Dual electron capture detector

Various alkyl and aryltin compounds were determined in aquatic matrices, namely sediments, biota and water by means of gas chromatographic methods. In this work, comparisons of single or dual flame photometric detectors and electron capture detectors were reported (Tolosa et al., 1991). Sample preparations included acid digestion, extraction, formation of methyl derivatives and clean-up with alumina prior to gas chromatographic analysis. With the electron capture detector, cold on-column injection of organo-tin chlorides was studied. The conclusion was that a single or dual flame photometric detector equipped with a 600 nm interference filter yielded the best performance for determinations of tin species as methyl derivatives. Detection limits for the method using flame... 

The 5 to 6 L of DCM recovered from the extractor was evaporated to 25 mL in a mantel-heated flask equipped with a 12-ball Snyder condenser. Final concentration to 1 mL was made in a water-bath-heated smaller flask with a Kuderna-Danish condenser. The suspended sediments were soxhiet extracted overnight with an acetone/hexane mixture. After back extraction with water to remove the acetone, the extract was concentrated to 1 mL by the above procedure. The extract was cleaned up on a minicolumn packed with 2 cm Na2S04/4 cm 40% H2SO4 in silica gel/2 cm florisil. Final gas chromatographic analysis was performed using dual capillary columns (SE54 and OV17) with electron capture detectors. Further method details and recovery efficiencies of the procedures have been previously reported (Oliver and Nicol 1982). 

Dual Detectors. Most dual detectors are run in parallel, the column effluent being split and run through both of them simultaneously. In GC the technique is known as dual channel GC usually, one of the detectors chosen is universal and the other is highly selective. Figure 6.6 shows the analysis of a commerical gasoline sample with dual detection by flame ionization (FID) and electron capture (ECD). The FID detects all the hydrocarbons, but the ECD is selective for the alkyl lead additives in gasoline and permits their detection without interference from the hydrocarbons. 

SP-2401" and 3% SP-2250. ° Detectors used by EPA standards procedures, include photoionization (PID)," electron capture (ECD)," Eourier transform infrared spectrometry (PTIR), " and mass spectrometry detectors (MSD)." ° Method 8061 employs an ECD, so identification of the phthalate esters should be supported by al least one additional qualitative technique. This method also describes the use of an additional column (14% cyanopropyl phenyl polysiloxane) and dual ECD analysis, which fulfills the above mentioned requirement. Among MSDs, most of the procedures employ electron impact (El) ionization, but chemical ionization (CI) ° is also employed. In all MSD methods, except 1625, quantitative analysis is performed using internal standard techniques with a single characteristic m/z- Method 1625 is an isotope dilution procedure. The use of a FTIR detector (method 8410) allows the identification of specific isomers that are not differentiated using GC-MSD. 

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