Method validation for the determination of propellant components by Soxhlet extraction and gas chromatography/mass spectrometry
Language English Country Germany Media print-electronic
Document type Journal Article, Research Support, Non-U.S. Gov't, Validation Study
- MeSH
- Amines analysis MeSH
- Chemical Fractionation methods MeSH
- Nitro Compounds analysis MeSH
- Esters analysis MeSH
- Gas Chromatography-Mass Spectrometry MeSH
- Reproducibility of Results MeSH
- Publication type
- Journal Article MeSH
- Research Support, Non-U.S. Gov't MeSH
- Validation Study MeSH
- Names of Substances
- Amines MeSH
- Nitro Compounds MeSH
- Esters MeSH
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.
References provided by Crossref.org