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J Chromatogr A. 2015 May 15;1394:154-8. doi: 10.1016/j.chroma.2015.03.006. Epub 2015 Mar 9.

Minimizing thermal degradation in gas chromatographic quantitation of pentaerythritol tetranitrate.

Author information

1
Nova Research, Inc., 1900 Elkin St., Suite 230, Alexandria, VA 22308, United States.
2
US Naval Research Laboratory, Naval Technical Center for Safety and Survivability, Code 6180, 4555 Overlook Ave SW, Washington, DC 20375, United States.
3
US Naval Research Laboratory, 4555 Overlook Ave SW, Washington, DC 20375, United States.
4
US Naval Research Laboratory, Naval Technical Center for Safety and Survivability, Code 6180, 4555 Overlook Ave SW, Washington, DC 20375, United States. Electronic address: kevin.johnson@nrl.navy.mil.

Abstract

An analytical method for establishing calibration curves for the quantitation of pentaerythriol tetranitrate (PETN) from sorbent-filled thermal desorption tubes by gas chromatography with electron capture detection (TDS-GC-ECD) was developed. As PETN has been demonstrated to thermally degrade under typical GC instrument conditions, peaks corresponding to both PETN degradants and molecular PETN are observed. The retention time corresponding to intact PETN was verified by high-resolution mass spectrometry with a flowing atmospheric pressure afterglow (FAPA) ionization source, which enabled soft ionization of intact PETN eluting the GC and subsequent accurate-mass identification. The GC separation parameters were transferred to a conventional GC-ECD instrument where analytical method-induced PETN degradation was further characterized and minimized. A method calibration curve was established by direct liquid deposition of PETN standard solutions onto the glass frit at the head of sorbent-filled thermal desorption tubes. Two local, linear relationships between detector response and PETN concentration were observed, with a total dynamic range of 0.25-25ng.

KEYWORDS:

Electron capture detection; Gas chromatography; High-resolution mass spectrometry; Pentaerythriol tetranitrate (PETN); Thermal desorption

PMID:
25841610
DOI:
10.1016/j.chroma.2015.03.006
[Indexed for MEDLINE]

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