The distribution of noble metal nanoparticles in hydrogels are influencing their nanoplasmonic response and signal used for biosensor purposes. By controlling the particle distribution, it is possible to obtain new nanoplasmonic features with new sensing modalities. Particle distributions can be characterized by using volume-imaging methods such as the focused ion beam-scanning electron microscope (FIB-SEM) and the serial block-face scanning electron microscopy (SBFSEM) techniques . Since the pore structure of hydrogels is contained by the water absorbed in the polymer network it may pose challenges for volume-imaging based on electron microscope techniques since the sample must be in a vacuum chamber. The structure of hydrogels can be conserved by choosing appropriate preparation methods, which also depends on the composition of the hydrogel used. In this paper, we have prepared low-weight percentage hydrogels, with and without gold nanorods (GNR) for conventional SEM imaging by using two different drying techniques; (1) the critical point drying (CPD) technique and (2) hexamethyldisilazane (HMDS) drying of hydrogels. A qualitative characterization of the GNR-hydrogels was carried out to study the GNRs positioned in the polymer network. The effect of the two different drying methods on the hydrogel morphology were also compared. The use of HMDS as an alternative to the CPD has several advantages involving less parametrical variables for drying, involving less effort, being cost-effective, and requires no equipment use. In addition, choosing an optimized sample preparation method for SEM with optimized imaging parameters is highly important for obtaining accurate information about materials that is not correlated to artifacts. Hence, the results obtained from the preparation methods and SEM imaging parameters in this paper are useful for developing methods for mapping the metal particle distributions in micro-hydrogels by using FIB-SEM and SBFSEM techniques.