改性壳聚糖在环境痕量元素及其形态分析中的应用
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摘要
环境问题是全球共同关注的一个热点,对环境污染物的监测分析已成为当今分析化学领域的一大热门。在各种环境污染物中,环境痕量元素由于其对生命物质的营养和毒害双重作用而广受重视。环境痕量元素的生物有效性和毒性大小不仅与其总量有关,更主要取决于其存在的化学形态。对环境痕量元素进行形态分析对于掌握其毒性和了解其生物有效性具有重大的现实意义,元素形态分析目前已成为分析化学的一个前沿研究课题。
环境痕量元素由于其含量非常低,一般在分析测定前都要进行预富集分离,常用的预富集分离技术有萃取、共沉淀、离子交换、吸附等。利用生物吸附剂吸附的预富集分离方法由于其取材来源广、成本低、操作简单而吸引了众多研究者的兴趣。壳聚糖(CTS)就是这样的一种生物吸附剂,关于壳聚糖已有大量研究报道,但是将改性壳聚糖应用于痕量元素形态分析的研究却比较少。本论文以壳聚糖的改性及其在环境痕量元素形态分析中的应用为研究内容,主要工作和创新点如下：
(1)、合成了二乙烯三胺交联壳聚糖(DCCTS),并将其应用于无机硒和砷的形态分析。利用红外光谱和扫描电镜对DCCTS进行了结构表征,研究了DCCTS对Se(Ⅵ)和Se(Ⅳ)、As(Ⅴ)和As(Ⅲ)的吸附行为,结果表明,在pH=3.6时,DCCTS对Se(Ⅵ)的吸附率达94%,对Se(Ⅳ)的吸附率只有5%左右,所以在pH=3.6时,DCCTS能选择性富集分离Se(Ⅵ)；在pH=3.0时,DCCTS对As(V)的吸附率达96%,对As(Ⅲ)的吸附率小于10%,所以在pH=3.0时,DCCTS能选择性富集分离As(V)。以DCCTS为富集分离剂,电感耦合等离子体发射光谱法(ICP-OES)和石墨炉原子吸收光谱法(GFAAS)为检测手段,分别测定了环境水样中Se(Ⅵ)和Se(Ⅳ)、As(Ⅴ)和As(Ⅲ)形态,获得了满意的结果。(2)、制备了氯化胆碱接枝壳聚糖(HGCTS),并将其应用于无机铬的形态分析。研究了HGCTS对Cr(Ⅵ)和Cr(Ⅲ)的吸附行为,结果表明,在pH=4.0时,HGCTS对Cr(Ⅵ)的吸附率达97%,对Cr(Ⅲ)的吸附率只有5%左右,所以在pH=4.0时,HGCTS能选择性富集分离Cr(Ⅵ)。HGCTS对Cr(Ⅵ)的吸附机理为静电引力和离子交换作用,吸附符合Langmuir模型和准二级动力学模型。以HGCTS为富集分离剂,火焰原子吸收光谱法为检测手段,构建了一种新的测定环境水样中Cr(Ⅵ)和Cr(Ⅲ)形态的方法。
(3)、制备了氨基硫脲接枝壳聚糖(AGCTS),并将其应用于Mn(Ⅱ)和Mn(Ⅶ)的形态分析。研究了AGCTS对Mn(Ⅶ)和Mn(Ⅱ)的吸附行为,结果表明,在pH=3.3时,HGCTS对Mn(Ⅶ)的吸附率达96%,对Mn(Ⅱ)的吸附率只有4%左右,所以在pH=3.3时,AGCTS能选择性富集分离Mn(Ⅶ)。考察了溶液pH、温度和接触时间等因素对吸附的影响。以AGCTS为富集分离剂,石墨炉原子吸收光谱法为检测手段,构建了一种新的测定环境水样中Mn(Ⅶ)和Mn(Ⅱ)形态的方法。
(4)、合成了氨基乙酸交联壳聚糖(ACCTS),并将其应用于Sb(Ⅲ)和Sb(Ⅴ)的形态分析。研究结果表明,未用吡咯烷二硫代氨基甲酸铵(APDC)络合时,ACCTS对Sb(Ⅲ)和Sb(Ⅴ)的吸附率都不高,用APDC络合后,在pH=5.0时,ACCTS对Sb(Ⅲ)-APDC的吸附率达98%,而对Sb(Ⅴ)-APDC的吸附率小于10%,所以,用APDC络合后,在pH=5.0时,ACCTS能选择性富集分离Sb(Ⅲ)。以ACCTS为富集分离剂,石墨炉原子吸收光谱法为检测手段,构建了一种新的测定环境水样中Sb(Ⅲ)和Sb(Ⅴ)形态的方法。
(5)、合成了铁(Ⅲ)模板-硫脲交联壳聚糖(Fe(Ⅲ)-TCCTS),考察了Fe(Ⅲ)和Fe(Ⅱ)在Fe(Ⅲ)-TCCTS上的吸附行为。研究结果表明,Fe(Ⅲ)-TCCTS对Fe(Ⅲ)和Fe(Ⅱ)的吸附行为非常相似,但对Fe(Ⅲ)的吸附容量比Fe(Ⅱ)大,吸附符合Langmuir模型和准二级动力学模型。Fe(Ⅲ)-TCCTS能选择性吸附Fe(Ⅲ),可将其应用于除去废水中的铁离子。
The problem of environment has already become a global focus. The analysis of environmental pollution has attracted large attention in current analytical chemistry region. The environmental trace elements are very important pollutants for their effect of nutrition and toxicity on life. The effect of nutrition and toxicity of the environmental trace elements is decided not only by their amounts but also by their speciation. It is very important to know the effect of nutrition and toxicity of the environmental trace elements by speciation of the environmental trace elements. Speciation analysis of element has become an advanced region.
