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使用λ_(19)分光光度计研究HNO_3介质中U(Ⅵ)和Pu(Ⅳ)的吸收光谱、四次微分谱以及共存的杂质离子对微分谱的影响,并分别采用微分谱上415nm处峰零值和472.5-479.5nm间的峰面积值计算U(Ⅵ)和Pu(Ⅳ)的含量。结果表明:当体系NO或HNO_3浓度处在1.5-3.0mol/l之间时,用微分法测定U(Ⅵ)不必预先测定体系中的NO或HNO_3浓度,相对偏差<5.5%;对于Pu(Ⅳ)的测定,相对偏差<5.0%;对于U(Ⅵ)和Pu(Ⅳ)混合体系,当U/Pu比达到200时,采用微分法仍可鉴定Pu(Ⅳ)的存在,这时,Pu(Ⅳ)测定的相对偏差<6.0%。Pu(Ⅳ)的检测下限为5×l0 ̄(-4)mol/l。
The effect of U (Ⅵ) and Pu (Ⅳ) absorption spectra, fourth derivative spectra and coexisting impurity ions on the differential spectra of HNO_3 in HNO_3 media were investigated by λ_ (19) spectrophotometer. Values of U (Ⅵ) and Pu (Ⅳ) were calculated from the peak areas between 472.5 and 479.5 nm. The results showed that when the concentration of NO or HNO 3 was 1.5-3.0 mol / l, the determination of U (Ⅵ) by differential method did not need to pre-determine the concentration of NO or HNO 3 in the system, the relative deviation was less than 5.5% ; For the determination of Pu (Ⅳ), the relative deviation is less than 5.0%; for U (Ⅵ) and Pu (Ⅳ) mixed systems, the differential expression of Pu At this moment, the relative deviation of Pu (Ⅳ) determination is less than 6.0%. Pu (Ⅳ) detection limit of 5 × l0 ~ (-4) mol / l.