海底热液探测的电化学传感器制备与海上试验应用研究
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摘要
近年来,化学传感器应用于海洋领域的在线测量越来越受到重视。本课题研究主要针对pH传感器的改进和实验室性能测试,以及课题组研制的包括改进后的pH电极的多参数化学传感器系统在深海、浅海多个热液系统的海试研究结果。研究结果对如何结合化学传感器的实验室研究成果,与化学传感器在海洋在线测量领域的应用研究方面,具有重要实践意义。
pH值作为表征深海热液环境以及扩散流区域溶液化学性能的基本参数,是实现化学传感器在线测量的基础问题,受到海洋科学研究者的广泛关注。以前试制的电化学原位传感器,在实际海试中虽然对海底异常信号有响应,但由于电极信号的不稳定因素,限制了电极在海洋领域的应用范围。本研究基于熔融碳酸锂氧化金属原理,提出了改进传统熔融碳酸锂法制备IrOx电极的方法。对改进后IrOx电极的性能测试与相应的表面扫描电镜测试发现,改进方法后电极保持了原电极的优点,并在各响应性能方面都有显著提高。特别是熔融碳酸锂混合过氧化钠制备的IrOx电极,具备重复性好,在大跨度pH溶液之间的响应快速稳定,长时问连续监测的漂移小于5mV,同一批次所制备电极性能几乎相同,使用寿命长等优点。实验室测试研究发现,熔融碳酸锂混合过氧化钠方法制备的IrOx电极不仅在常温常压和高压,室温到90℃条件下,可作为可靠的pH电极使用,在高压、100～150℃条件下,也具备成为可靠pH电极的可能性。
基于电极在实验室的测试研究成果,集成了实验室自行开发的Eh、Ag/Ag2S和pH电极,组成了多参数化学传感器,在深海和浅海热液地区寻找活动热液喷口和对热液羽状流三维结构分布调查等领域进行了海上试验研究。在寻找热液喷口的海上试验研究中,集成了Eh、Ag/Ag2S和pH电极的多参数化学传感器首次在大洋一号20航次的洋中脊地区热液调查中,在东太平洋中脊(EPR)赤道区域和西南印度洋中脊(SWIR)的60条测线中投入使用,其中有效测线55条,共在29条测线上发现存在或可能存在的热液异常,获得了一批珍贵数据。在台湾龟山岛地区寻找新热液口过程中,多参数化学传感器组成的传感器链在拖曳航线中获得了一系列与热液活动相对应的化学异常信号,确定了几处可能存在热液口的地区,获得了一批有效数据,并确定了下一步进行再拖曳的几个目标位置。海试研究表明,应用多参数化学传感器探测化学异常进行海底热液探测,是一种有效的方法。电极可灵敏地检测出由热液异常引起的化学量变化,并在长达半年的多次使用中表现出其稳定性好、寿命长的特点。多参数化学传感器系统已作为大洋一号的常规设备使用。
集成了Eh和pH电极的多参数化学传感器在对龟山岛地区对浅海型热液口典型羽状流的三维结构分布调查应用中,第一次比较完整地获得了典型的黄泉口和白泉口羽状流结构的pH与Eh的三维等值线图。通过对黄泉口和白泉口上方羽状流区域拖曳数据的处理分析发现,热液对周边海域的影响不仅局限在热液口附近的底层水域,更多地是附近海域海水的表层。这项工作,为进一步开展该地区生态、化学环境等研究工作,提供了重要的基础资料。
In recent years, application of chemical sensors in in-situ measurement has attracted more and more attentions in marine science. This study is focused on the preparation improvement, lab-test of pH electrode, and application of lab-developed multi-parameter chemical sensors in in-situ measurements in deep-sea and shallow water hydrothermal systems.
