We demonstrate, for the first time, the chemical/electrochemical synthesis of uniformly dispersed nickel hydroxide nanoparticles (Ni(OH)(2)-NPs) embedded in an adsorbed lignosulfonate layer (LS) deposited on a glassy carbon (GC) electrode. This approach is based on the oxidative deposition of Ni(II) lignosulfonates (Ni-LS) followed by Ni(OH)(2)-NP precipitation in alkaline electrolyte. The morphology of this composite was investigated by scanning electron microscopy (SEM). The SEM results show that the NPs have a nano-globular structure in the range ca. 50-200 nm. The composite displays reversible electrochemical transition due to a Ni(II)/Ni(III) redox couple and electrocatalytic activity leading to the oxidation of methanol in alkaline solution. The electrochemical properties of the resulting material deposited as a redox film were investigated by cyclic voltammetry and chronoamperometry techniques. Using Laviron's theory, the electron-transfer rate constant and the transfer coefficient were determined to be k(s) = 4.1 s(-1) and alpha =0.42 respectively for a modifier film (Gamma(Ni) = 2.5 x 10(-9) mol cm(-2)) in 0.1 M sodium hydroxide electrolyte. Chronoamperometric studies were used to determine the catalytic rate constant for the catalytic reaction of the tested modifier with methanol (k(ch) = 1.0 x 104 cm(3) mo1(-1) s(-1)). The dependence of the methanol oxidation current on alcohol concentration is discussed. The modified electrode for methanol oxidation offers simple preparation, good stability and reproducibility. (C) 2014 Elsevier Ltd. All rights reserved.