钛基晶须材料固相萃取分离/富集无机环境激素及机理研究
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摘要
环境激素,也称为环境内分泌干扰剂,系由于人类活动而释放到环境中的、能影响和扰乱生物内分泌系统的有害化学物质的总称。环境激素可以分为有机环境激素和无机环境激素。无机环境激素主要指镉、铅、汞等一类具有明显生物效应的无机污染物。由于方法的灵敏度限制和基体效应的影响,利用仪器直接测定无机环境激素一般很困难,因此预富集/分离无机环境激素显得十分必要。固相萃取法因其具有操作简单、分离/富集倍数高、相分离速度快和易与不同的检测技术相结合等优点而受到广大分析工作者的关注。
钛基晶须材料具有特定强度、模量、尺寸稳定性等优良性能,不仅在光电材料方面有广泛的应用,而且在吸附、分离等领域也具有重要的应用价值。分子印迹技术是近年发展起来的制备对目标化合物具有特定识别能力的聚合物的新技术。本研究选择利用钛基晶须/表面修饰钛基晶须/表面离子印迹钛基晶须固相萃取无机环境激素。
本论文主要包括以下三个方面的内容:
(1)钛基晶须固相萃取预分离/富集无机环境激素的研究
ⅰ.以四钛酸钾(K_2Ti_4O_9)晶须为固相萃取剂,火焰原子吸收光谱法(FAAS)为检测手段,详细研究了K_2Ti_4O_9对无机环境激素铅、镉、镍的吸附行为,考察了共存离子的影响情况及可能的吸附机理。在优化的实验条件下,将其用于环境水样中Cd(Ⅱ)、Pb(Ⅱ)、Ni(Ⅱ)的测定,检出限分别为:2.5μg·L~(-1)、3.6μg·L~(-1)、56μg·L~(-1);相对标准偏差(RSD)分别为2.6%、3.1%、2.9%。结果表明,所提出的新方法具有稳定性好、吸附和解吸性能好的特点。
ⅱ.建立了一种以电感耦合等离子体原子发射光谱法(ICP-AES)为检测手段,六钛酸钾(K_2Ti_6O_(13))为固相萃取剂分离/富集Co(Ⅱ)、Ni(Ⅱ)、Cr(Ⅲ)的方法,探讨了影响分离/富集过程的主要因素、共存离子的干扰以及可能的吸附机理,考察了吸附容量。在优化的实验条件下,本法用于磷化废水中Co(Ⅱ)、Ni(Ⅱ)、Cr(Ⅲ)的测定,检出限分别为:9.2μg·L~(-1)、5.3μg·L~(-1)、8.9μg·L~(-1);相对标准偏差(RSD)分别为0.98%、0.75%、0.87%。结果表明:所提出的新方法具有稳定性好、吸附和解吸性能好的特点。
(2)钛基晶须表面修饰分离/富集无机环境激素研究
ⅰ.以K_2Ti_4O_9为载体,γ-(2、3环氧丙氧)丙基三甲氧基硅烷(KH-560)为表面修饰剂,溶胶-凝胶法(sol-gel)制备负载型、疏水性固相萃取剂KH-560/K_2Ti_4O_9。采用傅立叶变换红外光谱法(FF-IR)、扫描电镜(SEM)、X-射线衍射(XRD)对KH-560/K_2Ti_4O_9表面形貌和结构进行表征;以FAAS为检测手段,考察了吸附酸度、吸附剂用量、静置时间等对KH-560/K_2Ti_4O_9吸附Pb(Ⅱ)的影响;研究了在混合溶液中KH-560/K_2Ti_4O_9对Pb(Ⅱ)的选择性。结果表明:在K_2Ti_4O_9表面修饰KH-560可以有效增加K_2Ti_4O_9的疏水性能。
ⅱ.以六钛酸钾晶须(K_2Ti_6O_(13))为载体,采用浸渍法制备了双硫腙(Dithizone,C_(13)H_(12)N_4S)负载型六钛酸钾(C_(13)H_(12)N_4S/K_2Ti_6O_(13))。采用FT-IR、SEM对C_(13)H_(12)N_4S/K_2Ti_6O_(13)表面形貌和结构进行表征。以ICP-AES为检测手段,考察了吸附酸度、吸附剂用量、静置时间等对C_(13)H_(12)N_4S/K_2Ti_6O_(13)吸附Cd(Ⅱ)、Pb(Ⅱ)的影响。在优化的条件下,本法用于环境水样中Cd(Ⅱ)、Pb(Ⅱ)的测定,检出限为1.2μg·L~(-1)、1.6μg·L~(-1),加标回收率为92～101%。结果表明:C_(13)H_(12)N_4S/K_2Ti_6O_(13)可以有选择的吸附Cd(Ⅱ)、Pb(Ⅱ)等离子。
(3)钛基晶须表面离子印迹聚合物分离/富集无机环境激素研究
