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Development of a large volume injection method using a programmed temperature vaporization injector – gas chromatography hyphenated to ICP-MS for the simultaneous determination of mercury, tin and lead species at ultra-trace levels in natural waters
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2018-02-27 , DOI: 10.1016/j.chroma.2018.02.056
J. Terán-Baamonde , S. Bouchet , E. Tessier , D. Amouroux

The current EU legislation lays down Environmental Quality Standards (EQS) for 45 priority substances in surface waters; among them levels for (organo)metallic species of Hg, Sn and Pb are set between ng L−1 (for Hg and Sn) and μg L−1 (for Pb). To date, only a few analytical methods can reach these very restrictive limits and there is thus a need for comprehensive methods able to analyze these species down to these levels in natural waters. The aim of this work was to develop an online automated pre-concentration method using large volume injections with a Programmed Temperature Vaporization (PTV) injector fitted with a sorbent packed liner coupled to GC-ICP-MS to further improve the detection limits associated to this well-established method. The influence of several parameters such as the PTV transfer temperature and time, carrier gas flow rate and amount of packing material was investigated. Finally, the maximum volume injected through single or multiple injection modes was optimized to obtain the best compromise between chromatographic resolution and sensitivity. After optimization, very satisfactory results in terms of absolute and methodological detection limits were achieved, down to the pg L−1 level for all species studied. The potential of the method was exemplified by determining the concentrations of organometallic compounds in unpolluted river waters samples from the Adour river basin (SW France) and results were compared with conventional (splitless) GC-ICP-MS. The strength of this analytical method lies in the low detection limits reached for the simultaneous analysis of a wide group of organometallic compounds, and the potential to transfer this method to other gas chromatographic applications with inherent lower sensitivity.



中文翻译:

使用程控温度汽化进样器开发的大体积进样方法– ICP-MS联用的气相色谱仪,用于同时测定天然水中超痕量的汞,锡和铅物种

欧盟现行法规为地表水中的45种优先物质制定了环境质量标准(EQS);其中Hg,Sn和Pb的(有机)金属种类的水平设置在ng L -1(对于Hg和Sn而言)和μgL -1之间(对于Pb)。迄今为止,只有极少数的分析方法可以达到这些非常严格的限制,因此需要能够在天然水域中对这些物种进行低至这些水平分析的综合方法。这项工作的目的是开发一种在线自动预浓缩方法,该方法使用大体积进样,并配有程序温度汽化(PTV)进样器,该进样器配有与GC-ICP-MS耦合的吸附剂填充衬管,以进一步提高与此相关的检测限完善的方法。研究了PTV传输温度和时间,载气流速和填料量等几个参数的影响。最后,对通过单次或多次进样方式进样的最大体积进行了优化,以获得色谱分离度和灵敏度之间的最佳平衡。所有研究物种的-1级。该方法的潜力通过确定来自Adour流域(法国西南部)的未污染河水样品中有机金属化合物的浓度来举例说明,并将结果与​​常规(分流式)GC-ICP-MS进行了比较。该分析方法的优势在于,可以同时分析多种有机金属化合物,且检测限较低,并且具有将该方法转移至其他气相色谱应用程序的潜力,而固有的灵敏度较低。

更新日期:2018-02-27
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