Method validation for the determination of propellant components by Soxhlet extraction and gas chromatography/mass spectrometry
Jazyk angličtina Země Německo Médium print-electronic
Typ dokumentu časopisecké články, práce podpořená grantem, validační studie
PubMed
21793207
DOI
10.1002/jssc.201100279
Knihovny.cz E-zdroje
- MeSH
- aminy analýza MeSH
- chemická frakcionace metody MeSH
- dusíkaté sloučeniny analýza MeSH
- estery analýza MeSH
- plynová chromatografie s hmotnostně spektrometrickou detekcí MeSH
- reprodukovatelnost výsledků MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
- validační studie MeSH
- Názvy látek
- aminy MeSH
- dusíkaté sloučeniny MeSH
- estery 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.
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