摘 要:本文研究了高壓消解三七，巰基棉富集砷及原子熒光光譜法測定的條件。高壓消解三七的時間在2-6小時內，砷含量隨著時間延長而增大，當消解溫度在120℃-160℃期間，保持相同的消解時間，則測得的砷含量略有波動，波動范圍在1.8%-6.6%之間。用巰基棉富集溶液中的微量砷時，富集率很好，但用5ml HNO3（1+1）及2.0ml HCl（3.0mol/L）在80℃下洗脫巰基棉上的砷時，卻較難洗脫。在常用的儀器條件下，用原子熒光光譜儀測定溶液中的砷含量時，在0-10ug/L范圍內，熒光強度與砷含量呈很好的線性關系，相關系數r＝0.9978. 用AFS法測定，三七中的砷含量范圍為0.95mg/kg-1.15mg/kg。
ABSTRACT:The conditions of high pressure treatment Sanqi, enrichment arsenic(As) from its dilute solution and determination of arsenic by atomic fluorescence spectrometry(AFS) was studied. During the time range of 2 hours to 6 hours for dissolve Sanqi at high pressure, arsenic content increased with time increased. During the temperature range of 120℃ to 160℃ for dissolve Sanqi at the same time, arsenic content fluctuation was range of 1.8%-6.6%. The rate of concentration arsenic from the solution by sulfhydryl cotton was very good, but eluting arsenic from sulfhydryl cotton was difficult used 5 mL HNO3 (1+1) and 2.0 mL HCl (3.0mol/L) at 80℃. At normal the instrument conditions used AFS, the fluorescence intensity changes linearly with arsenic content at range of 0-10ug/L arsenic, r=0.9978. Arsenic content in the Sanqi was at range from 0.95mg/kg to 1.15mg/kg detected by AFS.
Keywords: Sanqi, atomic fluorescence spectrometry, arsenic, sulfhydryl cotton