功能化纳米吸附材料的合成及其在痕量金属离子分析中的应用
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摘要
随着经济的不断发展,各种环境污染事件层出不穷,大气污染、水体污染、全球变暖、能源匮乏、固体废弃物污染和物种灭绝等问题时刻威胁着我们的生存环境。特别是重金属离子造成的水体、土壤和食品污染已经一次又一次地损害了我们的生活环境。然而,由于分析方法的灵敏度不够以及复杂基质的干扰,对金属离子直接进行分析测定是比较困难的。因此,如何对环境中的金属污染物进行有效治理就成为环境分析化学工作者所面临的一大挑战。本论文以富集分离和测定环境样品中痕量金属元素为目的,设计新的固相萃取吸附剂及分析方法,通过对多壁碳纳米管、埃洛石纳米管和氧化石墨烯进行修饰改性,得到了几种新的固相萃取吸附剂材料,并对材料的选择性吸附性能进行了系统研究。同时,根据氧化石墨烯的特性,建立了荧光传感器,用于直接分析和测定溶液样品中痕量的Th4+。具体工作分为以下五个部分：
1.紫脲酸铵功能化的埃洛石纳米管对痕量Pd(Ⅱ)的高选择性固相萃取性能研究
在此工作中,首次成功地合成了一种新型吸附剂(HNTs-Mu),通过FT-IR,XRD,SEM,TEM和BET分析对HNTs-Mu的结构进行了表征。把HNTs-Mu作为固相萃取吸附剂,用于分离和预富集溶液中的痕量Pd(Ⅱ),通过ICP-AES进行测定,研究其分析性能。结果表明,HNTs-Mu对Pd(Ⅱ)具有很好的亲和力、较高的选择性以及好的捕捉能力。在pH=1.0时,痕量Pd(Ⅱ)能够被定量吸附,同时在流速为2.0mL min-1的时候,被吸附的Pd(Ⅱ)可以用2.5mL的0.01molL-1HCl-3%硫脲溶液定量洗脱。在样品溶液最大体积为300mL时,计算得到该方法的最大富集因子为120。HNTs-Mu对Pd(Ⅱ)的最大吸附容量为42.86mgg-1。Pd(Ⅱ)/Cd(Ⅱ),Pd(Ⅱ)/Hg(Ⅱ),Pd(Ⅱ)/Au(Ⅲ),Pd(Ⅱ)/Pt(Ⅳ)和Pd(Ⅱ)/Ir(Ⅳ)的选择性因子分别是3572.6,29.6,13.7,76.3和207。并且HNTs-Mu实验室合成方法简单,耗费较低。该方法被成功用于富集分离实际样品中的痕量Pd(Ⅱ),回收率大于95%。精密度和检出限都令人满意。
2.水杨酸修饰的埃洛石纳米管对痕量Fe(Ⅲ)的高选择性吸附性能的研究
使用水杨酸成功修饰埃洛石纳米管(HNTs-HBA),并用FT-IR,XRD,TEM和元素分析对其进行表征。把合成的HNTs-HBA用于溶液样品中痕量Fe(Ⅲ)的选择性分离,并用ICP-AES进行测定。通过静态和动态分析条件,对富集酸度、振荡时间、样品溶液的流速和体积及其洗脱剂等实验条件进行了优化。同时考察了一些常见共存离子对Fe(Ⅲ)的干扰问题。得到的富集因子为75。HNTs-HBA对Fe(Ⅲ)的吸附很快达到平衡。Fe(Ⅲ)的最大吸附容量是45.54mg g-1,方法的检出限是0.21ng mL-1,相对标准偏差是2.7%。把HNTs-HBA用于国家标准样品、生物样品以及环境水样中痕量Fe(Ⅲ)的富集测定,结果令人满意。
3.2-氨基苯并噻唑修饰的碳纳米管对痕量铅的选择性预富集分离研究
合成了2-氨基苯并噻唑修饰的多壁碳纳米管(MWCNTs-ABTZ),并把MWCNTs-ABTZ作为一种新的吸附剂,用于选择性富集分离痕量Pb(Ⅱ),实验结果用ICP-AES进行测定。通过静态和动态分析条件,对富集酸度、振荡时间、样品溶液的流速和体积、洗脱条件和共存离子的影响等实验条件进行了优化。得到的富集因子是100。常见的共存离子对痕量Pb(Ⅱ)的富集分离没有影响。MWCNTs-ABTZ对Pb(Ⅱ)的最大吸附容量是60.32mg g-1,方法的检出限是0.27ng mL-1,相对标准偏差是2.7%(n=8)。把MWCNTs-ABTZ用于国家标准样品以及环境水样中痕量Pb(Ⅱ)的分析测定,结果令人满意。
4.基于氧化石墨烯的荧光效应研究
我们通过化学方法成功地合成了氧化石墨烯,并且用TEM,UV-Vis,FT-IR和XRD对其结构进行了探究。同时,我们发现氧化石墨烯能够有效地猝灭罗丹明6G水溶液的荧光效应。依据氧化石墨烯的UV-Vis谱图以及罗丹明6G的荧光谱图,我们证明了荧光猝灭是由以下两个原因引起的：第一,罗丹明6G的电子转移到氧化石墨烯表面；第二,罗丹明6G被氧化石墨烯吸附。尽管如此,痕量的Th4+能够使被氧化石墨烯猝灭的罗丹明6G水溶液的荧光信号增强。
5.二乙烯三胺功能化的氧化石墨烯对痕量Cr(Ⅲ)和Pb(Ⅱ)的吸附性能研究
合成了二乙烯三胺功能化的氧化石墨烯(GO-DETA),并把GO-DETA用于富集分离溶液中的重金属离子。研究发现,GO-DETA对溶液中Cr(Ⅲ)和Pb(Ⅱ)具有良好的吸附能力。按照分析程序,对实验参数进行了优化。同时证明了常见共存离子对痕量Cr(Ⅲ)和Pb(Ⅱ)的富集分离没有干扰。GO-DETA对Cr(Ⅲ)和Pb(Ⅱ)的最大吸附容量分别是60.9和142.86mg g-1。把GO-DETA用于国家标准样品及环境水样中痕量Cr(Ⅲ)和Pb(Ⅱ)的分离富集和测定,实验结果令人满意。
