A method of monitoring the evolution of polymer and/or colloid stimuli responsiveness during synthesis of polymers and/or colloids, including postpolymerization modifications on natural and synthetic polymers, includes providing a reactor in which the polymers and/or colloids are synthesized; and providing a means of monitoring the stimuli responsiveness of the polymers and/or colloids during said synthesis. Preferably, the method also includes monitoring the evolution of the characteristics of the polymers and/or colloids during said synthesis. Preferably, evolution of polymer and/or colloid stimuli responsiveness is correlated to the evolution of the properties of the polymers and/or colloids themselves. Also, preferably the conditions of the fluid in the reactor in which the synthesis occurs is determined. The determination can be by detection, choice of materials and temperature conditions, for example, and combinations thereof. The method and instrumentation disclosed can lead to optimization and control of processes and synthetic and modification strategies leading to polymers and colloids with desired stimuli responsiveness.