Reaction heats measured in a microcalorimeter between varying amounts of human serum and 700 IU of lipase (EC 3.1.1.3) and those between serum and 8 U of cholesterol oxidase (EC 1.1.3.6) were significantly linear with the contents of triglycerides (r=1.00) and cholesterol (r=0.99), respectively. However, when sera from 13 human volunteers were subject to comparative study between the micro-calorimetric and spectrophotometric methods, the correlation became less appreciable (r=0.70 and r=0.71) presumably due to the individual variations in free glycerol and cholesterol ester-constituents that were deliberately omitted in the microcalorimetric method but were routinely included in the standard (multi-enzymatic) spectro-photometric clinical method. The contribution of interfering substances, if any, is not totally ruled out.