A test-rig closed-loop flotation column was used to observe the effect of diesel oil (collector) and Flomin F-425 (frother) on mass yield and ash content for two Colombian coals: Caypa (northern zone) and Guachinte (southwestern zone). The coal samples of less than 38 µm (-400 M) were processed in a collector concentration range of 0,32 to 1,60 kg/ton of coal, as well as a frother concentration range of 10 to 50 ppm. The response surface methodology was used for the experimental test runs. The results showed that the maximum mass yield obtained by Caypa coal was 98,39% at 1,28 kg of collector/ton of coal and 40 ppm of frother concentration, whereas Guachinte coal obtained a maximum mass yield of 94,71% at 0,96 kg of collector/ton of coal and 30 ppm of frother concentration. In general, for Caypa coal, the mass yield tends to increase (low ash removal) with the collector and frother concentration increase; while the mass yield tends to decrease (high ash removal) for Guachinte coal when the collector concentration increases (low ash removal) at high frother concentrations. It is worth highlighting that the ash content of 0,65% obtained for Caypa coal is the lowest value reported in the literature while employing a test-rig loop flotation column in a single stage, which is considered to be an ultra-clean coal obtained by a physical cleaning process.