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FuzzyBoots
FuzzyBoots
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It looks like it happened in the March 1963 issue, "Menace to Society".

Three panels of a Spider-Man comic. One, the Chameleon, disguised as a police-man, is about to pull a fuse as Spider-Man realizes Chameleon's disguise. Two, the lights are out, but Spider-Man can still sense Chameleon. Three, Spider-Man realizes he's out of the fluid that makes his webbing.

Valorum also provided two images of other times it has happened, but I haven't found the source thereof:

In the middle of a crisis, Spider-Man runs out of web-fluid and cries, "Nuts!" Spider-Man checks the cartridges at his waist and realizes he used up his entire supply to web up "Juggy" that morning.

FuzzyBoots
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