悬浮进样/离子液体萃取在原子荧光光谱中的应用
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摘要
本文将悬浮进样、酸消解和离子液体萃取分别与氢化物发生原子荧光光谱分析结合,用于食品和保健品中硒的形态分析和白洋淀水质中的痕量镉的检测,建立了灵敏有效的分析新方法。
全文共分四章：
第一章：引用41篇文献论述氢化物原子荧光光谱分析的进展,悬浮进样技术,元素价态分析,离子液体萃取的应用。
第二章：提出了一种悬浮进样-氢化物发生原子荧光法直接测定总Se,无机Se和Se(Ⅵ)的新方法。样品中的总硒以盐酸提取,用悬浮进样氢化物发生原子荧光法加以测定。以环己烷萃取分离无机硒和有机硒,而水相中的Se(Ⅳ)用亚硫酸钠作掩蔽剂。利用差减法可求得有机硒和Se(Ⅳ)的含量。本方法用于小麦面粉、大米面粉和富硒盐中总硒、无机硒和Se(Ⅵ)的测定,及保健品中总硒的测定。本方法具有准确,操作简易、快速,灵敏度高等特点,可用于实际样品中硒的形态分析。
第三章：采用三氯乙酸沉淀蛋白和环己烷萃取实现了富硒鸡蛋中的有机硒和无机硒的有效分离,建立了氢化物发生原子荧光法测定硒的形态分析新方法。本方法己用于富硒鸡蛋样品中总硒、无机硒和有机硒的含量,富硒鸡蛋试样中有机硒的含量约为无机硒的3-7倍。
第四章：介绍和讨论了室温离子液体的理化特性及其作为萃取剂在分离富集金属离子的应用。综述了室温离子液体在火焰原子吸收、蒸汽发生原子吸收、石墨炉原子吸收、原子荧光光谱和原子发射光谱的应用研究进展。选用1-丁基-3-甲基咪唑六氟磷酸盐离子液体萃取镉-双硫腙的络合物,离子液体层经反萃取将镉进入水相,用氢化物原子荧光法测定了水中的痕量镉。
In this paper, hydride generation-atomic fluorescence spectrometry combined with slurry sampling, acid digestion and ionic liquids extraction, respectively, was used for for speciation analysis of Se in food and dietary supplements, and trace amounts of Cd in Baiyang lake water. The new, sensitive and effective methods were developed.
This paper includes four chapters:
Chapter one:The advancement of hydride generation atomic fluorescence spectrometry, speciation analysis of trace element, the application of slurry-sampling technique and ionic liquid extraction were reviewed with 41 references.
Chapter two:A new method is developed for directly determination of total Se, inorganic Se and Se(VI) by slurry sampling-hydride generation atomic fluorescence spectrometry (SS-HGAFS). The total Se was extracted with HC1 and determined by SS-HGAFS. The inorganic Se and organic Se were separated by extracting with cyclohexane, Se(VI) in the aqueous phase were masked by Na2 SO3. The organic Se could be calculated by difference of the total Se and the inorganic Se, and the Se(IV) could be calculated by difference of the inorganic Se and the Se(VI). This method was used for the determination of total Se, inorganic Se and Se(VI) in rice flour, wheat flour,selenium-richen salt and dietary supplements.The proposed method has the characteristics of accuracy, facility,celerity and sensitivity, can be used for speciation analysis of selenium in real samples.
Chapter three:Effective separation of organic selenium and inorganic selenium in selenium-enriched eggs was achieved by precipitating protein with trichloroacetic acid and extraction with cyclohexane, and a new method was established for the speciation of selenium by hydride generation-atomic absorption fluorescence spectrometry. The proposed method has been used for the determination of organic selenium, inorganic selenium and total selenium in selenium-enriched eggs. The content of organic selenium was 3-7 times that of inorganic selenium.
Chapter four:The physicochemical performance of room-temperature ionic liquid and its application as extraction reagent in separation and concentration of metal ions were described. The research advancement for applications of room-temperature ionic liquid in flame atomic absorption, vapor generation atomic absorption, graphite furnace atomic absorption spectrometry and atomic fluorescence spectrometry as well as atomic emission spectrometry was reviewed. The 1-Butyl-3-Methylimidazolium
Hexafluorophosphate was chosen as extractant for the extraction of Cd-dithizone.complex, Cd in water phase obtained by the anti-phase extraction from ionic liquid layer was was determined by hydride generation atomic fluorescence spectrometry.
