization into the LP-He ICP-MS has also been conducted.
机译:超声雾化器(USNs)是血浆光谱分析中液体样品分析的有用分析工具。由于其高雾化效率,它提供了更好的灵敏度和检测极限。这项工作涉及超声雾化器的设计和构造,用于将样品引入感应耦合等离子体(ICP)中。已经开发了直接风冷的USN,并对其进行了评估,用于在2%硝酸中使用多元素溶液的电感耦合等离子体原子发射光谱法(ICP-AES)。已为USN获得了相关的性能指标,例如信号背景,灵敏度检测极限和线性动态范围,并与气动和玻璃料雾化器的性能指标进行了比较。还比较了响应时间,并进行了稳定性和再现性测试。此外,对于含盐量高的溶液(即合成海水),还对USN的性能进行了评估。设计了另一种采用间接水冷却方法的换能器,并通过电感耦合等离子体质谱(ICP-MS)对非水溶液进行了分析评估;已开发出低压电感耦合等离子体(LP-ICP)并表征为质谱的替代离子源。 LP-ICP提供的优势包括:(1)较低的气体消耗量,这使使用高纯度气体更加经济实惠;(2)较低的功率要求;(3)易于点火;(4)消除了由于夹带大气引起的干扰; (5)等离子气体的灵活性,以及​​(6)对现有仪器的适应性。特别重要的是产生低压He ICP。由于氦的高电离能,氦等离子体是更好的电离源。然而,在大气压下产生稳定的He-血浆并非易事。通过在低压条件下生成He ICP,可以获得稳定的等离子体。已对LP-He ICP-MS的性能进行了气相色谱(GC)洗脱液形式的气态样品分析的评估,这导致卤代(溴和氯)测试化合物的检测限在低pg范围内。此外,低压空气ICP也已用于检测含卤素(碘)的GC洗脱液。已尝试使用LP-He ICP-MS检测超临界流体色谱产物(二茂铁和二茂铁衍生物)。还对通过溶液雾化到LP-He ICP-MS中进行液体样品分析的可行性进行了研究。

著录项

  • 作者单位

    University of Cincinnati.;

  • 授予单位 University of Cincinnati.;
  • 学科 Chemistry Analytical.
  • 学位 Ph.D.
  • 年度 1994
  • 页码 147 p.
  • 总页数 147
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

  • 入库时间 2022-08-17 11:49:49

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