ⅰ.以Pb(Ⅱ)为模板离子,壳聚糖(CTS)为功能单体,三钛酸钠(Na_2Ti_3O_7)为载体,KH-560为偶联剂,利用表面分子印迹技术(SMIT)和溶胶-凝胶法(sol-gel)在稀醋酸溶液中制备了Pb(Ⅱ)离子印迹聚合物(Pb(Ⅱ)-ion Imprinted Polymer,Pb(Ⅱ)-ⅡP)。采用FT-IR、SEM、XRD等表征手段对Pb(Ⅱ)-ⅡP的表面形貌和结构进行表征;以FAAS为检测手段,考察了吸附酸度、吸附剂用量、吸附时间等对聚合物吸附性能的影响;研究了印迹聚合物在混合溶液中对Pb(Ⅱ)的选择性,比较了印迹和非印迹聚合物(Non imprinted polymer,NIP)的吸附容量;提出了印迹聚合物可能的印迹吸附机理。结果表明:Pb(Ⅱ)-ⅡP具有较好的疏水性能,对Pb(Ⅱ)离子具有较高的选择性。
ⅱ.在醋酸溶液中,以Ni(Ⅱ)为模板离子,CTS为功能单体,KH-560为偶联剂,利用表面印迹技术和溶胶-凝胶技术结合制备了Ni(Ⅱ)离子印迹聚合物(Ni(Ⅱ)-ion Imprinted Polymer,Ni(Ⅱ)-ⅡP)。采用FT-IR、SEM等手段对Ni(Ⅱ)-ⅡP的性质和结构进行了表征。并以其为固相萃取吸附剂,以FAAS为检测手段,考察了溶液酸度、吸附时间、吸附剂用量等对聚合物吸附性能的影响。采用ICP-AES研究了聚合物对Ni(Ⅱ)的选择性和吸附容量。对Ni(Ⅱ)-ⅡP的印迹机理进行了探讨。结果表明:Ni(Ⅱ)-ⅡP具有较高的选择性。
研究表明:钛基晶须分离/富集无机环境激素具有广谱性、选择性不理想等特性。对钛基晶须材料实施表面离子印迹,得到表面离子印迹改性钛基晶须固相萃取材料,用于预分离/富集样品中无机环境激素的研究,实现对无机环境激素专属性/高选择性吸附;研究了表面离子印迹改性钛基晶须材对无机环境激素的吸附行为和分离/富集机理。实现了表面离子印迹改性钛基晶须固相萃取材料预分离/富集与仪器分析方法联用,建立了环境样品中痕量/超痕量无机环境激素仪器分析新方法。
Environmental hormones,also known as environmental endocrine disrupters,are harmful chemical substances released into environment because of human activities and can disrupt biological endocrine system. Environmental hormones can be divided into organic environmental hormones and inorganic environmental hormones.Inorganic environmental hormones(IEHs) mainly include cadmium,lead,mercury,etc.Owing to restriction of selectivity and influence of samples,inorganic environmental hormones cannot be analyzed directly with equipment.Therefore, separation/enrichment of inorganic environmental hormones from samples is very important.Solid-phase extraction has gained attention of many analytic researchers for its several advantages,including operating simply, high pre-concentration factor,rapid phase separation,and the ability of combining with different detection techniques.
Titanate whisker materials have some good performances such as specific strength,modulus,dimensional stability,etc.It has widely application not only on photoelectric materials,but also on adsorption, separation and other fields.
