摘要
由于锌冶炼工业是一个重要的大气汞污染源，而再生锌原料是锌的一个重要来源之一，因此再生锌中汞的准确测定具有重要的意义。实验采用先加入10mL盐酸加热分解并除去硫后，再加入5mL硝酸的溶样方式，以盐酸（1＋19）作载流，硼氢化钾溶液作为还原剂，实现了氢化物发生原子荧光光谱对再生锌原料中质量分数为0．0001％～O．060％汞的测定。实验中，为了使汞标准溶液稳定保存较长的时间，采用O．5g／L重铬酸钾-5％硝酸作为汞保护剂。在选定的工作条件下，汞质量浓度在2～20ng／mL范围内呈线性关系，相关系数R^2=O．9996。方法检出限为O．20ng／mL，测定下限为2．0ng／mL。干扰试验表明，样品中的共存元素不干扰汞的测定。按照实验方法测定含锌废料、瓦斯灰、氧化锌、烟灰、锌浮渣多个实际样品，结果与冷原子吸收光谱法的基本一致，相对标准偏差（RSD，”一6）在1．6％～3．5％之间。将实验方法应用于瓦斯灰和含锌废料中汞的测定，
The zinc smelting industry is an important source of mercury pollution in air.The regenerated zinc raw material is one of important sources of zinc.Therefore,the accurate determination of mercury in regenerated zinc is of great significance.In this study,10 mL of hydrochloric acid was firstly added to removal sulfur by heating.Then,5mL of nitric acid was added to dissolve the sample.The mercury in regenerated zinc raw material with mass fraction in range of 0.000 1%-0.060% was determined by atomic fluorescence spectrometry using hydrochloric acid(1+19)as carrier and using potassium borohydride solution as reducing agent.In experiments,0.5g/L potassium dichromate-5% nitric acid was used as protective agent of mercury to store the standard solution for long time.Under the selected working conditions,the mass concentration of mercury in range of 2-20ng/mL showed linear relationship with correlation coefficient of R2=0.999 6.The detection limit of method was 0.20ng/mL,and the lower determination limit was 2.0ng/mL.The interference tests indicated that the coexisting elements in sample did not interfere with the determination of mercury.Several actual samples such as zinc-bearing waste material,gas dust,zinc oxide,zinc ash and dross were determined according to the experimental method.The found results were basically consistent with those obtained by cold atomic absorption spectrometry.The relative standard deviations(RSD,n=6)were between 1.6%and 3.5%.The proposed method had been applied to the determination of mercury in gas dust and zinc-bearing waste material.The recoveries were between 96%and 101%.
出处
《冶金分析》
CAS
CSCD
北大核心
2016年第5期35-38,共4页
Metallurgical Analysis
基金
广东省金属材料与加工专业镇联合创新公共平台(2013B091602002)
广东省主体科研机构创新能力建设专项项目(粤科规财字[2014]208号)
关键词
原子荧光光谱法
再生锌原料
汞
汞保护剂
atomic fluorescence spectrometry
regenerated zinc raw material
mercury
protective agent of mercury