Enrichment and separation are necessary prior to determination of trace elements because their content is low. The methods of enrichment and separation include extraction, precipitation, ion-exchange and adsorption. The bio-adsorbents have attracted more attention for their advantages of large source, low cost and easy operation. Chitosan is one of these bio-adsorbents, there are many reports about chitosan, however, the reports about application of modified chitosan to speciation of trace elements are few. This thesis concentrates research on chitosan modification and their application to speciation of trace elements. The major contents and novelty of this thesis are given in the following.
(1) The cross-linked chitosan was synthesized with Diethylene Triamine (DCCTS), and applied to speciation of inorganic selenium and arsenic. The characterization of DCCTS was performed by FTIR and SEM. The adsorption behavior of Se(Ⅵ) and Se(Ⅳ), As(Ⅴ) and As(Ⅲ) on DCCTS was studied. The results indicated that the adsorption efficiency of Se(Ⅵ) was94%at pH3.6, whereas5%of Se(Ⅳ). Thus DCCTS can concentrate and separate Se (Ⅵ) from Se (Ⅳ) solution at pH3.6. The results also showed that the adsorption efficiency of As(Ⅴ) was96%at pH3.0, whereas which of As(Ⅲ) was lower than10%. DCCTS can concentrate and separate As(Ⅴ) from As(Ⅲ) solution at pH3.0. Speciation of Se(Ⅵ) and Se(Ⅳ), As(Ⅴ) and As(Ⅲ) in environmental water samples was performed using DCCTS as adsorbent and ICP-OES, GFAAS as determination means, respectively. The result was approving.
(2) The grafting chitosan was prepared with2-Hydroxyethyl trimethyl ammonium chloride(HGCTS), and applied to speciation of inorganic chromium. The adsorption behavior of Cr(Ⅵ) and Cr(Ⅲ) on HGCTS was studied. The results indicated that the adsorption efficiency of Cr(Ⅵ) was97%at pH4.0, whereas5%of Cr(Ⅲ). Thus HGCTS can concentrate and separate Cr(Ⅵ) from Cr(Ⅲ) solution at pH4.0. The adsorption mechanism of Cr(VI) on HGCTS was electrostatic attraction and ion exchange. The adsorption agreed very well with the Langmuir model and the Pseudo second-order kinetic model. A novel method for speciation of Cr(Ⅵ) and Cr(Ⅲ) in environmental water samples has been developed using HGCTS as adsorbent and FAAS as determination means.
