The nitrogen should be flowing in the space above the solution, not bubbling through the solution. Pierce the rubber septum and introduce a nitrogen flow through the flask. Place a rubber stopper into the center neck of the flask, and a rubber septum over one of the other necks. If extract concentration is low relative to the limit of detection, transfer the filtered hexanes into a clean, dry three-necked round-bottom flask, 100 mL in size. If the extract concentration is sufficient for detection, the filtered hexanes may be transferred to a clean, dry flask for storage and later analysis. Once a clear solution has been achieved, separate the hexanes from CaCl 2 using gravity filtration. If the solution is translucent and the CaCl 2 is free flowing, then do not repeat step 3.1. If the solution is still cloudy and/or all of the CaCl 2 is clumped, there is still water remaining, and step 3.1 should be repeated. Swirl the solution and observe for a minimum of 15 min. To dry the n-hexane solution, add one small spatula of CaCl 2.
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