With the continuous development of the economy, the growing incidence of environmental pollution, air pollution, water pollution, global warming, energy shortages, solid waste pollution and species extinction and other issues have threated our living environment. Especially water, soil and food contamination caused by the heavy metal ions have maken our life destroyed once again. However, because complex matrix interference is complex and the sensitivity of the exsiting methods is not enough, it's difficult to analyze trace and ultra-trace element in actual samples. Thus, it is very important to open efficient methods for detecting metal ions in the environment. In this paper, in order to separate trace metals from the environmental samples, we designed the new SPE adsorbents and analytical methods. Through the modification of multiwall carbon nanotubes, graphene oxide and halloysite nanotubes, we obtained several new SPE adsorbents material, and systematically studied the selective adsorption property of the material. At the same time, according to characteristics of graphene oxide, we developed a fluorescence sensor to directly analysis trace Th4+in the solution samples. Our work is divided into the following five parts:
1. Highly selective solid-phase extraction of trace Pd(Ⅱ) by murexide functionalized halloysite nanotubes
The originality on the high efficiency of murexide modified halloysite nanotubes (HNTs-Mu) as a new solid-phase extractant has been reported to preconcentrate and separate Pd(Ⅱ) in solution samples. The structure of HNTs-Mu was confirmed by FT-IR, XRD, SEM, TEM and BET. Effective determination conditions of Pd(Ⅱ) were examined using column procedures before detection by inductive coupled plasma atomic emission spectrometry (ICP-AES). The effects of pH, sample flow rate and volume, amount of adsorbent, elution condition and interfering ions were optimized. Under the optimized conditions, trace Pd(Ⅱ) could be retained on the column at pH1.0and quantitatively eluted by2.5mL of0.01mol L-1HCl-3%thiourea solution at a flow rate of2.0mL min-1.An enrichment factor of120was achieved. Common interfering ions did not interfere in determination and separation. The maximum adsorption capacity of HNTs-Mu at optimum conditions was42.86mg g-1for Pd(II). The detection limit (3a) of the method was0.29ng mL-1, and the relative standard deviation was3.1%(n=11). The method was validated using certified reference material, and then has been applied for the determination of trace Pd(II) in actual samples with satisfactory results.