In recent years,Molecular Imprinting Technique(MIT) has been developed as the new technology for the preparation of polymer with specific ability for identification of targeted compound.
In this work,IEHs were pre-concentration/separation by using whisker titanium/modified whisker titanium/surface ion imprinted titanate polymer as solid-phase extractant.
The work mainly included the following items:
(1) Study on the pre-concentration/separation of IEHs using titanate whisker as solid-phase extractant
ⅰ.The absorption behaviors of K_2Ti_4O_9 towards Cd(Ⅱ),Pb(Ⅱ), Ni(Ⅱ) using FAAS as sensitive detector was studied.Under optimum conditions,the possiblility of absorption mechanism was investigated and applied to the speciation analysis of Cd(Ⅱ),Pb(Ⅱ),Ni(Ⅱ) in environmental water samples and the detection limits were 2.5μg·L~(-1) with relative standard deviation(RSD) of 2.6%for Cd,3.6μg·L~(-1)with RSD of 3.1%for Pb and 56μg·L~(-1) with RSD of 2.9%for Ni,respectively.It was found that the proposed method used in the paper had many advantages such as good stability and good performance of absorption and desorption.
ⅱ.A new method was proposed for the separation/enrichment of Co(Ⅱ),Ni(Ⅱ),Cr(Ⅲ) using K_2Ti_6O_(13) as solid-phase extractant and ICP-AES as sensitive detector.The major factors influencing the process of separation and enrichment were investigated,including the interference of co-existing ions and the possible sorption mechanism.Under optimum conditions,the detection limits were 9.2μg·L~(-1) with relative standard deviation(RSD) of 0.98%for Co,5.3μg·L~(-1) with RSD of 0.75%for Ni and 8.9μg·L~(-1) with RSD of 0.87%for Cr,respectively.It was found that the proposed method used in the article had many advantages including good stability and good performance of absorption and desorption.The result showed that the method was suit for the analysis of industrial waste water samples.
(2) Study on the pre-concentration/separation of IEHs using surface modification -titanate whisker as solid-phase extractant
ⅰ.The new solid-phase extractant(KH-560/K_2Ti_4O_9) was prepared by using sol-gel method with KH-560 as the surface modification agent, K_2Ti_4O_9 as the carrier.KH-560/K_2Ti_4O_9 was characterized by using SEM, FI-IR、XRD.The absorption behavior of KH-560/K_2Ti_4O_9 towards Pb using FAAS as sensitive detector was studied.Under optimum conditions, the selectivity for Pb(Ⅱ) of KH-560/K_2Ti_4O_9 was also discussed in mixed aqueous solution.The detection limit was 2.5μg·L~(-1) with relative standard deviation(RSD) of 2.6%for Pb(Ⅱ),respectively.It was found that the surface modification of K_2Ti_4O_9 using KH-560 could effectively increase the hydrophobic properties.
ⅱ.In this paper,the C_(13)H_(12)N_4S/K_2Ti_6O_(13) as solid sorbent was prepared by using impregnation method,and characterized by using SEM、FI-IR.Effects of adsorption acidity,sorbent dosage and resting time on adsorption rate to Cd(Ⅱ),Pb(Ⅱ) on C_(13)H_(12)N_4S/K_2Ti_6O_(13) were investigated by ICP-AES.Under optimum conditions,the method was applied to the determination of real water samples,and the detection limits were 1.2μg·L~(-1),1.6μg·L~(-1) for Cd(Ⅱ) and Pb(Ⅱ),respectively.The results indicated that the C_(13)H_(12)N_4S/K_2Ti_6O_(13) can adsorb some ions like Cd(Ⅱ) and Pb(Ⅱ).
(3) Study on the pre-concentration/separation of IEHs using surface ion-imprinted titanate polymer as solid-phase extractant
ⅰ.The Pb(Ⅱ) ion imprinted polymer particles were prepared by surface molecular imprinting technique and sol-gel process in acetic acid solution,with Pb(Ⅱ) ion as the template,chitosan(CTS) as the functional monomer,Na_2Ti_3O_7 as the carder,and KH-560 as the crosslinking agent. The ion-imprinted polymer particles were characterized by FT-IR,XRD, SEM and TEM.Effects of adsorption acidity,sorbent dosage and resting time on adsorption rate were investigated by FAAS.Selectivity of the prepared polymer for Pb(Ⅱ) ions was also discussed in mixed aqueous solution.Adsorption capacity of Pb(Ⅱ)-ⅡP was compared with that of non-imprinted polymer(NIP).The imprint and adsorption mechanism were also put forward.The results indicated that Pb(Ⅱ)-ⅡP exhibited high selectivity for Pb(Ⅱ) ions and hydrophobic properties.
