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Mercury determination in soil by CVG-ICP-MS after volatilization using microwave-induced combustion

机译:微波诱导燃烧挥发后CVG-ICP-MS测定土壤中的汞

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摘要

Microwave-induced combustion (MIC) was applied for mercury volatilization from soil with subsequent determination by cold vapor generation coupled with inductively coupled plasma mass spectrometry (CVG-ICP-MS). Samples of soil were mixed with microcrystalline cellulose (300 mg), pressed as pellets and combusted in closed quartz vessels pressurized with 20 bar of oxygen. Mercury was volatilized from the sample matrix during combustion and quantitatively absorbed in a suitable solution. The type and concentration of absorbing solution (diluted or concentrated nitric or hydrochloric acids, or even water) as well as the use of a reflux step after combustion were studied. Accuracy was evaluated using soil certified reference materials. Using 0.25 mol L~(-1) HNO3 as absorbing solution with a reflux step of 5 min the agreement with reference values was better than 95%. The limit of detection was 0.006 μg g~(-1) Hg (using 300 mg of sample mass) and the residual carbon content for MIC digests was always below 1%. The main advantage of the proposed method is related to the complete separation of the analyte from the sample matrix. Up to eight samples could be simultaneously combusted in only 25 min. Taking into account that only 6 ml of very diluted nitric acid solution (0.25 mol L~(-1)) were used, the proposed MIC method coupled with CVG-ICP-MS can be considered in good agreement with green analytical chemistry recommendations.
机译:微波诱导燃烧(MIC)用于土壤中的汞挥发,随后通过冷蒸气产生与电感耦合等离子体质谱(CVG-ICP-MS)进行测定。将土壤样品与微晶纤维素(300 mg)混合,压成小丸,并在密闭的石英容器中燃烧,该容器用20 bar的氧气加压。在燃烧过程中,汞从样品基质中挥发出来,并在适当的溶液中定量吸收。研究了吸收溶液(稀或浓的硝酸或盐酸,甚至水)的类型和浓度,以及燃烧后回流步骤的使用。使用土壤认证参考材料评估准确性。使用0.25 mol L〜(-1)HNO3作为吸收溶液,回流步骤为5分钟,与参考值的一致性优于95%。检测极限为0.006μgg〜(-1)Hg(使用300 mg样品质量),MIC消化液的残留碳含量始终低于1%。所提出方法的主要优点与将分析物与样品基质完全分离有关。仅25分钟内即可同时燃烧多达8个样品。考虑到仅使用了6 ml的非常稀的硝酸溶液(0.25 mol L〜(-1)),建议的MIC方法与CVG-ICP-MS结合使用可以认为与绿色分析化学建议非常吻合。

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