2. Functionalized halloysite nanotubes with2-hydroxybenzoic acid for selective solid-phase extraction of trace iron(III)
Functionalized halloysite nanotubes with2-hydroxybenzoic acid (HNTs-HBA) has been synthesized and characterized by FT-IR, XRD, TEM and Elemental analysis. The capability of HNTs-HBA has been developed for selective separation and preconcentration of trace Fe(III) before detection by ICP-AES. The effects of pH, shaking time, flow rate and volume of the sample, elution condition and interfering ions were examined using column and batch procedures. An enrichment factor of75was obtained. HNTs-HBA exhibited fairly fast kinetics for the adsorption of Fe(Ⅲ) and common coexisting ions did not interfere in the determination. The maximum adsorption capacity of HNTs-HBA for Fe(Ⅲ) was45.54mg g-1at optimum conditions. The detection limit (3σ) of the method was0.21ng mL-1. The relative standard deviation under optimum condition was2.7%(n=11). The developed method has been successfully applied for the determination of trace Fe(Ⅲ) in biological and natural water samples.
3. Multiwalled carbon nanotubes modified with2-aminobenzothiazole for uniquely selective solid-phase extraction and determination of trace Pb(Ⅱ) ion in water samples
A solid phase extraction method is presented for the selective preconcentration and/or separation of trace Pb(Ⅱ) by2-aminobenzothiazole modified multiwalled carbon nanotubes (MWCNTs-ABTZ). ICP-AES was used for detection. The effects of pH, shaking time, sample flow rate and volume, elution condition and interfering ions were examined by column and batch procedures. An enrichment factor of100was obtained. Common coexisting ions did not interfere in the determination. The maximum adsorption capacity of MWCNTs-ABTZ for Pb(Ⅱ) was60.32mg g-1. The detection limit (3σ) of the method was0.27ng mL-1. And the relative standard deviation was1.6%(n=8). The method was validated using a certified reference material, and has been applied for the determination of trace Pb(II) in water samples with satisfactory results.
4. Fluorescence determination based on graphene oxide
Graphene oxide (GO) has been prepared and the structure of the prepared GO was characterized by XRD, UV-Vis, FT-IR and TEM, respectively. And then we demonstrated that GO could quench the fluorescence of Rhodamine6G (Rh6G) in aqueous solution. According to the UV-vis absorption spectrum of GO and the fluorescence spectrum of Rh6G, we found that GO quenched the fluorescence of Rh6G due to two factors. Firstly, the electrons moved from the Rh6G to the surface GO; secondly, Rh6G adsorbed onto the GO surface. However, trace Th4+enhanced the fluorescent signal of Rh6G, which was quenched by GO prior to metal ions addition.
5. Adsorption of trace Cr(Ⅲ)and Pb(Ⅱ) by diethylenetriamine functionalized graphene oxide
Graphene oxide chemically modified with diethylenetriamine (GO-DETA) was fabricated and used to determine trace metal ions in solution. The results showed that the material exhibited a highly selective adsorption of trace Cr(Ⅲ) and Pb(Ⅱ) at pH4. The maximum adsorption capacity of GO-DETA was be60.9mg g-1and142.86mg g-1for Cr(Ⅲ) and Pb(Ⅱ), respectively. The facile chemical route and high adsorption capacity made this material practically useful for waste water treatment.
1.紫脲酸铵功能化的埃洛石纳米管对痕量Pd(Ⅱ)的高选择性固相萃取性能研究
在此工作中,首次成功地合成了一种新型吸附剂(HNTs-Mu),通过FT-IR,XRD,SEM,TEM和BET分析对HNTs-Mu的结构进行了表征。把HNTs-Mu作为固相萃取吸附剂,用于分离和预富集溶液中的痕量Pd(Ⅱ),通过ICP-AES进行测定,研究其分析性能。结果表明,HNTs-Mu对Pd(Ⅱ)具有很好的亲和力、较高的选择性以及好的捕捉能力。在pH=1.0时,痕量Pd(Ⅱ)能够被定量吸附,同时在流速为2.0mL min-1的时候,被吸附的Pd(Ⅱ)可以用2.5mL的0.01molL-1HCl-3%硫脲溶液定量洗脱。在样品溶液最大体积为300mL时,计算得到该方法的最大富集因子为120。HNTs-Mu对Pd(Ⅱ)的最大吸附容量为42.86mgg-1。Pd(Ⅱ)/Cd(Ⅱ),Pd(Ⅱ)/Hg(Ⅱ),Pd(Ⅱ)/Au(Ⅲ),Pd(Ⅱ)/Pt(Ⅳ)和Pd(Ⅱ)/Ir(Ⅳ)的选择性因子分别是3572.6,29.6,13.7,76.3和207。并且HNTs-Mu实验室合成方法简单,耗费较低。该方法被成功用于富集分离实际样品中的痕量Pd(Ⅱ),回收率大于95%。精密度和检出限都令人满意。
