放射性核素在固—液界面吸附行为研究
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摘要
放射性废物的安全处理和妥善处置是制约我国核能战略顺利实施的关键因素之一。开展放射性核素在固-液界面宏观吸附热力学、动力学行为,以及化学种态与微观结构变化规律等相关研究,是评价放射性核素在环境介质中物理化学行的基础。另外,放射性核素在固-液界面吸附行为研究可为高放废物地质处置库的性能评价和安全评价提供基础数据。本论文主要探讨放射性核素在凹凸棒石、石灰性土壤表面的相互作用机制；考察pH值、离子强度、腐殖酸、温度等因素对放射性核素在固-液界面上吸附种态、微观结构和机理等影响,构建放射性核素在固-液界面吸附模型和机理。
(1)利用连续电位滴定对凹凸棒石和高温活化凹凸棒石进行表面酸碱性质进行研究,计算凹凸棒石表面反应本征常数和表面位点密度。低pH值下凹凸棒石表面主要以离子交换位(=XNa/K)、可变电荷位点=SWOH,=SSOH和=SSOH2为主而高pH值下,=SWO-和=SSO-两种种态占主导。高温活化凹凸棒石表面在低pH范围内主要以=SSOH和=SWOH种态存在为主；而在高pH则可变电荷位点的去质子化位(=SSO-和=SWO-)占主导。
(2)考察了pH和离子强度对放射性核素在固-液界面吸附的影响。发现Th(Ⅳ)、Eu(Ⅲ)和U(Ⅵ)在固体材料(凹凸棒石、磁性凹凸棒石复合材料、土壤)上吸附受pH和离子强度显著,表明Th(Ⅳ)、Eu(Ⅲ)、U(Ⅵ)在固-液界面上吸附机理比较复杂,涉及表面配位、离子交换、静电作用和表面沉淀等多种吸附机理；而Cs(Ⅰ)在石灰性土壤上的吸附却几乎不受pH影响,受离子强度影响却较为强烈,影响次序为K+>Na+>Li+及Mg2+>Ca2+≈Na+。
(3)Th(Ⅳ)在凹凸棒石表面吸附主要以离子交换作用和内层配合作用为主；而在高温活化凹凸棒石表面上则主要形成内层配合物。两种单齿配合物=X2UO20和=SWOUO2(OH)0可描述U(Ⅵ)在凹凸棒石表面吸附行为,但=X2UO20,=SSOUO2+=SWOUO2CO3-及=SWOUO2(CO3)23-的组合亦可解释U(Ⅵ)在凹凸棒石上的吸附边界,说明U(Ⅵ)在固-液界面吸附机理非常复杂。相比U(Ⅵ)在凹凸棒石表面吸附,U(Ⅵ)在ATP/IOM复合材料上吸附种态发生明显的改变,其中无离子交换作用的贡献,主要形成内层配合物(=SSOUO2+和=SWOUO2(CO3)23-)。Eu(Ⅲ)在凹凸棒石表面上吸附种态主要为离子交换作用(=X3Eu0)、外层配合物(=SWOHEu3+)和内层配合物(=SOEu(OH)20)。
(4)腐殖酸可改变放射性核素在液相和固体表面的种态,从而影响或改变放射性核素在固-液界面上微观结构和吸附机理。低pH下,腐殖酸可促进放射性核素在固-液界面吸附；而高pH范围内,腐殖酸可能会表现出明显的抑制作用。HA的存在改变了Th(Ⅳ)在凹凸棒石表面吸附种态(=SSO-CO-HA-Th和=SSOTh)。当pH<4.0时,腐殖酸对Eu(Ⅲ)在凹凸棒石表面吸附有一定促进作用；而pH4.0-6.0范围内,腐殖酸却抑制Eu(Ⅲ)吸附；当pH高于7.0时,吸附率出现明显增大,但没有达到相同条件下二元体系的吸附水平。另外,腐殖酸的存在可促进Th(Ⅳ)和U(Ⅵ)在高温活化凹凸棒石和DCS表面上的解吸作用。
(5)利用EXAFS研究了不同pH值下HA-Eu(Ⅲ)的配位作用,发现中心原子Eu周围O原子构成的配位环境(第一配位壳层)明显随pH变化而发生改变,当pH值从1.76增大至9.50,R(Eu-O)从2.415A减小至2.360A,且配位数从9.94迅速减小至8.56。表明在低pH值下(pH<2.40),Eu原子的第一配位壳层O原子来源于水合氛围,而此时HA实际上没有参与Eu(Ⅲ)的配位作用：但随pH值升高HA逐渐参与配位作用,逐渐取代H2O的位置,导致R和N值的减小(6)EuLⅢ边EXAFS吸收谱证明HA介入次序不同可导致Eu(Ⅲ)在凹凸棒石表面微观结构的改变和吸附机理的变化。对于batch 1 (ATP+HA-Eu(Ⅲ)),原子间距R(Eu-O)大约为2.411A(N=11.91)：bacth 2 (Eu(Ⅲ)+HA--ATP)勺原子间距R(Eu-O)约为2.399A(N=11.66)；而batch 3的R(Eu-O)约为2.321A(N=8.866)。其中值得注意的是batch 3 (ATP+Eu(Ⅲ)--HA)的结构参数非常与二元体系(Eu(Ⅲ)+ATP)非常相似(R(Eu-O)=2.314A.N=8.24)：而batch 1和batch 2的结构参数相似。说明Eu(Ⅲ)在凹凸棒石表面上的吸附种态、空间构型和微观机理等随HA介入次序不同而发生根本性的变化。
(7)pH>6.0时,吸附体系中CO2存在与否对U(Ⅵ)的吸附有显著影响,红外和静态实验数据均表明土壤中碳酸盐组分对U(Ⅵ)吸附起到至关重要的作用。
