为准确、快速测定粗硒中金、银、铂、钯的含量，建立了氧化焙烧除硒、铅试金法结合电感耦合等离子体原子发射光谱法测定粗硒中金、银、铂、钯的方法。实验采用二氧化硅铺底，阶段升温至600 ℃，焙烧时间2 h，除硒效果较好，且不会造成金、银、铂、钯的损失；当试样量为10.0 g，试金硅酸度为1.0时，熔渣流动性良好，能够得到光滑圆润的贵金属合粒，经硝酸溶解后以盐酸沉淀分离银；选择Pt 265.945 nm、Pd 340.458 nm作为测定谱线进行电感耦合等离子体原子发射光谱法测定，铂和钯校准曲线的线性相关系数均大于0.999，检出限分别为0.002 0 mg/L和0.001 8 mg/L，测定下限分别为0.006 7 mg/L和0.006 1 mg/L。本方法测定结果的相对标准偏差（RSD，n=7）为0.47 %~5.9 %，加标回收率为97.3 %~103.0 %，准确度和精密度满足生产控制要求。

In order to accurately and rapidly determine the content of gold,silver,platinum,and palladium in crude selenium,a method for the determination of gold,silver,platinum,and palladium in crude selenium by oxidation roasting and lead assay combined with inductively coupled plasma atomic emission spectrometry (ICP-AES) was established.In the experiment,silicon dioxide was used to lay the bottom.The sample was heated up to 600 ℃ in stages and roasted for 2 h,the effect of removing selenium was fairly good,without losing gold,silver,platinum,and palladium;when the sample was 10.0 g and the silicon acidity in fire assay was 1.0,the fluidity of molten slag was good.Smooth and round precious metal granules can be obtained.Silver was precipitated and separated by hydrochloric acid after the precious metal particles were dissolved in nitric acid.Pt 265.945 nm and Pd 340.458 nm were selected as the determination lines of ICP-AES.The linear correlation coefficients of platinum and palladium calibration curves were all more than 0.999.The detection limits of platinum and palladium were 0.002 0 mg/L and 0.001 8 mg/L,and the detection limits were 0.006 7 mg/L and 0.006 1 mg/L,respectively.The relative standard deviation (RSD,n=7) of the results was 0.47 %-5.9 %,and the spike recovery rate was 97.3 %-103.0 %.The accuracy and precision met the requirements of production control.