This study developed a method to produce uniform captan surface films on a disposable nitrile glove for quantitation with a portable attenuated total reflection Fourier transform infrared (ATR-FTIR) spectrometer. A permeation test was performed using aqueous captan formulation. Uniform captan surface films were produced using solvent casting with 2-propanol and a 25 mm filter holder connected to a vacuum manifold to control solvent evaporation. The coefficient of variation of the reflectance at 1735 ± 5 cm−1 was minimized by selection of the optimum solvent volume, airflow rate, and evaporation time. At room temperature, the lower to upper quantifiable limits were 0.31–20.7 μg/cm2 ( r = 0.9967; p ≤ 0.05) for the outer glove surface and 0.55–17.5 μg/cm2 ( r = 0.9409; p ≤ 0.05) for the inner surface. Relative humidity and temperature did not affect the uncoated gloves at the wavelength of captan analysis. Glove screening using ATR-FTIR was necessary as a control for between-glove variation. Captan permeation, after 8 hours exposure to an aqueous concentration of 217 mg/mL of Captan 50-WP, was detected at 0.8 ± 0.3 μg/cm2 on the inner glove surface. ATR-FTIR can detect captan permeation and can determine the protectiveness of this glove in the field.