A greater understanding of precessional dynamics in magnetic systems is central to several emerging technologies. This thesis presents the design, construction and development of a Vector Network Analyser based Ferromagnetic Resonance measurement instrument (VNA-FMR), and its application in characterising dynamic material properties in hybrid anisotropy [CoPd]8-NiFe films, produced by remote plasma sputtering. Potential applications for hybrid films include Spin Torque Oscillators (STOs) or Vortex Oscillators (VO) for use as microwave emitters in, for example in Microwave Assisted Magnetic Recording (MAMR). The VNA-FMR system was first used to measure thin films of NiFe (permalloy) which allowed its capabilities to be quantified and compared to systems reported in the literature. The instrument demonstrated the capability of measuring permalloy films down to a thickness of 3 nm and was used to measure resonance and damping behaviour which agreed well with theory. The results obtained forMs were in agreement with measurement using Vibrating Sample Magnetometry. The effect of interlayer exchange on FMR was explored in hybrid films using a sample series with varying Pd spacer layer thickness, t, [Co/Pd]-Pd(t)-NiFe. As Pd spacer thickness increased, a transition was observed from near complete coupling with a single resonance mode to separate acoustic and optical branches of resonance. As spacing was further increased, the branches converged towards the resonances of the individual component layers of the hybrid films. The results suggest exchange coupling has a range of less than 2 nm, and is completely extinguished at 5 nm, in agreement with previous measurements. However, a change in damping behaviour was observed between 10 and 20 nm spacer thickness, independent of field orientation.