Alkyl methylphosphonic acids, the degradation products of organophosphorous CWA — preparation and direct quantitative GC-FID analysis

• Published in: Central European journal of chemistry Vol. 8; no. 6; pp. 1251 - 1265
• Main Authors: Połeć, Iwona, Kiełczewska, Anna, Konopski, Leszek, Oleksa, Grażyna, Krukowska, Hanna Nowacka, Legocki, Jan
• Format: Journal Article
• Language: English
• Published: Heidelberg SP Versita 01.12.2010; Versita; De Gruyter
• Subjects: Alkyl methylphosphonic acids; Biochemistry; Biological and Medical Physics; Biophysics; Chemistry; Chemistry and Materials Science; Chemistry/Food Science; Degradation products; Gas chromatography; Geochemistry; Organophosphorus chemical warfare agents; Reference materials; Research Article; Organophosphorus chemical warfare agents; Alkyl methylphosphonic acids; Gas chromatography; Degradation products; Reference materials
• ISSN: 1895-1066; 2391-5420; 1644-3624; 2391-5420
• DOI: 10.2478/s11532-010-0102-3

Seven alkyl methylphosphonic acids, products of hydrolytic degradation of organophosphorus chemical warfare agents, were obtained with a high purity (mostly above 98%), with the aim of being applyed as future certified reference materials. Ethyl (EMPA), isopropyl (IMPA), pinacolyl (PMPA), butyl (BUMPA), isobutyl (IBUMPA), cyclohexyl (CHMPA) and 2-ethylhexyl (EHMPA) monoesters of MPA were synthesized and characterized by MS EI, FTIR and NMR ( 1 H, 13 C, 31 P), TLC, as well as GC and GC-MS after derivatization. The conditions for a direct quantitative GC FID analysis on CP-FFAP CB column of non-derivatized alkyl methylphosphonic acids were developed. This is the first successful attempt of a directed GC analysis of free alkyl phosphonic acids. Their chemical purity was determined and limit of quantification (LOQ) values for some of them were evaluated for the GC-FID method.