A novel approach is presented to determine 4‐nitrobenzaldehyde in water samples. The procedure is based on switchable solvent based liquid‐liquid microextraction (SS‐LLME) and then determination by differential pulse voltammetry at multi‐walled carbon nanotubes modified glassy carbon electrode. Dipropylamine, a solvent with switchable polarity, was used as an extraction solvent that can be miscible/immiscible upon the changes of pH of sample solution. Effects of experimental conditions on SS‐LLME were investigated using a one‐factor‐at‐a‐time methodology. Under optimized conditions, a calibration curve was linear in the concentration range of 1.0 and 350 μg L−1. Limits of quantification and detection were empirically 1.0 μg L−1 and 0.3 μg L−1, respectively. Intraday and Interday RSDs%, calculated in three concentration levels, were in the range of 6.2–7.8 % confirm the proper precision of the method. Finally, the performance of the method was evaluated successfully in real samples including drinking water, tap water and river water.
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