This paper describes a method to determine the equilibrium transformation temperatures in low C steels using the in situ high-temperature X-ray diffraction technique. The samples were heated and then cooled from 1000 to 720 °C in a stepwise manner decreasing to −10 °C. Austenite and ferrite fractions were determined by a quantitative method using the integrated intensities of austenite (111)γ and ferrite (110)α peaks from X-ray diffraction patterns. The effect of the temperature on interplanar d spacings of (111) and (110) crystallographic planes was determined using 2θ maximum positions of the austenite (111)γ and ferrite (110)α peaks. The equilibrium transformation temperatures were determined to be Ae1=720 °C and Ae3=950 °C. The results are in excellent agreement with those obtained by dilatometric analysis and Thermo-Calc phase diagram simulation software. In addition, the results were supported by microstructural observations: the formation of thin ferrite films (5–10 μm) was observed at temperatures near to experimental Ae3.