Conventional and high-throughput experimentation (HTE) techniques were used for the synthesis, characterization, and catalytic testing of Pt/Mn–WO x –ZrO 2 materials. The catalysts were prepared by surfactant-assisted coprecipitation and screened for catalytic activity in a multi-channel fixed bed (MCFB) micro-reactor for the hydroisomerization of n-hexane. Conventional coprecipitation route leads mainly to the segregation of the WO 3 crystalline phase (XRD). On the other hand, the use of the automated HTE route allows the formation of catalysts with a highly dispersed WO x phase on the zirconia surface and a high surface area (60–100m 2 /g) when calcined at 800°C (N 2 physisorption, XRD, Raman, UV–vis, HRTEM). These polytungstates with different coordination symmetry are accessible to the reactants and they lead to an increase in the catalytic activity and selectivity to the bi-ramified products (2,2-DMB and 2,3-DMB) in the n-hexane isomerization. In addition, it was found that the incorporation of Mn modifies the nanostructural properties of the tungstated zirconia favoring the catalytic activity of these materials.