不同消解方式对土壤中锑的原子荧光法检测影响

Effects of Different Digestion Methods on Determination of Antimony in Soil by AFS

氢化物发生-原子荧光光谱法是土壤环境中锑检测所广泛使用的方法．土壤的消解前处理分别采用王水微波消解（半消解）、混酸全消解（硝酸＋高氯酸＋氢氟酸）方式．研究结果表明王水微波消解对锑的检测效果较好，标准土壤9次测定值的相对标准偏差为3．6％，实际样品的回收率为96％-102％．而采用混酸全消解的方式测定值偏低，实际样品的回收率为78％～86％，而且精密度超过5％，这是由于在赶酸过程中样品易被蒸干而造成痕量锑元素的损失．

The concentration of antimony is usually determined by hydride generation-atomic fluorescence spectrometry in soil monitoring. Two different digestion methods [ aqua regia microwave digestion and mixed acid （HNO3 ＋HCIO4 ＋HF） digestion ] were introduced to digest the soil samples. Results suggested that aqua regia microwave digestion was effective in detecting the concentration of antimony in soils, and the results of antimony were in good agreement with reference values. The relative standard deviation （RSD） of 9 standard soil detections was 3.6% , and the recoveries of real samples was 96% -102%. The recovery of antimony was only 78% - 86% and the RSD value was over 5% processed by mixed acid digestion, which might because the samples were entirely dried out in the process of evaporation.