微波消解-氢化物发生原子荧光法测定紫阳高硒区土壤硒含量的方法研究

Determination of Se in Soils of Ziyang High Selenium Region by Microwave Digested-Hydride Generation Atomic Fluorescence Spectrometry

[目的]利用微波消解-氢化物发生原子荧光法,测定紫阳高硒区土壤中的硒含量.[方法]以浓硝酸和双氧水（10＋2）为消解剂,采取以微波消解的方法对紫阳富硒区土壤样品进行处理,采取氢化物发生-原子荧光光谱法测定土壤中硒含量,并设定最佳的样品处理条件和仪器测定条件.利用加标回收试验,对试验方法进行了验证.[结果]紫阳富硒区土壤硒含量为16.28 mg/kg,达到高硒土壤标准.该方法硒的检出限达到0.15 μg/L,硒回收率为92.0％ ～ 101.8％,相关系数达0.9999,线性范围为0～ 100 mg/kg.[结论]该微波消解的方法对土壤总硒的测定结果准确且稳定,线性范围宽,节约时间.

[Objective] Determination of Se in the soil with high selenium in Ziyang area by Microwave Digested-Hydride Generation Atomic Fluorescence Spectrometry.[Method] The samples were first treated by nitric acid and hydrogen peroxide （10 ＋ 2） of microwave digestion,then the trace arsenic and selenium in soil of Ziyang high selenium region were determined by hydride generation-atomic fluorescence spectrometry.The experimental conditions for treating and analyzing samples were optimized.[Result] The results indicated that the selenium content in soil of Ziyang high selenium region is 16.28 mg/kg,the detection limits were 0.15 g/L,the selenium recovery rate was 92％-101.8％,the correlation coefficient was 0.999 9,the linear range 0-100 mg/kg.[Conclusion] The method of microwave digestion of total selenium determination result is accurate and stable.It also saves the chemical reagents and time.