摘要
采用硼氢化钠还原法将试样中硒还原为挥发性硒化氢 ,氩为载气将硒化氢吹出并导入火焰原子化器进行原子荧光测定。以正交设计法对该还原反应、氢化物转移、原子化及原子荧光测定条件等进行了详细研究。实验结果表明 ,在佳化条件下 ,该法检出限为 0 .0 72μ g/ dm3,相对标准偏差为 2 .0 %。标准曲线表明 ,在 0 .0 0 0~ 1.0 0 0μ g/ dm3Se浓度范围内 ,有理想的线性关系。本法测定海洋生物样品硒的回收率为 95.8%~ 10 2 .4 %。
The method is based on the reduction of Selenium to volatile SeH 2 which is bubbled out by a carrier gas of pure argon and then swept to an Ar H 2 flame quartz atomizer to measure its atomic fluorescence. The hydride generation, transportation, atomisation and some instrumental Parameters were studied by a kind of orthogonal design. The optimum conditions selected are as follows: reactive acidity, 20% HCl; the amount of NaBH 4, 0.7% 4.9ml in 5ml sample; the gas flow of Argon, 600m/min; atomize temperature, 200; lamp current, 100 mA; negative voltage, 300V. The detection limit is 0.072μg/dm 3. The calibration curve shows an ideal linearity in the concentration range of 0.000~0.1000μg/dm 3 Se, The recovery is 95.8%~102.4%.
出处
《青岛海洋大学学报(自然科学版)》
CSCD
北大核心
2001年第3期375-381,共7页
Journal of Ocean University of Qingdao