The safety and reasonable treatment of radio-waste is a key factor for the Chinese nuclear power program. The speciation in environmental medium (include aqueous and solid speciation) could strongly affect radiounclides' dissolvability, biotoxicity, sorption and diffusion and so on. The studies on physiochemical behaviors of radionuclides on solid-water interface are of importance for the performance and safety assessment of high-level radioactive repository. In this work, the sorption of radionuclides on attapulgite (ATP) and calcareous soil (CS) was investigated under various physiochemical conditions (such as pH, ion strengthen, humic substances, temperature etc.) to discuss the sorption mechanism and speciation of radionuclides on solid-water interface combined advanced spectroscopies (EDS, XPS and EXAFS).
(1) Sorption site densities and intrinsic acidity constants of sorbents were studied here using continuous potential titration and surface complexation model. The results indicated that sorption sites of intrinsic ATP involved in sorption process were main ion exchange site (=XNa/K), strong site (=SSOH) and weak site (=SWOH), while only strong site (=SSOH) and weak site (=SWOH) were predominant for activated ATP.
(2) Influences of pH and ionic strength on radionuclides sorption onto solid-water interface were discussed in detail. Th(IV), Eu(III) and U(VI) sorption on solid-water interface were strongly dependent on pH and ionic strength indicating that the sorption mechanisms were actually complex, which may be attributed to the synergistic effects of ion exchange, surface complexation and surface precipitation. Cs(I) sorption on CS was influenced significantly by ionic strength, however, hardly independent of pH; and the foreign cations competed with Cs(I) in the following order: K+>Mg2+>Ca2+≈Na+>Li+
(3) Ion exchange reaction and inner-sphere complexes dominated Th(IV) sorption on ATP, but only inner-sphere complexes could be found for Th(VI) sorption on activated ATP. The sorption edges of U(Ⅵ) on ATP could be described well by monodentate complexes (=X2UO20 and=SWOUO2(OH)0) or the combination of four sorption speciation (=X2UO20,=SSOUO2+,=SWOUO2CO3-and=SWOUO2(CO3)23-). Compared with ATP, both sorption mechanism and speciation of U(VI) changed obviously, the prevalent speciation were both=SSOUO2+ and=SWOUO2(CO3)23- on ATP/IOM composites in the observed pH range. The sorption of Eu(III) might be expressed as =X3Eu0=SWOHEu3+(outer-sphere complexes) and=SOEu-OOC-/HA in the ternary Eu/HA/ATP system.
