电感耦合等离子体原子发射光谱法测定铅锑合金中12种元素

Determination of twelve elements in lead-antimony alloy by inductively coupled plasma atomic emission spectrometry

采用硝酸分解样品,柠檬酸抑制Sb水解,全谱直读电感耦合等离子体发射光谱仪同时测定铅锑合金样品中常量的Sb、次量和微量的As、Cu、Sn、Se、Ag、Bi、Fe、Zn、Ni、Cd、Mn等12种元素。筛选了不同溶样方法和仪器参数,在优选条件下,测得方法检出限如下:Sn、Ag和Fe为0.01μg/g,Mn为0.02μg/g,Bi和Cd为0.03μg/g,Sb、As和Zn为0.04μg/g,Se和Ni为0.05μg/g,Cu为0.08μg/g。基体铅对测定产生背景干扰,但可以通过硫酸铅沉淀除去。方法用于铅锑合金样品中上述12种元素的测定,结果与原子荧光光谱法或原子吸收光谱法相符,相对标准偏差(RSD,n=11)为0.87%～3.8%,加标回收率在95.2%～107.4%之间。

Totally 12 elements in lead-antimony alloy,including the major element（Sb）,minor and trace elements（As,Cu,Sn,Se,Ag,Bi,Fe,Zn,Ni,Cd,Mn） were simultaneously determined by full spectrum directly reading inductively coupled plasma atomic emission spectrometer.Nitric acid was used to decompose the sample,while citric acid was added to inhibit the hydrolysis of Sb.Different sample dissolution methods and instrumental parameters were tested.Under the optimized conditions,the detection limits of elements were as follows：0.01 μg/g for Sn,Ag and Fe;0.02 μg/g for Mn;0.03 μg/g for Bi and Cd;0.04 μg/g for Sb,As and Zn;0.05 μg/g for Se and Ni;0.08 μg/g for Cu.The matrix lead caused background interference in the determination.However,it could be eliminated by lead sulfate precipitation.The proposed method had been applied to the determination of twelve elements described above in lead-antimony alloy,and the results were consistent with those obtained by atomic fluorescence spectrometry or atomic absorption spectrometry.The relative standard deviations（RSD,n=11） were 0.87 %-3.8 %,and the recoveries of standard addition were 95.2 %-107.4 %.