The efficacy of sulfuryl fluoride was evaluated for control of fourth-instar pecan weevil, Curculio caryae (Horn), at 25°C for a 24-h exposure. Larvae, collected as they naturally emerged from pecans, were used to artificially infest pecan nuts. Infested nuts were fumigated with six concentration by time (CT) treatment dosages of sulfuryl fluoride (0–750 g-h/m³) within air-tight, glass containers. The sulfuryl fluoride concentration in each fumigation container was analyzed 30 min after sulfuryl fluoride introduction and just prior to termination of the experiment. Mean sulfuryl fluoride CT dosages were calculated from sulfuryl fluoride measurements and were used for probit analysis. The lethal accumulated dosage (LAD₉₉) of sulfuryl fluoride for pecan weevil was 1052.0 g-h/m³ with a 95% C.I. of 683.21–2,573.0 g-h/m³. For the confirmatory trial, we used two sulfuryl fluoride CT dosage treatments, 1,100 and 1,300 g-h/m³, and a nonfumigated control. All larvae were dead in both fumigation treatments by 14-d postfumigation. Due to higher mortality in the nonfumigated control in the confirmatory trial compared to that of the dose–response trial, 1300 g-h/m³ was selected as the sulfuryl fluoride CT dosage for a proposed quarantine treatment schedule. Fumigating pecans with sulfuryl fluoride can control larval pecan weevil infestations in commercially traded nuts and maintain compliance with quarantine regulations both within and outside the United States.