Electrocatalytic oxidation of hydroxylamine was investigated at silver (Ag) paste nanocomposite electrode. This electrode is a very good alternative for hydroxylamine determination compared with previously described electrodes because the electrocatalytic effect was achieved without any electrode modification. was determined over a wide linear concentration range of 1.0 –5.0 mM with double potential step amperometry. The limit of detection was obtained as 0.3 . This new method of determination is reproducible, selective, sensitive, and can be used for real sample analysis. The independence of the system from most of the interferences is the other advantageous feature of this sensor.