In this study, we propose an approach using the gamma transmission technique based on the combination of the experimental and simulated data for determining the percentage concentration of the acid solution. The experiment consists of a collimated 137Cs radioactive source emitting a narrow gamma beam of 662 keV and a NaI(Tl) detector. Monte Carlo simulation data is used to construct the calibration curve of lnR versus the percentage concentration of acid solution at different temperatures (R is the ratio of the area under a transmission peak for an acid solution relative to that for water). The percentage concentration of the acid solution is determined based on the calibration curve and the experimental ratio R. The obtained results showed that this approach was feasible in which the percent concentration of 7 in total 8 samples of the sulfuric acid solution are less than 5% in comparison with one of the reference samples. There is only one sample with a relative deviation of 7.6%. These preliminary results suggest that it is possible to develop nondestructive testing for the rapid determination of the percentage concentration of acid solutions based on the gamma transmission technique.