摘要
重金属精矿中汞会排入环境,加剧生态环境恶化,因此铅精矿中汞的检测意义重大.称取0.05～0.30 g样品,利用塞曼测汞仪将样品在空气气氛中高温灼烧,控制热释温度为800℃,热释时间为150 s,将汞释放并原子化,汞蒸气被空气带入检测器,基于塞曼效应扣除样品基体中硫的干扰,在波长253.7 nm处对汞进行测定,建立了铅精矿中汞的测定方法.实验表明,汞含量分别在1～500 ng和500～15 000 ng范围内与其对应的峰面积呈良好的线性关系,相关系数均为0.999 9;方法检出限为0.24 ng,定量限为0.80 ng.按照实验方法测定铅精矿样品,测定结果的相对标准偏差(RSD,n=11)为1.2％～5.0％,加标回收率为85％～114％.采用标准方法GB/T 8152.11-2006中的原子荧光光谱法进行方法比对,结果表明,实验方法的测定值与标准方法基本一致.该方法采用固体直接进样,无需对样品进行前处理,与汞齐富集型测汞仪相比,检测范围较宽.
Abstract
Mercury in heavy metal concentrates could be discharged into environment,which will exacerbate ecological environment.Therefore,it is of great significance to determine mercury in lead concentrate.Af-ter 0.05-0.30 g of sample was weighed,it was burned at high temperature in air atmosphere by Zeeman mercury analyzer.Mercury was released and atomized with heat release temperature of 800 ℃ for 150 s,and then mercury vapor was introduced into the detector by air.The interference of sulfur in sample matrix was deducted based on Zeeman effect.The content of mercury was determined at wavelength of 253.7 nm.Thus,a determination method of mercury in lead concentrate was established.The results showed that the contents of mercury in range of 1-500 ng and 500-15 000 ng had a good linear relationship with their corre-sponding peak areas respectively,and the correlation coefficients were both 0.999 9.The limit of detection of this method was 0.24 ng,and the limit of quantification was 0.80 ng.The lead concentrate samples was determined according to the proposed method.The relative standard deviations(RSDs,n=11)of determi-nation results were between 1.2％and 5.0％,and the recoveries were between 85％and 114％.Atomic fluorescence spectrometry in GB/T 8152.11-2006 was used for method comparison,and the results of the two above methods were basically consistent.The proposed method adopted direct solid injection without sample pretreatment.The detection range was wider compared to the mercury enrichment mercury analy-zer.
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