The course of instrumental analysis experiment is the main means to cultivate students’ performance ability. We took the instrument of Flow Injection Chemiluminescence as an example to explore the reform of instrumental analysis experiment course. Based on the obvious sensitization of potassium bromide on the chemiluminescent reaction in the system of luminol-H2O2–chromium (CrⅢ),a sensitive chemiluminescent method for fast determination of (CrⅢ) in water with flow injection technique is developed as the undergraduate students’ chemical experimental subject. Well-developed methods in scientific research are also imported into instrumental analysis experiment teaching, and students have to explore the instrument and experimental conditions by themselves.