(3) The grafting chitosan was prepared with aminothiourea (AGCTS), and applied to speciation of Mn(Ⅶ) and Mn(Ⅱ). The adsorption behavior of Mn(Ⅶ) and Mn(Ⅱ) on AGCTS was studied. The results indicated that the adsorption efficiency of Mn(Ⅶ) was96%at pH3.3, whereas4%of Mn(Ⅱ). Thus AGCTS can concentrate and separate Mn(Ⅶ) from Mn(Ⅱ) solution at pH3.3. The effect of pH, temperature and contact time was investigated. A novel method for speciation of Mn(Ⅶ) and Mn(Ⅱ) in environmental water samples has been developed using AGCTS as adsorbent and GFAAS as determination means.
(4) The cross-linked chitosan was synthesized with aminoacetic (ACCTS), and applied to speciation of Sb(Ⅲ) and Sb(Ⅴ). The results showed that the adsorption efficiency of Sb(Ⅲ) and Sb(Ⅴ) was low on ACCTS before chelated with ammonium pyrrolidine dithiocarbamate (APDC) and after chelated with APDC, the adsorption efficiency of Sb(Ⅲ)-APDC was98%at pH5.0, whereas which of Sb(Ⅴ)-APDC was lower than10%. Thus, ACCTS can concentrate and separate Sb(Ⅲ) at pH5.0after chelated with APDC. A novel method for speciation of Sb(Ⅲ) and Sb(Ⅴ) in environmental water samples has been developed using ACCTS as adsorbent and GFAAS as determination means.
(5) The thiourea cross-linked chitosan with Fe(Ⅲ) as template (Fe(Ⅲ)-TCCTS) was synthesized. The adsorption behavior of Fe(III) and Fe(Ⅱ) on Fe(Ⅲ)-TCCTS was studied. The results indicated that the adsorption behavior of Fe(Ⅲ) and Fe(Ⅱ) on Fe(Ⅲ)-TCCTS was similar, but the adsorption content of Fe(Ⅲ) was higher than which of Fe(Ⅱ). The adsorption agreed very well with the Langmuir model and the Pseudo second-order kinetic model. Fe(Ⅲ)-TCCTS can adsorb Fe(Ⅲ) selectively. It can be applied to remove iron ion from waste water.
环境痕量元素由于其含量非常低,一般在分析测定前都要进行预富集分离,常用的预富集分离技术有萃取、共沉淀、离子交换、吸附等。利用生物吸附剂吸附的预富集分离方法由于其取材来源广、成本低、操作简单而吸引了众多研究者的兴趣。壳聚糖(CTS)就是这样的一种生物吸附剂,关于壳聚糖已有大量研究报道,但是将改性壳聚糖应用于痕量元素形态分析的研究却比较少。本论文以壳聚糖的改性及其在环境痕量元素形态分析中的应用为研究内容,主要工作和创新点如下：
(1)、合成了二乙烯三胺交联壳聚糖(DCCTS),并将其应用于无机硒和砷的形态分析。利用红外光谱和扫描电镜对DCCTS进行了结构表征,研究了DCCTS对Se(Ⅵ)和Se(Ⅳ)、As(Ⅴ)和As(Ⅲ)的吸附行为,结果表明,在pH=3.6时,DCCTS对Se(Ⅵ)的吸附率达94%,对Se(Ⅳ)的吸附率只有5%左右,所以在pH=3.6时,DCCTS能选择性富集分离Se(Ⅵ)；在pH=3.0时,DCCTS对As(V)的吸附率达96%,对As(Ⅲ)的吸附率小于10%,所以在pH=3.0时,DCCTS能选择性富集分离As(V)。以DCCTS为富集分离剂,电感耦合等离子体发射光谱法(ICP-OES)和石墨炉原子吸收光谱法(GFAAS)为检测手段,分别测定了环境水样中Se(Ⅵ)和Se(Ⅳ)、As(Ⅴ)和As(Ⅲ)形态,获得了满意的结果。(2)、制备了氯化胆碱接枝壳聚糖(HGCTS),并将其应用于无机铬的形态分析。研究了HGCTS对Cr(Ⅵ)和Cr(Ⅲ)的吸附行为,结果表明,在pH=4.0时,HGCTS对Cr(Ⅵ)的吸附率达97%,对Cr(Ⅲ)的吸附率只有5%左右,所以在pH=4.0时,HGCTS能选择性富集分离Cr(Ⅵ)。HGCTS对Cr(Ⅵ)的吸附机理为静电引力和离子交换作用,吸附符合Langmuir模型和准二级动力学模型。以HGCTS为富集分离剂,火焰原子吸收光谱法为检测手段,构建了一种新的测定环境水样中Cr(Ⅵ)和Cr(Ⅲ)形态的方法。
