The whole scene with Shelob pouncing on Frodo, and then Sam being left all alone. And having to get past the Watchers and go through Cirith Ungol looking for Frodo.
Pippin and Merry in the hands of the Uruk-Hai.
Also the suicide of Denethor and the attempted murder of Faramir.
I guess nothing in LOTR is really scary in the typical "Stephen King" scary way. But you care so much for the characters that you hate watching them suffer.
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