The destruction of ammonium by the semi-continuous addition of sodium nitrite during acidic evaporation can be achieved with a wide range of waste compositions. The efficiency of nitrite utilization for ammonium destruction was observed to vary from less than 20% to 60% depending on operating conditions. The effects of nitric acid concentration and nitrite addition rate are dominant factors that affect the efficiency of nitrite utilization for ammonium destruction. Reducing the acid concentration by performing acid recovery via steam stripping prior to performing nitrite destruction of ammonium will require more nitrite due to the low destruction efficiency. The scale-up of the baseline rate nitrite addition rate from the 100 mL to the 1600 gallon batch size has significant uncertainty and poses the risk of lower efficiency at the plant scale. Experience with plant scale processing will improve confidence in the application of nitrite destruction of ammonium to different waste streams.