原子荧光光度法测定固体废物中砷的方法验证

Verification of Atomic Fluorescence Photometric Method for Determining Arsenic in Solid Waste

为对我国环境保护与控制提供技术支持,进一步完善固体废物中重点参数,本文对HJ 702—2014《固体废物砷、汞、硒、铋、锑的测定微波消解/原子荧光法》中砷的测定进行6个方面的验证:线性关系、方法检出限、测定下限、精密度、准确度和实际样品加标回收率。结果表明,线性关系达到0.9998;当称取0.5 g固体废物样品验证砷(全量)时,测得0.009μg/g检出限、0.036μg/g的测定下限,当移取40 m L固体废物浸出液验证砷(浸出液)时,测得0.08μg/L的检出限、0.32μg/L的测定下限;砷(全量)、砷(浸出液)的相对标准偏差分别为0.35%~1.0%、1.2%~2.9%;实验室砷(全量)有证标准物质相对误差分别为-4.6%~0.85%,砷(浸出液)标准浓度的相对误差分别为0.25%~3.0%;固体废物砷(全量)加标回收率分别为93.7%~97.5%,固体废物砷(浸出液)加标回收率分别为96.0%~98.1%。各项指标均满足标准方法要求,证实实验室具备原子荧光光度法测定固体废物中砷的试验条件和技术能力。

In order to provide technical support for environmental protection and control in China,and further improve the key parameters in solid waste,this article verifies the determination of arsenic in HJ 702-2014 Determination of Arsenic,Mercury,Selenium,Bismuth,and Antimony in Solid Waste by Microwave Digestion/Atomic Fluorescence Method from six aspects:linear relationship,method detection limit,determination lower limit,precision,accuracy,and actual sample spiked recovery rate.The results show that the linear relationship reaches 0.9998.When weighing 0.5 g of solid waste sample to verify arsenic(full amount),detection limit of 0.009μg/g was measured,and the lower limit is 0.036μ.When transferring 40 mL of solid waste leachate to verify arsenic(leachate),detection limit of 0.08μg/L was measured,and the lower limit for measuring is 0.32μg/L.The relative standard deviations of arsenic(total amount)and arsenic(leaching solution)are 0.35%to 1.0%and 1.2%to 2.9%,respectively.The relative errors of certified reference materials for laboratory arsenic(full amount)are-4.6%to 0.85%,and the relative errors of standard concentrations for arsenic(leaching solution)are 0.25%to 3.0%,respectively.The recovery rates of solid waste arsenic(full amount)with added standards are 93.7%to 97.5%,and the recovery rates of solid waste arsenic(leaching solution)with added standards are 96.0%to 98.1%,respectively.All indicators meet the requirements of the standard method,confirming that the laboratory has the experimental conditions and technical ability to determine arsenic in solid waste by atomic fluorescence spectrophotometry.