A microwave plasma was generated by N 2 gas. Synthesis gases (H 2 and CO) were produced by the interaction of CH 4 and CO 2 under plasma conditions at atmospheric pressure. The experimental pilot plant was set up, and the gases were sampled and analysed by gas chromatography-mass spectrometry. The Box-Behnken design (BBD) method was used to find the optimising conditions based on the experimental results. The response surface methodology based on a three-parameter and three-level BBD has been developed to find the effects of independent process parameters, which were represented by the gas flow rates of CH 4 , CO 2 , and N 2 and their effects on the process performance in terms of CH 4 , CO 2 , and N 2 conversion and selectivity of H 2 and CO. In this work, four models based on quadratic polynomial regression have been determined to understand the connection between the limits of the feed gas flow rate and the performance of the process.The results show that the most important factor influencing the CO 2 , CH 4 , and N 2 conversion and the selectivity of H 2 and CO was "CO 2 feed gas flow rate." At the maximum desirable value of 0.92, the optimum CH 4 , CO 2 , and N 2 conversion were 84.91%, 44.40%, and 3.37%, respectively, and the selectivities of H 2 and CO were 51.31% and 61.17%, respectively. This was achieved at a gas feed flow rate of 0.19, 0.38, and 1.49 L min −1 for CH 4 , CO 2 , and N 2 , respectively.