2.水杨酸修饰的埃洛石纳米管对痕量Fe(Ⅲ)的高选择性吸附性能的研究
使用水杨酸成功修饰埃洛石纳米管(HNTs-HBA),并用FT-IR,XRD,TEM和元素分析对其进行表征。把合成的HNTs-HBA用于溶液样品中痕量Fe(Ⅲ)的选择性分离,并用ICP-AES进行测定。通过静态和动态分析条件,对富集酸度、振荡时间、样品溶液的流速和体积及其洗脱剂等实验条件进行了优化。同时考察了一些常见共存离子对Fe(Ⅲ)的干扰问题。得到的富集因子为75。HNTs-HBA对Fe(Ⅲ)的吸附很快达到平衡。Fe(Ⅲ)的最大吸附容量是45.54mg g-1,方法的检出限是0.21ng mL-1,相对标准偏差是2.7%。把HNTs-HBA用于国家标准样品、生物样品以及环境水样中痕量Fe(Ⅲ)的富集测定,结果令人满意。
3.2-氨基苯并噻唑修饰的碳纳米管对痕量铅的选择性预富集分离研究
合成了2-氨基苯并噻唑修饰的多壁碳纳米管(MWCNTs-ABTZ),并把MWCNTs-ABTZ作为一种新的吸附剂,用于选择性富集分离痕量Pb(Ⅱ),实验结果用ICP-AES进行测定。通过静态和动态分析条件,对富集酸度、振荡时间、样品溶液的流速和体积、洗脱条件和共存离子的影响等实验条件进行了优化。得到的富集因子是100。常见的共存离子对痕量Pb(Ⅱ)的富集分离没有影响。MWCNTs-ABTZ对Pb(Ⅱ)的最大吸附容量是60.32mg g-1,方法的检出限是0.27ng mL-1,相对标准偏差是2.7%(n=8)。把MWCNTs-ABTZ用于国家标准样品以及环境水样中痕量Pb(Ⅱ)的分析测定,结果令人满意。
4.基于氧化石墨烯的荧光效应研究
我们通过化学方法成功地合成了氧化石墨烯,并且用TEM,UV-Vis,FT-IR和XRD对其结构进行了探究。同时,我们发现氧化石墨烯能够有效地猝灭罗丹明6G水溶液的荧光效应。依据氧化石墨烯的UV-Vis谱图以及罗丹明6G的荧光谱图,我们证明了荧光猝灭是由以下两个原因引起的：第一,罗丹明6G的电子转移到氧化石墨烯表面；第二,罗丹明6G被氧化石墨烯吸附。尽管如此,痕量的Th4+能够使被氧化石墨烯猝灭的罗丹明6G水溶液的荧光信号增强。
5.二乙烯三胺功能化的氧化石墨烯对痕量Cr(Ⅲ)和Pb(Ⅱ)的吸附性能研究
合成了二乙烯三胺功能化的氧化石墨烯(GO-DETA),并把GO-DETA用于富集分离溶液中的重金属离子。研究发现,GO-DETA对溶液中Cr(Ⅲ)和Pb(Ⅱ)具有良好的吸附能力。按照分析程序,对实验参数进行了优化。同时证明了常见共存离子对痕量Cr(Ⅲ)和Pb(Ⅱ)的富集分离没有干扰。GO-DETA对Cr(Ⅲ)和Pb(Ⅱ)的最大吸附容量分别是60.9和142.86mg g-1。把GO-DETA用于国家标准样品及环境水样中痕量Cr(Ⅲ)和Pb(Ⅱ)的分离富集和测定,实验结果令人满意。
With the continuous development of the economy, the growing incidence of environmental pollution, air pollution, water pollution, global warming, energy shortages, solid waste pollution and species extinction and other issues have threated our living environment. Especially water, soil and food contamination caused by the heavy metal ions have maken our life destroyed once again. However, because complex matrix interference is complex and the sensitivity of the exsiting methods is not enough, it's difficult to analyze trace and ultra-trace element in actual samples. Thus, it is very important to open efficient methods for detecting metal ions in the environment. In this paper, in order to separate trace metals from the environmental samples, we designed the new SPE adsorbents and analytical methods. Through the modification of multiwall carbon nanotubes, graphene oxide and halloysite nanotubes, we obtained several new SPE adsorbents material, and systematically studied the selective adsorption property of the material. At the same time, according to characteristics of graphene oxide, we developed a fluorescence sensor to directly analysis trace Th4+in the solution samples. Our work is divided into the following five parts:
1. Highly selective solid-phase extraction of trace Pd(Ⅱ) by murexide functionalized halloysite nanotubes
The originality on the high efficiency of murexide modified halloysite nanotubes (HNTs-Mu) as a new solid-phase extractant has been reported to preconcentrate and separate Pd(Ⅱ) in solution samples. The structure of HNTs-Mu was confirmed by FT-IR, XRD, SEM, TEM and BET. Effective determination conditions of Pd(Ⅱ) were examined using column procedures before detection by inductive coupled plasma atomic emission spectrometry (ICP-AES). The effects of pH, sample flow rate and volume, amount of adsorbent, elution condition and interfering ions were optimized. Under the optimized conditions, trace Pd(Ⅱ) could be retained on the column at pH1.0and quantitatively eluted by2.5mL of0.01mol L-1HCl-3%thiourea solution at a flow rate of2.0mL min-1.An enrichment factor of120was achieved. Common interfering ions did not interfere in determination and separation. The maximum adsorption capacity of HNTs-Mu at optimum conditions was42.86mg g-1for Pd(II). The detection limit (3a) of the method was0.29ng mL-1, and the relative standard deviation was3.1%(n=11). The method was validated using certified reference material, and then has been applied for the determination of trace Pd(II) in actual samples with satisfactory results.
