用于海洋碳酸盐体系参数测定的微电极的研制与应用
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摘要
碳酸盐体系是深海沉积物、海洋贝类生物微环境以及海底热液和冷泉研究的重要内容,对研究全球碳循环和全球气候变迁具有重要意义。利用化学传感器精确地确定各无机碳种类(包括CO2气体、碳酸氢根离子和碳酸根离子)的浓度,是研究海洋无机碳酸盐体系的核心技术手段之一。论文在pH电极的基础上,研制了溶解二氧化碳电极和碳酸根离子选择性电极,为确定海洋无机碳酸盐体系的溶解二氧化碳和碳酸根离子浓度,提供了理论基础与技术支持。
论文基于已有的制作海洋原位地球化学传感器的经验和工艺,制作了溶解二氧化碳电极。该电极的核心响应部位是pH电极,内电解质溶液为0.002mol/L NaHC03和3.5%NaCl的混合溶液,整个测试体系密封,仅通过聚四氟乙烯气透膜与被测溶液进行气体交换,从而改变内部体系的pH值。该电极在NaHC03溶液10-3mol/L～10-1mol/L的浓度区间内满足能斯特响应定律。然而,由于电极的响应过程主要受气体扩散作用控制,电极响应缓慢,可测试的线性区间有限。
为提高电极响应的灵敏性,扩展其可测线性区间,论文制作了基于有机复合膜的碳酸根离子选择性电极。该碳酸根离子选择性电极的膜溶液以胆酸衍生物为离子选择性敏感试剂,以三-十二烷基甲基氯化铵膜添加剂,以2-硝基苯基辛基醚为膜溶剂,以聚氯乙烯为增塑剂,该电极的内电解质溶液为pH约为9的硼酸盐与碳酸盐混合溶液。采用三种不同的溶液和标定方法分别对电极进行了标定,结果表明该电极的性能大大提高,其响应时间<30s,检测限在10-5mol/L～10-2.5mol/L。为了实现电极的集成封装与深海探测,使液膜型电极固态化：将Ag丝外表层涂覆聚二氧乙烯噻吩,固化后将前述液膜型电极的膜溶液涂覆至电极表面。该固态碳酸根离子选择性电极体积更小,具有高机械强度和韧性,工作性能重现性良好,但其能斯特方程的斜率未能符合能斯特定律。
为改进碳酸根离子选择性电极的性能,论文制作了基于锌铝型水滑石(ZA-LDH)为离子载体的微型C02电极。该电极采用pH Ir/IrOx电极为基材,其碳酸(氢)根离子敏感膜成份以共沉淀法自制的ZA-LDH为离子载体,以氯仿或四氢呋喃为溶剂,以硅烷偶联剂为表面活性剂,聚二甲基硅氧烷或聚氯乙烯为成膜剂。该电极对不同浓度的NaHC03和NaCl昆合溶液响应良好,其响应时间为30s-1min,检测限在10一4～10-1mol/L.
论文将基于有机复合膜的碳酸根离子选择性微电极应用于沉积物和珊瑚生长微环境的测试,得到沉积物-孔隙水界面以下和珊瑚口附近的高分辨率的pH和C032-离子浓度剖面。沉积物经过长时间培养,其深层缺乏氧气供给,同时微表层由于细菌的厌氧分解产生大量还原性硫化物,从而造成pH值和C032-离子浓度急剧下降。珊瑚生长受周围海水微环境的DIC和文石饱和度等因素的影响,这与珊瑚生长过程中需要大量C032-和Ca2+有关。上述结果表明,液膜型pH和碳酸根离子选择性微电极是测试沉积物和珊瑚等微环境良好的探针。基于锌铝型水滑石的微型CO2电极与其它pH、Eh、H2S及温度传感器构成传感器链,按一定轨迹在台湾东北部龟山岛热液区进行探测,获得了海底热液扩散流三维空间分布规律。并且将其中一组传感器应用于研究白色热泉,得到87h的pH、Eh、H2S、C032离子浓度及温度等化学、物理参数的原位观测序列。通过小波变换和经验模分解变换的方法,从原位观测时间序列中解析出潮汐周期。由于碳酸根离子选择性电极膜材料的耐酸性欠佳,仅得到不足24h的C032-离子浓度序列,但C032-离子电极从另一个角度(除Eh、H2S探测等)为寻找海底热液喷口给出了依据,同时为研究热液喷发对周围海洋环境影响提供了一种可行的方法。
Inorganic carbon system is an important part of studying deep sea sediment, shellfish microenvironment, and the hydrothermal and cold seep. It is also of great significance to study the global carbon cycle and the global climate change. To utilize chemical sensor to accurately determine the concentration of each inorganic carbon species (CO2gas, bicarbonate ions, and carbonate ions) is one technique for studying the ocean inorganic carbon system. This study fabricated the dissolved CO2electrodes and carbonate ion selective microelectrodes based on pH microelectrode. The microelectrodes were utilized to determine the concentration of the dissolved CO2and the carbonate ions in the ocean, and provide theoretical basis and technique support.
