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Abstract An untapped source of amorphous SiO₂, industrially generated Indian biomass ash (SA)—90% amorphous, with composition of ~60% SiO₂and ~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)₂wt% 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.