Microwave pyrolysis of pecan nutshell (Carya illinoinensis) biomass was used to produce carbon-based solid products with potential application in contaminated water treatment.A range of analytical techniques were applied to characterize the intermediate products of microwave pyrolysis in order to monitor the physio-chemical effects of the interacting energy on the biomass.The performance of the carbon-based products was tested through evaluation of lead ion removal capacity from solution. Further analyses demonstrated that ion-exchange by calcium ions on the material surface was the main mechanism involved in lead removal. Calcium compound development was directly correlated to the interaction of the electromagnetic waves with the biomass.Through monitoring the physio-chemical effects of biomass-microwave interactions during microwave pyrolysis, we have shown for the first time that the intermediate products differ from those of conventional pyrolysis. We hypothesise that selective heating leads to the (hemi)cellulosic and lignin degradation processes occurring simultaneously, whereas they are largely sequential in conventional pyrolysis.This work provides optimization parameters essential for the large scale design of microwave processes for this application as well as an understanding of how the operating parameters impact on functionality of the resulting carbon-based materials.