Simple derivatization technique for determination of Schedule III chemicals of the Chemical Weapon Convention by Gas Chromatography-Mass Spectrometry

ALTAMIRANO, JORGELINA C.; KILJUNEN, HARRI; KOSKELA, HARRI; SÖDERSTRÖM, MARTIN; HÄKKINEN, VESA; KUITUNEN, MARJA-LEENA; VANINEN, PAULA

2008-10-01/2009-01-01

1-39

Química

Defensa y seguridad-Otros

A simple derivatization technique was studied for the derivatization and analysis by gas chromatography-mass spectrometry (GC-MS) of several Schedule III chemicals and one Schedule II chemical included in the Chemical Weapons Conventions (CWC). The derivatization technique is based on the use of 40% pyridine in 1-propanol solution. The studied target analytes were COCl2, POCl3, PCl3, PCl5, SOCl2, SCl2, S2Cl2 and AsCl3. All of them were successfully derivatized and analyzed by GC-MS. The stability of the target analytes and their derivatives were studied in different solvents and as a function of time. Some of them were complemented with the 31P-NMR studies. Different variables were evaluated in order to determine the best working conditions in order to achieve the maximum yield of the derivatives for each target analyte. The studied variables were reaction time, reaction temperature, sonication of the reaction mixture, concentration of the reaction mixture and addition order of the reagents. Schedule III chemicals showed a linear response within the concentration range of 0.1-2 mmol L-1 with correlation coefficient higher than 0.9900.