In modern microelectronics progress has been made towards low power ultra large-scale integration (ULSI), and nano-structure devices such as single electron transistors and quantum dots. In this technology application of new materials, which includes high-κ dielectrics for the MOSFET transistors, with extraordinary purity and uniformity is required. Failure analysis and reliability investigations of such films very often requires highresolution local measurements of electrical surface parameters. This kind of experiments can be performed using conductive atomic force microscopy, which provides simultaneous measurement of surface topography and current ?owing through the investigated layer. In order to acquire reliable data, there was designed a precise measurement and control system, which included a low-noise current-to-voltage converter of picoampere resolution, a scanning stage with control electronics and a data acquisition system. In the paper we describe the architecture of the designed and applied experimental set-up. We also present results of simultaneous measurements of topography and current on gold and highly oriented pyrolytic graphite (HOPG).