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Hydroxylamine (HX) is a reactive chemical with formula NH2OH, as well as a functional group where one or more of the hydrogens are replaced by substituents. Hydroxylamine tends to be explosive, and the nature of the hazard is not entirely understood. Hydroxylamine is used as a reducing agent in a myriad of organic and inorganic reactions. It can also act as antioxidants for fatty acids. Some non-chemical uses include removal of hair from animal hides and photography developing solutions . Hydroxylamine may explode on heating. At least two factories dealing in hydroxylamine have been destroyed since 1999 with loss of life. It is known, however, that ferrous and ferric iron salts accelerate the decomposition of 50% NH2OH solutions. Hydroxylamine and its derivatives are more safely handled in the form of salts . Determination of HZ is important in many environmental and industrial situations. Several methods have been developed for the determination of HX. Phenol and its vapors are corrosive and harmful for eyes, skin, and the respiratory tract . Repeated or prolonged skin contact with phenol may cause dermatitis, or even second and third-degree burns due to phenol's caustic and defatting properties . Inhalation of phenol vapor may cause lung edema . Therefore, determination of this compound is also very important. To our knowledge, no any paper has been reported for simultaneous electrocatalytic determination of HX and phenol using mediator (electrocatalysis). In this paper, we studied the preparation and suitability of a p-aminophenol-modified carbon nanotubes paste electrode (p-APMCNTPE) as a new electrocatalyst in the determination of HX and phenol in aqueous solution. Then we evaluated the analytical performance of the proposed method in quantification of HX in the presence of phenol. The method is fast, simple, and enough sensitive to measure those species in real samples such as waste water.