The Amazing Spider-Man #032 (1966)
“Man on a Rampage!”
Writer: Stan Lee
Artist: Steve Ditko
Aunt May is in hospital with radiation poisoning in her blood due to a transfusion from Peter. Doc Ock turns out to be the one behind the goons on the submarine. Dr. Connors helps Spider-Man develop a serum to cure Aunt May. Spider-Man gets trapped under a bunch of fallen machinery during a fight with Doc Ock. Second of three-parter.