过硫酸铵恒温水浴消解-原子荧光法测定尿铅

Determination of Urine Lead Using Ammonium Persulfate Constant Temperature Water Bath Digestion with Atomic Fluorescence Spectrometer Method

目的 探讨通过湿法恒温消解尿样,利用原子荧光测定尿铅的方法。方法 采用过硫酸铵恒温水浴消解-原子荧光法测定尿铅。通过对尿样消解条件及测定条件的优化,得出最佳条件如下：尿样/过硫酸铵体积比为1∶1,沸水浴,消解1h;还原剂硼氢化钠（NaBH4）浓度为1%（0.2%氢氧化钠做碱性介质）,载流为2%盐酸。结果 测定的尿铅含量在浓度范围25~500μg/L内呈良好线性关系,相关系数为0.999 8,检出限为0.3μg/L,6次测定相对标准偏差小于3%,加标回收率为97.8%~107.2%。结论 该方法消解条件易于操控、样品前处理简单、试验结果快速、准确,适于应用推广。

Objective To explore to establish a method for urine sample by wet constant temperature digestion coupling with atomic fluorescence spectrometer. Methods After pretreatment with ammonium persutfate constant temperature water bath digestion,atomic fluorescence spectrometer methodology was used to detect lead in urine sample. Under the optimized digestion and detection conditions：urine/ammonium persulfate ratio 1 ： 1, boiling water bath digestion 1 h;NaBH4 concentration, 1 % （w/w） （0.2 % NaOH as the alkaline medium）, current-carrying, 2 % HCl. Results Wide linear rela- tionship was achieved in the range of 25-500 μg/L with coefficient of 0. 999 8 and the detection limit was estimated to be 0.3 μg/L, RSD of six replicate experiment less than 3% ,recovery rates of urine sample of 97.8%-107.2%. Conclusion The digestion method is easy to control, the sample pretreatment is simple,the method is precise, rapid and sensitive enough, suitable for application.