Carbon materials are promising candidates for sensors to detect heavy metal ions. This paper reported an effective method of fabricating nanofiber membrane sensor for detection of heavy metal ions by electrospinning with the carbon nanoparticles and PANi (polyaniline) as additives. The results revealed that the PANi/C/PAN nanofiber membrane was the most economical approach to adsorbing and detecting metal ions with highly sensitive property. This paper sheds a light on an economic fabrication of nanofiber membrane sensor with well-defined characteristics in electrical sensors and adsorption applications.