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首页> 外文期刊>Spectrochimica Acta, Part B. Atomic Spectroscopy >Determination of Se at low concentration in coal by collision/reaction cell technology inductively coupled plasma mass spectrometry
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Determination of Se at low concentration in coal by collision/reaction cell technology inductively coupled plasma mass spectrometry

机译:通过碰撞/反应电池技术电感耦合等离子体质谱法测定煤中低浓度的Se

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摘要

A method is proposed for the determination of selenium at low concentration in coal by collision/reaction cell technology inductively coupled plasma mass spectrometry (CRC-ICP-MS). Samples were decomposed by high pressure microwave-assisted wet digestion (MAWD) using 250 mg of coal, a mixture of 5 mL of 14.4 mol L-1 HN0(3) and 1 mL of 40% HF and 70 min of heating program (200 degrees C and 40 bar). Hydrogen gas used in the colli-sion/reaction cell was investigated to minimize the argon-based interferences at m/z 77,78 and 80. The rejection parameter (RPq) and the H-2 gas flow rate were set to 0.45 and 4.8 mL min(-1), respectively. The use of H-2 in the cell resulted in other polyatomic interferences, such as (GeH+)-Ge-76-H-1, (BrH+)-Br-79-H-1 and (BrH+)-Br-81-H-1, which impaired Se determi-nation using Se-77, Se-80 and Se-82 isotopes, thus Se determination was carried out by monitoring only Se-78 isotope. Selenium was determined in certified reference materials of coal (NIST 1635 and SARM 20) and an agreement better than 95% was observed between the results obtained by CRC-ICP-MS and the certified values. Under opti-mized conditions, the instrumental limit of detection was 0.01 mu g L-1 and the method limit of detection was 0.01 mu g g(-1) which was suitable for Se determination at very low concentration in coal. (C) 2018 Elsevier B.V. All rights reserved.
机译:通过碰撞/反应电池技术电感耦合等离子体质谱(CRC-ICP-MS)在煤中低浓度测定硒的硒的方法。使用250mg煤的高压微波辅助湿法消化(MAWD)分解样品,用5ml 14.4mol 1 -1 HN0(3)和1mL 40%HF和70分钟的加热程序(200度C和40 bar)。研究了在煤酮/反应细胞中使用的氢气,以最小化M / Z 77,78和80的氩基干扰。排斥参数(RPQ)和H-2气流速率设定为0.45和4.8 ml min(-1)分别。在电池中使用H-2导致其他多种原子干扰,例如(Geh +) - Ge-76-H-1,(BRH +) - BR-79-H-1和(BRH +) - BR-81-H. -1,使用SE-77,SE-80和SE-82同位素受损的SE确定,因此通过仅监测SE-78同位素进行SE测定。在CRC-ICP-MS和认证价值获得的结果和认证价值获得的结果和经认证价值获得的结果中,在煤(NIST 1635和SARM 20)的认证参考资料中确定了硒的参考资料和综合。在光调条件下,检测的仪器极限为0.01μgl-1,并且检测方法限制为0.01μgg(-1),其适用于在煤中非常低浓度的Se测定。 (c)2018 Elsevier B.v.保留所有权利。

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