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外贸工作要求检测工业硫磺中小于1ppm的硒量,现用的3,3′-二氨基联苯胺比色法的灵敏度已不够。荧光法测硒的灵敏度很高,但用于工业硫磺中痕量硒的测定尚未见报道。我们在P. R. Haddad等人研究荧光法测定植物体中痕量硒的基础上,对试样分解和测定条件进行了试验。试样经发烟硝酸分解,所含硒被氧化为四价和六价硒,并以盐酸还原六价硒成四价。在酸性条件下四价硒与2,3-二氨基萘(2,3-Diaminonaphthalene,缩写为DAN)反应,生成能产生荧光的络合物4,5-苯并苤硒脑(4,5-Benzopiaselenol),用环己烷萃取,然后在荧光分光光度计上测其荧光强度,根据荧光强度计算硒的含量。
Foreign trade requires detection of less than 1 ppm of selenium in industrial sulfur, and the sensitivity of the currently available 3,3’-diaminobenzidine colorimetric method is insufficient. Fluorescence detection of selenium is very sensitive, but the determination of trace amounts of selenium in industrial sulfur has not been reported. On the basis of the study of fluorescence spectrometry for the determination of trace selenium in plants by P. R. Haddad et al., The conditions of sample decomposition and determination were tested. The sample was fuming nitric acid decomposition, the selenium is oxidized to tetravalent and hexavalent selenium, and hydrochloric acid hexavalent selenium reduction. Under acidic conditions, tetravalent selenium reacts with 2,3-diaminonaphthalene (abbreviated to DAN) to generate a fluorescent 4,5-benzodiazepine selenium (4,5- Benzopiaselenol) was extracted with cyclohexane, then the fluorescence intensity was measured on a fluorescence spectrophotometer, and the content of selenium was calculated on the basis of the fluorescence intensity.