ⅱ.Ni(Ⅱ) ion imprinted polymer(Ni(Ⅱ)-ⅡP) particles was prepared by the combination of surface molecular imprinting technique and sol-gel process in acetic acid solution,with Ni(Ⅱ) ion as a template,CTS as functional monomer,and KH-560 as the cross-linker.The configuration of Ni(Ⅱ) ion imprinted polymer and its materials were characterized by FT-IR spectra,UV-spectra,SEM,TEM and XRD.The optimal adsorption conditions,such as acidity,resting time,amount of sorbent etc,were investigated by FAAS.Selectivity of the prepared Ni(Ⅱ) ion imprinted polymer in dilute aqueous solution was examined by ICP-AES.The mixed solution was consisted of Cd(Ⅱ),Co(Ⅱ),Cu(Ⅱ),Hg(Ⅱ),Mn(Ⅱ),Cu(Ⅱ), Pb(Ⅱ) and Zn(Ⅱ) ions.Finally,the imprint mechanism of Ni(Ⅱ) ions on Ni(Ⅱ) ion imprinted polymer was discussed in detail.The adsorption capacity of Ni(Ⅱ) ion imprinted and non-imprinted polymer particles were discussed,respectively.Ni(Ⅱ) ion imprinted polymer exhibited higher selectivity for Ni(Ⅱ) ions than non-imprinted polymer in the mixed aqueous solution.
The results indicated that the pre-concentration/separation of inorganic environmental hormones by titanate whisker has the disadvantage of poor selectivity.Titanate whisker was modified by surface ion imprinting technique and sol-gel process.The surface ion imprinted titanate polymer was used as the solid-phase extraction materials to pre-separation/ enrichment inorganic environmental hormone with high selectivity.The adsorption behavior and mechanism were also studied.
A new method for determination of trace Inorganic Environmental Hormones in environmental samples was established by combination of the SPE on surface ion imprinted titanate polymer and equipment directly through detection techniques.
钛基晶须材料具有特定强度、模量、尺寸稳定性等优良性能,不仅在光电材料方面有广泛的应用,而且在吸附、分离等领域也具有重要的应用价值。分子印迹技术是近年发展起来的制备对目标化合物具有特定识别能力的聚合物的新技术。本研究选择利用钛基晶须/表面修饰钛基晶须/表面离子印迹钛基晶须固相萃取无机环境激素。
本论文主要包括以下三个方面的内容:
(1)钛基晶须固相萃取预分离/富集无机环境激素的研究
ⅰ.以四钛酸钾(K_2Ti_4O_9)晶须为固相萃取剂,火焰原子吸收光谱法(FAAS)为检测手段,详细研究了K_2Ti_4O_9对无机环境激素铅、镉、镍的吸附行为,考察了共存离子的影响情况及可能的吸附机理。在优化的实验条件下,将其用于环境水样中Cd(Ⅱ)、Pb(Ⅱ)、Ni(Ⅱ)的测定,检出限分别为:2.5μg·L~(-1)、3.6μg·L~(-1)、56μg·L~(-1);相对标准偏差(RSD)分别为2.6%、3.1%、2.9%。结果表明,所提出的新方法具有稳定性好、吸附和解吸性能好的特点。
ⅱ.建立了一种以电感耦合等离子体原子发射光谱法(ICP-AES)为检测手段,六钛酸钾(K_2Ti_6O_(13))为固相萃取剂分离/富集Co(Ⅱ)、Ni(Ⅱ)、Cr(Ⅲ)的方法,探讨了影响分离/富集过程的主要因素、共存离子的干扰以及可能的吸附机理,考察了吸附容量。在优化的实验条件下,本法用于磷化废水中Co(Ⅱ)、Ni(Ⅱ)、Cr(Ⅲ)的测定,检出限分别为:9.2μg·L~(-1)、5.3μg·L~(-1)、8.9μg·L~(-1);相对标准偏差(RSD)分别为0.98%、0.75%、0.87%。结果表明:所提出的新方法具有稳定性好、吸附和解吸性能好的特点。
(2)钛基晶须表面修饰分离/富集无机环境激素研究
