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This paper reports on developing a low cost but efficient paired emitter–detector diode (PEDD)-based photometer. The photometer consists of a white light-emitting diode (LED) as the emitter diode, an RGB LED as the detector diode, and a multimeter for recoding the signal. The developed PEDD-based photometer was utilized for the determination of liquid bleach adulteration in cow milk samples. N,N-Diethyl-p-phenylenediamine sulfate aqueous solution of pH 6 was used as a probe to monitor the presence of residual active chlorine in milk. The results showed that the developed method could be used to determine sodium hypochlorite in the concentration range of 0.5 to 20.0 ppm Cl2 with 0.14 and 0.46 ppm Cl2 limit of detection and limit of quantification, respectively. The intraday and interday precisions of the method at two concentration levels of 5.5 and 13.7 ppm Cl2 were 1.04% and 0.52%, and 1.81% and 1.02%, respectively. The recoveries of 114.2% and 106.9% were obtained for 5.5 and 13.7 ppm Cl2 concentrations levels, respectively. Real sample analyzes results showed that “maybe” liquid bleach adulteration in milk is the case for local distributors of raw milk.