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Chambre d'Analyse Spectrométrique en Transmission ou en Réflexion (Analysis Chamber for Transmission or Reflection Spectrometry) (CASTOR) is a new instrument, operated at the SOLEIL synchrotron facility, dedicated to the metrological characterization of thin films with thicknesses in the nanometer range. The instrument can combine two X‐ray techniques, namely, the reflectivity (XRR) measurements with fluorescence (XRF) acquisitions and especially total‐reflection X‐ray fluorescence (TXRF)‐related techniques such as grazing‐incidence XRF (GIXRF). The instrument is most often installed on the hard X‐ray branch of the Metrology beamline. Geometrical characterization is presented, reproducibility of measurements is studied, and the reference‐free GIXRF analysis is described. Some representative examples are given to illustrate the capabilities of the setup and the combined analysis procedure. Herein, the precise characterization of the depth profile of thin films with a new methodology that combines X‐ray reflectivity with X‐ray fluorescence in grazing incidence is dealt with. It shows results of a reference‐free approach on model samples.