In the Anime, the episode is "Transformed at Last". In the games, it's usually the final battle in the Frieza Saga if it counts 100% Frieza. If not, it's the second to last.
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35. goku's ascension
Transformed At Last.
Episode 230 "Super Saiyan 3"
Goku does not turn super saiyan 6 or 5 in fact. and it only goes up to super saiyan 3 in the manga and super saiyan 4 in the cartoon.
Goku goes super saiyan 3 episode 246 in dragon ball z the episode name is super saiyan 3?! So its kinda hard to miss