Determination of gold,silver,platinum,and palladium in crude selenium by oxidation roasting-lead assay-ICP-AES
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.
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