First choice: I like the "Zip-A-Dee-Doo-Dah" scene in Splash Mountain a lot. It caps off a great bit of storytelling and ends the ride on a satisfying note.
Second choice: The hallway scene in Tower of Terror is superb, particularly with the floating picture. Creeeeepppyyyy....
I used to LOVE the trolls sending you backwards down a slope in the old Maelstrom ride. That, and the ride's beginning with Odin's strobing eye. So cool. Simple things, but well done.
I like the ship battle in Pirates too, but I think it needs to be majorly plussed. It's a bit dated looking.
And I like flying over London in Peter Pan's Flight. Although I think I like the idea better than its actual execution.