建立了一种基于固体热解-高频偏振塞曼效应背景校正技术的原子吸收光谱快速测定粉煤灰样品中总汞的方法。对样品基体、取样量、气体流量、记忆效应等实验影响因素进行了研究,在优化的实验条件下,方法的相对标准偏差为3.2%~3.8%(峰面积)和5.2%~6.9%(峰高),检出限为0.002 0μg·g^-1(3σ),加标回收率为94.2%~98.5%。采用本方法测量3个粉煤灰实际样品和3个国家土壤标准物质,并与冷原子吸收测汞仪法进行对照,t检验结果表明两种方法间无显著性差异。该方法简便快捷,定量准确,重现性好,适用于高通量检测粉煤灰样品中的汞含量。
In this paper a rapid and simple method using pyrolysis High Frequency Modulated light polarization coupled with Zeeman Atomic Absorption Spectrometry (ZAAS-HFM) was employed for the analysis of total mercury in fly ash samples. The factors those influence the experiment results, such as the sample matrix, quantity of samples, gas flow, memory effect, were studied. Under optimum conditions, the reproducibility of the method was within the range of 3.2% ~ 3.8% for peak area and 5.2% - 6.9% for peak height. The detection limit (3σ) was 0. 002 0μg·g^-1 and the recoveries were within the range of 94.2% -98.5%. Three fly ash samples and three standard reference materials were analyzed. These results were consistent with those obtained by the Cold Vapor Atomic Absorption mercury analyzer (CVAAS) , as shown by the result of t-test, no significant difference was found between these two methods. The method was simple, efficient and suitable for high throughput determination of total mercury in fly ash samples.