CN102590540A - In-situ detection system for concentration of deep sea micro-ions - Google Patents
In-situ detection system for concentration of deep sea micro-ions Download PDFInfo
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- CN102590540A CN102590540A CN2012100335805A CN201210033580A CN102590540A CN 102590540 A CN102590540 A CN 102590540A CN 2012100335805 A CN2012100335805 A CN 2012100335805A CN 201210033580 A CN201210033580 A CN 201210033580A CN 102590540 A CN102590540 A CN 102590540A
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Abstract
The invention relates to an in-situ detection system for concentration of deep sea micro-ions. The in-situ detection system comprises two sub-systems including a liquid path system and a control system. According to the system, a flow injection analysis technology is taken as an automatic continuous flow analysis method to realize feeding, mixed reaction and automation of detection, and the system has four working modes including calibration, detection, flushing and standby, the self-maintenance flushing and calibration are realized, and the system can be resided in the deep sea environment to carry out the in-situ detection. A liquid core waveguide with the length of 5 meters is taken as a detection pool of the system, so that the pre-concentration or pre-enrichment process in the conventional detection method is reduced, the system is simplified, the detection efficiency is improved, the sample consumption is decreased, the sensitivity of the system is effectively increased, and the detection limit is lowered, and the system is suitable for detecting the trace elements in the deep sea.
Description
Technical Field
The invention relates to the field of deep sea detection electromechanical equipment, in particular to a deep sea trace ion concentration in-situ detection system capable of in-situ detecting the concentration of seawater ions in a deep sea environment for a long time.
Background
The concentration change of the trace elements such as iron, manganese, copper, cobalt, aluminum and the like in the deep sea water can influence the processes of chloroplast photosynthesis, animal and plant respiration, biosynthesis, nitrate and nitrite reduction and the like in the sea water, thereby influencing the ecological balance of the sea and the carbon cycle in the global environment, and the detection of the concentration of the trace elements in the deep sea water becomes the focus of the international ocean community. The traditional detection method of the trace elements in the seawater comprises the steps of sampling at regular time or irregular time by using an investigation ship, pretreating a sample, sealing, storing at low temperature, and transferring to a land laboratory for chemical detection; or the sample is collected and then detected on a sea ship. Both methods need to invest a large amount of manpower and material resources, and pollutants may be introduced in sampling, preprocessing and storing links of the sample, so that the sample is polluted and the true value of the ion concentration cannot be reflected; another disadvantage of both methods is that only discrete limited data is available and no real-time data with high spatial and temporal resolution is available. In addition, due to the extremely low content of trace elements in seawater, the traditional method needs to perform pre-concentration or pre-enrichment treatment on samples during detection, so that the operation link of detection is increased, a large amount of seawater samples need to be consumed, and the detection efficiency is not high. Therefore, the deep sea trace element in-situ detection system with simple research operation, quick analysis, high sensitivity and low detection limit is the development direction of marine geochemical detection.
Disclosure of Invention
The invention aims to provide an in-situ detection system for the concentration of trace ions in deep sea aiming at the defects of the prior art, and the in-situ detection system for the concentration of trace ions in deep sea has the advantages of simple operation, quick analysis, high sensitivity, low detection limit, self-maintenance flushing and calibration functions, and capability of in-situ detecting the concentration of trace ions in the sea in a deep sea environment for a long time.