In view of the ready experience and technique to make the in-situ oceanic geochemicstry sensors, we made the dissolved CO2electrode based on the ready experience and technique to make oceanic in-situ geochemical sensor. The key part of the dissolved CO2electrode that response the electromotive force is Ir/IrOx pH electrode. The internal electrolyte of this electrode is0.002mol/L NaHCO3and3.5%NaCl mixed solution which was sealed. And this sealed system exchanged gas with external measured solution by polytetrafluoroethylene membrane through which only gas could permeate and altered the pH of the internal electrolyte. This electrode reponse by the Nernst Law in the range of10-3mol/L to10-1mol/L. However, the work process of dissolved CO2electrode is controled by the diffusion, and it severely slows the electrode response. And the available linear range of the electrode is limited.
This study also tried to make the carbonate ion selective microelectrodes based on the organic composed membrane hydrotalcite as for enhancing the response rapid and extending the available linear range. The carbonate ion selective electrode based on the organic composed membrane utilized cholic derivative as the ion selective sensitive reagent, tridodecylmethyl-ammonium chloride as membrane additive reagent,2-nitrophenyloctyl ether as membrane solvent, poly (vinyl chloride) as plastisizer, together to make the membrane solution. Borate and carbonate salt solution of pH9was the internal electrolyte. We calibrated the microelectrode applying three distinct solution and calibration methods. The results indicate that response time of the electrode is less than 30s, and the detection limitation is from10-5mol/L to10-2.5mol/L. For the purpose of realizing integration and package of the electrodes and detection in the deep ocean, we solidified the liquid membraned electrode:depositing poly (2,3-dihydrothieno-1,4-dioxin)-poly(styrenesulfonate) to Ag wire surface, coating the above-mentioned membrane solution to the electrode surface after it solidification. This solid carbonate ion selective electrode is more miniature, strong and robust in mechanical characteristics, and it performs good stability.
This study makes micro-CO2electrode based on Zinc aluminum type hydrotalcite (ZA-LDH) to improve the characteristic of the carbonate ion-selective microelectrode. We utilize pH Ir/IrOx electrode as the matrix. And the carbonate (or bicarbonate) ions sensitive membrane solution uses self-coprecipitated prepared ZA-LDH as carbonate ion carrier, chloroform or tetrahydrofuran as solvent, silane coupling agent as surface active agent, N,N-dimethyltrimethylsilylamine or poly (chloride vinyl) as membrane-forming agent. The calibration results show that the electrode response well to NaCl and different-concentration of NaHCO3mixed solutions. The response time is30s～1min, and the detection limitation is10-4～10-1mol/L.
We applied the carbonate ion selective electrode of organic composed membrane to study the sediment and the survival microenvironment of coral. High-resolution pH and CO32-profile under the sediment-porewater interface and arround the coral mouth were obtained. After long time cultivation, the sediment was lack in O2in the deep. pH and CO32-concentration drop quickly under the sediment-porewater interface due to a great deal of reductive sulfide produced by bacterial anaerobic decay. Coral survival need CO32-and Ca2+. And it is limited by the factors of DIC and aragonite saturation. All evidenced that liquid-membraned pH and CO32-microelectrodes are good indicatiors to reflect the microenvironment of the sediment and the coral. We also utilize the miniature ZA-LDH type CO2electrode, with pH、Eh、H2S and temperature sensor, to detect the hydrothermal at Kueishan Tao, Northeast of Taiwan. The three-dimensional spatial distribution of the seabed hydrothermal diffusion of the white spring vent were observed. We applied a set of sensor to study the white spring, and obtained87hours long chemical and physical parameter time series of of pH, Eh, H2S concentration、CO32-concentration and temperature. The tidal period is decomposed from the in-situ observation time series through wavelet transform analysis and empirical mode decomposition. However, only less than24hours CO32-concentration time series were obtained, due to the poor acid resistance of the membrane material. Besides Eh and H2S detection, the carbonate ion-selective electrode offers another evidence to in search of submarine hydrothermal vent, and provides an available method to study the erupted hydrothermal influence on the surrounding oceanic environment.