(3)、制备了氨基硫脲接枝壳聚糖(AGCTS),并将其应用于Mn(Ⅱ)和Mn(Ⅶ)的形态分析。研究了AGCTS对Mn(Ⅶ)和Mn(Ⅱ)的吸附行为,结果表明,在pH=3.3时,HGCTS对Mn(Ⅶ)的吸附率达96%,对Mn(Ⅱ)的吸附率只有4%左右,所以在pH=3.3时,AGCTS能选择性富集分离Mn(Ⅶ)。考察了溶液pH、温度和接触时间等因素对吸附的影响。以AGCTS为富集分离剂,石墨炉原子吸收光谱法为检测手段,构建了一种新的测定环境水样中Mn(Ⅶ)和Mn(Ⅱ)形态的方法。
(4)、合成了氨基乙酸交联壳聚糖(ACCTS),并将其应用于Sb(Ⅲ)和Sb(Ⅴ)的形态分析。研究结果表明,未用吡咯烷二硫代氨基甲酸铵(APDC)络合时,ACCTS对Sb(Ⅲ)和Sb(Ⅴ)的吸附率都不高,用APDC络合后,在pH=5.0时,ACCTS对Sb(Ⅲ)-APDC的吸附率达98%,而对Sb(Ⅴ)-APDC的吸附率小于10%,所以,用APDC络合后,在pH=5.0时,ACCTS能选择性富集分离Sb(Ⅲ)。以ACCTS为富集分离剂,石墨炉原子吸收光谱法为检测手段,构建了一种新的测定环境水样中Sb(Ⅲ)和Sb(Ⅴ)形态的方法。
(5)、合成了铁(Ⅲ)模板-硫脲交联壳聚糖(Fe(Ⅲ)-TCCTS),考察了Fe(Ⅲ)和Fe(Ⅱ)在Fe(Ⅲ)-TCCTS上的吸附行为。研究结果表明,Fe(Ⅲ)-TCCTS对Fe(Ⅲ)和Fe(Ⅱ)的吸附行为非常相似,但对Fe(Ⅲ)的吸附容量比Fe(Ⅱ)大,吸附符合Langmuir模型和准二级动力学模型。Fe(Ⅲ)-TCCTS能选择性吸附Fe(Ⅲ),可将其应用于除去废水中的铁离子。
The problem of environment has already become a global focus. The analysis of environmental pollution has attracted large attention in current analytical chemistry region. The environmental trace elements are very important pollutants for their effect of nutrition and toxicity on life. The effect of nutrition and toxicity of the environmental trace elements is decided not only by their amounts but also by their speciation. It is very important to know the effect of nutrition and toxicity of the environmental trace elements by speciation of the environmental trace elements. Speciation analysis of element has become an advanced region.
Enrichment and separation are necessary prior to determination of trace elements because their content is low. The methods of enrichment and separation include extraction, precipitation, ion-exchange and adsorption. The bio-adsorbents have attracted more attention for their advantages of large source, low cost and easy operation. Chitosan is one of these bio-adsorbents, there are many reports about chitosan, however, the reports about application of modified chitosan to speciation of trace elements are few. This thesis concentrates research on chitosan modification and their application to speciation of trace elements. The major contents and novelty of this thesis are given in the following.
