首页|两种湿消解法消解-原子荧光法测定尿中总砷

两种湿消解法消解-原子荧光法测定尿中总砷

扫码查看
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 1h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 1h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.
Two wet digestion methods for the determination of total arsenic in urine by digestion-atomic fluorescence spectrometry
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 sys-tem 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.

wet digestionammonium persulfatemixed acidatomic fluorescence spectrometrytotal arsenic

杨志羡、包玉龙、李科、王慧、郭志伟

展开 >

内蒙古自治区疾病预防控制中心地方病实验室,呼和浩特 010080

湿消化 过硫酸铵 混酸 原子荧光 总砷

中央引导地方科技发展资金项目西部青年学者项目内蒙古自治区科技计划内蒙古自治区卫生健康科技计划

2021ZY0047人字[2022]4号2021GG0383202201161

2024

环境卫生学杂志
中国疾病预防控制中心

环境卫生学杂志

CSTPCD
影响因子:0.735
ISSN:2095-1906
年,卷(期):2024.14(6)
  • 10