A novel approach to isolation of semivolatile organic compounds from aqueous media is proposed based on combined distillation and solid phase extraction. A model compound, 1,3,5-trimethylbenzene, was concentrated with good yield on polyurethane foam coating of a cooler positioned above the boiling aqueous mixture. It was found that terpenes are released very slowly from intact Norway Spruce (Picea abies) needles even at the boil. Also microwave-assisted extraction with hexane was inefficient. The vibrational circular dichroism spectrum of compounds isolated from the needles by distillation and solid phase extraction was too complex to be easily interpreted.