悬浮液进样-氢化物发生原子荧光光谱法测定土壤中痕量砷锑硒

Determination of Trace Arsenic,Antimony,Selenium in Soil Samples by Hydride Generation-Atomic Fluorescence Spectrometry with Slurry Sample Introduction

在原子荧光光谱法传统样品前处理的基础上，提出了悬浮液进样技术。用琼脂作为悬浮剂，水溶液作为校正曲线，对土壤标准样品和实际样品进行测定，结果令人满意，并且省去了冗长的样品化学前处理过程。检出限分别为砷0．33μg／L、锑0．13μg／L、硒0．06μg／L；相对标准偏差分别为：砷3．92％～6．32％、锑1．76％～3．11％、硒3．08％～5．54％；回收率分别为砷98．7％～105．7％、锑99．5％-103．3％和硒94．6％-107．2％。国家一级标准物质的测定结果与标准值相符，实际样品的测定值与传统消化法相比较，结果基本一致。

A method for direct determination of arsenic, antimony and selenium in soil samples by hydride generation atomic fluorescence spectrometry （HG-AFS） with ultrasonic-mixed slurry sample introduction was developed. Agar was selected as a suspending agent and aqueous solution was used for preparation of calibration solutions. The operation condition for hydride generation and AFS determination are optimized. The detection limits are 0.33 μg/L for As, 0.13 μg/L for Sb and 0.06 μg/L for Se. The recoveries are 98.7% - 105.7% for As, 99.5% -103.3% for Sb and 94.6% - 107.2% for Se with precision （RSD） of 3.92% -6.32% for As, 1.76% -3.11% for Sb and 3.08% -5.54% for Se. The method had been applied to the determination of trace arsenic, antimony and selenium in National Reference Materials and soil samples with satisfactory results.