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以H2 SO4 HNO3 H2 O2 作氧化剂 ,采用湿式灰化法将UO2 C2 O4 ·TRPO配合物中的有机磷氧化成磷酸盐 ,并在 0 14mol/LH2 SO4 介质中 ,以水溶性聚乙烯醇为稳定剂 ,用碱性染料乙基紫与磷钼杂多蓝形成较高灵敏度的离子缔合物 ,在波长 6 2 0nm处用分光光度法测定磷含量。结果表明 ,当溶液中质量比Rm(UO2 2 + /P)≤ 1 4× 10 3 ,Rm(C2 O4 2 - /P)≤ 8 8× 10 2 和Rm(C2 O2 2 - /P)≤ 3 6×10 4 (1次湿式灰化 )时 ,可在水相中直接显色测定磷。与聚乙烯醇 罗丹明B 磷钼杂多蓝测定磷的方法进行对照 ,结果符合良好。本法对有机磷转化为无机磷的平均转化率为 99 8%~ 10 1 1% ,磷的检测限为 0 0 2mg/L ,相对标准偏差为 3% ,回收率为 97%~ 10 3%
With H2 SO4 HNO3 H2 O2 as oxidant, the organophosphorus in UO2 C2 O4 · TRPO complex was oxidized to phosphate by wet ashing method and water-soluble polyvinyl alcohol was used as stabilizer in 0 14 mol / LH2 SO4 medium , The basic dye ethyl violet and phosphomolybdenum heteropoly blue to form a higher sensitivity of the ion-association, at a wavelength of 6 20nm determination of phosphorus content by spectrophotometry. The results show that when the mass ratio Rm (UO2 2 + / P) ≤ 14 × 10 3, Rm (C2 O4 2 - / P) ≤ 8 8 × 10 2 and Rm (C2 O2 2 - / P) ≤ 3 6 × 10 4 (1 wet ashing), the color can be directly measured in the water phosphorus. And polyvinyl alcohol Rhodamine B phosphomolybdate heteropoly blue method for the determination of phosphorus, the results are in good agreement. The average conversion of organic phosphorus to inorganic phosphorus was 99 8% -101 1%, the detection limit of phosphorus was 0.02 mg / L, the relative standard deviation was 3% and the recovery was 97% -103%