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The combination of magnetic and nonmagnetic interactions between the colloidal particles in ferrofluids results in various local inter-particle correlations that, in turn, change the macroscopic properties of the whole system. Therefore, characterization of the particle ensemble is a crucial point, allowing optimization of a ferrofluid for a particular application. Here it is shown how the crystal structure of the particles can be easily obtained in a fast synchrotron light diffraction experiment without any special treatment of the ferrofluid sample. Moreover, from the same diffraction patterns, such important parameters as particle mean size and dispersion are retrieved; these are compared with the corresponding parameters obtained from electron microscopy data. A particular problem of magnetite-maghemite transformation in nanoparticles stabilized by the surfactant shell is pointed out.