A sequential injection analysis/immunosensor system is proposed for the analysis of thyroxine (L-T4) in serum and in pharmaceutical formulations with a rate of 75 samples/hour. The immunosensor design is based on the physical immobilization of anti-L-T4 in carbon paste. The working concentration range of the immunosensor in the sequential injection analysis system is between 36 and 1080 ng/mL with a limit of detection of 24.6 ng/mL. The system is very reliable and very easy to design and operate.