Cyanide in wastewater is an important parameter to measure for health requirements. Free, weakly complexed, and strongly complexed cyanide can be differentiated. Direct measurement in the wastewater is not feasible due to the matrix itself. Therefore, total cyanide is determined after acidification of the sample, which releases all cyanide from complexes, and subsequent distillation and absorption of cyanide in an alkaline solution. Amperometric detection is applied using a gold working electrode. This electrode is advantageous over the silver electrode due to less contamination issues and better long-term stability.