<p>Carbon dioxide (CO₂) is one of the significant artificial greenhouse gases (GHGs) that produces complex trouble facing the Earth’s planet today. The volume of CO₂ discharged into the environment as a consequence of the consumption of fossil fuels rises, and there is a tremendous potential for increasing the average Earth’s surface temperature and catastrophic climate change. Regarding the research, attempts are made to curb CO₂ from primary single-point contributors, such as (a) internal combustion (IC) engines, (b)&#xa0;mobile generator systems, and (c)&#xa0;dispersed power production units. By capturing CO₂ after combustion, some research has been carried out on minimizing CO₂ emissions in IC engines and passenger vehicles. Agro-based capture material has been explored as an adsorbent for sequestrating CO₂ pollutants from a test engine’s exhaust unit. Three potential agro-based CO₂ capture materials, including (i) palm shell, (ii) barley straw, and (iii) corn cob, are used in the capture system of this experimental investigation to trap the pollutants from the test engine. The adsorption efficiency of the three adsorbents is explored by linking a capture unit filled with adsorbents to the test engine. Temperature Swing Adsorption (TSA) regeneration technique is employed in the capture unit to renew the used adsorbents. They are utilized several times to assess cyclic adsorption and desorption efficiency to test the adsorption capacity of the regenerated adsorbents. The adsorption capability of the adsorbent samples is determined over multiple experiments. The adsorbed gas components get liberated from the adsorbent’s surface during TSA operation, which is once more acquired and collected in a cylinder. The collected adsorbed gas is further analyzed in Gas Chromatography-Mass Spectroscopy (GC–MS) characterization to estimate and ascertain the gas uptake peaks of the adsorbent samples. The findings of the experimental work are addressed and presented in the current study.</p>