Dilute aqueous pertechnic acid has long been known as strong monoprotic acid that behaves as a simple pertechnetate ion in aqueous solution. As pertechnic acid concentrates by evaporation, it becomes yellow and then dark red, and dark-red crystalline material may ultimately be obtained. We show that as pertechnic acid concentrates, at least three compounds are formed: a yellow viscous liquid, a colorless (not red) crystalline solid, and a small amount of an intensely colored red-purple compound. The colorless crystalline compound melts at 118 °C and can be melted and recrystallized several times with little decomposition. The red-purple compound is apparently not stable at room temperature and quickly decomposes if it is isolated. UV-vis spectra show that Beer's law does not hold as pertechnic acid concentrates by evaporation. We report densities, 99Tc nuclear magnetic resonance spectra, and ultraviolet-visible absorption spectra for highly pure aqueous pertechnic acid (accompanied by the other technetium compounds that form) ranging from 1 to 14 M in technetium concentration.