A novel chemiluminescence(CL) sensor, which can be used for hydroxylamine determination in combination with flow injection analysis, was developed by electrostatically immobilizing luminol and periodate on anion-exchange resin respectively. Hydroxylamine was sensed by its enhancing effect on the weak CL reaction between luminol and periodate, which were eluted from the ion exchange column. The response of the sensor to hydroxylamine was linear in the concentration range of 8.0×10-8-2.0×10-6 mol/L with a detection limit of 4.0×10-8 mol/L hydroxylamine(3σ). The relative standard deviation(RSD) was 2.0% for 9 repetitive determinations at a hydroxylamine concentration of 5.0×10-7 mol/L. The sensor could be reused for over 400 times with a good reproducibility and was used to determine hydroxylamine in wastewater.