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Serum aluminum levels were determined by instrumental neutron activation analysis in 31 patients undergoing long-term haemodialysis. Aluminum-28 1.778 MeV (T 1/2=2.24 min) γ-rays produced by the thermal neutron reaction27Al(n,γ)28Al were detected. Successive irradiation of the samples at epithermal neutron fluence was performed to correct for the interference from the fast neutron reaction31P(n,α)28Al. Serum aluminum level in this group of subjects was adequately represented by a lognormal distribution with a mean and variance of 16.5 μg/l and 16.8 μg/l, respectively. The results obtained were found to be in agreement with serum aluminum determination performed by electrothermal atomic absorption spectrophotometry (r 2=0.97). Instrumental neutron activation can provide a rapid technique to routinely monitor long-term haemodialysis patients in order to identify individuals at greater risk to develop aluminum toxicity.