论文基于已有的制作海洋原位地球化学传感器的经验和工艺,制作了溶解二氧化碳电极。该电极的核心响应部位是pH电极,内电解质溶液为0.002mol/L NaHC03和3.5%NaCl的混合溶液,整个测试体系密封,仅通过聚四氟乙烯气透膜与被测溶液进行气体交换,从而改变内部体系的pH值。该电极在NaHC03溶液10-3mol/L～10-1mol/L的浓度区间内满足能斯特响应定律。然而,由于电极的响应过程主要受气体扩散作用控制,电极响应缓慢,可测试的线性区间有限。
为提高电极响应的灵敏性,扩展其可测线性区间,论文制作了基于有机复合膜的碳酸根离子选择性电极。该碳酸根离子选择性电极的膜溶液以胆酸衍生物为离子选择性敏感试剂,以三-十二烷基甲基氯化铵膜添加剂,以2-硝基苯基辛基醚为膜溶剂,以聚氯乙烯为增塑剂,该电极的内电解质溶液为pH约为9的硼酸盐与碳酸盐混合溶液。采用三种不同的溶液和标定方法分别对电极进行了标定,结果表明该电极的性能大大提高,其响应时间<30s,检测限在10-5mol/L～10-2.5mol/L。为了实现电极的集成封装与深海探测,使液膜型电极固态化：将Ag丝外表层涂覆聚二氧乙烯噻吩,固化后将前述液膜型电极的膜溶液涂覆至电极表面。该固态碳酸根离子选择性电极体积更小,具有高机械强度和韧性,工作性能重现性良好,但其能斯特方程的斜率未能符合能斯特定律。
为改进碳酸根离子选择性电极的性能,论文制作了基于锌铝型水滑石(ZA-LDH)为离子载体的微型C02电极。该电极采用pH Ir/IrOx电极为基材,其碳酸(氢)根离子敏感膜成份以共沉淀法自制的ZA-LDH为离子载体,以氯仿或四氢呋喃为溶剂,以硅烷偶联剂为表面活性剂,聚二甲基硅氧烷或聚氯乙烯为成膜剂。该电极对不同浓度的NaHC03和NaCl昆合溶液响应良好,其响应时间为30s-1min,检测限在10一4～10-1mol/L.
论文将基于有机复合膜的碳酸根离子选择性微电极应用于沉积物和珊瑚生长微环境的测试,得到沉积物-孔隙水界面以下和珊瑚口附近的高分辨率的pH和C032-离子浓度剖面。沉积物经过长时间培养,其深层缺乏氧气供给,同时微表层由于细菌的厌氧分解产生大量还原性硫化物,从而造成pH值和C032-离子浓度急剧下降。珊瑚生长受周围海水微环境的DIC和文石饱和度等因素的影响,这与珊瑚生长过程中需要大量C032-和Ca2+有关。上述结果表明,液膜型pH和碳酸根离子选择性微电极是测试沉积物和珊瑚等微环境良好的探针。基于锌铝型水滑石的微型CO2电极与其它pH、Eh、H2S及温度传感器构成传感器链,按一定轨迹在台湾东北部龟山岛热液区进行探测,获得了海底热液扩散流三维空间分布规律。并且将其中一组传感器应用于研究白色热泉,得到87h的pH、Eh、H2S、C032离子浓度及温度等化学、物理参数的原位观测序列。通过小波变换和经验模分解变换的方法,从原位观测时间序列中解析出潮汐周期。由于碳酸根离子选择性电极膜材料的耐酸性欠佳,仅得到不足24h的C032-离子浓度序列,但C032-离子电极从另一个角度(除Eh、H2S探测等)为寻找海底热液喷口给出了依据,同时为研究热液喷发对周围海洋环境影响提供了一种可行的方法。
Inorganic carbon system is an important part of studying deep sea sediment, shellfish microenvironment, and the hydrothermal and cold seep. It is also of great significance to study the global carbon cycle and the global climate change. To utilize chemical sensor to accurately determine the concentration of each inorganic carbon species (CO2gas, bicarbonate ions, and carbonate ions) is one technique for studying the ocean inorganic carbon system. This study fabricated the dissolved CO2electrodes and carbonate ion selective microelectrodes based on pH microelectrode. The microelectrodes were utilized to determine the concentration of the dissolved CO2and the carbonate ions in the ocean, and provide theoretical basis and technique support.
