An untapped source of amorphous SiO2, industrially generated Indian biomass ash (SA)—90% amorphous, with composition of ~60% SiO2 and ~20% unburnt carbon—can be used to produce cementitious and alkali-activated binders. This study reports dissolution of amorphous Si from SA in 0.5 mol/L and 1 mol/L aqueous NaOH, with and without added Ca(OH)2, at SA:Ca(OH)2 wt% ratios of 100:0, 87.5:12.5, and 82.5:17.5. Monitoring of elemental dissolution and subsequent/simultaneous product uptake by ICP-OES offers an effective process for evaluating utility of industrial wastes in binder-based systems. After 28 days in solution, up to 68% of total Si is dissolved from SA in 1 mol/L NaOH, with values as much as 38% lower in the presence of Ca(OH)2, due to the formation of tobermorite-like C-S-H. FTIR, 29Si MAS-NMR, and XRD are used to characterize solid reaction products and observe reaction progress. Product chemistries calculated from ICP-OES results and verified by selective dissolution in EDTA/NaOH—namely, Ca/Si of 0.6-1 and Na adsorption of 1-2 mmol/g—are found to be consistent with those indicated by aforementioned techniques. This indicates the efficacy of ICP-OES in estimating product chemistry via such a methodology. © 2019 The American Ceramic Society