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In this study, we use an experimental model of bilateral nephrectomy in rats to identify an advanced, yet simple nanoscale-based approach to discriminate between exhaled breath of healthy states and of chronic renal failure (CRF) states. Gas chromatography/mass spectroscopy (GC−MS) in conjugation with solid-phase microextraction (SPME) of healthy and CRF breath, collected directly from the trachea of the rats, identified 15 common volatile organic compounds (VOCs) in all samples of healthy and CRF states and 27 VOCs that appear in CRF but not in healthy states. Online breath analysis via an array of chemiresistive random network of single-walled carbon nanotubes (SWCNTs) coated with organic materials showed excellent discrimination between the various breath states. Stepwise discriminate analysis showed that enhanced discrimination capacity could be achieved by decreasing the humidity prior to …