快速石墨消解测定废水中总磷的方法改进
An Improvement of Determination Method of Total Phosphorus in Wastewater by Using Rapid Graphite Digestion
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摘要:目的 利用快速石墨消解器对废水中总磷测定进行前处理。方法 采用Hot Block快速石墨消解器, 水样中含磷化合物在120℃, 过硫酸钾消解转化为正磷酸盐, 在酸性条件下, 正磷酸盐与钼酸铵、酒石酸锑氧钾反应, 生成磷钼杂多酸, 被抗坏血酸还原变成蓝色络合物, 用1 cm比色皿于波长700 nm测定。结果 方法的相关系数为0.9997, 方法检出限为0.01 mg/L, 相对标准偏差为0.34%, 回收率97.0%~102.5%。结论 改进后的方法快速安全, 准确度、精密度、灵敏度等均能符合相关标准要求。Abstract:Objectives A rapid graphite digestion device is used for total phosphorus in wastewater pre-treatment.Methods Potassium-persulfade was applied to digest phosphorus compounds in water into orthophosphate at 120℃.In acidic condition, phosphorus-molybdenum heteropoly acid was produced by the reaction among orthophosphate, ammonium molybdate and potassium antimony tartrate. Phosphorus-molybdenum heteropoly acid was reduced into blue complex by Vitamin C. The blue complex was determined by using 1cm cuvette under the wavelength of 700 nm.Results The correlation coefficient of this method was 0.9997. The detection limits were 0.01mg/L. Returns-ratio varied from 97.0%~102.5%, and RSD was 0.34%.Conclusions The improved method was rapid and safe. The accuracy, precision and sensitivity were able to meet the requirement of the related standards.
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