The purpose of the invention is realized by the following technical scheme: an in-situ detection system for deep sea trace ion concentration comprises a liquid path system and a control system; wherein,
the fluid path system includes: seven reagent bags, eight filter screens, eight electromagnetic valves, an electromagnetic valve seat, three metering pumps, two chemical reaction coils, two light-liquid couplers, a liquid core waveguide tube, a detector, a light source and the like; the first reagent bag 1 is connected with an inlet of a first electromagnetic valve, the second reagent bag is connected with an inlet of a second electromagnetic valve, the third reagent bag is connected with an inlet of a third electromagnetic valve, the fourth reagent bag is connected with an inlet of a fifth electromagnetic valve, the fifth reagent bag is connected with an inlet of a sixth electromagnetic valve, the sixth reagent bag is connected with an inlet of a seventh electromagnetic valve, the seventh reagent bag is connected with an inlet of an eighth electromagnetic valve, a filter screen is arranged at the inlet of each electromagnetic valve, outlets of the first electromagnetic valve and the second electromagnetic valve are connected with an inlet of a first metering pump, an outlet of the third electromagnetic valve is connected with an inlet of a second metering pump, outlets of the fourth electromagnetic valve, the fifth electromagnetic valve, the sixth electromagnetic valve, the seventh electromagnetic valve and the eighth electromagnetic valve are connected with an inlet of a third metering pump, and eight electromagnetic valves are all arranged on an electromagnetic valve seat; outlets of the second metering pump and the third metering pump are connected with one end of a first chemical reaction coil, the other end of the first chemical reaction coil and an outlet of the first metering pump are connected with one end of a second chemical reaction coil, the other end of the second chemical reaction coil is sequentially connected with a first light-liquid coupler, a liquid core waveguide tube and a second light-liquid coupler, the first light-liquid coupler is connected with a light source through an optical fiber, and the second light-liquid coupler is connected with a detector through an optical fiber;
the control system includes: the system comprises a controller unit, a real-time clock, a memory card, a digital acquisition card, an energy supply module, a power supply conversion module, a pump valve control panel and the like; the energy supply module supplies power to the controller unit and the pump valve control panel through the power supply conversion module, the real-time clock and the storage card are all connected with the controller unit, the light source, the eight electromagnetic valves and the three metering pumps of the liquid path system are all connected with the pump valve control panel, the pump valve control panel is connected with the digital acquisition card, and the digital acquisition card and the detector of the liquid path system are all connected with the controller unit through the USB interface.
The invention has the beneficial effects that: the deep sea trace ion concentration in-situ detection system adopts the liquid core waveguide tube to increase the optical path length of light, greatly improves the sensitivity of sample detection and reduces the detection limit without a preconcentration or preconcentration link of the traditional detection method, simplifies the design of a liquid path system and improves the sample processing capacity; the flow injection analysis technology is adopted as an automatic continuous flow analysis method, and the system has four working modes of calibration, detection, flushing and standby, has the functions of self-maintenance flushing and calibration, and can be used for detection in a deep sea environment for a long time.
Drawings
FIG. 1 is a schematic view of a fluid path system of the present invention;
FIG. 2 is a schematic view of the control system of the present invention;
in the figure, a first reagent bag 1, a second reagent bag 2, a third reagent bag 3, a fourth reagent bag 4, a fifth reagent bag 5, a sixth reagent bag 6, a seventh reagent bag 7, a filter screen 8, a first electromagnetic valve 9, a second electromagnetic valve 10, a third electromagnetic valve 11, a fourth electromagnetic valve 12, a fifth electromagnetic valve 13, a sixth electromagnetic valve 14, a seventh electromagnetic valve 15, an eighth electromagnetic valve 16, an electromagnetic valve seat 17, a first metering pump 18, a second metering pump 19, a third metering pump 20, a first chemical reaction coil 21, a second chemical reaction coil 22, a liquid core waveguide 23, a first optical-liquid coupler 24, a second optical-liquid coupler 25, a detector 26, and a light source 27 are shown.
Detailed Description
The invention is discussed in detail below with reference to the figures and examples.
The deep sea trace ion concentration in-situ detection system comprises a liquid path system shown in figure 1 and a control system shown in figure 2.
Referring to fig. 1, the fluid path system includes: seven reagent bags, eight filter screens, eight electromagnetic valves, an electromagnetic valve seat 17, three metering pumps, two chemical reaction coils, two light-liquid couplers, a liquid core waveguide 23, a detector 26 and a light source 27. Wherein, the first reagent bag 1 is connected with the inlet of a first electromagnetic valve 9, the second reagent bag 2 is connected with the inlet of a second electromagnetic valve 10, the third reagent bag 3 is connected with the inlet of a third electromagnetic valve 11, the fourth reagent bag 4 is connected with the inlet of a fifth electromagnetic valve 13, the fifth reagent bag 5 is connected with the inlet of a sixth electromagnetic valve 14, the sixth reagent bag 6 is connected with the inlet of a seventh electromagnetic valve 15, the seventh reagent bag 7 is connected with the inlet of an eighth electromagnetic valve 16, a filter screen 8 is arranged at the inlet of each electromagnetic valve, the outlets of the first electromagnetic valve 9 and the second electromagnetic valve 10 are connected with the inlet of a first metering pump 18, the outlet of the third electromagnetic valve 11 is connected with the inlet of a second metering pump 19, the outlets of the fourth electromagnetic valve 12, the fifth electromagnetic valve 13, the sixth electromagnetic valve 14, the seventh electromagnetic valve 15 and the eighth electromagnetic valve 16 are connected with the inlet of a third metering pump 20, the eight electromagnetic valves are arranged on an electromagnetic valve seat 17, the device and the electromagnetic valve seat 17 realize combination and control of reagents and samples, outlets of a second metering pump 19 and a third metering pump 20 are connected with one end of a first chemical reaction coil 21, the other end of the first chemical reaction coil 21 and an outlet of a first metering pump 18 are connected with one end of a second chemical reaction coil 22, the other end of the second chemical reaction coil 22 is sequentially connected with a first light-liquid coupler 24, a liquid core waveguide tube 23 and a second light-liquid coupler 25, the first light-liquid coupler 24 is connected with a light source 27 through an optical fiber, and the second light-liquid coupler 25 is connected with a detector 26 through an optical fiber.
