The authors describe a new and unique nanosensing system: a derivative of poly(acrylic acid) (PAA, M-w = 1.250.000) possessing a comb-like structure. This structure is achieved by attaching perfluorinated (-O-C8F17) functions and chemically linked pyrene fluorescent units to the PAA backbone. The average composition of the new materials was investigated by UV/vis absorption spectroscopy, DOG, and elementary (CHN) analysis. Gel permeation chromatography (GPC) led to the conclusion that the new polymeric materials are almost monodisperse, The change of pH from the basic to the acidic range causes a collapse of the macromolecules in an aqueous environment, and consequently the formation of preformed excimers is suppressed. These novel materials are designed for use in sensor heads for the photochemical detection of the pH and CO2 content of water solutions. Using a model experiment, we show how these characteristics can be used for the measurement principles.