ⅰ.以K_2Ti_4O_9为载体,γ-(2、3环氧丙氧)丙基三甲氧基硅烷(KH-560)为表面修饰剂,溶胶-凝胶法(sol-gel)制备负载型、疏水性固相萃取剂KH-560/K_2Ti_4O_9。采用傅立叶变换红外光谱法(FF-IR)、扫描电镜(SEM)、X-射线衍射(XRD)对KH-560/K_2Ti_4O_9表面形貌和结构进行表征;以FAAS为检测手段,考察了吸附酸度、吸附剂用量、静置时间等对KH-560/K_2Ti_4O_9吸附Pb(Ⅱ)的影响;研究了在混合溶液中KH-560/K_2Ti_4O_9对Pb(Ⅱ)的选择性。结果表明:在K_2Ti_4O_9表面修饰KH-560可以有效增加K_2Ti_4O_9的疏水性能。
ⅱ.以六钛酸钾晶须(K_2Ti_6O_(13))为载体,采用浸渍法制备了双硫腙(Dithizone,C_(13)H_(12)N_4S)负载型六钛酸钾(C_(13)H_(12)N_4S/K_2Ti_6O_(13))。采用FT-IR、SEM对C_(13)H_(12)N_4S/K_2Ti_6O_(13)表面形貌和结构进行表征。以ICP-AES为检测手段,考察了吸附酸度、吸附剂用量、静置时间等对C_(13)H_(12)N_4S/K_2Ti_6O_(13)吸附Cd(Ⅱ)、Pb(Ⅱ)的影响。在优化的条件下,本法用于环境水样中Cd(Ⅱ)、Pb(Ⅱ)的测定,检出限为1.2μg·L~(-1)、1.6μg·L~(-1),加标回收率为92～101%。结果表明:C_(13)H_(12)N_4S/K_2Ti_6O_(13)可以有选择的吸附Cd(Ⅱ)、Pb(Ⅱ)等离子。
(3)钛基晶须表面离子印迹聚合物分离/富集无机环境激素研究
ⅰ.以Pb(Ⅱ)为模板离子,壳聚糖(CTS)为功能单体,三钛酸钠(Na_2Ti_3O_7)为载体,KH-560为偶联剂,利用表面分子印迹技术(SMIT)和溶胶-凝胶法(sol-gel)在稀醋酸溶液中制备了Pb(Ⅱ)离子印迹聚合物(Pb(Ⅱ)-ion Imprinted Polymer,Pb(Ⅱ)-ⅡP)。采用FT-IR、SEM、XRD等表征手段对Pb(Ⅱ)-ⅡP的表面形貌和结构进行表征;以FAAS为检测手段,考察了吸附酸度、吸附剂用量、吸附时间等对聚合物吸附性能的影响;研究了印迹聚合物在混合溶液中对Pb(Ⅱ)的选择性,比较了印迹和非印迹聚合物(Non imprinted polymer,NIP)的吸附容量;提出了印迹聚合物可能的印迹吸附机理。结果表明:Pb(Ⅱ)-ⅡP具有较好的疏水性能,对Pb(Ⅱ)离子具有较高的选择性。
ⅱ.在醋酸溶液中,以Ni(Ⅱ)为模板离子,CTS为功能单体,KH-560为偶联剂,利用表面印迹技术和溶胶-凝胶技术结合制备了Ni(Ⅱ)离子印迹聚合物(Ni(Ⅱ)-ion Imprinted Polymer,Ni(Ⅱ)-ⅡP)。采用FT-IR、SEM等手段对Ni(Ⅱ)-ⅡP的性质和结构进行了表征。并以其为固相萃取吸附剂,以FAAS为检测手段,考察了溶液酸度、吸附时间、吸附剂用量等对聚合物吸附性能的影响。采用ICP-AES研究了聚合物对Ni(Ⅱ)的选择性和吸附容量。对Ni(Ⅱ)-ⅡP的印迹机理进行了探讨。结果表明:Ni(Ⅱ)-ⅡP具有较高的选择性。
研究表明:钛基晶须分离/富集无机环境激素具有广谱性、选择性不理想等特性。对钛基晶须材料实施表面离子印迹,得到表面离子印迹改性钛基晶须固相萃取材料,用于预分离/富集样品中无机环境激素的研究,实现对无机环境激素专属性/高选择性吸附;研究了表面离子印迹改性钛基晶须材对无机环境激素的吸附行为和分离/富集机理。实现了表面离子印迹改性钛基晶须固相萃取材料预分离/富集与仪器分析方法联用,建立了环境样品中痕量/超痕量无机环境激素仪器分析新方法。
Environmental hormones,also known as environmental endocrine disrupters,are harmful chemical substances released into environment because of human activities and can disrupt biological endocrine system. Environmental hormones can be divided into organic environmental hormones and inorganic environmental hormones.Inorganic environmental hormones(IEHs) mainly include cadmium,lead,mercury,etc.Owing to restriction of selectivity and influence of samples,inorganic environmental hormones cannot be analyzed directly with equipment.Therefore, separation/enrichment of inorganic environmental hormones from samples is very important.Solid-phase extraction has gained attention of many analytic researchers for its several advantages,including operating simply, high pre-concentration factor,rapid phase separation,and the ability of combining with different detection techniques.
Titanate whisker materials have some good performances such as specific strength,modulus,dimensional stability,etc.It has widely application not only on photoelectric materials,but also on adsorption, separation and other fields.
