报道了以ＨＮＯ３＿ＨＦ＿ＨＣｌＯ４分解多金属结核样品，用日立１８０＿８０偏振塞曼原子吸收分光光度计测定Ｃｕ、Ｃｏ和Ｎｉ的方法。试验了介质及共存元素对测定的影响，选择了最佳测定条件。用该法测定了大洋锰结核标准物质中的Ｃｕ、Ｃｏ、Ｎｉ，结果与标准值符合，且方法已应用于大批量样品分析中。对这些标样６次测定的ＲＳＤ分别是Ｃｕ０４９％～１９９％，Ｃｏ１８６％～２６６％，Ｎｉ０４６％～１９６％。 A method for the determination of Cu, Co and Ni with HNO3_HF_HClO4 to decompose polymetallic nodules was reported with a Hitachi 180_80 polarized Zeeman atomic absorption spectrophotometer. The effects of media and co-existing elements on the determination were tested, and the best determination conditions were selected. This method was used to determine the contents of Cu, Co and Ni in oceanic manganese nodules, and the results are in accordance with the standard values. The method has been applied to the analysis of large quantities of samples. The RSDs of these samples were 6 times of Cu049% ~ 199%, Co186% ~ 266%, Ni046% ~ 196%.