流动注射化学发光法测定水中焦性没食子酸
FI-Chemiluminescence Determination of Pyrogallol in Water
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摘要: 在0.05 mol·L-1氢氧化钠溶液中,高碘酸钾与鲁米诺产生化学发光,焦性没食子酸对该发光有显著的增强作用.基于此,并结合流动注射技术,提出了在水样中测定焦性没食子酸的方法.在选定的条件下,化学发光信号的增加值与焦性没食子酸质量浓度之间在1.0~100 μg·L-1及0.1~2.0 mg·L-1之间呈线性关系,该方法的检出限为0.78 μg·L-1(3σ);对10 μg·L-1焦性没食子酸平行测定11次,其相对标准偏差为3.9%.该方法已应用于工业废水和环境水样中焦性没食子酸的测定,并用标准加入法作了回收试验,测得回收率在95.7%~104.1%之间.Abstract: It was found that in an alkaline medium of 0.05 mol·L-1 NaOH solution,the intensity of chemiluminescence (CL) produced by the reaction between KIO4 and luminol was notably enhanced by the presence of pyrogallol.On the base of this fact,a FI-CL method for determination of pyrogallol in water was proposed.Under optimum condition for the CL reaction,linear relationship was obtained between the magnitude of increase in CL intensity (ΔI) and the concentration of pyrogallol (C in mg·L-1) in the ranges of 1.0-100 μg·L-1 and 0.1-2.0 mg·L-1,with detection limit of 0.78 μg·L-1 (3σ).Precision of the method was tested at the concentration level of 10 μg·L-1 of pyrogallol for 11 determinations,value of RSD obtained was 3.9%.The proposed method was used in the determination of pyrogallol in samples of tap water,river water and industrial waste water,and recovery was tested by standard addition method giving values of recovery in the range from 95.7%-104.1%.