CAPILLARY SUPERCRITICAL-FLUID CHROMATOGRAPHY WITH NITRO-SPECIFIC AND NITROSO-SPECIFIC CHEMILUMINESCENCE DETECTION

The thermal energy analyzer (TEA), a gas-phase chemiluminescence detector which is specific for nitro and nitroso compounds, was evaluated as a detector for use with capillary supercritical fluid chromatography. The potential use of the TEA for thermally labile compounds and environmental samples was demonstrated. The TEA showed good sensitivity and broad linear dynamic range; minimum detectable quantities (MDQ) were below 20 pg for pentaerythritol tetranitrate (PETN) with a dynamic range of over 4 orders of magnitude. The analysis of cyclotetramethylene tetranitramine (HMX) was accomplished by using modified (CO2) with a corresponding MDQ of 67 pg. The selectivity of the TEA for nitro and nitroso compounds can be adjusted by changing the pyrolysis temperature. The SFC/TEA system was applied to a variety of nitro and nitroso compounds, and evaluated more extensively for routine analysis of propellant and explosive residues.