We report the electroanalytical detection of n-butylamine at a nickel/carbon nanotube (Ni/CNT) composite. Scanning Electron Microscopy (SEM) characterisation of the composite demonstrated that it consisted of bulk nickel particles ca. 2 μm in diameter entangled in CNT bundles. The spontaneous formation of Ni(OH)2 was optimised, and comparison with a 3 mm nickel electrode showed that ca. 4 μg of the Ni/CNT composite cast on a 3 mm GC electrode possessed bulk nickel characteristics while also having higher activity and higher sensitivity towards the electro-chemical detection of n-butylamine. However, the Ni/CNT composite showed no response to ammonia, in contrast to the macro-nickel-electrode.© 2010 Wiley-VCH Verlag GmbHandCo. KGaA, Weinheim.