电感耦合等离子体原子发射光谱法测定铅精矿中砷铜锌

采用盐酸和硝酸溶解样品,高氯酸冒烟除碳,20%(V/V)酸介质中,采用As 188.980 nm、Cu 327.395 nm、Zn 328.233 nm为分析线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定铅精矿中砷、铜、锌。结果表明,基体效应对砷、铜、锌的测定结果没有显著影响,使用无铅基体匹配的方法绘制校准曲线。各元素校准曲线的线性相关系数均不小于0.999 8;方法中砷、铜、锌的检出限分别为0.032 7、0.024 0、0.130 mg/L。按照实验方法测定铅精矿标准样品中砷、铜、锌,结果的相对标准偏差(RSD,n=7)为0.64%～1.1%;测定值与认定值一致,并且与碱熔-电感耦合等离子体原子发射光谱法的测定值也相吻合。

Determination of arsenic,copper and zinc in lead concentrate by inductively coupled plasma atomic emission spectrometry

The sample was dissolved by hydrochloric acid and nitric acid. After removing carbon by perchloric acid fume, the content of arsenic, copper and zinc in lead concentrate was determined in 20% (V/V) acid medium by inductively coupled plasma atomic emission spectrometry (ICP-AES) using As 188.980 nm, Cu 327.395 nm and Zn 328.233 nm as analytical lines. The results showed that the determination results of arsenic, copper and zinc were not significantly affected by matrix effect. The calibration curves were prepared by lead-free matrix matching method. The linear correlation coefficients of calibration curves were higher than 0.999 8. The detection limit of arsenic, copper and zinc was 0.032 7 mg/L, 0.024 0 mg/L and 0.130 mg/L, respectively. The arsenic, copper and zinc in lead concentrate standard sample were determined according to the experimental method. The relative standard deviations (RSD,n=7) were between 0.64% and 1.1%. The found results were consistent with the certified values and those obtained by alkali fusion ICP-AES.