氢化物发生-原子荧光光谱法测定居住区大气砷化物

Determination of Arsenides in Air of Residential Areas by Hydride Generation-Atomic Fluorescence Spectrometry

目的建立氢化物原子荧光光谱测定居住区大气中砷化物的方法。方法利用浸渍微孔滤膜采集居住区大气中蒸气态以及气溶胶态砷化物,酸消解或微波消解;活性碳采集居住区大气中气砷化氢以及蒸气态等砷化物,酸性溶液解吸。在最佳仪器、反应条件下测定。结果方法检出限0.16μg/L,方法检测下限0.53μg/L。线性范围0ng/mL～30ng/mL(As),相关系数0.9998。精密度:测试液砷浓度为3.0μg/L、15.0μg/L、27.0μg/L(As)时,7次测定的相对标准偏差(RSD)分别为5.5%、3.9%和1.5%。样品加标回收率在92.7%～101.5%之间。活性碳管采集砷化物的平均采样效率为93.7%(RSD2.7%)、盐酸溶液(2+8)解吸的平均解吸效率为93.1%(RSD2.9%)。浸渍微孔滤膜和活性碳管采集砷化物,在室温下至少可保存7d。结论该方法具有较高的准确度、采样效率和解吸效率,较低的检出限,较好的精密度和稳定性,能满足居住区大气中砷化物浓度的测定要求。

Objective To establish a method for the determination of arsenides in air of residential areas by hydride generation-atomic fluorescence spectrometry.Methods Arsenide vapor and arsenide aerosol in air of residential areas were sampled by using impregnated micropore filter films and digested in acids or under microwave.Arsine and vapor arsenides in air of residential areas were collected by using activated carbon tubes and desorbed in acidic solution.The determination was performed under the optimal instrument and reaction conditions.Results Of the method,the limit of detection was 0.16 μg/L and the limit of quantification was 0.53 μg/L.The linearity range was 0 ng/mL ～30 ng/mL（As）（r=0.9998）.As regards the precision,when the arsenic concentration of the test solution was 3.0 μg/L,15.0 μg/L and 27.0 μg/L（As）,the relative standard deviations（RSD）of 7 determinations were 5.5%,3.9% and 1.5% respectively.The recovery of spiked samples was in the range of 92.7%-101.5%.The mean arsenide sampling efficiency of activated carbon tubes was 93.7%（RSD=2.7%）,and the mean adsorption efficiency of hydrochloric acid solution（2＋8）was 93.1%（RSD=2.9%）.Impregnated micropore filter films and activated carbon tubes could keep stable for at least 7 days at room temperature after arsenide sample collection.Conclusion The method has high low limit of detection,high precision and favorable stability.It can meet the determination requirement of arsenides in air of residential areas,which can be applied in the determination of arsenides in indoor air and air of public places.