The Batman/Superman Hour: Season 1, Episode 2
The Cool, Cruel Mr. Freeze/The Joke's on Robin/Can a Luthor Change His Spots?/Superboy Meets Mighty Lad (21 Sep. 1968)
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All of Gotham's water will turn to ice unless Mr. Freeze can be stopped but will posing as a criminal work for Batman? / Batman decides to go solo after Robin gets in his way while trying to apprehend the Joker.