Electrical impedance measurements of PZT nanofiber sensors were performed using a variety of methods over a frequency spectrum ranging from DC to 1.8 GHz. The nanofibers formed by electrospinning with diameters ranging from 10 to 150 nm were collected and integrated into sensors using microfabrication techniques. Special matching circuits with ultrahigh input impedance were fabricated to produce low noise, measurable sensor outputs. Material properties including resistivity and dielectric constant are derived from the impedance measurements. The resulting material properties are also compared with those of individual nanofibers being tested using conductive AFM and Scanning Conductive Microscopy.