Abstract: | In this research, we used a new redox free radical initiation system consisting of potassium persulfate (K2S2O8) and sodium hypophosphite (NaH2PO2). In the presence of NaH2PO2, the thermal decomposition of K2S2O8 is accelerated, and the temperature required for the formation of free radical is reduced. We polymerized maleic acid (MA) using the K2S2O8/NaH2PO2 initiation system in an aqueous solution, and monitored the polymerization process with FT‐Raman spectroscopy. The Raman spectroscopy data indicate the formation of a saturated carboxylic acid with the disappearance of the characteristic bands of MA as the thermal decomposition of K2S2O8 progresses, thus indicating the formation of poly(maleic acid) (PMA). We also found that itaconic acid (IA) polymerizes in the presence of the new initiation system. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 81: 223–228, 2001 |