Standard reference material and different geological samples were dissolved by system A (the mixture of nitric and perchloric acids) and system B (mixture of nitric, perchloric and hydrofluoric acids), and total Se in...Standard reference material and different geological samples were dissolved by system A (the mixture of nitric and perchloric acids) and system B (mixture of nitric, perchloric and hydrofluoric acids), and total Se in all samples was measured by hydride-generation atomic fluorescence spectrometry (HG-AFS) after concentration with thiol cotton fiber (TCF). The analytical results obtained by the two digestion method are in good agreement (within the limit of errors) for most of the samples, particularly for those having recommended values. The Se concentrations determined by the two methods are of no difference, and the correlation coefficient is 0.9986; the relative standard deviation (RSD) for the determination of 0.04 μg/g Se is 10.2%. The recovery rates of systems A and B by the stan- dard-addition method were 96%–106% and 99%–104%, respectively.展开更多
Flue gas from coal combustion contains significant amounts of volatile selenium （Se）. The capture of Se in the flue gas desulfurization （FGD） scrubber unit has resulted in a generation of metal-laden residues. It ...Flue gas from coal combustion contains significant amounts of volatile selenium （Se）. The capture of Se in the flue gas desulfurization （FGD） scrubber unit has resulted in a generation of metal-laden residues. It is important to determine Se speciation to understand the environmental impact of its disposal. A simple method has been developed for selective inorganic Se（IV）, Se（VI） and organic Se determination in the liquid-phase FGD residues by hydride generation atomic fluorescence spectrometry （AFS）. It has been determined that Se（IV）, Se（VI） and organic Se can be accurately determined with detection limits （DL） of 0.05, 0.06 and 0.06 μg/L, respectively. The accuracy of the proposed method was evaluated by analyzing the certified reference material, NIST CRM 1632c, and also by analyzing spiked tap-water samples. Analysis indicates that the concentration of Se is high in FGD liquid residues and primarily exists in a reduced state as selenite （Se（IV））. The toxicity of Se（IV） is the strongest of all Se species. Flue gas desulfurization residues pose a serious environmental risk.展开更多
目的:建立一种简便、高效、灵敏的硝酸-盐酸混合酸-石墨消解仪消解-氢化物发生原子荧光光谱法测定猪肝样品中(干粉)全硒含量。方法:使用HCl和HNO+3对猪肝样品(干粉)进行消解,采用原子荧光光度计测定猪肝中全硒含量。结果:硒工作曲线的...目的:建立一种简便、高效、灵敏的硝酸-盐酸混合酸-石墨消解仪消解-氢化物发生原子荧光光谱法测定猪肝样品中(干粉)全硒含量。方法:使用HCl和HNO+3对猪肝样品(干粉)进行消解,采用原子荧光光度计测定猪肝中全硒含量。结果:硒工作曲线的线性范围是2~20μg·L^(-1),相关系数为0.999 7;检出限和定量限分别是0.029μg·L^(-1)和0.098μg·L^(-1),不同浓度下的加标回收率在91.2%~111.4%,日内精密度为1.2%,日间精密度2.1%。同时对石墨消解仪消解样品条件进行了单因素条件优化,最优化条件为消解还原溶剂4 mL HCl和1 mL HNO+3,最佳料液比1/25(0.200 g/5 mL),消解温度采用离心管最大耐受温度120℃,消解时间3 h。结论:本研究为猪肝中全硒含量的测定提供了一种简单、快捷、高效、环保的方法。展开更多
基金the Knowledge-Innovation Program of the Chinese Academy of Sciences（KZCX3-SW-125）；the National Natural Science Foundation of China（Grant Nos.60633110,40003008）.
文摘Standard reference material and different geological samples were dissolved by system A (the mixture of nitric and perchloric acids) and system B (mixture of nitric, perchloric and hydrofluoric acids), and total Se in all samples was measured by hydride-generation atomic fluorescence spectrometry (HG-AFS) after concentration with thiol cotton fiber (TCF). The analytical results obtained by the two digestion method are in good agreement (within the limit of errors) for most of the samples, particularly for those having recommended values. The Se concentrations determined by the two methods are of no difference, and the correlation coefficient is 0.9986; the relative standard deviation (RSD) for the determination of 0.04 μg/g Se is 10.2%. The recovery rates of systems A and B by the stan- dard-addition method were 96%–106% and 99%–104%, respectively.
基金supported by the National Natural Science Foundation of China (No.90410018)the Shanxi Nature Science Foundation (No.20051017)+1 种基金the Shanxi Returned Scholar Research Project (No.2005-21)the Programfor Changjiang Scholars and Innovative Research Team at University in MOE,China (No.IRT0517)
文摘Flue gas from coal combustion contains significant amounts of volatile selenium （Se）. The capture of Se in the flue gas desulfurization （FGD） scrubber unit has resulted in a generation of metal-laden residues. It is important to determine Se speciation to understand the environmental impact of its disposal. A simple method has been developed for selective inorganic Se（IV）, Se（VI） and organic Se determination in the liquid-phase FGD residues by hydride generation atomic fluorescence spectrometry （AFS）. It has been determined that Se（IV）, Se（VI） and organic Se can be accurately determined with detection limits （DL） of 0.05, 0.06 and 0.06 μg/L, respectively. The accuracy of the proposed method was evaluated by analyzing the certified reference material, NIST CRM 1632c, and also by analyzing spiked tap-water samples. Analysis indicates that the concentration of Se is high in FGD liquid residues and primarily exists in a reduced state as selenite （Se（IV））. The toxicity of Se（IV） is the strongest of all Se species. Flue gas desulfurization residues pose a serious environmental risk.
文摘目的:建立一种简便、高效、灵敏的硝酸-盐酸混合酸-石墨消解仪消解-氢化物发生原子荧光光谱法测定猪肝样品中(干粉)全硒含量。方法:使用HCl和HNO+3对猪肝样品(干粉)进行消解,采用原子荧光光度计测定猪肝中全硒含量。结果:硒工作曲线的线性范围是2~20μg·L^(-1),相关系数为0.999 7;检出限和定量限分别是0.029μg·L^(-1)和0.098μg·L^(-1),不同浓度下的加标回收率在91.2%~111.4%,日内精密度为1.2%,日间精密度2.1%。同时对石墨消解仪消解样品条件进行了单因素条件优化,最优化条件为消解还原溶剂4 mL HCl和1 mL HNO+3,最佳料液比1/25(0.200 g/5 mL),消解温度采用离心管最大耐受温度120℃,消解时间3 h。结论:本研究为猪肝中全硒含量的测定提供了一种简单、快捷、高效、环保的方法。