2. Functionalized halloysite nanotubes with2-hydroxybenzoic acid for selective solid-phase extraction of trace iron(III)
Functionalized halloysite nanotubes with2-hydroxybenzoic acid (HNTs-HBA) has been synthesized and characterized by FT-IR, XRD, TEM and Elemental analysis. The capability of HNTs-HBA has been developed for selective separation and preconcentration of trace Fe(III) before detection by ICP-AES. The effects of pH, shaking time, flow rate and volume of the sample, elution condition and interfering ions were examined using column and batch procedures. An enrichment factor of75was obtained. HNTs-HBA exhibited fairly fast kinetics for the adsorption of Fe(Ⅲ) and common coexisting ions did not interfere in the determination. The maximum adsorption capacity of HNTs-HBA for Fe(Ⅲ) was45.54mg g-1at optimum conditions. The detection limit (3σ) of the method was0.21ng mL-1. The relative standard deviation under optimum condition was2.7%(n=11). The developed method has been successfully applied for the determination of trace Fe(Ⅲ) in biological and natural water samples.
3. Multiwalled carbon nanotubes modified with2-aminobenzothiazole for uniquely selective solid-phase extraction and determination of trace Pb(Ⅱ) ion in water samples
A solid phase extraction method is presented for the selective preconcentration and/or separation of trace Pb(Ⅱ) by2-aminobenzothiazole modified multiwalled carbon nanotubes (MWCNTs-ABTZ). ICP-AES was used for detection. The effects of pH, shaking time, sample flow rate and volume, elution condition and interfering ions were examined by column and batch procedures. An enrichment factor of100was obtained. Common coexisting ions did not interfere in the determination. The maximum adsorption capacity of MWCNTs-ABTZ for Pb(Ⅱ) was60.32mg g-1. The detection limit (3σ) of the method was0.27ng mL-1. And the relative standard deviation was1.6%(n=8). The method was validated using a certified reference material, and has been applied for the determination of trace Pb(II) in water samples with satisfactory results.
4. Fluorescence determination based on graphene oxide
Graphene oxide (GO) has been prepared and the structure of the prepared GO was characterized by XRD, UV-Vis, FT-IR and TEM, respectively. And then we demonstrated that GO could quench the fluorescence of Rhodamine6G (Rh6G) in aqueous solution. According to the UV-vis absorption spectrum of GO and the fluorescence spectrum of Rh6G, we found that GO quenched the fluorescence of Rh6G due to two factors. Firstly, the electrons moved from the Rh6G to the surface GO; secondly, Rh6G adsorbed onto the GO surface. However, trace Th4+enhanced the fluorescent signal of Rh6G, which was quenched by GO prior to metal ions addition.
5. Adsorption of trace Cr(Ⅲ)and Pb(Ⅱ) by diethylenetriamine functionalized graphene oxide
Graphene oxide chemically modified with diethylenetriamine (GO-DETA) was fabricated and used to determine trace metal ions in solution. The results showed that the material exhibited a highly selective adsorption of trace Cr(Ⅲ) and Pb(Ⅱ) at pH4. The maximum adsorption capacity of GO-DETA was be60.9mg g-1and142.86mg g-1for Cr(Ⅲ) and Pb(Ⅱ), respectively. The facile chemical route and high adsorption capacity made this material practically useful for waste water treatment.
引文
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