Magnetic Particle Imaging (MPI) is capable of imaging the spatial distribution of superparamagnetic iron oxide (SPIO) nanoparticles with a high sensitivity and high resolution. A Magnetic Particle Spectrometer (MPS) can be used to estimate the magnetic response of the SPIO nanoparticles and achieve the system matrix for the calibration of imaging devices. A one-dimensional and two-dimensional MPS have been introduced and shown good usability. A three-dimensional transmit coil setup was optimized, and its corresponding signal chains have been partially described. This paper is a continuation work and aims at presenting the first measured results of the three-dimensional MPS.