摘要
建立微波消解原子荧光法同时测定土壤中硒与锑的含量。以硝酸–盐酸–过氧化氢作为消解体系,用微波消解方法对土壤样品进行前处理。对实验条件进行了优化,灯电流硒灯为50 mA,锑灯为60 mA,载气流量为300mL/min,光电倍增管负高压为270 V,原子化器高度为8 mm,气态物发生的还原剂选择20 g/L硼氢化钾–5 g/L氢氧化钠溶液。硒、锑的质量浓度分别在0～20,0～8μg/L范围内与其荧光强度呈良好的线性,线性相关系数r分别为0.999 5,0.999 7,检出限分别为0.009 7,0.008 7mg/kg。用该方法对土壤标准物质进行测定,硒、锑测定结果的相对误差分别为–0.7%～2.5%,0.8%～2.9%,相对标准偏差分别为2.6%～4.2%,1.8%～4.0%(n=6),样品加标回收率分别为93.6%～95.0%,94.8%～104.0%。该方法试剂用量小,干扰少,适用于大量土壤样品中硒和锑的同时测定。
Simultaneous determination of selenium and antimony in soil sample by microwave digestion–atomic fluorescence spectrometry(AFS)was developed.Soil samples were pretreated by microwave digestion with nitric acid– hydrochloric acid–hydrogen peroxide as the digestion system.The determination conditions were optimized as follows:current was 50 mA for selenium lamp and 60 mA for antimony lamp,carrier gas flow was 300 mL/min,negative pressure of photomultiplier tube was 270 V,and atomizer height was 8 mm.20 g/L potassium borohydride–5 g/L sodium hydroxide solution was selected as reduction agent.The mass concentration of selenium and antimony showed good linearity with the fluorescence intensity in the range of 0–20 ug/L,0–8μg/L,respectively.The linear correlation coefficients(r)were 0.999 5,0.999 7,and the detection limits were 0.009 7,0.008 7 mg/kg,respectively.The soil certified reference materials were determined by this method,the relative errors of Se and Sb were–0.7%–2.5%,0.8%– 2.9%,the relative standard deviations of the results were 2.6%–4.2%,1.8%–4.0%(n=6),respectively.The recovery rates of sandard addition in samples were 93.6%–95.0%,94.8%–104.0%,respectively.The method has advantages of small dosage of reagent and small interference,it is suitable for the simultaneous determination of selenium and antimony in a large number of soil samples.
作者
李美秀
齐少华
LI Meixiu;QI Shaohua(Environmental Monitoring Station of Xi'an,Xi'an 710119,China)
出处
《化学分析计量》
CAS
2018年第6期81-86,共6页
Chemical Analysis And Meterage
关键词
微波消解
原子荧光法
土壤
硒
锑
同时测定
microwave digestion
atomic fluorescence spectrometry
soil
selenium
antimony
simultaneous determination
作者简介
通讯作者,李美秀,硕士,工程师,从事水质与土壤等环境监测分析工作,E-mail:mx2003mx@163.com
