Sample application cryogenic traps

A method which uses supercritical fluid/solid phase extraction/supercritical fluid chromatography (SE/SPE/SEC) has been developed for the analysis of trace constituents in complex matrices (67). By using this technique, extraction and clean-up are accomplished in one step using unmodified SC CO2. This step is monitored by a photodiode-array detector which allows fractionation. Eigure 10.14 shows a schematic representation of the SE/SPE/SEC set-up. This system allowed selective retention of the sample matrices while eluting and depositing the analytes of interest in the cryogenic trap. Application to the analysis of pesticides from lipid sample matrices have been reported. In this case, the lipids were completely separated from the pesticides. 

Second, no work has yet been done on the application of the transpiration method to the preparation of samples for chemical analysis. In this area the same strictures on odour sampling apply, even where sub-ambient-temperature trapping techniques are used. Especially where cryogenic trapping is proposed, preparation of the odour sample in the laboratory is a considerable advantage. 

Cryogenic traps are convenient accumulation and injection devices for fast gas chromatography and interfaces for coupled-column gas chromatography, where a heartcut sample is collected and focused from the first column, and reinjected into the second column. The main requirement for a cryogenic trap used in these applications is efficient accumulation over time with rapid injection of the collected analytes as a narrow pulse in both time and space. Commercially available systems using a capacitance discharge for heating provide injection bandwidths of 5-20 ms. 

Depending on the application, the derivatized sample can either be introduced directly into the GC unit [11,13,15,16] or be preconcentrated on a Tenax or cryogenic trap, followed by thermal desorption for introduction into the column [12, 20]. Although capillary columns are now the most widely applied ]11,13,15,16,20], the use of packed columns has also been reported [12]. 

Supercritical fluid extraction (EPA 3540, for total recoverable petroleum hydrocarbons EPA 3561 for polynuclear aromatic hydrocarbons) is applicable to the extraction of semivolatile constituents. Supercritical fluid extraction involves heating and pressuring a mobile phase to supercritical conditions (where the solvent has the properties of a gas and a liquid). The supercritical fluid is passed through the soil sample, and the analytes are concentrated on a sorbent or trapped cryogenically. The analytes are eluted with a solvent and analyzed using conventional techniques. Carbon dioxide is the most popular mobile phase. 

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