The full-spectrum least-squares(FSLS) method is introduced to perform quantitative energy-dispersive X-ray fluorescence analysis for unknown solid samples.Based on the conventional least-squares principle, this spectr...The full-spectrum least-squares(FSLS) method is introduced to perform quantitative energy-dispersive X-ray fluorescence analysis for unknown solid samples.Based on the conventional least-squares principle, this spectrum evaluation method is able to obtain the background-corrected and interference-free net peaks, which is significant for quantization analyses. A variety of analytical parameters and functions to describe the features of the fluorescence spectra of pure elements are used and established, such as the mass absorption coefficient, the Gi factor, and fundamental fluorescence formulas. The FSLS iterative program was compiled in the C language. The content of each component should reach the convergence criterion at the end of the calculations. After a basic theory analysis and experimental preparation, 13 national standard soil samples were detected using a spectrometer to test the feasibility of using the algorithm. The results show that the calculated contents of Ti, Fe, Ni, Cu, and Zn have the same changing tendency as the corresponding standard content in the 13 reference samples. Accuracies of 0.35% and 14.03% are obtained, respectively, for Fe and Ti, whose standard concentrations are 8.82% and 0.578%, respectively. However, the calculated results of trace elements (only tens of lg/g) deviate from the standard values. This may be because of measurement accuracy and mutual effects between the elements.展开更多
本研究建立了利用原子荧光光度计测定蜜蜂和蜂产品中汞含量的方法。0.25 g蜜蜂样品和0.5 g蜂蜜样品通过微波消解,消解试剂为5 mL HCl和2 mL HNO_(3),最终体积调至15 mL。当样品质量为0.25 g时,检测限低于0.03μg·kg^(-1),回收率为7...本研究建立了利用原子荧光光度计测定蜜蜂和蜂产品中汞含量的方法。0.25 g蜜蜂样品和0.5 g蜂蜜样品通过微波消解,消解试剂为5 mL HCl和2 mL HNO_(3),最终体积调至15 mL。当样品质量为0.25 g时,检测限低于0.03μg·kg^(-1),回收率为74%~107.7%,RSD<3%。此法简便、快速且灵敏度高,适用于多种基质中汞的检测,为环境监测和食品安全提供了有效工具。展开更多
基金supported by the National Key R&D Project of China(No.2017YFC0602100)the National Natural Science Foundation of China(No.41774147)Sichuan Science and Technology Support Program(No.2015GZ0272)
文摘The full-spectrum least-squares(FSLS) method is introduced to perform quantitative energy-dispersive X-ray fluorescence analysis for unknown solid samples.Based on the conventional least-squares principle, this spectrum evaluation method is able to obtain the background-corrected and interference-free net peaks, which is significant for quantization analyses. A variety of analytical parameters and functions to describe the features of the fluorescence spectra of pure elements are used and established, such as the mass absorption coefficient, the Gi factor, and fundamental fluorescence formulas. The FSLS iterative program was compiled in the C language. The content of each component should reach the convergence criterion at the end of the calculations. After a basic theory analysis and experimental preparation, 13 national standard soil samples were detected using a spectrometer to test the feasibility of using the algorithm. The results show that the calculated contents of Ti, Fe, Ni, Cu, and Zn have the same changing tendency as the corresponding standard content in the 13 reference samples. Accuracies of 0.35% and 14.03% are obtained, respectively, for Fe and Ti, whose standard concentrations are 8.82% and 0.578%, respectively. However, the calculated results of trace elements (only tens of lg/g) deviate from the standard values. This may be because of measurement accuracy and mutual effects between the elements.
文摘本研究建立了利用原子荧光光度计测定蜜蜂和蜂产品中汞含量的方法。0.25 g蜜蜂样品和0.5 g蜂蜜样品通过微波消解,消解试剂为5 mL HCl和2 mL HNO_(3),最终体积调至15 mL。当样品质量为0.25 g时,检测限低于0.03μg·kg^(-1),回收率为74%~107.7%,RSD<3%。此法简便、快速且灵敏度高,适用于多种基质中汞的检测,为环境监测和食品安全提供了有效工具。
文摘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。
