Steenbergen stuns O'Callaghan to win 100 free, Douglass dominates 200 backstroke
O'Callaghan has already won three gold medals this week, taking her overall tally to 11, and one more would see her move past Ian Thorpe to become the most successful Australian swimmer at the world championships.
However, she found herself in fourth place after the first 50 in Friday's final and was unable to claw back the deficit as Steenbergen touched first in 52.55 seconds, 0.12 ahead of O'Callaghan with American Torri Huske (52.89) third.
Steenbergen's victory made her the first swimmer to successfully defend their title from last year's world championships.
O'Callaghan, who won gold in the 200 on Wednesday, said her exertions from Thursday's programme affected her. In addition to the 100 semi-finals, she also anchored Australia home to win gold in the 4x200 relay.
"I'm tired, I'm not going to lie," she told Australian broadcaster Nine Network. "None of the girls did what I did last night. I'm happy to walk away with a medal.
"I'm pretty happy, and it just shows the strength that I have and the work I can do in the future knowing that I've barely done any training for this."
South African Pieter Coetze was also denied a double in the men's backstroke as reigning Olympic and 2023 world champion Hubert Kos powered to victory in the 200, posting a time of 1:53.19.
Both swimmers were on world record pace at the 150 metres mark before the Hungarian inched ahead and touched the wall first by 0.17 seconds. Frenchman Yohann Ndoye-Brouard took bronze.
With Olympic champion Leon Marchand skipping the 200 breaststroke, China's Qin Haiyang powered home from lane eight to win gold and make it a double after his victory in the 100.
The world record holder, who swept the 50, 100 and 200 breaststroke titles at the 2023 championships in Fukuoka, looked a spent force coming into the home stretch but got his second wind to power past the competition on the outside.
Qin clocked a winning time of 2:07.41 ahead of Japan's Ippei Watanabe and Caspar Corbeau of the Netherlands.
Qin's performance in Singapore went some way towards making up for his poor showing at last year's Olympics, where he ended seventh in the 100 and failed to even qualify for the 200 final.
American Douglass was absolutely dominant in the women's 200 breaststroke, swimming a scorching 2:18.50 to record the second-fastest time in the event.
The 23-year-old was relentless, surging further and further ahead of the field to win gold by a body length ahead of Russian Evgeniia Chikunova, the world record holder who is competing as a neutral athlete. South African Kaylene Corbett was third.
Douglass credited Chikunova for pushing her to a personal best, saying: "I was really excited to race her tonight.
"Honestly, if I wasn't racing her, I don't know if I would have gone a 2:18. I think that really helped push me to be my best."
Douglass was afforded barely any time to recover from her explosive effort, returning to the pool just 15 minutes later for the 50 butterfly semi-finals.
The turnaround proved too quick for the American, however, as she finished 14th fastest and failed to make Saturday's final, where compatriot Gretchen Walsh will be favourite to add the 200 title to the 100 gold she won on Monday.
In the final event of the evening, Duncan Scott put in a crucial shift in the anchor leg of the men's 4x200 freestyle relay as Olympic and 2023 world champions Britain won gold in a time of 6:59.84.
China were second and Australia took bronze, while France were only sixth after Marchand was left with too much to do in the final leg.
Australian Kaylee McKeown remains on track for a double in the women's backstroke, posting the fourth-fastest time in the 200 semi-finals, just ahead of rival Regan Smith.
On Saturday, American great Katie Ledecky will once again face off against Canadian sensation Summer McIntosh in the women's 800 freestyle final in one of six golds up for grabs on the penultimate day of the championships.
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