The extraction of polycyclic aromatic hydrocarbons (PAH) from sediments and from an urban dust standard reference material (SRM 1649) was compared using two methods; ultrasonication and Soxhlet extraction. Sample weights ranging from 0.5 g to 5 g were extracted using ultrasonication. The yield of organic material from sediment samples using ultrasonication with two solvents was 2.53 ± 0.10% while the Soxhlet method yielded 2.41 ± 0.14% of the initial sample weight. Sequential ultrasonic extraction with two solvents was much more rapid (45 minutes) than Soxhlet extraction (two days) and resulted in equal extraction efficiency. The levels of PAH extracted by ultrasonication from the urban dust standard reference material varied by no more than 15% from the certified values.