This book introduce synthesis of some thiols surfactants and thier nano-structure with Gold Nano particles which confirmed with spectroscopic techniques such as (FTIR, 1HNMR, TEM, UV). The synthesized dithiol and paraaminothiol surfactants and their nanostructures with gold nanoparticles were used for detection of Zn and Ni ions in aqueous solution.In addition investigate the fabrication of Surface Plasmon Resonance nano sensor using gold nanoparticles (AuNPs) chemisorbed onto self-assembled monolayer of amino thiol surfactants on gold substrate. The fabricated SPR nanosensor was used for detection of Cu(II)ions in an aqueous solution.Also, In the present study newly developed potentiometric sensors for determination of zinc (II) are presented.The modified potentiometric method was based on the fabrication of modified thiol-carbon paste and modified gold-thiols nano particles-carbon paste sensors.