(1) The cross-linked chitosan was synthesized with Diethylene Triamine (DCCTS), and applied to speciation of inorganic selenium and arsenic. The characterization of DCCTS was performed by FTIR and SEM. The adsorption behavior of Se(Ⅵ) and Se(Ⅳ), As(Ⅴ) and As(Ⅲ) on DCCTS was studied. The results indicated that the adsorption efficiency of Se(Ⅵ) was94%at pH3.6, whereas5%of Se(Ⅳ). Thus DCCTS can concentrate and separate Se (Ⅵ) from Se (Ⅳ) solution at pH3.6. The results also showed that the adsorption efficiency of As(Ⅴ) was96%at pH3.0, whereas which of As(Ⅲ) was lower than10%. DCCTS can concentrate and separate As(Ⅴ) from As(Ⅲ) solution at pH3.0. Speciation of Se(Ⅵ) and Se(Ⅳ), As(Ⅴ) and As(Ⅲ) in environmental water samples was performed using DCCTS as adsorbent and ICP-OES, GFAAS as determination means, respectively. The result was approving.
(2) The grafting chitosan was prepared with2-Hydroxyethyl trimethyl ammonium chloride(HGCTS), and applied to speciation of inorganic chromium. The adsorption behavior of Cr(Ⅵ) and Cr(Ⅲ) on HGCTS was studied. The results indicated that the adsorption efficiency of Cr(Ⅵ) was97%at pH4.0, whereas5%of Cr(Ⅲ). Thus HGCTS can concentrate and separate Cr(Ⅵ) from Cr(Ⅲ) solution at pH4.0. The adsorption mechanism of Cr(VI) on HGCTS was electrostatic attraction and ion exchange. The adsorption agreed very well with the Langmuir model and the Pseudo second-order kinetic model. A novel method for speciation of Cr(Ⅵ) and Cr(Ⅲ) in environmental water samples has been developed using HGCTS as adsorbent and FAAS as determination means.
(3) The grafting chitosan was prepared with aminothiourea (AGCTS), and applied to speciation of Mn(Ⅶ) and Mn(Ⅱ). The adsorption behavior of Mn(Ⅶ) and Mn(Ⅱ) on AGCTS was studied. The results indicated that the adsorption efficiency of Mn(Ⅶ) was96%at pH3.3, whereas4%of Mn(Ⅱ). Thus AGCTS can concentrate and separate Mn(Ⅶ) from Mn(Ⅱ) solution at pH3.3. The effect of pH, temperature and contact time was investigated. A novel method for speciation of Mn(Ⅶ) and Mn(Ⅱ) in environmental water samples has been developed using AGCTS as adsorbent and GFAAS as determination means.
(4) The cross-linked chitosan was synthesized with aminoacetic (ACCTS), and applied to speciation of Sb(Ⅲ) and Sb(Ⅴ). The results showed that the adsorption efficiency of Sb(Ⅲ) and Sb(Ⅴ) was low on ACCTS before chelated with ammonium pyrrolidine dithiocarbamate (APDC) and after chelated with APDC, the adsorption efficiency of Sb(Ⅲ)-APDC was98%at pH5.0, whereas which of Sb(Ⅴ)-APDC was lower than10%. Thus, ACCTS can concentrate and separate Sb(Ⅲ) at pH5.0after chelated with APDC. A novel method for speciation of Sb(Ⅲ) and Sb(Ⅴ) in environmental water samples has been developed using ACCTS as adsorbent and GFAAS as determination means.
(5) The thiourea cross-linked chitosan with Fe(Ⅲ) as template (Fe(Ⅲ)-TCCTS) was synthesized. The adsorption behavior of Fe(III) and Fe(Ⅱ) on Fe(Ⅲ)-TCCTS was studied. The results indicated that the adsorption behavior of Fe(Ⅲ) and Fe(Ⅱ) on Fe(Ⅲ)-TCCTS was similar, but the adsorption content of Fe(Ⅲ) was higher than which of Fe(Ⅱ). The adsorption agreed very well with the Langmuir model and the Pseudo second-order kinetic model. Fe(Ⅲ)-TCCTS can adsorb Fe(Ⅲ) selectively. It can be applied to remove iron ion from waste water.
引文
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