Electroplating sludge and associated waste products comprise complex mixtures of metallic elements and may cause serious environmental pollution if discharged without treatment. An effective light industrial process is modified to selectively extract and recover copper and nickel from electroplating sludge. The procedure was developed on a laboratory scale and validated in a small pilot plant. Extraction yields of greater than 95% for Cu and Ni are achieved under optimum leaching conditions. To selectively recover copper and nickel from the leaching solution, they were extracted by N902 in kerosene, followed by selective stripping using sulfuric acid. The overall recoveries of copper and nickel were 93.6% and 88.9%, respectively, via a fast, simple, and inexpensive process. Partial recovery of ammonia in the process enables some cost savings. The technology can be used for metal resource recovery from solid wastes containing copper and nickel.