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本文研究了工业硫磺试样的溶解和试样中砷和硒的测定方法。经典方法系采用溴 四氯化碳溶解样品 ,试剂用量大、操作繁杂、污染环境 ,且导致微量砷、硒损失。本文提出用 1mLHNO3 +1mLHClO4 溶解硫磺试样 ,试剂用量少 ,在控温电热板上处理样品操作简单 ,砷、硒无损失。在盐酸介质中 ,用HG ICP AES法一次取样依次测定砷、硒。方法检出限分别为 0 6和 0 7ng·mL-1,方法的RSD(n =8)分别为 2 1%和 1 9% ,加标回收率分别为 99 6 %和 10 1%。
This article studies the dissolution of industrial sulfur samples and determination of arsenic and selenium in the sample. The classic method is the use of bromine carbon tetrachloride to dissolve the sample, a large amount of reagents, complicated operation, pollute the environment, and lead to trace arsenic, selenium loss. In this paper, we propose to use 1mLHNO3 + 1mLHClO4 to dissolve the sulfur sample, the reagent dosage is less, the samples are easy to handle on the temperature-controlled hotplate, and the arsenic and selenium are not lost. In hydrochloric acid medium, arsenic and selenium were determined by HG ICP AES method. The detection limits were 0 6 and 0 7 ng · mL -1, respectively. The RSDs (n = 8) were 21% and 19%, respectively. The recoveries were 99.6% and 101%, respectively.