全文共分四章：
第一章：引用41篇文献论述氢化物原子荧光光谱分析的进展,悬浮进样技术,元素价态分析,离子液体萃取的应用。
第二章：提出了一种悬浮进样-氢化物发生原子荧光法直接测定总Se,无机Se和Se(Ⅵ)的新方法。样品中的总硒以盐酸提取,用悬浮进样氢化物发生原子荧光法加以测定。以环己烷萃取分离无机硒和有机硒,而水相中的Se(Ⅳ)用亚硫酸钠作掩蔽剂。利用差减法可求得有机硒和Se(Ⅳ)的含量。本方法用于小麦面粉、大米面粉和富硒盐中总硒、无机硒和Se(Ⅵ)的测定,及保健品中总硒的测定。本方法具有准确,操作简易、快速,灵敏度高等特点,可用于实际样品中硒的形态分析。
第三章：采用三氯乙酸沉淀蛋白和环己烷萃取实现了富硒鸡蛋中的有机硒和无机硒的有效分离,建立了氢化物发生原子荧光法测定硒的形态分析新方法。本方法己用于富硒鸡蛋样品中总硒、无机硒和有机硒的含量,富硒鸡蛋试样中有机硒的含量约为无机硒的3-7倍。
第四章：介绍和讨论了室温离子液体的理化特性及其作为萃取剂在分离富集金属离子的应用。综述了室温离子液体在火焰原子吸收、蒸汽发生原子吸收、石墨炉原子吸收、原子荧光光谱和原子发射光谱的应用研究进展。选用1-丁基-3-甲基咪唑六氟磷酸盐离子液体萃取镉-双硫腙的络合物,离子液体层经反萃取将镉进入水相,用氢化物原子荧光法测定了水中的痕量镉。
In this paper, hydride generation-atomic fluorescence spectrometry combined with slurry sampling, acid digestion and ionic liquids extraction, respectively, was used for for speciation analysis of Se in food and dietary supplements, and trace amounts of Cd in Baiyang lake water. The new, sensitive and effective methods were developed.
This paper includes four chapters:
Chapter one:The advancement of hydride generation atomic fluorescence spectrometry, speciation analysis of trace element, the application of slurry-sampling technique and ionic liquid extraction were reviewed with 41 references.
Chapter two:A new method is developed for directly determination of total Se, inorganic Se and Se(VI) by slurry sampling-hydride generation atomic fluorescence spectrometry (SS-HGAFS). The total Se was extracted with HC1 and determined by SS-HGAFS. The inorganic Se and organic Se were separated by extracting with cyclohexane, Se(VI) in the aqueous phase were masked by Na2 SO3. The organic Se could be calculated by difference of the total Se and the inorganic Se, and the Se(IV) could be calculated by difference of the inorganic Se and the Se(VI). This method was used for the determination of total Se, inorganic Se and Se(VI) in rice flour, wheat flour,selenium-richen salt and dietary supplements.The proposed method has the characteristics of accuracy, facility,celerity and sensitivity, can be used for speciation analysis of selenium in real samples.
Chapter three:Effective separation of organic selenium and inorganic selenium in selenium-enriched eggs was achieved by precipitating protein with trichloroacetic acid and extraction with cyclohexane, and a new method was established for the speciation of selenium by hydride generation-atomic absorption fluorescence spectrometry. The proposed method has been used for the determination of organic selenium, inorganic selenium and total selenium in selenium-enriched eggs. The content of organic selenium was 3-7 times that of inorganic selenium.
Chapter four:The physicochemical performance of room-temperature ionic liquid and its application as extraction reagent in separation and concentration of metal ions were described. The research advancement for applications of room-temperature ionic liquid in flame atomic absorption, vapor generation atomic absorption, graphite furnace atomic absorption spectrometry and atomic fluorescence spectrometry as well as atomic emission spectrometry was reviewed. The 1-Butyl-3-Methylimidazolium
Hexafluorophosphate was chosen as extractant for the extraction of Cd-dithizone.complex, Cd in water phase obtained by the anti-phase extraction from ionic liquid layer was was determined by hydride generation atomic fluorescence spectrometry.
引文
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