(4) Humic substances could influence radionuclides speciation in both aqueous and solid phases, and affect sorption process and mechanism of radionuclides at soli/water interface. The sorption of Th(IV) on activated ATP was obviously enhanced in ternary system (HA/ATP/Th(Ⅳ)); and both=SSOH-HA-Th and=SSOTh were the predominant speciation. In the presence of FA and HA. Eu(Ⅲ) sorption was enhanced at pH<4.0. decreased at pH range of 4.0-6.0. and then raised again above pH～7.0. It was very interesting to note that the humic acid could enhance the desorption of U(Ⅵ) from ATP and decarbonated calcareous soil surface.
(5) Eu LⅢedge EXAFS analysis demonstrated that the interatomic distance R (Eu-O) (first coordination shell) in binary HA-Eu(Ⅲ) system decreased from 2.415 to 2.360 (?) with increasing pH from 1.76 to 9.50. and the coordination number (N) also reduced from 9.94 to 8.56. It can be attributed to the contribution of the hydration sphere Eu-OH2 and the carboxylate groups Eu-O(HA). The measured distances of 2.415 (?) (N=9.94) at pH 1.76 and 2.395 (?) (N=9.97) at pH 2.85 are attributed to the hydration inner-sphere Eu-OH_2, which suggests that HA does not participated in forming complexes with Eu3+. As pH increasing, the coordination positions of H2O were replaced by HA molecule resulting in the decreasing of N and R.
(6) The influence of humic acid addition sequence on radionuclides sorption mechanism is always controversy. The mean R(Eu-O) were 2.411 (?) (N=11.91) for batch 1 (ATP+HA—Eu(Ⅲ)),2.399 (?) (N=11.66) for batch 2(Eu(III)+HA-ATP).2.321 (?) (N=8.866) for batch 3 (Eu(III)+ATP-HA), and 2.314 (?) (N=8.24) for binary system(Eu(III)+ATP) at pH 4.50. The mean R(Eu-O) and N decreased slightly from batch 1 to batch 3. N and d (Eu-O) of batch 1 and 2 were very close to each other, whereas those of d (Eu-O) and N of batch 3 and binary Eu/attapulgite system were similar because Eu(Ⅲ) was adsorbed on attapulgite firstly in batch 3, which suggested that the configuration of Eu(Ⅲ) were different in various addition sequences of HA.
(7) Above pH～6.0, the CO2 and carbonates component of calcareous soil had obvious influence and attribution on U(Ⅵ) sorption speciation and mechanism.
(1)利用连续电位滴定对凹凸棒石和高温活化凹凸棒石进行表面酸碱性质进行研究,计算凹凸棒石表面反应本征常数和表面位点密度。低pH值下凹凸棒石表面主要以离子交换位(=XNa/K)、可变电荷位点=SWOH,=SSOH和=SSOH2为主而高pH值下,=SWO-和=SSO-两种种态占主导。高温活化凹凸棒石表面在低pH范围内主要以=SSOH和=SWOH种态存在为主；而在高pH则可变电荷位点的去质子化位(=SSO-和=SWO-)占主导。
