摘要
建立用氢化物发生–原子荧光光度计同时测定锌锭样品中砷和锑含量的方法。采用硝酸一次溶样,加入酒石酸防止锑水解。加入硫脲–抗坏血酸混合溶液作为还原剂和掩蔽剂,消除干扰元素的影响,对实验条件进行了优化。砷和锑的负高压分别为220,200 V,灯电流分别为80,60 mA,还原剂为1%硼氢化钾溶液(含0.5%KOH),载流为10%盐酸溶液,还原时间为30 min。测定砷的线性范围为0~80 ng/mL,相关系数r=0.999 8,检出限为0.35μg/L,测定结果的相对标准偏差为3.18%(n=11);测定锑的线性范围为0~80 ng/mL,相关系数r=0.999 6,检出限为0.42μg/L,测定结果的相对标准偏差为4.32%(n=11),砷和锑的加标回收率在97.46%~100.30%之间。用该方法对标准样品进行测定,测定结果与标准值相符。该方法基体干扰少,灵敏度高,适合于锌锭中砷和锑的日常测定。
The method for the simultaneous determination of arsenic and antimony in zinc ingot sample by hydride atomic fluorescence spectrophotometry was established.Nitric acid digestion was used,tartaric acid was added to prevent hydrolysis.Thiourea-ascorbic acid was used as reducing agent and masking agent to eliminate interference effects.Experimental conditions were optimized,arsenic and antimony negative high voltage were220,200V,respectively,lamp current were80,60mA,respectively,reducing agent was1%potassium borohydride solution(include0.5%KOH),current carrying was10%hydrochloric acid solution,and the reduction time was30min.The linear range of arsenic was0-80ng/mL with the correlation coefficient(r)of0.9998,the detection limit was0.35μg/L,and the relative standard deviation was3.18%(n=11).The linear range of antimony was0-80ng/mL with the correlation coefficient(r)of0.9996,the detection limit was0.42μg/L,and the relative standard deviation was4.32%(n=11).The standard addition recoveries of arsenic and antimony were in the range of97.46%-100.30%.The method was used to determine the standard sample,the detection result was consistent with the standard value.This method has high sensitivity,less matrix interference,it is suitable for the routine determination of arsenic and antimony in zinc ingot sample.
作者
杨占菊
李颜君
隆英兰
韩俊丽
王景凤
Yang Zhanju;Li Yanjun;Long Yinglan;Han Junli;Wang Jingfeng(The key Laboratory of Mineral Processing Engineering and Comprehensive Utilization in Qinghai, Analysis and Inspection Center, Western Mining Group Technology Development Co., Ltd., Xining 810007, China)
出处
《化学分析计量》
CAS
2017年第4期81-84,共4页
Chemical Analysis And Meterage
关键词
锌锭
砷
锑
原子荧光光谱法
zinc ingot
arsenic
antimony
atomic fluorescence spectrophotometry
