Monitoring by means of blood and urine analysis for methanol was successfully applied in 32 male workers who were exposed to methyl methacrylate (MMA) monomer at 6 ppm as a geometric mean and at 112 ppm as the maximum. Measurement of time-weighted average (TWA) intensity of the vapor exposure was successfully conducted with a diffusive sampler with activated carbon cloth as an adsorbent. Methanol concentrations in whole blood, serum, and urine samples were measured by headspace gas chromatography. The methanol concentrations in the three biological samples collected at the end of 8-h workshifts related linearly with the TWA MMA vapor concentrations, with correlation coefficients of 0.8-0.9. Quantitative evaluation of MMA in vapor and of methanol in urine suggests that only 1.5% of MMA inhaled will be excreted in urine as methanol. There were no significant clinical symptoms or abnormal hematological or serum biochemical findings at this exposure level, except that some workers complained throat irritation and frequent cough and sputa. The results indicate that biological monitoring by analysis for methanol is sensitive enough to detect MMA exposure at levels at which no serious health effects are to be expected.