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Ultra sensitive ammonia sensors based on microwave (MW) nanofrillar polyaniline (PANI) with ppb sensing range were developed. First PANIs synthesized by classical (CS) and MW assisted methods using different dopants (HCl, H₂SO₄) and oxidants – (ammonium persulfate (APS) and potassium iodate (KIO₃)) were exposed to 1 ppm (700 μg m⁻³) of ammonia to select the more sensitive. The couple dopant/oxidant (H₂SO₄/KIO₃) leads to PANIs presenting the best responses whatever the method of synthesis used. These selected samples have been further investigated and characterized from a metrological point of view in terms of response, sensitivity, quantification limit, repeatability and reversibility. Compared to CS method, the MW synthesized PANI gives rise to sensor presenting better metrological performances which can be correlated with the physical properties of the samples obtained by using FTIR …