Carey Dale Grayson, 50, was put to death on Thursday after being found guilty of capital murder in 1996 for the murder of Vickie Deblieux, who was 37 at the time.
His attorneys contended that the US Supreme Court should examine whether the new method of death was constitutional, but the high court denied a petition that would have prevented the execution.
Nitrogen hypoxia has not been used to execute the death penalty in any other state.
Members of Grayson’s victim’s family objected to his execution for the murder at the William C. Holman Correction Facility in Alabama.
Following the execution, Deblieux’s daughter, Jodi Haley, who was 12 at the time of the murder, informed reporters that Grayson had experienced abuse as a child. “Society failed this man as a whole,” she added.