Extremely carcinogenic diethylnitrosamine (DENA) was found to form in up to 75% yield from the reaction of nitrite with the two commonly used water tracing dyes. Rhodamine B and Rhodamine WT, DENA was detected at trace levels (0.13–7.02 μg −1) in river water samples after treatment with the dye and nitrite. Analysis of these chemically treated environmental water samples required extensive separation techniques prior to acquisition of reliable analytical data using highly sensitive instruments for detection. The occurrence of DENA in nitrite-rich water treated with Rhodamines may pose a health hazard to general populations.