Citation: HUANG Gui-Lan, YUAN Ling, LIU Shi-Lei, ZHOU Shi-Kun. In Situ Phosphitylation for Nuclear Magnetic Resonance Identification of Precursors of Chemical Warfare Agents[J]. Chinese Journal of Analytical Chemistry, ;2015, 43(12): 1927-1933. doi: 10.11895/j.issn.0253-3820.150178 shu

In Situ Phosphitylation for Nuclear Magnetic Resonance Identification of Precursors of Chemical Warfare Agents

1.
State key Laboratory of NBC Protection for Civilian, Research Institute of Chemical Defence, Beijing 102205, China

Corresponding author: HUANG Gui-Lan,
Received Date: 5 April 2015
Available Online: 20 July 2015

There is a trouble for ¹H NMR identification of non-phosphorus precursors of chemical warfare agents listed in Schedule 2, part B of Chemical Weapons Convention(CWC) in complex matrix. An alternative method was proposed for identification by in situ derivatization of the precursors containing hydroxyl functions with 2-chloro-4,4,5,5-tetramethyl-1,3,2-dioxaphospholane(CTMP) in a NMR tube followed by phosphorus-31 NMR detection. The specificity, stability, sensitivity and selectivity of the method were evaluated with pinacol and three aminoalcohols isomers, 2-(N,N-dipropylamino)ethanol, 2-(N-butyl-N-ethylamino)ethanol and 2-(N-isopropyl-N-propylamino) ethanol. The results showed that the phosphorylation products were single, stable and allowing clear distinction between aminoalcohols isomers. The method was used for the detection and identification of three mixed aminoalcohols isomers present(at original concentration of 10μg/mL) in an organic sample from 32^th OPCW Official Proficiency Tests.
- Phosphorus-31 nuclear magnetic resonance,
- In situ derivatization,
- Non-phosphorus precursors,
- Chemical warfare agents,
- Aminoalcohols,
- Phosphitylation
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沈阳化工大学材料科学与工程学院沈阳 110142