The filling behavior of a room temperature solvent, perfluoro-methyl-cyclohexane, in ∼20 nm nanoporous alumina membranes was investigated in-situ with small angle x-ray scattering. Adsorption in the pores was controlled reversibly by varying the chemical potential between the sample and a liquid reservoir via a thermal offset, ∆T . The system exhibited a pronounced hysteretic capillary filling transition as liquid was condensed into the nanopores. These results are compared with the Kelvin-Cohan prediction, with a prediction in which the effect of the van der Waals potential is combined with the Derjaguin approximation and also with recent predictions by Cole and Saam. [7]; not to mention more commonplace applications such as filtering and humidity sensors [8]. The breadth of nanopore research serves to underscore the need for a solid physical understanding of the evolution of liquids in such systems. Experimental studies have been done on porous network systems, such as the disordered Vycor [9] and M41S silica materials [10]. Unfortunately, these porous systems have very complicated network geometries that make it rather difficult to compare the measurements with simple theoretical predictions. Additionally, most of these studies are done at low temperatures that are impractical for all of the applications described above. Room temperature measurements on ordered nanoporous systems with nearly ideal geometry should provide insight into the physical processes governing liquid behavior in more general nanoporous systems.We describe here in-situ small angle x-ray scattering (SAXS) experiments of the equilibrium wetting and capillary condensation of a room temperature solvent, perfluoro-methyl-cyclohexane (PFMC), within nanoporous alumina (Al 2 O 3 , pore diameter ∼ 20 nm). The anodized alumina system had an ideal geometry described by a parallel arrangement of cylindrical nanopores with large aspect ratios ∼ 1:5,000, see Fig. 1. [11] Experiments were carried out within an environmental chamber that allowed precise control of the amount of solvent condensed within the pores via changes in the chemical potential, ∆µ, relative to liquid/vapor coexistence similar to studies of wetting on flat [12] and nanostructured surfaces [13]. Both adsorption and desorption processes were investigated reproducibly via this technique. Porous alumina membranes were prepared electrochemically using a two-step anodization technique [11,14] and cleaned as described elsewhere [4]. The resultant alumina membrane consisted of an array of cylindrical parallel pores running the entire thickness of the membrane and open on both ends. The macroscopic dimensions of the nanoporous membrane were about 1 cm × 1 cm × 90 microns. Pores formed a 2D local hexagonal order (see Fig. 1) with nearest neighbor distances (center to center) of 58±4 nm, and diameter of 21 ± 5 nm, determined via electron microscopy. After cleaning, samples were dried and loaded into a hermetically sealed environmental chamber under an atmosphere of "ultra-pure" grade N 2 .Th...