Ward, the British number two, led by a break in the final set but lost 6-3 3-6 6-4 to India's Somdev Devvarman.
Baltacha served for the match against Michelle Larcher de Brito of Portugal but eventually went down 4-6 7-5 6-1.
Dan Evans is the remaining Briton in qualifying and plays Spain's Adrian Menendez-Maceiras later on Friday.
Defending champion Andy Murray,
30th seed Laura Robson and world number 77 Heather Watson have qualified directly for the main singles draw.
Ward, 26, was visibly upset as he made his way off Court Seven after seeing a great chance to qualify at the US Open for the first time slip by.
The Londoner, ranked 175th, looked to have turned things around after battling back from a set and a break down, reeling off six straight games to lead 2-0 in the decider.
Devvarman, 28, remained a tough opponent to break down, however, and the world number 113's steadier play ultimately won the day as he broke back in game six and clinched victory after two hours and 15 minutes.
Baltacha, ranked 244 as she makes her way back from injury, went even closer than Ward, serving superbly as she took the first set and recovering from 3-0 down in the second to serve for victory at 5-4.
De Brito, who knocked Maria Sharapova out of Wimbledon in June, had been driven to distraction at times, smacking the net and the back fence with her racquet in anger, but she gathered herself to win three straight games and force a decider.
The final set was closer than the score suggests but Baltacha could not contain the 20-year-old Portuguese, who secured her place in the main draw after two hours and 31 minutes.
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