A couple of roller-bladers terrorize vendors in Central Park, with Spidey showing up too quickly deal with them. Medusa appears and confirms to the police that Spidey had nothing to do with the trouble. She claims to be just visiting New York, but has in fact been invited there by the Wizard, her old partner in crime. She refuses his offer of joining forces with him, so the Wizard gives Medusa an irremovable collar forcing her to work for him. Together, they steal cylinders of the rare metal element Niobium, so that the Wizard can construct an anti-gravity weapon. Medusa accidentally drops two of the cylinders and the alarm is sounded. Spidey turns up and fights the Wizard, not believing that Medusa is working for him again. The Wizard escapes, leaving Spider-Man and Medusa to talk about her problems, but she quickly leaves to join up with the Wizard before he does anything to the collar. The Wizard asks Medusa to steal an electronic component from a military base with Spider-Man's help. She tricks Spidey into helping her steal the component, and the Wizard then traps Spidey in his lair. Trapped in a room with increasingly hot walls, Spidey has to figure a way out in time to stop the Wizard and his anti-gravity weapon.

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Although this was the last episode produced, the adventures of this particular animated incarnation of Spider-Man were continued in Spider-Man And His Amazing Friends. The episodes "Origin Of The Iceman" and "Origin Of The Spider-Friends" detailed (in flashback) what happened in-between the two series. Aunt May was still a regular character in the series, but Jameson appeared in only four episodes.