[en] Bendiocarb (BEN) is an acutely toxic carbamate insecticide which used in public places and agriculture, it is also effective against a wide range of nuisance and disease vector insects. A new rapid and sensitive reverse flow injection spectrophotometric procedure coupled with on-line solid-phase reactor is designed in this article for the determination of BEN in its insecticidal formulations and water samples, by using three different solid-phase reactors containing bulk PbO/sub 2/ (B-SPR), PbO/sub 2/ nanoparticles (N-SPR) and grafted nanoparticles of SiO/sub 2/-PbO/sub 2/ (G-SPR) immobilized on cellulose acetate matrix (CA). This method of oxidative coupling is based on alkaline hydrolysis of the BEN pesticide, and then coupled with N,N dimethyl-p-phenylenediamine sulphate (DMPD) to give a blue color product which measured at λmax 675 nm. It worth to mentioned that under optimal conditions, Beer’s law is obeyed in the range of 1-175 μg mL/sup -1/ for B-SPR and 0.25-70 μg mL/sup -1/ of BEN for both N-SPR and G-SPR respectively within limit of detection (LOD) of 0.931, 0.234 and 0.210 μg mL/sup -1/ for B-SPR N-SPR and G-SPR respectively. The surface methodology of the solid phase was also investigated by using atomic force microscopy. (author)