Referring to fig. 2, the control system includes: the system comprises a controller unit, a real-time clock, a memory card, a digital acquisition card, an energy supply module, a power supply conversion module and a pump valve control panel; the energy supply module supplies power to the controller unit and the pump valve control panel through the power supply conversion module, the real-time clock and the storage card are connected with the controller unit, the light source, the eight electromagnetic valves and the three metering pumps of the liquid path system are connected with the pump valve control panel, the pump valve control panel is connected with the digital acquisition card, and the digital acquisition card and the detector of the liquid path system are connected with the controller unit through USB interfaces.
The controller unit is provided with a plurality of USB interfaces, a plurality of serial interfaces and a plurality of network interfaces; the real-time clock provides a real-time clock, and provides standard detection time information and a timing reference for system detection; the digital acquisition card is connected with the controller unit through a USB interface, is controlled by the controller unit and outputs a digital signal; the detector is connected with the controller unit through a USB interface, is controlled by the controller unit and stores acquired data into the memory card; the pump valve control panel controls the pump, the valve, the switch of the light source and the flow of the pump according to the digital signal of the digital acquisition card; the controller unit can receive instructions of an external controller through a serial port protocol or a network communication protocol (TCP/IP protocol), and can also transmit acquired data to the external controller through the serial port protocol or the network communication protocol.
The working process of the invention is illustrated below by taking the detection of the concentration of ferric ions and the concentration of ferrous ions in seawater as an example: and proportioning three parts of standard solution, and respectively filling the standard solution into a fifth reagent bag 5, a sixth reagent bag 6 and a seventh reagent bag 7, wherein the concentration of ferric ions and the concentration of ferrous ions in the first part of standard solution are both 0.1nmol/L, the concentration of ferric ions and the concentration of ferrous ions in the second part of standard solution are both 0.5nmol/L, and the concentration of ferric ions and the concentration of ferrous ions in the third part of standard solution are both 1.0 nmol/L. The rinse solution was ultrapure water having a resistivity of 18.2M Ω · cm, and was filled in the fourth reagent bag 4. The first reagent is ascorbic acid with the concentration of 0.01mol/L, and is filled in the third reagent bag 3 for reducing ferric ions in the seawater to be detected into ferrous ions. The second reagent is phenanthroline (C20H 13N4NAO6S 2. H20) with the concentration of 0.005g/ml, is filled into the second reagent bag 2, is obtained by mixing and diluting sodium acetate and glacial acetic acid according to a certain proportion, has the pH value of =5.5, and is filled into the first reagent bag 1. The flow rate of the third metering pump 20 was set to 0.8ml/min, and the flow rates of the first metering pump 18 and the second metering pump 19 were set to 0.3 ml/min. Before detection, a standard solution with known concentrations of ferric ions and ferrous ions is used for calibrating the system, a calibration curve is obtained through numerical calculation and processing, then the concentrations of the ferric ions and the ferrous ions of the seawater to be detected are detected, and the calibration operation steps are different according to the difference of the detected ions; after calibration is finished, detecting the ion concentration according to the operation steps set by the program; after each sample is detected, the system is flushed, so that the samples left on the wall of the pipeline of the system are flushed, and detection errors caused by sample residues are reduced.
