Premium
Method validation for the determination of propellant components by Soxhlet extraction and gas chromatography/mass spectrometry
Author(s) -
Fryš Ondřej,
Bajerová Petra,
Eisner Aleš,
Mudruňková Martina,
Ventura Karel
Publication year - 2011
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201100279
Subject(s) - chromatography , chemistry , calibration curve , diphenylamine , repeatability , extraction (chemistry) , gas chromatography , mass spectrometry , detection limit , analytical chemistry (journal) , dichloromethane , reproducibility , analyte , gas chromatography–mass spectrometry , organic chemistry , solvent
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.