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Analysis of elemental distributions in minerals and rocks by microwave-assisted continuous leaching on-line with inductively coupled plasma mass spectrometry.

机译:微波辅助连续浸出-电感耦合等离子体质谱在线分析矿物和岩石中的元素分布。

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摘要

Continuous on-line leaching with Inductively Coupled Plasma Mass Spectrometry (CL-ICP-MS) is a novel technique that can quickly assess the mobility and fractionation of elements in soils. It involves pumping different reagents sequentially through a micro-column containing the soil sample while continuously monitoring the released analytes by ICP-MS. Previous studies of CL-ICP-MS employed a high resolution ICP-MS (ICP-HRMS) instrument equipped with a micronebulizer to demonstrate its application to the analysis of minerals in ore samples. However, the long sample analysis time, from the slow mass scanning rate of HRMS, hinders its feasibility in exploration geochemistry.; Focused-microwave heating was used in combination with simultaneous multielemental detection through ICP-TOFMS (ICP-time-of-flight mass spectrometry) at a higher flow rate to speed up the continuous leaching of soils. Heating the micro-column to 90°C using focused-microwave energy significantly enhanced the release of analytes, by up to an order of magnitude. This was achieved without any increase in the time needed for the whole fractionation study, which is about 16 minutes and is substantially shorter than the several hours that are required for typical procedures using CL-ICP-HRMS.; Analysis of single minerals as well as a complex sample showed that the flow rate of reagents through the sample had an effect on the leaching profile, but the simultaneous application of microwave energy, which speeded up the kinetics of dissolution, essentially compensated for the shorter residence time, yielding profiles fairly similar to those obtained at low flow rate with a micronebulizer and ICP-HRMS.
机译:电感耦合等离子体质谱法(CL-ICP-MS)进行的连续在线浸提是一种可以快速评估土壤中元素的迁移率和分离度的新技术。它涉及依次通过包含土壤样品的微柱泵送不同的试剂,同时通过ICP-MS连续监测释放的分析物。以前对CL-ICP-MS的研究使用了配备有微型雾化器的高分辨率ICP-MS(ICP-HRMS)仪器,以证明其在矿石样品中矿物分析中的应用。然而,由于HRMS质量扫描速度慢,样品分析时间长,阻碍了其在勘探地球化学中的可行性。聚焦微波加热与通过ICP-TOFMS(ICP飞行时间质谱)同时进行多元素检测结合使用,可提高流速,以加快土壤的连续浸出。使用聚焦微波能量将微柱加热到90°C可以将分析物的释放提高多达一个数量级。无需增加整个分馏研究所需的时间即可实现这一目标,整个分馏研究大约需要16分钟,并且比使用CL-ICP-HRMS的典型程序所需的数小时要短得多。对单一矿物和复杂样品的分析表明,试剂流经样品的流速对浸出曲线有影响,但是同时施加微波能量可加快溶出动力学,基本上弥补了较短的停留时间时间,产生的曲线与使用微型雾化器和ICP-HRMS在低流速下获得的曲线相当相似。

著录项

  • 作者

    Silva M., Milithza O.;

  • 作者单位

    Queen's University at Kingston (Canada).;

  • 授予单位 Queen's University at Kingston (Canada).;
  • 学科 Chemistry Analytical.; Geochemistry.
  • 学位 M.Sc.
  • 年度 2005
  • 页码 112 p.
  • 总页数 112
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 化学;地质学;
  • 关键词

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