电感耦合等离子体原子发射光谱(ICP-AES)法测定银精矿中铜、铅、锌、砷、镉、钙、镁、锰含量

Determination of Copper,Lead,Zinc,Arsenic,Cadmium,Calcium,Magnesium and Manganese in Silver Concentrate by ICP-AES

针对银精矿样品复杂,难消解的特点,研究了不同酸溶法和碱熔法对样品的消解情况,建立了硝酸、盐酸、氢氟酸、高氯酸消解银精矿的方法。根据元素灵敏度和抗干扰性,选定各元素的测定波长。通过酸溶样和碱熔样测定结果比对,验证了方法准确性。建立了四酸消解-电感耦合等离子体原子发射光谱(ICP-AES)法测定银精矿中铜、铅、锌、砷、镉、钙、镁、锰含量的方法,元素的线性相关系数均在0.9999以上。通过共存元素干扰实验,确定了银精矿中高含量元素(铜、铅、锌、铁、锑、铋等)对测定元素结果没有影响。方法检出限:Cu 0.0063mg/L,Pb 0.0159mg/L,Zn 0.0090mg/L,As 0.0192mg/L,Cd 0.0093mg/L,Ca 0.0084mg/L,Mg 0.0075mg/L,Mn 0.0081mg/L。测定下限:Cu 0.0105mg/L,Pb 0.0265mg/L,Zn 0.0150mg/L,As 0.0320mg/L,Cd 0.0155mg/L,Ca 0.0140mg/L,Mg 0.0125mg/L,Mn 0.0135mg/L。3个样品的相对标准偏差在0.87%~3.6%,加标回收率在95.0%~104%。方法流程短,操作简单,快速,灵敏度和再现性高,结果准确可靠,可以满足银精矿中铜、铅、锌、砷、镉、钙、镁、锰含量在0.050%~6.00%的测定。

In view of the complex and difficult digestion characteristics of silver concentrate samples,the digestion of samples by different acid and alkali fusion methods was studied,and the digestion methods of silver concentrate by nitric acid,hydrochloric acid,hydrofluoric acid and perchloric acid were established.According to the sensitivity and anti-interference of the elements,the determination wavelengths of eight elements were selected.The accuracy of the method was verified by comparing the results of acid and alkali samples.A method for the determination of copper,lead,zinc,arsenic,septum,calcium,magnesium and manganese in silver concentrate by ICP-AES with a linear correlation coefficient of more than 0.9999 has been established.Through the interference experiment of coexisting elements,it is determined that the high content elements(Cu,Pb,Zn,Fe,Sb,Bi)in the silver concentrate have no effect on the determination of elements.The detection limit of the method:Cu 0.0063 mg/L,Pb 0.0159 mg/L,Zn 0.0090 mg/L,As 0.0192 mg/L,Cd 0.0093 mg/L,Ca 0.0084 mg/L,Mg 0.0075 mg/L,Mn 0.0081 mg/L.The lower limit of determination:Cu 0.0105 mg/L,Pb 0.0265 mg/L,Zn 0.0150 mg/L,As 0.0320 mg/L,Cd 0.0155 mg/L,Ca 0.0140 mg/L,Mg 0.0125 mg/L,Mn 0.0135 mg/L.The relative standard deviation of the three samples was between 0.87%—3.6%,and the recovery was between 95.0%—104%.The method has the advantages of short process,simple operation,high sensitivity and reproducibility,accurate and reliable results,and can be used for the determination of copper,lead,zinc,arsenic,septum,calcium,magnesium and manganese in silver concentrate.