分光光度法测定模拟高放废液中的磷含量

    Determination of Phosphorus in Simulated High Level Liquid Waste by Spectrophotometry

    • 摘要: 建立了模拟高放废液中磷含量的分析方法。该法是在铋盐存在下,溶液中的正磷酸与钼酸铵形成磷钼黄(磷钼杂多酸),磷钼黄经抗坏血酸还原后形成磷钼蓝,于分光光度计上测量吸光度从而获得样品中的磷含量。开展了磷钼蓝吸收波长、形成酸度、显色试剂用量、稳定时间、干扰离子、重加回收率、精密度等实验。结果表明:在0.8 mol/L硝酸溶液中,依次加入硝酸铋、钼酸铵、抗坏血酸能使磷完全形成磷钼蓝,在室温下、40 min内磷显色稳定,于分光光度计695 nm处有最大吸收,同时硅(0.3 mg/L)、铁(4.0 mg/L)、镍(2.9 mg/L)、铀(0.8 mg/L)、铈(0.8 mg/L)、镁(0.4 mg/L)、锰(1.0 mg/L)、铝(2.0 mg/L)、铜(1.6 mg/L)、铌(0.2 mg/L)、 锶(0.4 mg/L)不影响磷含量(0.2 mg/L)的测定。采用该法测定模拟高放废液中磷的含量,重加回收率为99.80%~103.34%,测量的相对标准偏差优于3.0%(n=6),满足分析要求,可用于真实高放废液中磷含量的测量。

       

      Abstract: A method for the determination of phosphorus in simulated high level liquid waste was established. In the presence of bismuth salt, orthophosphoric acid reacts with ammonium phosphomolybdate to produce phosphomolybdenum yellow(PMo12 heteropoly acid), which can be reduced to phosphomolybdenum blue by the ascorbic acid. The absorbance was measured on the spectrophotometer to obtain the phosphorus content in the sample. Experiments were carried out on the absorption wavelength of phosphorous molybdenum blue, the formation of acidity, the amount of color reagents, the stabilization time, interference ions, regain recovery, precision, etc. The results show that in 0.8 mol/L nitric acid solution, phosphorous molybdenum is formed completely after adding strontium nitrate, ammonium molybdate, ascorbic acid sequentially, which can stable 40 min in room temperature, λmax=695 nm. Under the selected experimental conditions, the influence of interfering ions on the determination of 0.2 mg/L phosphorus can be neglected, if the masses of the interfering ions are less than those as shown in the round brackets: Si(0.3 mg/L), Fe(4.0 mg/L),Ni(2.9 mg/L), U(0.8 mg/L), Ce(0.8 mg/L), Mg(0.4 mg/L), Mn(1.0 mg/L), Al(2.0 mg/L), Cu(1.6 mg/L), Nb(0.2 mg/L), Sr(0.4 mg/L). The relative standard deviation is less than 3.0%(n=6), and the recovery of standard addition is 99.80%-103.34%, which meets the requirement of analysis. The method can be used to measure the content of phosphorus in real high level liquid waste.

       

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