(2)考察了pH和离子强度对放射性核素在固-液界面吸附的影响。发现Th(Ⅳ)、Eu(Ⅲ)和U(Ⅵ)在固体材料(凹凸棒石、磁性凹凸棒石复合材料、土壤)上吸附受pH和离子强度显著,表明Th(Ⅳ)、Eu(Ⅲ)、U(Ⅵ)在固-液界面上吸附机理比较复杂,涉及表面配位、离子交换、静电作用和表面沉淀等多种吸附机理；而Cs(Ⅰ)在石灰性土壤上的吸附却几乎不受pH影响,受离子强度影响却较为强烈,影响次序为K+>Na+>Li+及Mg2+>Ca2+≈Na+。
(3)Th(Ⅳ)在凹凸棒石表面吸附主要以离子交换作用和内层配合作用为主；而在高温活化凹凸棒石表面上则主要形成内层配合物。两种单齿配合物=X2UO20和=SWOUO2(OH)0可描述U(Ⅵ)在凹凸棒石表面吸附行为,但=X2UO20,=SSOUO2+=SWOUO2CO3-及=SWOUO2(CO3)23-的组合亦可解释U(Ⅵ)在凹凸棒石上的吸附边界,说明U(Ⅵ)在固-液界面吸附机理非常复杂。相比U(Ⅵ)在凹凸棒石表面吸附,U(Ⅵ)在ATP/IOM复合材料上吸附种态发生明显的改变,其中无离子交换作用的贡献,主要形成内层配合物(=SSOUO2+和=SWOUO2(CO3)23-)。Eu(Ⅲ)在凹凸棒石表面上吸附种态主要为离子交换作用(=X3Eu0)、外层配合物(=SWOHEu3+)和内层配合物(=SOEu(OH)20)。
(4)腐殖酸可改变放射性核素在液相和固体表面的种态,从而影响或改变放射性核素在固-液界面上微观结构和吸附机理。低pH下,腐殖酸可促进放射性核素在固-液界面吸附；而高pH范围内,腐殖酸可能会表现出明显的抑制作用。HA的存在改变了Th(Ⅳ)在凹凸棒石表面吸附种态(=SSO-CO-HA-Th和=SSOTh)。当pH<4.0时,腐殖酸对Eu(Ⅲ)在凹凸棒石表面吸附有一定促进作用；而pH4.0-6.0范围内,腐殖酸却抑制Eu(Ⅲ)吸附；当pH高于7.0时,吸附率出现明显增大,但没有达到相同条件下二元体系的吸附水平。另外,腐殖酸的存在可促进Th(Ⅳ)和U(Ⅵ)在高温活化凹凸棒石和DCS表面上的解吸作用。
(5)利用EXAFS研究了不同pH值下HA-Eu(Ⅲ)的配位作用,发现中心原子Eu周围O原子构成的配位环境(第一配位壳层)明显随pH变化而发生改变,当pH值从1.76增大至9.50,R(Eu-O)从2.415A减小至2.360A,且配位数从9.94迅速减小至8.56。表明在低pH值下(pH<2.40),Eu原子的第一配位壳层O原子来源于水合氛围,而此时HA实际上没有参与Eu(Ⅲ)的配位作用：但随pH值升高HA逐渐参与配位作用,逐渐取代H2O的位置,导致R和N值的减小(6)EuLⅢ边EXAFS吸收谱证明HA介入次序不同可导致Eu(Ⅲ)在凹凸棒石表面微观结构的改变和吸附机理的变化。对于batch 1 (ATP+HA-Eu(Ⅲ)),原子间距R(Eu-O)大约为2.411A(N=11.91)：bacth 2 (Eu(Ⅲ)+HA--ATP)勺原子间距R(Eu-O)约为2.399A(N=11.66)；而batch 3的R(Eu-O)约为2.321A(N=8.866)。其中值得注意的是batch 3 (ATP+Eu(Ⅲ)--HA)的结构参数非常与二元体系(Eu(Ⅲ)+ATP)非常相似(R(Eu-O)=2.314A.N=8.24)：而batch 1和batch 2的结构参数相似。说明Eu(Ⅲ)在凹凸棒石表面上的吸附种态、空间构型和微观机理等随HA介入次序不同而发生根本性的变化。
(7)pH>6.0时,吸附体系中CO2存在与否对U(Ⅵ)的吸附有显著影响,红外和静态实验数据均表明土壤中碳酸盐组分对U(Ⅵ)吸附起到至关重要的作用。
The safety and reasonable treatment of radio-waste is a key factor for the Chinese nuclear power program. The speciation in environmental medium (include aqueous and solid speciation) could strongly affect radiounclides' dissolvability, biotoxicity, sorption and diffusion and so on. The studies on physiochemical behaviors of radionuclides on solid-water interface are of importance for the performance and safety assessment of high-level radioactive repository. In this work, the sorption of radionuclides on attapulgite (ATP) and calcareous soil (CS) was investigated under various physiochemical conditions (such as pH, ion strengthen, humic substances, temperature etc.) to discuss the sorption mechanism and speciation of radionuclides on solid-water interface combined advanced spectroscopies (EDS, XPS and EXAFS).
