吉首大学学报(自然科学版) ›› 2024, Vol. 45 ›› Issue (1): 56-60.DOI: 10.13438/j.cnki.jdzk.2024.01.010

• 化学 • 上一篇    下一篇

自动消解-原子荧光法测定有机锗和总锗

刘邦夫   

  1. (湖南省电子信息产业研究院,湖南 长沙 410011)
  • 出版日期:2024-01-25 发布日期:2024-01-31
  • 作者简介:刘邦夫(1978—),男,湖南娄底人,湖南省电子信息产业研究院高级工程师,主要从事分析检测研究.

Determination of Organic Germanium and Total Germanium Through Automatic Digestion and Fluorescence Spectrometry

LIU Bangfu   

  1. (Hunan Electronic Information Industry Institute,Changsha 410011,China)
  • Online:2024-01-25 Published:2024-01-31

摘要:以药材中有机锗和总锗为综合考察指标,利用GeCl4沸点低的性质,设计程序使用全自动石墨消解仪对药材中有机锗和无机锗进行消解和分离,并采用原子荧光法检测药材中锗含量.结果表明,样品用质量分数为1%的HNO3溶液处理后在50 ℃下振荡40 min,再将溶液倒入6 mol/L HCl溶液中于100 ℃下加热60 min,可实现无机锗和有机锗的分离.方法检出限为0.16 μg/L,加标回收率为92.5%~104.0%,RSD为2.01%~3.77%,符合检测要求.

关键词: 药材, 全自动石墨消解仪, 消解, 分离, 原子荧光, 有机锗, 总锗

Abstract: With organic germanium and total germanium as indexes in herbal medicine,and with the property of GeCl4 low boiling point,the organic germanium and inorganic germanium are separated and extracted by fully automated sample digestion system,and determined by atomic fluorescence spectrometry.We found that inorganic germanium could be extracted at 50 ℃,vibrating for 40 min in mass fraction of 1% HNO3.In 6 mol/L HCl heated at 100 ℃ for 60 min,the inorganic germanium and organic germanium can be separated.The LOD of Ge was 0.16 μg/L,the recoveries of germanium was 92.5%~104.0%,and the RSD was 2.01%~3.77%,which accords with the demand of analysis.

Key words: medicinal material, fully-automatic graphite digestion instrument, digestion, separation, atomic flourence spectrometry, organic germanium, total germanium

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