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The veteran Olympian stunned the favourite, Vladimir Morozov (Russia), with another blistering start to steal the gold medal in the men's 50m freestyle and clock an amazing 20.86 seconds.
Morozov was unable to close Schoeman down and ended second on 21.00 with Steffen Deibler (Germany) taking the bronze in 21.04.
Schoeman was unbeaten on Saturday in the 50m breaststroke (25.65) and 50m butterfly (22.05).
"This is amazing. To get almost everything right from the start was important to beat a field like this," said Schoeman afterwards.
"Three gold medals from three starts - that has not happened in a long time.
"But I must just say a huge thank you to those supporters who have continued to believe in me, this was for them."
Chad le Clos had to be content with two silver medals as American Thomas Shields provided an outstanding performance in the men's 100m butterfly, winning his first gold in 49.01.
Le Clos was close with a 49.48 swim with German Steffen Deibler earning another bronze in 49.72.
Le Clos came close again in the men's 200m individual medley just three events later.
Kenneth To (Australia) was the favourite and led from the start to win in 1 minute 52.01 seconds - but the final 50m freestyle leg from Le Clos saw him finish within 0.1 sec in a 1.52.11 with Japan's Daiya Seto taking third in 1.52.62.
