Despite of their toxic and carcinogenic properties, aniline and their derivatives are important because of wide use in many industrial processes. Therefore monitoring of their levels in environmental waters is important. These compounds have been included in the US environmental protection agency (EPA) list of priority pollutants. Many of these amines are known to be highly mutagenic and carcinogenic and to from adducts with proteins and DNA [1]. These amines are present in the environment at low parts per billion or less. Therefore a certain clean – up procedure for the sample matrix is necessary. Thus extraction and clean – up of the sample has been performed using a number of different purification techniques such as Solid Phase Microextraction (SPME) [2] and Liquid Phase Microextraction (LPME) [3-6]. In the present research liquid – liquid microextraction method was illustrated for the extraction of a mixture of 3 aniline derivatives; N-ethyl aniline, 2-nitroaniline and 2-bromoaniline from water, using spectrophotometry to determine the concentrations of extracted components, but the mixture showed overlapping spectra. Thus, for resolving mixtures of these components we have used of two simple and efficient methods. Mean Centering of Ratio Spectra and Partial Least Squares [7,8]. Finally, in order to evaluate the practical application of the method, recovery were determined and extraction precision, linearity and limits of detection (LOD’s) for selected analytes were evaluated.The results obtained in this work indicate the development and application of a novel method approach to extracting and determining aniline derivatives from water samples.

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