In view of the ready experience and technique to make the in-situ oceanic geochemicstry sensors, we made the dissolved CO2electrode based on the ready experience and technique to make oceanic in-situ geochemical sensor. The key part of the dissolved CO2electrode that response the electromotive force is Ir/IrOx pH electrode. The internal electrolyte of this electrode is0.002mol/L NaHCO3and3.5%NaCl mixed solution which was sealed. And this sealed system exchanged gas with external measured solution by polytetrafluoroethylene membrane through which only gas could permeate and altered the pH of the internal electrolyte. This electrode reponse by the Nernst Law in the range of10-3mol/L to10-1mol/L. However, the work process of dissolved CO2electrode is controled by the diffusion, and it severely slows the electrode response. And the available linear range of the electrode is limited.
This study also tried to make the carbonate ion selective microelectrodes based on the organic composed membrane hydrotalcite as for enhancing the response rapid and extending the available linear range. The carbonate ion selective electrode based on the organic composed membrane utilized cholic derivative as the ion selective sensitive reagent, tridodecylmethyl-ammonium chloride as membrane additive reagent,2-nitrophenyloctyl ether as membrane solvent, poly (vinyl chloride) as plastisizer, together to make the membrane solution. Borate and carbonate salt solution of pH9was the internal electrolyte. We calibrated the microelectrode applying three distinct solution and calibration methods. The results indicate that response time of the electrode is less than 30s, and the detection limitation is from10-5mol/L to10-2.5mol/L. For the purpose of realizing integration and package of the electrodes and detection in the deep ocean, we solidified the liquid membraned electrode:depositing poly (2,3-dihydrothieno-1,4-dioxin)-poly(styrenesulfonate) to Ag wire surface, coating the above-mentioned membrane solution to the electrode surface after it solidification. This solid carbonate ion selective electrode is more miniature, strong and robust in mechanical characteristics, and it performs good stability.
This study makes micro-CO2electrode based on Zinc aluminum type hydrotalcite (ZA-LDH) to improve the characteristic of the carbonate ion-selective microelectrode. We utilize pH Ir/IrOx electrode as the matrix. And the carbonate (or bicarbonate) ions sensitive membrane solution uses self-coprecipitated prepared ZA-LDH as carbonate ion carrier, chloroform or tetrahydrofuran as solvent, silane coupling agent as surface active agent, N,N-dimethyltrimethylsilylamine or poly (chloride vinyl) as membrane-forming agent. The calibration results show that the electrode response well to NaCl and different-concentration of NaHCO3mixed solutions. The response time is30s～1min, and the detection limitation is10-4～10-1mol/L.
We applied the carbonate ion selective electrode of organic composed membrane to study the sediment and the survival microenvironment of coral. High-resolution pH and CO32-profile under the sediment-porewater interface and arround the coral mouth were obtained. After long time cultivation, the sediment was lack in O2in the deep. pH and CO32-concentration drop quickly under the sediment-porewater interface due to a great deal of reductive sulfide produced by bacterial anaerobic decay. Coral survival need CO32-and Ca2+. And it is limited by the factors of DIC and aragonite saturation. All evidenced that liquid-membraned pH and CO32-microelectrodes are good indicatiors to reflect the microenvironment of the sediment and the coral. We also utilize the miniature ZA-LDH type CO2electrode, with pH、Eh、H2S and temperature sensor, to detect the hydrothermal at Kueishan Tao, Northeast of Taiwan. The three-dimensional spatial distribution of the seabed hydrothermal diffusion of the white spring vent were observed. We applied a set of sensor to study the white spring, and obtained87hours long chemical and physical parameter time series of of pH, Eh, H2S concentration、CO32-concentration and temperature. The tidal period is decomposed from the in-situ observation time series through wavelet transform analysis and empirical mode decomposition. However, only less than24hours CO32-concentration time series were obtained, due to the poor acid resistance of the membrane material. Besides Eh and H2S detection, the carbonate ion-selective electrode offers another evidence to in search of submarine hydrothermal vent, and provides an available method to study the erupted hydrothermal influence on the surrounding oceanic environment.
引文
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