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利用铈的变价以及Ce(Ⅳ)-Tiron配合物在不同酸度条件下颜色的特殊性,建立了无需预先分离而直接测定混合稀土中铈含量的分光光度法。在pH为9.0条件下,借助空气的氧化,Ce(Ⅲ)和Ce(Ⅳ)都与Tiron形成Ce(Ⅳ)-Tiron配合物。该配合物在pH为5.0时呈亮黄色,在435nm处有最大吸收。铈的浓度在0~80μg范围内,符合Beer定律:摩尔吸光系数ε=1.64×103L/(mol.cm-1;检出限为1.88μg/mL;线性回归方程为A=0.0117C-0.018(C以μg/mL表示),线性相关系数γ=0.9992。对稀土样品平行测定6次,变异系数CV≤2.3%。共存的轻稀土离子对铈的测定无干扰。用于稀土氧化物及稀土盐中铈的测定,结果与KMnO4法比较,相对误差≤0.55%。
Based on the change of cerium and the particularity of the color of Ce (Ⅳ) -Tiron complex under different acidity conditions, a spectrophotometric method was established for the direct determination of cerium content in mixed rare earth without prior separation. At pH 9.0, both Ce (Ⅲ) and Ce (Ⅳ) formed Ce (Ⅳ) -Tiron complex with Tiron by air oxidation. The complex showed a bright yellow color at pH 5.0 and a maximum absorption at 435 nm. The concentration of cerium in the range of 0 ~ 80μg, in line with Beer’s Law: molar extinction coefficient ε = 1.64 × 103L / (mol.cm-1; detection limit of 1.88μg / mL; linear regression equation A = 0117C-0.018 (C in μg / mL), the linear correlation coefficient γ = 0.9992. The samples were measured 6 times in parallel and the coefficient of variation CV was less than or equal to 2.3%. The coexistence of light rare earth ions on the determination of cerium Interference. Used for the determination of rare earth oxides and rare earth salts of cerium, the results compared with the KMnO4 method, the relative error ≤ 0.55%.