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目的建立一种快速准确灵敏的微波消解-原子荧光光谱法,用于测定干松茸中汞含量。方法采用硝酸微波消解体系对样品进行前处理,氢化物-原子荧光光谱法测定样品中汞,同时优化仪器的工作条件。结果在选定条件下,还原剂硼氢化钾(KBH4)浓度为10 g/L;灯电流20 mA;载气流量400 m l/m in;酸性介质为2%的盐酸;汞浓度在0.300~10.00μg/L时,方法的线性关系好。相关系数r=0.999 4,检出限为0.025μg/L,加标回收率91.3%~97.1%,相对标准偏差(RSD)1.34%~2.89%。结论该方法灵敏,耗时少,准确度高,适用于干松茸中汞含量的测定。
Objective To establish a rapid, accurate and sensitive microwave digestion - atomic fluorescence spectrometry for the determination of mercury in dried matsutake. Methods The sample was pretreated by nitric acid microwave digestion system, and the mercury in the sample was determined by hydride generation - atomic fluorescence spectrometry. The working conditions of the instrument were also optimized. Results Under the selected conditions, the reducing agent KBH4 concentration was 10 g / L; the lamp current was 20 mA; the carrier gas flow rate was 400 ml / min; the acidic medium was 2% hydrochloric acid; the mercury concentration was between 0.300 and 10.00 μg / L, the method has a good linear relationship. The correlation coefficient r = 0.999 4, the detection limit was 0.025 μg / L, the spiked recoveries ranged from 91.3% to 97.1%, and the relative standard deviations (RSDs) ranged from 1.34% to 2.89%. Conclusion The method is sensitive, time-consuming and accurate, suitable for the determination of mercury content in dried matsutake.