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首页> 外文期刊>Fuel >Investigation of the Grignard reaction and experimental conditions for the determination of inorganic mercury and methylmercury in crude oils by GC-ICP-MS
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Investigation of the Grignard reaction and experimental conditions for the determination of inorganic mercury and methylmercury in crude oils by GC-ICP-MS

机译：GC-ICP-MS测定原油中无机汞和甲基汞的格氏反应和实验条件的研究

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摘要

A method proposed by Bouyssiere et al. [3] for mercury speciation in gas condensates by GC-ICP-MS was investigated for the determination of Hg~(2+) (as inorganic mercury) and MeHg~+ in crude oil samples. The Grignard reaction conditions and instrumental parameters were optimized. The original volume (0.5 mL) of the Grignard reagent was duplicated, and a sample/toluene ratio of 1:19 was used to avoid the total consumption and/or destruction of the Grignard reagent by the components of the oil matrices. Furthermore, the split injection mode was applied. When BuMgCl was used for the derivatization reaction, a limit of detection of 0.03 μg L~(-1) Hg~(2+) was obtained. Precision was always better than 12%. Quantitative recoveries (80-117%) of Hg~(2+) (as MeBuHg and Bu_2Hg) were obtained for the determination of MeHg~+ and inorganic mercury in spiked samples, respectively. Besides BuMgCl, other Grignard reagents such as MeMgCl, EtMgCl and PrMgCl can be used for the determination of Hg~(2+) as inorganic mercury and MeHg~+. Moreover, mercury species such as Me_2Hg, MeEtHg, Et_2Hg, Pr_2Hg and MePrHg can be determined by direct injection into the CG-ICP-MS using Bu_2Hg standard solutions for external calibration.
机译：Bouyssiere等人提出的方法。文献[3]研究了气相色谱-ICP-MS测定冷凝水中汞的形态，以测定原油样品中的Hg〜（2 +）（作为无机汞）和MeHg〜+。优化了格氏反应条件和仪器参数。重复了格氏试剂的原始体积（0.5 mL），并使用了1:19的样品/甲苯比率，以避免格氏试剂的总消耗和/或被油基质的组分破坏。此外，采用分流喷射模式。使用BuMgCl进行衍生化反应时，检出限为0.03μgL〜（-1）Hg〜（2+）。精度始终优于12％。分别测定了Hg〜（2 +）（作为MeBuHg和Bu_2Hg）的定量回收率（80-117％），用于测定加标样品中的MeHg〜+和无机汞。除BuMgCl外，其他格氏试剂如MeMgCl，EtMgCl和PrMgCl也可用于测定Hg〜（2+）中的无机汞和MeHg〜+。此外，可以通过使用Bu_2Hg标准溶液直接注入CG-ICP-MS中进行外部校准，从而确定诸如Me_2Hg，MeEtHg，Et_2Hg，Pr_2Hg和MePrHg等汞种类。

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  • 来源
    《Fuel》 |2014年第1期|421-426|共6页
  • 作者

    Fernanda Veronesi M. Pontes; Manuel C. Carneiro; Delmo S. Vaitsman; Maria Ines C. Monteiro; Arnaldo A. Neto; Maria Luiza B. Tristao;

  • 作者单位

    Coordenao de Analises Minerals, Centro de Tecnologia Mineral - CETEM, Av. Pedro Calmon 900, Cidade Universitaria, CEP 21941-908 Rio de Janeiro, RJ, Brazil,Departamento de Quimica Analitica, Institute de Quimica, Universidade Federal do Rio de Janeiro, Av. Athos da Silveira Ramos, 149, Cidade Universitaria, CEP 21941-909 Rio de Janeiro, RJ, Brazil;

    Coordenao de Analises Minerals, Centro de Tecnologia Mineral - CETEM, Av. Pedro Calmon 900, Cidade Universitaria, CEP 21941-908 Rio de Janeiro, RJ, Brazil;

    Departamento de Quimica Analitica, Institute de Quimica, Universidade Federal do Rio de Janeiro, Av. Athos da Silveira Ramos, 149, Cidade Universitaria, CEP 21941-909 Rio de Janeiro, RJ, Brazil;

    Coordenao de Analises Minerals, Centro de Tecnologia Mineral - CETEM, Av. Pedro Calmon 900, Cidade Universitaria, CEP 21941-908 Rio de Janeiro, RJ, Brazil;

    Coordenao de Analises Minerals, Centro de Tecnologia Mineral - CETEM, Av. Pedro Calmon 900, Cidade Universitaria, CEP 21941-908 Rio de Janeiro, RJ, Brazil;

    Petrobras/CENPES, Av. Horatio de Macedo 950, Cidade Universitaria, CEP 21941-915 Rio de Janeiro, RJ, Brazil;

  • 收录信息 美国《科学引文索引》(SCI);美国《工程索引》(EI);
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

    GC-ICP-MS; Mercury speciation; Crude oils; Grignard reaction;

    机译：GC-ICP-MS;汞形态;原油;格氏反应;

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