两种湿消解法消解-原子荧光法测定尿中总砷

杨志羡; 包玉龙; 李科; 王慧; 郭志伟

doi:10.13421/j.cnki.hjwsxzz.2024.06.008

两种湿消解法消解-原子荧光法测定尿中总砷

Two wet digestion methods for the determination of total arsenic in urine by digestion-atomic fluorescence spectrometry

摘要

摘要:
目的比较硝酸、硫酸、高氯酸混酸与过硫酸铵两种消解法-原子荧光测定尿中总砷的方法。
方法前处理分别用硝酸、高氯酸、硫酸混酸在310 ℃下对尿样消解1 h后加硫脲-抗坏血酸还原样品和用饱和过硫酸铵溶液在310 ℃下对尿样消解1 h后加入硫脲-抗坏血酸还原，进入原子荧光仪检测。
结果在1.00~20.00 μg/L砷含量范围内，标准曲线回归方程：y=106.587x-11.979，相关系数优于0.999 0，混酸消解法的精密度2.06%~3.03%，平均加标回收率101.2%~104.3%，检出限0.012 μg/L；饱和过硫酸铵消解法的精密度3.31%~4.05%，平均加标回收率97.9%~101.6%，检出限0.006 μg/L。
结论两种方法的准确度、精密度均符合卫生标准《尿中砷的测定氢化物发生原子荧光法》(WS/T 474-2015)的要求，适于大批量尿中总砷含量的检测。

Abstract:
Objective To compare the two digestion methods of ammonium persulfate and the mixed acid system of nitric acid, sulfuric acid, and perchloric acid in determining total arsenic in urine by digestion-atomic fluorescence spectrometry.
Methods Urine samples were digested by the mixed acid system of nitric acid, sulfuric acid, and perchloric acid and saturating ammonium persulfate at 310 ℃ for 1 hour, then thiourea-ascorbic acid was added to reduce the sample, and the samples were placed in the atomic fluorescence spectrometry analyzer for determination.
Results Within the range of 1.00-20.00 μg/L for the content of arsenic, the standard curve regression equation was y=106.587x-11.979, with a correlation coefficient of >0.999 0. The digestion method of the mixed acid system had a precision of 2.06%-3.03%, an average spike recovery of 101.2%-104.3%, and a detection limit of 0.012 μg/L. The saturating ammonium persulfate digestion method had a precision of 3.31%-4.05%, an average spike recovery of 97.9%-101.6%, and a detection limit of 0.006 μg/L.
Conclusion The accuracy and precision of both methods meet the requirements in Determination of arsenic in urine by hydride generation atomic fluorescence spectrometry(WS/T 474-2015), and the two methods are suitable for large-scale determination of total arsenic content in urine.

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