Stijve T, Cardinale E
J Chromatogr. 1975 Jun 18;109(2):239-45. doi: 10.1016/s0021-9673(01)91795-9.
In the proposed procedure for the determination of selenium, 0.5-1 g of sample is wet ashed with concentrated nitric acid. After adding 1,2-diamino-4,5-dichlorobenzene to the digest at pH 1, the resulting dichloropiazselenol derivatives is extracted with toluene. The extract is purified by column chromatography over Florisil and analyzed by gas-liquid chromatography with electron capture detection. Recoveries of selenium added to various substrates ranged from 72 to 102%. The limit of detection is approximately 0.01 ppm, but smaller amounts can be determined by increasing the sample size or by concentration of the final extract.
在拟议的硒测定方法中，称取0.5 - 1克样品，用浓硝酸进行湿灰化。在pH值为1的消化液中加入1,2 - 二氨基 - 4,5 - 二氯苯后，所得的二氯对苯二硒酚衍生物用甲苯萃取。萃取液通过弗罗里硅土柱色谱法进行纯化，并采用电子捕获检测的气相色谱法进行分析。添加到各种底物中的硒的回收率在72%至102%之间。检测限约为0.01 ppm，但通过增加样品量或浓缩最终萃取液可以测定更少量的硒。