pH is a fundamental parameter in understanding the chemical processes in hydrothermal vents and diffuse flow systems. Hence, accurate access of in-situ pH is a common concern of marine scientists. Although signals have been acquired by the former pH electrodes, the drifting problem greatly constrain the application of them. Improvements on preparation of IrOx electrode have been proposed based on the mechanism of molten alkali metal carbonate. Results of lab-experiments and SEM surface analysis indicate that the response characteristics of the improved IrOx electrode are better, including good reproducibility and sensitivity, small OCP(open circuit potential) drift (<5mV) of7-day continuous measurement, long life time and remarkable agreement with respect to potential/pH slopes and apparent standard electrode potentials of electrodes from the same batch. Good results of lab-test permit IrOx electrode prepared by molten mixed carbonate lithium with sodium peroxide be suitable for in-situ pH measurement at pressures up to50MPa and temperatures up to90℃. Furthermore, the IrOx electrode could be potentially used at temperatures up to150℃.
Based on the good results of lab-test, multi-parameter chemical sensor, which integrates Eh, Ag/Ag2S and pH electrode, has been applied in several marine investigations, including hydrothermal detection in deep-sea and shallow water systems. During applications in DY115-20Cruise, Dayangyihao Research Vessel, multi-parameter chemical sensor has measured60times in both East Pacific Ridge (EPR) and Southwest Indian Ridge (SWIR). Among the60measurements,55groups of valid data were gained, in which29records indicate potential active hydrothermal vents. Besides, the electrodes exhibit good sensitivity, stability and long lifetime during the six-month measurements. Multi-parameter chemical sensor system has become a common instrument in Dayangyihao Research Vessel. During the investigation on detecting hydrothermal vents in Kueishan Tao area, batches of valid chemical data, which are in good agreement with anomalies caused by hydrothermal vent fluids, were acquired by the multi-parameter sensor chain. Potential spots of new hydrothermal vents have been inferred according to the in-situ chemical measurements. It has been proved by sea trial results on many occasions that the multi-parameter chemical sensor can help detecting the chemical anomalies of the plumes. The chemical sensor system is an effective tool in hydrothermal activity detection.
Chemical sensor system integrating Eh and pH electrodes was used to measure the structure of hydrothermal plume at shallow-water hydrothermal vents in Kueishan Tao area, Taiwan. Three dimensional distributions of pH and Eh were firstly acquired at two typical types of hydrothermal plumes. Investigation reveals that the influence of hydrothermal is not limited in vicinity of hydrothermal vents, but on the total water column with most pronounced layers at the surface.
pH值作为表征深海热液环境以及扩散流区域溶液化学性能的基本参数,是实现化学传感器在线测量的基础问题,受到海洋科学研究者的广泛关注。以前试制的电化学原位传感器,在实际海试中虽然对海底异常信号有响应,但由于电极信号的不稳定因素,限制了电极在海洋领域的应用范围。本研究基于熔融碳酸锂氧化金属原理,提出了改进传统熔融碳酸锂法制备IrOx电极的方法。对改进后IrOx电极的性能测试与相应的表面扫描电镜测试发现,改进方法后电极保持了原电极的优点,并在各响应性能方面都有显著提高。特别是熔融碳酸锂混合过氧化钠制备的IrOx电极,具备重复性好,在大跨度pH溶液之间的响应快速稳定,长时问连续监测的漂移小于5mV,同一批次所制备电极性能几乎相同,使用寿命长等优点。实验室测试研究发现,熔融碳酸锂混合过氧化钠方法制备的IrOx电极不仅在常温常压和高压,室温到90℃条件下,可作为可靠的pH电极使用,在高压、100～150℃条件下,也具备成为可靠pH电极的可能性。
基于电极在实验室的测试研究成果,集成了实验室自行开发的Eh、Ag/Ag2S和pH电极,组成了多参数化学传感器,在深海和浅海热液地区寻找活动热液喷口和对热液羽状流三维结构分布调查等领域进行了海上试验研究。在寻找热液喷口的海上试验研究中,集成了Eh、Ag/Ag2S和pH电极的多参数化学传感器首次在大洋一号20航次的洋中脊地区热液调查中,在东太平洋中脊(EPR)赤道区域和西南印度洋中脊(SWIR)的60条测线中投入使用,其中有效测线55条,共在29条测线上发现存在或可能存在的热液异常,获得了一批珍贵数据。在台湾龟山岛地区寻找新热液口过程中,多参数化学传感器组成的传感器链在拖曳航线中获得了一系列与热液活动相对应的化学异常信号,确定了几处可能存在热液口的地区,获得了一批有效数据,并确定了下一步进行再拖曳的几个目标位置。海试研究表明,应用多参数化学传感器探测化学异常进行海底热液探测,是一种有效的方法。电极可灵敏地检测出由热液异常引起的化学量变化,并在长达半年的多次使用中表现出其稳定性好、寿命长的特点。多参数化学传感器系统已作为大洋一号的常规设备使用。
