A Small Punch Test method with 3 mm diameter and 0.5 mm thick specimens was utilized to characterize 3003-H14 aluminum, 2618-T61 aluminum, and Ti-6Al-4V alloys. The method was found to be repeatable and the effect of surface roughness negligible within the range of 0.450–3.011 μm. In addition, the titanium has shown higher strength and elastic modulus than the aluminum specimens. The addition of iron, copper, and nickel elements to Al makes the alloy stronger and more ductile. The research shows that the Small Punch Test can be used to qualitatively compare such mechanical properties as surface hardness, ductility, toughness, yield strength, and ultimate tensile strength of small volume test specimens in aluminum and titanium alloys. The advantage of such a method is its ability to obtain consistent evaluation of mechanical properties from small specimen volumes effectively.