Nanoparticles of acidic cesium salt of Preyssler by a one-step solid-state reaction at room temperature, were synthesised and characterised by Fourier transform infrared spectroscopy, titration, inductively coupled plasma and transmission electron microscopy (TEM), respectively. These uniform nanoparticles showed an average size of 2–10 nm. Multi-walled carbon nanotubes (MWCNTs) were synthesised by the catalytic chemical vapour deposition method and used as nanostructured porous supports for the immobilisation of the nanoparticles of the acidic cesium salt of Preyssler. The TEM image showed a bamboo-like structure with inner and outer diameters of about 20 and 35 nm, respectively. The modification of the MWCNTs by the synthesised nanoparticles was successfully achieved via the impregnation method. The infrared analysis showed that the basic structure of Preyssler is preserved and left intact. The TEM images also showed an endohedral functionalisation of the MWCNTs.

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