In recent years,Molecular Imprinting Technique(MIT) has been developed as the new technology for the preparation of polymer with specific ability for identification of targeted compound.
In this work,IEHs were pre-concentration/separation by using whisker titanium/modified whisker titanium/surface ion imprinted titanate polymer as solid-phase extractant.
The work mainly included the following items:
(1) Study on the pre-concentration/separation of IEHs using titanate whisker as solid-phase extractant
ⅰ.The absorption behaviors of K_2Ti_4O_9 towards Cd(Ⅱ),Pb(Ⅱ), Ni(Ⅱ) using FAAS as sensitive detector was studied.Under optimum conditions,the possiblility of absorption mechanism was investigated and applied to the speciation analysis of Cd(Ⅱ),Pb(Ⅱ),Ni(Ⅱ) in environmental water samples and the detection limits were 2.5μg·L~(-1) with relative standard deviation(RSD) of 2.6%for Cd,3.6μg·L~(-1)with RSD of 3.1%for Pb and 56μg·L~(-1) with RSD of 2.9%for Ni,respectively.It was found that the proposed method used in the paper had many advantages such as good stability and good performance of absorption and desorption.
ⅱ.A new method was proposed for the separation/enrichment of Co(Ⅱ),Ni(Ⅱ),Cr(Ⅲ) using K_2Ti_6O_(13) as solid-phase extractant and ICP-AES as sensitive detector.The major factors influencing the process of separation and enrichment were investigated,including the interference of co-existing ions and the possible sorption mechanism.Under optimum conditions,the detection limits were 9.2μg·L~(-1) with relative standard deviation(RSD) of 0.98%for Co,5.3μg·L~(-1) with RSD of 0.75%for Ni and 8.9μg·L~(-1) with RSD of 0.87%for Cr,respectively.It was found that the proposed method used in the article had many advantages including good stability and good performance of absorption and desorption.The result showed that the method was suit for the analysis of industrial waste water samples.
(2) Study on the pre-concentration/separation of IEHs using surface modification -titanate whisker as solid-phase extractant
ⅰ.The new solid-phase extractant(KH-560/K_2Ti_4O_9) was prepared by using sol-gel method with KH-560 as the surface modification agent, K_2Ti_4O_9 as the carrier.KH-560/K_2Ti_4O_9 was characterized by using SEM, FI-IR、XRD.The absorption behavior of KH-560/K_2Ti_4O_9 towards Pb using FAAS as sensitive detector was studied.Under optimum conditions, the selectivity for Pb(Ⅱ) of KH-560/K_2Ti_4O_9 was also discussed in mixed aqueous solution.The detection limit was 2.5μg·L~(-1) with relative standard deviation(RSD) of 2.6%for Pb(Ⅱ),respectively.It was found that the surface modification of K_2Ti_4O_9 using KH-560 could effectively increase the hydrophobic properties.
