摘要
采用微量高温灼烧法制备样品气,运用同位素质谱测定稳定性同位素13 C、15 N双标记氨基脲(13C、15 N3-SEM)产品的13C、15 N同位素丰度。通过实验对影响测定结果准确度的相关因素进行了考察,确定了最佳质谱转化条件为:称取1mg 13C、15 N3-SEM.HCl样品,10mg微粒状氧化铜,放入玻璃样品管,于真空状态下熔封样品管。将样品管放入马弗炉,530℃反应4h。实验表明:测定结果具有良好的精密度、重复性及再现性,满足了稳定性同位素13 C、15 N双标记氨基脲产品的同位素丰度测定的要求。
A microscale high temperature burning-MS method for determining isotope abundance of 13C、15N3-semicarbazide products was established.The conditions with relation to accuracy of results were investigated by experiments,and the optimum transform reaction conditions of mass spectrometry were： taking 1 mg 13C、15N3-SEM·HCl with 10 mg CuO（particle） in glass sample tube,sealing the tube in vacuum condition and putting it into muffle furnace into 530 ℃ for 4 h.Experiments showed that the determination results had good precision,repeatability and reproducibility,which met the determination requirements of 13C,15N labeled semicarbazide products＇ isotope abundance.
出处
《化学世界》
CAS
CSCD
北大核心
2012年第11期645-647,658,共4页
Chemical World
基金
上海市科委技术标准专项项目(10DZ0502700)
