The extraordinary mechanical and swelling/deswelling properties of nanocomposite (NC) gels are attributed to their unique organic (polymer)/inorganic (clay) network structure. In this study, poly(N‐isopropylacrylamide) (PNIPA) was successfully separated from an NC gel network by decomposing the clay (hectorite) using hydrofluoric acid (HF). A very low HF concentration (0.2 wt.‐%) was adequate for the decomposition of the clay without causing any damage to PNIPA. The separated PNIPA had a high (=5.5 × 106 g · mol−1). Also, was almost constant regardless of the clay concentration (Cclay = 1–25 × 10−2 mol · l−1), even though the properties of the NC gel varied widely over this Cclay range. Comparisons of NC gels, PNIPA, and SiO2‐NC gels indicated that the clay platelets specifically play an important role in NC gels.
(=5.5 × 106 g · mol−1). Also, 
was almost constant regardless of the clay concentration (Cclay = 1–25 × 10−2 mol · l−1), even though the properties of the NC gel varied widely over this Cclay range. Comparisons of NC gels, PNIPA, and SiO2‐NC gels indicated that the clay platelets specifically play an important role in NC gels. 