水杨基荧光酮荧光猝灭法测定钼原矿中钼

钼的加入会使水杨基荧光酮(SAF)的荧光发生猝灭, 且猝灭的程度与钼的浓度呈线性关系, 据此建立了钼原矿中低含量钼的测定方法。实验选用4.0 mL 1.0% OP和1.0%吐温-80体积比为0.8∶0.2的混合溶液进行增敏, 加入2.0 mL 1.0×10^-3 mol/L SAF溶液, 2.0 mL 0.1 mol/L HCl, 在常温下反应30 min后于λ_ex/λ_em =460/520 nm处测定荧光发射强度, 结果表明, 钼浓度在 0.013~0.20 μg/mL范围之内与ΔF呈线性关系, 线性方程为ΔF=2 865.0ρ－10.667, 相关系数(R²)为0.998 8, 方法检出限为0.013 μg/mL。方法应用于测定钼原矿企业管理样中低含量的钼, 结果与参考值一致, 相对标准偏差为1.1%～1.8%, 回收率为93%～113%。

Determination of molybdenum in molybdenum ore by salicylfluorone fluorescence quenching method

The addition of molybdenum quenched the fluorescence of salicyl fluorone (SAF) and the quenching degree constituted a linear relationship with the concentration of molybdenum, so a method was established for determination of low content of molybdenum in molybdenum ore. The experiment used a mixture solution of 4.0 mL of 1.0% OP and 1.0% Tween-80 with a volume ratio of 0.8∶0.2 for sensitization, then 2.0 mL of 1.0×10^-3 mol/L SAF solution and 2.0 mL of 0.1 mol/L HCl were added. After the reaction was carried out for 30 min at room temperature, the fluorescence emission intensity was determined at λ_ex/λ_em = 460/520 nm. The results showed that the molybdenum (VI) concentration in the range of 0.013-0.20 μg/mL established a linear relationship with ΔF with the linear equation of ΔF = 2 865.0ρ-10.667, the correlation coefficient (R²) of 0.998 8 and detection limit of 0.013 μg/mL. The method was applied to determination of low content of molybdenum in the management samples of molybdenum ore plants. The results were consistent with the reference values, the relative standard deviations were 1.1%-1.8% and the recoveries were 93%-113%.