title: Method validation for the determination of propellant components by Soxhlet extraction and gas chromatography/mass spectrometry.
abstract: A fast, sensitive, and accurate GC/MS method for the quantification of aliphatic nitroesters (ethylene glycol dinitrate, nitroglycerin, and triethylene glycol dinitrate) and aromatic amines (diphenylamine, 2-nitrodiphenylamine, and triphenylamine) in propellants was developed and validated. This method comprises a Soxhlet extraction step with dichloromethane, followed by separation on a capillary column MDN-5. Ionization of the analytes is carried out using electron ionization. The limit of quantification of the method was 1% w/w for aliphatic nitroesters and 0.1% w/w for aromatic amines (diphenylamine and triphenylamine). Values of repeatability and reproducibility for analyzed compounds were smaller than values of the maximum allowed tolerances of the Horwitz-equation RSD(max) and 2/3 RSD(max). Values of accuracy for selected compounds were below the acceptable threshold of 15% for all tested levels in the range of calibration curve excepting the lowest concentration of calibration curve for nitroglycerin and aromatic amines. During the validation of method, temperature instability in injection port of gas chromatograph and column was observed for 2-nitrodiphenylamine. Hence, it follows worse results of accuracy and linearity and 2-nitrodiphenylamine was not validated successfully.
authors.affiliation: University of Pardubice, Faculty of Chemical Technology, Department of Analytical Chemistry, Pardubice, Czech Republic.
authors.forename: Ondřej
authors.initials: O
authors.lastname: Fryš
authors.forename: Petra
authors.initials: P
authors.lastname: Bajerová
authors.forename: Aleš
authors.initials: A
authors.lastname: Eisner
authors.forename: Martina
authors.initials: M
authors.lastname: Mudruňková
authors.forename: Karel
authors.initials: K
authors.lastname: Ventura
mesh_terms: D000588:Amines / Q000032:analysis*; D005591:Chemical Fractionation / Q000379:methods*; D004952:Esters / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry; D009574:Nitro Compounds / Q000032:analysis*; D015203:Reproducibility of Results
chemical_list: D000588:Amines; D004952:Esters; D009574:Nitro Compounds