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原子荧光光度法测定固体废物中砷的方法验证

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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 0.009 μg/g检出限、0.036 μg/g的测定下限,当移取 40 mL固体废物浸出液验证砷(浸出液)时,测得0.08 μg/L的检出限、0.32 μg/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.
Verification of Atomic Fluorescence Photometric Method for Determining Arsenic in Solid Waste
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 0.999 8.When weighing 0.5 g of solid waste sample to verify arsenic(full amount),detection limit of 0.009 μg/g was measured,and the lower limit is 0.036 μ.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 0.32 μg/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.

atomic fluorescence spectrophotometrysolid wastearsenicmethod validation

傅晓燕、朱建发、黄紫君

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中铁二院成都工程检测有限责任公司, 四川 成都 610000

原子荧光光度法 固体废物 方法验证

2024

山西化工
山西省煤化工发展促进中心 山西省化工学会

山西化工

影响因子:0.293
ISSN:1004-7050
年,卷(期):2024.44(1)
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