集成了Eh和pH电极的多参数化学传感器在对龟山岛地区对浅海型热液口典型羽状流的三维结构分布调查应用中,第一次比较完整地获得了典型的黄泉口和白泉口羽状流结构的pH与Eh的三维等值线图。通过对黄泉口和白泉口上方羽状流区域拖曳数据的处理分析发现,热液对周边海域的影响不仅局限在热液口附近的底层水域,更多地是附近海域海水的表层。这项工作,为进一步开展该地区生态、化学环境等研究工作,提供了重要的基础资料。
In recent years, application of chemical sensors in in-situ measurement has attracted more and more attentions in marine science. This study is focused on the preparation improvement, lab-test of pH electrode, and application of lab-developed multi-parameter chemical sensors in in-situ measurements in deep-sea and shallow water hydrothermal systems.
pH is a fundamental parameter in understanding the chemical processes in hydrothermal vents and diffuse flow systems. Hence, accurate access of in-situ pH is a common concern of marine scientists. Although signals have been acquired by the former pH electrodes, the drifting problem greatly constrain the application of them. Improvements on preparation of IrOx electrode have been proposed based on the mechanism of molten alkali metal carbonate. Results of lab-experiments and SEM surface analysis indicate that the response characteristics of the improved IrOx electrode are better, including good reproducibility and sensitivity, small OCP(open circuit potential) drift (<5mV) of7-day continuous measurement, long life time and remarkable agreement with respect to potential/pH slopes and apparent standard electrode potentials of electrodes from the same batch. Good results of lab-test permit IrOx electrode prepared by molten mixed carbonate lithium with sodium peroxide be suitable for in-situ pH measurement at pressures up to50MPa and temperatures up to90℃. Furthermore, the IrOx electrode could be potentially used at temperatures up to150℃.
Based on the good results of lab-test, multi-parameter chemical sensor, which integrates Eh, Ag/Ag2S and pH electrode, has been applied in several marine investigations, including hydrothermal detection in deep-sea and shallow water systems. During applications in DY115-20Cruise, Dayangyihao Research Vessel, multi-parameter chemical sensor has measured60times in both East Pacific Ridge (EPR) and Southwest Indian Ridge (SWIR). Among the60measurements,55groups of valid data were gained, in which29records indicate potential active hydrothermal vents. Besides, the electrodes exhibit good sensitivity, stability and long lifetime during the six-month measurements. Multi-parameter chemical sensor system has become a common instrument in Dayangyihao Research Vessel. During the investigation on detecting hydrothermal vents in Kueishan Tao area, batches of valid chemical data, which are in good agreement with anomalies caused by hydrothermal vent fluids, were acquired by the multi-parameter sensor chain. Potential spots of new hydrothermal vents have been inferred according to the in-situ chemical measurements. It has been proved by sea trial results on many occasions that the multi-parameter chemical sensor can help detecting the chemical anomalies of the plumes. The chemical sensor system is an effective tool in hydrothermal activity detection.
Chemical sensor system integrating Eh and pH electrodes was used to measure the structure of hydrothermal plume at shallow-water hydrothermal vents in Kueishan Tao area, Taiwan. Three dimensional distributions of pH and Eh were firstly acquired at two typical types of hydrothermal plumes. Investigation reveals that the influence of hydrothermal is not limited in vicinity of hydrothermal vents, but on the total water column with most pronounced layers at the surface.
引文
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