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Simple and Rapid Method for the Determination of Trace Bismuth in Sulfur Samples by Hydride Generation Atomic Fluorescence Spectrometry With Microwave Digestion

机译:微波消解-氢化物发生原子荧光光谱法快速测定硫样品中痕量铋

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摘要

A new, simple, rapid, and sensitive method was developed for the direct determination of trace bismuth (Bi) in sulfur samples by hydride generation atomic fluorescence spectrometry with microwave digestion in closed Teflon vessels. In the microwave oven, the samples were completely digested in 35 minutes using 3 mL concentrated nitric acid and 1 mL hydrogen peroxide at a pressure of 0.2-1.5 MPa. The analytical parameters, such as argon flow rate, acidity of the medium, the amount of NaBH4 and interfering ions on the recovery of bismuth were investigated. The detection limit (3 sigma) of bismuth was 0.027 mu g L-1. The relative standard deviation (%RSD) for seven replicate measurements of the sulfur samples was 1.43%-2.21% (n = 7); the standard addition recovery was 96.7-106.7%. The proposed method for the determination of bismuth in sulfur samples is simple, accurate, and there is a low risk of environmental contamination.
机译:开发了一种新的,简单,快速,灵敏的方法,通过氢化物发生原子荧光光谱法和密闭的特氟隆容器中的微波消解,直接测定硫样品中的痕量铋(Bi)。在微波炉中,使用3 mL浓硝酸和1 mL过氧化氢在0.2-1.5 MPa的压力下,在35分钟内将样品完全消化。研究了氩气流量,介质的酸度,NaBH4的含量和干扰离子对铋的回收率等分析参数的影响。铋的检测极限(3 sigma)为0.027μg L-1。硫样品的七个重复测量的相对标准偏差(%RSD)为1.43%-2.21%(n = 7);标准添加回收率为96.7-106.7%。所提出的测定硫样品中铋的方法简便,准确,环境污染风险低。

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