ⅱ.In this paper,the C_(13)H_(12)N_4S/K_2Ti_6O_(13) as solid sorbent was prepared by using impregnation method,and characterized by using SEM、FI-IR.Effects of adsorption acidity,sorbent dosage and resting time on adsorption rate to Cd(Ⅱ),Pb(Ⅱ) on C_(13)H_(12)N_4S/K_2Ti_6O_(13) were investigated by ICP-AES.Under optimum conditions,the method was applied to the determination of real water samples,and the detection limits were 1.2μg·L~(-1),1.6μg·L~(-1) for Cd(Ⅱ) and Pb(Ⅱ),respectively.The results indicated that the C_(13)H_(12)N_4S/K_2Ti_6O_(13) can adsorb some ions like Cd(Ⅱ) and Pb(Ⅱ).
(3) Study on the pre-concentration/separation of IEHs using surface ion-imprinted titanate polymer as solid-phase extractant
ⅰ.The Pb(Ⅱ) ion imprinted polymer particles were prepared by surface molecular imprinting technique and sol-gel process in acetic acid solution,with Pb(Ⅱ) ion as the template,chitosan(CTS) as the functional monomer,Na_2Ti_3O_7 as the carder,and KH-560 as the crosslinking agent. The ion-imprinted polymer particles were characterized by FT-IR,XRD, SEM and TEM.Effects of adsorption acidity,sorbent dosage and resting time on adsorption rate were investigated by FAAS.Selectivity of the prepared polymer for Pb(Ⅱ) ions was also discussed in mixed aqueous solution.Adsorption capacity of Pb(Ⅱ)-ⅡP was compared with that of non-imprinted polymer(NIP).The imprint and adsorption mechanism were also put forward.The results indicated that Pb(Ⅱ)-ⅡP exhibited high selectivity for Pb(Ⅱ) ions and hydrophobic properties.
ⅱ.Ni(Ⅱ) ion imprinted polymer(Ni(Ⅱ)-ⅡP) particles was prepared by the combination of surface molecular imprinting technique and sol-gel process in acetic acid solution,with Ni(Ⅱ) ion as a template,CTS as functional monomer,and KH-560 as the cross-linker.The configuration of Ni(Ⅱ) ion imprinted polymer and its materials were characterized by FT-IR spectra,UV-spectra,SEM,TEM and XRD.The optimal adsorption conditions,such as acidity,resting time,amount of sorbent etc,were investigated by FAAS.Selectivity of the prepared Ni(Ⅱ) ion imprinted polymer in dilute aqueous solution was examined by ICP-AES.The mixed solution was consisted of Cd(Ⅱ),Co(Ⅱ),Cu(Ⅱ),Hg(Ⅱ),Mn(Ⅱ),Cu(Ⅱ), Pb(Ⅱ) and Zn(Ⅱ) ions.Finally,the imprint mechanism of Ni(Ⅱ) ions on Ni(Ⅱ) ion imprinted polymer was discussed in detail.The adsorption capacity of Ni(Ⅱ) ion imprinted and non-imprinted polymer particles were discussed,respectively.Ni(Ⅱ) ion imprinted polymer exhibited higher selectivity for Ni(Ⅱ) ions than non-imprinted polymer in the mixed aqueous solution.
The results indicated that the pre-concentration/separation of inorganic environmental hormones by titanate whisker has the disadvantage of poor selectivity.Titanate whisker was modified by surface ion imprinting technique and sol-gel process.The surface ion imprinted titanate polymer was used as the solid-phase extraction materials to pre-separation/ enrichment inorganic environmental hormone with high selectivity.The adsorption behavior and mechanism were also studied.
A new method for determination of trace Inorganic Environmental Hormones in environmental samples was established by combination of the SPE on surface ion imprinted titanate polymer and equipment directly through detection techniques.
引文
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