Natural organic matter present in raw waters reacts with chlorine to form disinfection byproducts (DBPs). As a result, chloramination is now a common method of disinfection in the water industry because it results in the formation of fewer DBPs than chlorine. However, there is some evidence that cyanogen chloride (CNCl) may be formed in greater amounts during chloramination than chlorination. In light of these findings, the USEPA requested all utilities participating in the Information Collection Rule reporting to include CNCl concentrations in their monthly reports. However, CNCl is highly toxic and very volatile. In addition, aqueous CNCl, required to generate stock standards, is expensive. This paper describes an alternative method of in situ analysis of CNCl which was developed to provide a safe and economical method for utilities to generate calibration and quality control standards.