This dataset contains FTIR and NMR spectra for the successful purification of acrylonitrile (AN) monomer by a simple column technique which is related to our published paper with DOI 10.3390/polym13040660 1. Fig. 2a FTIR non-Pure AN (httpswebbook.nist.govcgicbook.cgiID=C107131&Units=SI&Mask=80#IR-Spec) 2. FTIR_ Pure AN_ Raw Data (Excel) 3. SigmaPlot FTIR_ Pure AN_ Raw Data 4. Pure AN_1H (1) 5. Pure AN_1H (2) 6. Pure AN_13C(1) 7. Pure AN_13C (2) 8. Non Pure AN_1H (1) 9. Non Pure AN_1H (2) 10. Non Pure AN_13C (1) 11. Non Pure AN_13C (2) 12. Figure (1) -A schematic diagram of a simple column's advantages versus the distillation technique's drawbacks 13. Figure (6)- Experimental setup of monomer purification procedure 14. Editing Figures (1) & (6) 15. Fig. 3. Chemial Structure of AN, AA, and MeHQ 16. Related research paper dataset In fact, As known, purification is of the utmost significance in any chemistry process. Besides, eliminating impurities enhances the quality and standard of the product. The primary method for monomer purification, like acrylonitrile (AN), is the distillation technique. However, this technique is unsafe and hard to set up or handle. A straightforward, risk-free, and low-cost method like the column technique resolves these issues. Therefore, the data will be helpful in numerous applications, especially in polymerization reactions that require the removal of inhibitors before the polymerization initiation process.