Thermoanalytical (TA) studies including differential scanning calorimetric (DSC) and thermogravimetric (TG) analyses were carried out to measure characteristics of dried mixtures based on two unsaturated polycarboxylic acids. Model 9% treatment (pad) solutions of maleic (M) and/or itaconic (1) acid, with and without potassium peroxydisulfate (K) as the free-radical initiator, were prepared with sodium hypophosphite (H) as the catalyst and vacuum oven-dried. DSC thermograms varied with each component; even the presence of a small amount of component K was evident. TG residue production and maximum rates of weight loss were the most useful thermal parameters. Residue/rate factors, used previously as predictors, were calculated. Previous studies indicated that high residues and low rates were indicators of combinations of reactants that resulted in good durable press treatments for fabrics. Residue/rate factors were used to rank the six mixtures that reflect actual fabric treatment combinations : MH, IH, MIH, and those same three with the initiator present. Rankings indicated that the presence of the initiator significantly increased the residue/rate factor for IHK and for MIHK. The presence of the initiator appears more beneficial to itaconic acid than to maleic acid. The rankings by the TA predictor agreed with textile properties measuring appearance and strength.