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Title: Separation and characterization of nitrated polycyclic aromatic hydrocarbons by high resolution gas chromatography, thermionic ionization detection, and mass spectrometry

Abstract

The gas chromatographic retention characteristics of fifty-six nitrated polycyclic aromatic hydrocarbons (nitro-PAH) have been determined on fused-silica capillary columns coated with SE-52 during linear-temperature-programming and isothermal experiments. The linear-temperature-programmed retention indices were calculated according to the relationship of van Den Dool and Kratz using the bracketing standards naphthalene, phenanthrene, chyrsene, and picene. The high degree of reproducibility of these retention indices from column to column and instrument to instrument led to optimism that these calculated values will be valuable in interlaboratory comparisons of retention information of nitro-PAH. Initial column temperature, as well as capillary column inner diameter, were varied to determine their effects on retention indices. The effect of operating temperature on retention was determined while operating isothermally at 130/sup 0/, 140/sup 0/ and 150/sup 0/C. Relationships between physical and chemical properties of nitro-PAH and their gas chromatographic retention characteristics were formulated. Nitro-PAH were found to elute as a function of the compound's vapor pressure and thus of its boiling point. The selectivity and sensitivity of a thermionic ionization detector employing a pure nitrogen atmosphere (TID-1-N/sub 2/) towards nitrated aromatics were investigated. Specifically, the detector's response, linear dynamic range, limits of detection, and selectivity towards some nitro-PAH were evaluated. Thismore » detector was shown to be of great potential utility in detecting trace amounts of nitro-PAH in samples from various sources. The electron impact mass spectra of fifty-five nitrated polycyclic aromatic hydrocarbons were determined. Comparison of these spectra revealed fragmentation patterns common to all nitro-PAH. Among the isomeric nitro-PAH studied, the mass spectral fragmentation patterns were very similar. 74 refs., 18 figs., 15 tabs.« less

Authors:
Publication Date:
Research Org.:
Tufts Univ., Medford, MA (USA)
OSTI Identifier:
5563691
Report Number(s):
DOE/OR/00033-T100
ON: DE85015021
DOE Contract Number:  
AC05-76OR00033
Resource Type:
Technical Report
Resource Relation:
Other Information: Portions of this document are illegible in microfiche products. Thesis
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; POLYCYCLIC NITRO COMPOUNDS; GAS CHROMATOGRAPHY; MASS SPECTRA; EXPERIMENTAL DATA; HIGH TEMPERATURE; MASS SPECTROSCOPY; SENSITIVITY; SPECIFICITY; TEMPERATURE DEPENDENCE; CHROMATOGRAPHY; DATA; INFORMATION; NITRO COMPOUNDS; NUMERICAL DATA; ORGANIC COMPOUNDS; ORGANIC NITROGEN COMPOUNDS; SEPARATION PROCESSES; SPECTRA; SPECTROSCOPY; 400102* - Chemical & Spectral Procedures; 400104 - Spectral Procedures- (-1987)

Citation Formats

Hoes, R M. Separation and characterization of nitrated polycyclic aromatic hydrocarbons by high resolution gas chromatography, thermionic ionization detection, and mass spectrometry. United States: N. p., 1983. Web.
Hoes, R M. Separation and characterization of nitrated polycyclic aromatic hydrocarbons by high resolution gas chromatography, thermionic ionization detection, and mass spectrometry. United States.
Hoes, R M. Sun . "Separation and characterization of nitrated polycyclic aromatic hydrocarbons by high resolution gas chromatography, thermionic ionization detection, and mass spectrometry". United States.
@article{osti_5563691,
title = {Separation and characterization of nitrated polycyclic aromatic hydrocarbons by high resolution gas chromatography, thermionic ionization detection, and mass spectrometry},
author = {Hoes, R M},
abstractNote = {The gas chromatographic retention characteristics of fifty-six nitrated polycyclic aromatic hydrocarbons (nitro-PAH) have been determined on fused-silica capillary columns coated with SE-52 during linear-temperature-programming and isothermal experiments. The linear-temperature-programmed retention indices were calculated according to the relationship of van Den Dool and Kratz using the bracketing standards naphthalene, phenanthrene, chyrsene, and picene. The high degree of reproducibility of these retention indices from column to column and instrument to instrument led to optimism that these calculated values will be valuable in interlaboratory comparisons of retention information of nitro-PAH. Initial column temperature, as well as capillary column inner diameter, were varied to determine their effects on retention indices. The effect of operating temperature on retention was determined while operating isothermally at 130/sup 0/, 140/sup 0/ and 150/sup 0/C. Relationships between physical and chemical properties of nitro-PAH and their gas chromatographic retention characteristics were formulated. Nitro-PAH were found to elute as a function of the compound's vapor pressure and thus of its boiling point. The selectivity and sensitivity of a thermionic ionization detector employing a pure nitrogen atmosphere (TID-1-N/sub 2/) towards nitrated aromatics were investigated. Specifically, the detector's response, linear dynamic range, limits of detection, and selectivity towards some nitro-PAH were evaluated. This detector was shown to be of great potential utility in detecting trace amounts of nitro-PAH in samples from various sources. The electron impact mass spectra of fifty-five nitrated polycyclic aromatic hydrocarbons were determined. Comparison of these spectra revealed fragmentation patterns common to all nitro-PAH. Among the isomeric nitro-PAH studied, the mass spectral fragmentation patterns were very similar. 74 refs., 18 figs., 15 tabs.},
doi = {},
journal = {},
number = ,
volume = ,
place = {United States},
year = {1983},
month = {5}
}

Technical Report:
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