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Gschwend%20thesis.pdf

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-81-<br />

o<br />

(heated to 60 C to reduce the relative humidity), before reaching a<br />

charcoal trap. The microcharcoal trap consists. of a glass tube in<br />

which about I mg of charcoal has been fixed between two stainless steel<br />

screens glass-blown into the tube. After passing through the trap, the<br />

air returns to the pump for recirculation through the system, The<br />

sample was stripped for 2 hours at a flow rate of about 1.5 liter/min.<br />

o<br />

The water sample was heated to 35 C by a water bath. All water samples<br />

were restripped onto a fresh trap for an additional 2 hours immediately<br />

after the first strip (henceforth referred to as a restrip) i<br />

After stripping, the trap was removed from its holder and<br />

with is ~l CS2 (figure 3-3).<br />

extracted<br />

This was done by adding another internal<br />

standard (2 ~l of 20 ng l-chloro-n-octane/~l CS2) onto the trap and then<br />

adding 6 ~l CS2. Cooling the vial of the assembled extraction apparatus<br />

drew the solvent plug down through the charcoal. Warming the vial<br />

pushed<br />

the solvent back up through the charcoaL. After several such passes ,the<br />

solvent was drawn down and away from the charcoal by prolonged cooling,<br />

and with a quick flick was shaken down into the bottom of the vial.<br />

Repeating the extraction with an additional 6 ~l CS2 efficiently completed<br />

the removal of the volatiles from the trap and provided a concentrated<br />

solution for further analysis.<br />

Gas Chromatography and Gas Chromatography ~ Mass Spectrometry<br />

The volatiles were analyzed using gas chromatography (GC) and<br />

combined gas chromatography-mass spectrometry (GCMS). A single SE54<br />

glass capillary column (0.3 mm i.d. x 20 m long; purchased from Jaeggi,<br />

9043 Trogen, Switzerland) was used. A Carlo Erba Model 215l ACgas<br />

chromatograph equipped with a flame ionization detector (FID) and<br />

special Grob inj ec tor was used. Injections were made with the split<br />

a

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