Determination of nitrated polycyclic hydrocarbons in aerosols using capillary gas chromatography combined with different electron capture detection methods

Abstract

A method is described which allows the determination of subnanogram concentrations of mono‐ and dinitrated polyaromatic hydrocarbons with two to four ring systems in aerosol samples. High performance liquid chromatography is used to separate the nitro compounds from other classes of substances. Carbozoles elute in the same fraction. Both electron capture detection and negative ion chemical ionization mass spectrometry combined with capillary gas chromatography are used for quantification. Use of these two methods leads to a considerable improvement of selectivity and sensitivity for nitrated compounds. In contrast to the situation with a nitrogen‐sensitive detector, carbazoles do not interfere and detection limits in the order of 10–200 pg/m3 are possible. The applicability of the method is critically discussed. Determination of nitrated polyaromatic hydrocarbons in aerosol samples from an aluminum smelter serves as an example.

Coupled LC-GC-NPD for Determination of Carbazole-Type PANH and Its Application to Personal Exposure Measurement

“…Another source of carbazoles is their formation during incomplete combustion of nitrogen-containing organic matter. Carbazoles have thus been detected in cigarette smoke condensate [25] and particulate air samples from aluminum reduction plants [13,26].…”

Mutagenicity testing of HPLC fractions from wood-stove emission samples using a modified Salmonella assay requiring smaller sample volumes

“…Normal-phase high performance liquid chromatography (HPLC) was chosen for chemical fractionation. This method has recently been used for separating extracts from diesel exhaust particles [Schuetzle et al, 1981, 19821 and ambient air particles [Eisenberg, 1978;Oehme et al, 1982;Ramdahl et al, 1982bl into classes of compounds. Usually more than 90% of the mass and the mutagenic activity injected into the column was recovered in these studies.…”

Sub-parts-per-billion determination of nitro-substituted polynuclear aromatic hydrocarbons in airborne particulate matter and soil by electron capture-Tandem mass spectrometry

“…Different mass spectrometric procedures were compared. The best performance was observed when the nitro-PAH mol ecular ions [M]-were mas s-selected by the first analyzer under multiple reaction monitoring conditions and then fragmented to NO ; ( mlz 46). Detection limits were on the order of hundreds of femtograms, as determined in extracts of real environmental samples.…”

“…As a matter of fact, the detection limits often declared from experiments on nitro-PAH standard solutions did not hold when real environmental samples were considered. Among the techniques utilized to detect nitro-PAHs, the most frequently used are gas chromatography combined with, respectively, a thermionic (TID) or nitrogen-phosphorus (NPD) selective detector [13,IS,47,50,59], chemiluminescence-based thermal energy analyzer (TEA) [31][32][33][34] and electron capture detector (ECD) [44,46,57], HPLC with either fluorescence [40][41][42]45], chemiluminescence [36,51,56], or electrochemical [37,42,43,58] detector, gas chromatography-mass spectrometry (GC-MS) in electron impact (EI) [13, 16-19, 32, 34, 35, 59], positive ion chemical ionization (PCI) [9], or negative ion chemical ionization (NCI) electron capture (EC) us. 39,46,48,55,59].…”