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A patient developed a right pleural effusion soon after starting a program of continuous ambulatory peritoneal dialysis. The etiology of the effusion was unclear. ^99mTc-labelled macroaggregated albumin was administered intrapentoneally, followed by 2 liters of dialysate. Trans-diaphragmatic leakage was clearly demonstrated, and confirmed by high count rates of pleural fluid with negligible blood count. This method can safely be used to demonstrate trans-diaphragmatic fluid leakage in peritoneal dialysis patients.