火焰原子吸收光谱法测定高锑烟尘中的银、铅、镉

建立了火焰原子吸收光谱法测定高锑烟尘中的银、铅、镉的分析方法。试样经王水、高氯酸溶解后,利用四价锑的溴化物沸点较低的性质,将锑挥发除去,以消除基体锑对测定的干扰,在盐酸-高氯酸-硫脲介质中实现了银、铅、镉的连续测定。方法检出限:Ag为0.003 7μg/mL,Pb为0.019 8μg/mL,Cd为0.001 6μg/mL。相对标准偏差(RSD,n=11):Ag为0.92%~1.04%,Pb为1.29%~2.21%,Cd为1.99%~2.22%。加标回收率:Ag为99.30%~101.8%,Pb为98.60%~102.5%,Cd为98.40%~104.0%。方法准确、可靠、简便、快速,完全适用于高锑烟尘中银、铅、镉的测定。

Determination of silver, lead, cadmium in high antimony smoke by flame atomic absorption spectrometry

An analytical method was proposed to determine silver,lead,and cadmium in high antimony smoke dust by flame atomic absorption spectrometry（FAAS）.The samples were first treated by aqua regia and perchloric acid.The matrix interference of antimony was eliminated according to the relatively lower boiling point of tetravalent antimony bromide volatilization.The contents of silver,lead and cadmium were analyzed simultaneously in hydrochloric acid-perchloric acid-thiourea medium.The detection limits（μg/mL）for Ag,Pb and Cd were 0.003 7 0.019 8and 0.001 6,and the relative standard deviation（RSD,n=11）：were 0.92%-1.04%,1.29%-2.21%and 1.99%-2.22%,respectively.The recoveries were in the range of 98.40% -104.0%.The method is accurate,reliable,simple and quick to meet the analytical requirement for the determination of silver,lead and cadmium in high antimony smoke dust samples.