- Sandman (Flint Marko) (First appearance as Sandman) (Apparent death)
- The Big Man (Mentioned)
- Alex O'Hirn
- Norman Osborn
- "Flash" Thompson
- Glory Grant
- Kenny Kong
- Hobie Brown (First appearance)
- Otto Octavius
- Emily Osborn (First appearance)
- Anna Watson (Mentioned)
- Anna's Niece (Mentioned)
Peter, as Spider-Man, effectively defeats two common thugs - Flint Marko and Alex O'Hirn - and puts them in prison. While discussing their outrage towards Spider-Man, their bail is paid by Hammerhead and they go into a limousine outside. Inside the limousine, Hammerhead tells them he has big plans for them, taking them to a secret base.
The next day, Peter practices his web slinging in his bedroom, when Aunt May walks in. He stops and she suggests he takes their neighbor Mary Jane Watson to the upcoming Fall Formal. Since Mary Jane had been referenced previously for her "wonderful personality", Peter cringes at the idea and heads off to school. There, it is announced football practices will be held that day and Harry wants to try out. Peter passes on joining him as he feels it will reveal his abilities. When he hears Flash Thompson planning on specifically going after Harry tryouts, he decides to keep him safe and try out anyways. They each do good at tryout - Harry impresses the coach and the other player while Peter does the same using his extra abilities.
Meanwhile, Norman Osborn arrives at the warehouse to supervise an experiment on Marko, which will insert silicon into his DNA. Dr. Octavius says that the experiment has too many flaws but Osborn commands him to go with it anyways. The experiment malfunctions and the silicon violently mutates him. His body evaporates into sand and Octavius, terrified, thinks he has just killed him. Suddenly, Marko reshapes himself, still made of sand, and viciously thrashes against the walls for them to let him out. Hammerhead and Osborn take him outside in their limousine, where Marko is able to reform himself in his old appearance. They tell him he will work for "the Big Man," but he instead goes to commit more crime while happily evading Spider-Man (for once). Hammerhead is fine with that as it means they will now have a distraction for Spider-Man.
Now codenamed "Sandman," Marko robs a bank and Spider-Man arrives immediately. He is overpowered by Marko's new powers and finds himself out of web fluid. After defeating Spider-Man, Sandman escapes through a sewer drain, after accidentally mentioning the "Big Man's" name. The next day, Peter goes to tryouts again, doing well once more and being invited for the last day of tryouts along with Harry. Harry is upset that he outshined him and invites the other players to hang out at a soda shop. Meanwhile, Peter goes on the city bus and sits next to Gwen, whom he apologizes to for ignoring her lately and she accepts. She also hints that he should take her to the fall formal, but he does not get the clue and tells her he is going to ask Betty Brant, a woman who works at the Daily Bugle.
After departing from the bus, Peter goes off as Spider-Man to an armored truck, which Sandman is robbing. In their struggle, the truck goes out of control and lands in a construction site. When Spider-Man tries to web him up, it proves to be ineffective as Sandman can slip through them; the villain then starts to attack Spider-Man with girders. Meanwhile, at the soda shop, Harry tries to impress the jocks, catching Kenny's girlfriend Glory's attention. Kenny plays a prank on Harry, which enrages Glory and she asks Harry to take her home. Back on the construction site, Spider-Man gets out from the pile of girders and gets the head on Sandman. He lures him up to the roof and encases him in cement from the nearby cement maker before spitting out some sand.
That night, Harry comes home to tell his father that he's tried out for the football team, but he is unimpressed. Harry walks off, darkly remarking that he will "show them tomorrow." At final tryouts the next day, Harry makes the team, and Peter purposely does terrible so he doesn't outshine his friend. Gwen then cheers him up with ice cream.
- Production Code 105