Volatile agents for anaesthesia are widely used for anaesthetizing laboratory primates, and isoflurane is one of the most frequently used agents. Sevoflurane has been shown to offer a more rapid recovery than isoflurane in a number of species, but no comparisons have been made in non-human primates. This study compared the recovery characteristics of isoflurane and sevoflurane in rhesus macaques undergoing experimental neurosurgery. Twelve primates (7 males and 5 females) were randomly allocated to the treatment groups. They were sedated with ketamine (10 mg/kg) and anaesthesia was induced with propofol (usually 8 mg/kg intravenously [IV]). Anaesthesia was maintained with either sevoflurane (SEVO) (2.2 ± 0.4%) or isoflurane (ISO) (1.2 ± 0.2%) and alfentanil (0.2-0.5 µg/kg/min IV) for 332-592 min. Animals were mechanically ventilated. Meloxicam (0.3 mg/kg) and methylprednisolone infusion (5.4 mg/kg/h) were also administered. Time to extubation after cessation of anaesthesia was significantly shorter with sevoflurane (ISO: 7.0 ± 1.8 min; SEVO: 3.6 ± 1.5; *P = 0.005) as was the time to the animal sitting unaided (ISO: 15.7 ± 8.2 min; SEVO: 7.1 ± 1.7 min; *P = 0.004) . No significant difference in the quality of recovery following isoflurane or sevoflurane anaesthesia was found. In conclusion, isoflurane and sevoflurane are both suitable volatile agents for the maintenance of general anaesthesia in rhesus macaques undergoing experimental neurosurgical procedures. The two volatile agents presented a similar emergence quality profile, however sevoflurane anaesthesia was associated with a faster recovery, offering the possibility of conducting earlier post-operative neurological assessment.