超声提取—顺序注射氢化物发生-原子荧光光谱法测定煤中无机砷

来源期刊：冶金分析2011年第3期

论文作者：王长芹 刘贵勤

文章页码：46 - 49

关键词：超声提取； 氢化物发生-原子荧光光谱法； 煤； 无机砷

Key words：ultrasonic extraction； hydride generation atomic fluorescence spectrometry； coal； inorganic arsenic

摘    要：利用6 mol/L盐酸作为提取试剂,样品经超声提取后,用顺序注射氢化物发生-原子荧光光谱法测定煤中无机砷的含量。对超声提取条件(提取试剂浓度、时间、温度)进行了优化。在优化的实验条件下,砷的浓度在0.20~100μg/L范围内与荧光强度呈线性关系,相关系数为0.999 7,砷的检出限为0.025μg/L,对10μg/L砷标准溶液进行重复11次测量,得出相对标准偏差(RSD)为0.9%。用该法对煤飞灰成分分析标准物质GBW08401和煤样进行分析,测得回收率在95%~102%之间,标准样品的测定值和认定值相符。

Abstract: A determination method of inorganic arsenic in coal was established by sequence injection hydride generation-atomic fluorescence spectrometry (HG-AFS),after the ultrasonic extraction with 6 mol/L HCl as extraction reagent.The ultrasonic extraction conditions were optimized,including extraction reagent,time and temperature.Under the optimized experimental condition,arsenic in concentration range of 0.20-100 μg/L showed linearity to the fluorescence intensity with correlation coefficient of 0.999 7.The detection limit of arsenic was 0.025 μg/L.The relative standard deviation(RSD) for 10 μg/L As was 0.9%(n=11).The proposed method has been applied to the analysis of coal fly ash component analysis certified reference material (GBW08401) and coal samples with recoveries of 95%-102%,and the result of GBW08401 was consist with the certified value.