(1) Sorption site densities and intrinsic acidity constants of sorbents were studied here using continuous potential titration and surface complexation model. The results indicated that sorption sites of intrinsic ATP involved in sorption process were main ion exchange site (=XNa/K), strong site (=SSOH) and weak site (=SWOH), while only strong site (=SSOH) and weak site (=SWOH) were predominant for activated ATP.
(2) Influences of pH and ionic strength on radionuclides sorption onto solid-water interface were discussed in detail. Th(IV), Eu(III) and U(VI) sorption on solid-water interface were strongly dependent on pH and ionic strength indicating that the sorption mechanisms were actually complex, which may be attributed to the synergistic effects of ion exchange, surface complexation and surface precipitation. Cs(I) sorption on CS was influenced significantly by ionic strength, however, hardly independent of pH; and the foreign cations competed with Cs(I) in the following order: K+>Mg2+>Ca2+≈Na+>Li+
(3) Ion exchange reaction and inner-sphere complexes dominated Th(IV) sorption on ATP, but only inner-sphere complexes could be found for Th(VI) sorption on activated ATP. The sorption edges of U(Ⅵ) on ATP could be described well by monodentate complexes (=X2UO20 and=SWOUO2(OH)0) or the combination of four sorption speciation (=X2UO20,=SSOUO2+,=SWOUO2CO3-and=SWOUO2(CO3)23-). Compared with ATP, both sorption mechanism and speciation of U(VI) changed obviously, the prevalent speciation were both=SSOUO2+ and=SWOUO2(CO3)23- on ATP/IOM composites in the observed pH range. The sorption of Eu(III) might be expressed as =X3Eu0=SWOHEu3+(outer-sphere complexes) and=SOEu-OOC-/HA in the ternary Eu/HA/ATP system.
(4) Humic substances could influence radionuclides speciation in both aqueous and solid phases, and affect sorption process and mechanism of radionuclides at soli/water interface. The sorption of Th(IV) on activated ATP was obviously enhanced in ternary system (HA/ATP/Th(Ⅳ)); and both=SSOH-HA-Th and=SSOTh were the predominant speciation. In the presence of FA and HA. Eu(Ⅲ) sorption was enhanced at pH<4.0. decreased at pH range of 4.0-6.0. and then raised again above pH～7.0. It was very interesting to note that the humic acid could enhance the desorption of U(Ⅵ) from ATP and decarbonated calcareous soil surface.
(5) Eu LⅢedge EXAFS analysis demonstrated that the interatomic distance R (Eu-O) (first coordination shell) in binary HA-Eu(Ⅲ) system decreased from 2.415 to 2.360 (?) with increasing pH from 1.76 to 9.50. and the coordination number (N) also reduced from 9.94 to 8.56. It can be attributed to the contribution of the hydration sphere Eu-OH2 and the carboxylate groups Eu-O(HA). The measured distances of 2.415 (?) (N=9.94) at pH 1.76 and 2.395 (?) (N=9.97) at pH 2.85 are attributed to the hydration inner-sphere Eu-OH_2, which suggests that HA does not participated in forming complexes with Eu3+. As pH increasing, the coordination positions of H2O were replaced by HA molecule resulting in the decreasing of N and R.
(6) The influence of humic acid addition sequence on radionuclides sorption mechanism is always controversy. The mean R(Eu-O) were 2.411 (?) (N=11.91) for batch 1 (ATP+HA—Eu(Ⅲ)),2.399 (?) (N=11.66) for batch 2(Eu(III)+HA-ATP).2.321 (?) (N=8.866) for batch 3 (Eu(III)+ATP-HA), and 2.314 (?) (N=8.24) for binary system(Eu(III)+ATP) at pH 4.50. The mean R(Eu-O) and N decreased slightly from batch 1 to batch 3. N and d (Eu-O) of batch 1 and 2 were very close to each other, whereas those of d (Eu-O) and N of batch 3 and binary Eu/attapulgite system were similar because Eu(Ⅲ) was adsorbed on attapulgite firstly in batch 3, which suggested that the configuration of Eu(Ⅲ) were different in various addition sequences of HA.
(7) Above pH～6.0, the CO2 and carbonates component of calcareous soil had obvious influence and attribution on U(Ⅵ) sorption speciation and mechanism.
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