Among polymerization techniques, conventional radical polymerization in solution is widely used. Polymerization is composed at least of three main steps known as initiation, propagation and termination [1]. However, undesired reactions, named as chain transfer reaction can cause the formation of polymers with undesirable properties (large Chain length distribution) [2]. To solve this drawback, Living radical polymerization is a promising solution. A Chain Transfer Agent (CTA) is added to the mixture for limiting the irreversible termination reactions [3]. Among Living polymerization strategies, Reversible Addition-Fragmentation Chain Transfer (RAFT) is based on reversible exchange of end group function between a dormant and an active macro radical. This technique may be potentially applied to any polymerizable monomers using operating conditions close to the ones used in conventional radical polymerization[2]. Kinetic parameters of each individual step of the polymerization reaction, in particular propagation constant (kp) can give valuable information in order to optimize the properties of the final polymer (chain lenght distribution, Molar Weight). The knowledge of these kinetic parameters is also essential to evaluate heat released by these reactions, enabling to design a cooling system to reduce thermal runaway risk of reactor. Indeed the reactions of polymerization are implied in industrial accident according to statistics [4]. Most of kinetic studies met in literature are carried out up to low reaction extent, although industrial process are run up to higher extent. Pulsed laser polymerization coupled to size-exclusion chromatography (PLP-SEC) [5] or electron spin resonance (ESR) [6] enable to investigate radical polymerization kinetic with non-stationary conditions. Both techniques can determine kp. Other techniques such as FTIR spectroscopy and calorimetric measurements [7] are also used and are based on the kinetic consumption of monomer. The latter give a global kinetic constant of polymerization reaction (Kpoly) using quasisteady state assumption measurement. These techniques do not allow a quantitative analysis and cannot separate the three different main steps of radical polymerization. In opposition to classical polymerization kinetic studies, the determination of thermokinetic parameters with a calorimetric method using a reaction calorimeter RC1–RTCal allows having operating conditions close to industrial processes and reaching a high reaction extent [4]. This method consists in comparing thermal power profiles measured during experiments with profiles calculated by means of differential equations representing instantaneous mass and energy balances of a mass and energy models. Thus, kinetic parameters of each individual step can be estimated through an inverse method [4]. This present work focuses on the determination of kinetics parameters of RAFT polymerization in solution of dodecyl methacrylate monomers (DDMA) with a calorimetric method using a reaction calorimeter RC1–RTCal. Polymerization is initiated with liquid monofunctional organic peroxide Tert-Butylperoxy 2-ethylhexyl carbonate (TBEC). Anisole is chosen as a solvent according to the fact that Anisole dissolves monomer and the produced polymer and it is also inert with regard to the formed radicals. The reagent 2-Cyano-2-propyl dodecyl trithiocarbonate is selected as CTA because it reacts with methacrylated monomers [3]. The reaction is led under Argon atmosphere as Oxygen is a powerful polymerization inhibitor. The power profile released by the reaction is measured by means of a RC1–RT Cal reaction calorimeter from Mettler. The kinetic parameters of each steps of RAFT polymerization will be estimated using the inverse method, described above.