Calixresorcinarenes and calixarenes have seen extensive usage as receptors for cations, anions and even neutral molecules. Incorporation of binding capabilities and chemical groups that respond to analytes complexation has given these macrocycles additional advantages in applications as efficient selective chemical sensors. Three major types of macrocyclic calixresorcinarenes namely C-dec-9-en-1-ylcalixresorcinarene (CAL 11U), C-trans-2, cis-6-octa-1,5-dien-1-ylcalixresorcinarene (CAL 9U) and C-nonylcalixresorcinarene (CAL 10) were synthesized. They differ in the alkyl/alkenyl side chains. They were characterized by different techniques (melting point measurements, Fourier Transform Infra-Red spectroscopy FT-IR, Thermal Gravimetric analysis and Differential Scanning Calorimetry coupled with Mass Spectrometry TG-DSC-MS, Nuclear Magnetic Resonance spectroscopy NMR, and Powder X-Ray Diffraction measurements PXRD). Calixresorcinarene derivatives, immobilized onto Au surfaces of quartz crystal resonators, have been successfully applied to detect the presence of lead in aqueous solution.