After the sample was dissolved with aqua regia-hydrofluoric acid and selenium in the sample solution was thus volatilized and removed by sulfuric acid fuming at high temperature, a determination method of copper in hydrometallurgical mud, slag and other selenium-rich materials by iodometry was established. The experiment showed that, selenium could also react with iodine reagent to interfere with the determination of copper in glacial acetic acid medium. After treatment with aqua regia-hydrofluoric acid, the residual amount of selenium in the sample was higher than the maximum allowable amount of selenium for the determination of copper. However, after further treatment with sulfuric acid fuming, there was almost no residual selenium, so the interference of selenium with the determination of copper could be eliminated. The optimal dosage of sulfuric acid for volatilizing selenium was 3 mL. The removal mechanism of selenium was also discussed. The content of copper (2%-35%) in copper anode slime 1# , copper anode slime 2# , acid mud, iron replaced slag and selenium-rich material samples was determined by the proposed method. The results were consistent with those obtained by national standard method of GB/T3884. 1-2000,and the relative standard deviations (RSDs, n = 6) was less than 4 %.%采用王水-氢氟酸溶解样品,加硫酸高温冒烟挥发除去硒,建立了碘量法测定冶金泥、渣等富硒物料中铜的方法.实验表明,在冰醋酸介质中采用碘量法测定铜时,硒也可发生碘量反应从而干扰铜的测定；采用王水-氢氟酸处理样品后,硒的残留量超过了测定铜时硒的最大允许量,而再经硫酸高温冒烟挥发法处理后,硒几乎无残留,可消除硒对测定铜的干扰.确定了挥发法除硒的最佳硫酸用量为3 mL;对挥发除硒的机理进行了探讨.采用本方法测定铜阳极泥1#、铜阳极泥2#、酸泥、铁置换渣和富硒渣样品中2％～35％范围内的铜,所得结果与国标法GB/T3884.1-2000一致,相对标准偏差(RSD,n=6)均小于4％.
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