System calibration: when ferric ions are calibrated, starting up to turn on a light source and a detector and enable all pump valves to be in an initial state, turning on an eighth electromagnetic valve 16, a third electromagnetic valve 11, a second metering pump 19 and a third metering pump 20, pumping a first part of standard solution and ascorbic acid into a first chemical reaction coil 21 for mixing reaction, pumping mixed solution into a second chemical reaction coil 22, turning on a first electromagnetic valve 9, a second electromagnetic valve 10 and a first metering pump 18, pumping buffer solution and a phenanthroline reagent into the second chemical reaction coil 22 for mixing with the existing mixed solution, pumping the mixed solution into a liquid core waveguide tube 23 after the chemical reaction is completely performed, acquiring detection signals by the detector and storing the detection signals, and enabling all pump valves to be in the initial state after the system is completely flushed. Repeating the above processes until three detection signals of the ferric ions in the standard solution are obtained, drawing and storing a calibration curve by the controller unit according to the ferric ion concentrations and the corresponding detection signals of the three standard solutions, and completing the calibration of the ferric ions; when ferrous ions are calibrated, the eighth electromagnetic valve 16 and the third metering pump 20 are opened, a first part of standard solution is pumped into the second chemical reaction coil 22, then the first electromagnetic valve 9, the second electromagnetic valve 10 and the first metering pump 18 are opened, a buffer solution and a phenazine reagent are pumped into the second chemical reaction coil 22 to be mixed with the existing standard solution, after the chemical reaction is completely carried out, the mixed solution is pumped into the liquid core waveguide tube 23, at the moment, the detector collects and stores detection signals, and after the system is flushed, all the pump valves are in an initial state. And repeating the processes until detection signals of the ferrous ions of the three standard solutions are obtained, drawing and storing a calibration curve according to the ferrous ion concentrations of the three standard solutions and the corresponding detection signal controller units, and completing the ferrous ion calibration.
System detection: when the ferric ion concentration is detected, the fourth electromagnetic valve 12, the third electromagnetic valve 11, the second metering pump 19 and the third metering pump 20 are opened, seawater to be detected and ascorbic acid are pumped into the first chemical reaction coil 21 for mixing reaction, the mixed solution is pumped into the second chemical reaction coil 22, then the first electromagnetic valve 9, the second electromagnetic valve 10 and the first metering pump 18 are opened, the buffer solution and the phenanthroline alloxazine reagent are pumped into the second chemical reaction coil 22 to be mixed with the existing seawater to be detected, the mixed solution is pumped into the liquid core waveguide tube 23 after the chemical reaction completely occurs, at the moment, the detector collects a detection signal, the controller unit obtains the ferric ion concentration in the seawater to be detected according to the analysis of a calibration curve, and all the pump valves are in an initial state after the system is flushed. When the ferrous ion concentration is detected, the fourth electromagnetic valve 12 and the third metering pump 20 are opened, seawater to be detected is pumped into the second chemical reaction coil 22, then the first electromagnetic valve 9, the second electromagnetic valve 10 and the first metering pump 18 are opened, a buffer solution and a phenanthroline reagent are pumped into the second chemical reaction coil 22 to be mixed with the existing seawater to be detected, after the chemical reaction is completely performed, the mixed solution is pumped into the liquid core waveguide tube 23, at the moment, a detection signal is collected by a detector, the controller unit obtains the ferrous ion concentration in the seawater to be detected according to the analysis of a calibration curve, and all pump valves are in an initial state after the system flushing is completed.
In the embodiment, the diameter of the holes of the filter screen 8 is 0.45 μm, which is smaller than the diameter of all the holes in the system, so that the micro particles in the seawater or the reagent can be effectively prevented from entering the liquid path system, and the blockage can be prevented; the liquid core waveguide tube 23 is a 5-meter quartz tube, the outer layer of which is wrapped by Teflon (Teflon AF 2400) material with lower refractive index than water, and is used for increasing the optical path length of light, the sensitivity is 500 times that of a traditional 10-centimeter wide cuvette, meanwhile, the inner diameter of the liquid core waveguide tube 23 is only 550 micrometers, the total volume of the 5-meter liquid core waveguide tube is not more than 1.25mL, and the consumption of samples and reagents is low; the first chemical reaction coil 21 and the second chemical reaction coil 22 are spirally surrounded pipelines, and some of the pipelines contain glass marbles inside, which are main fields for mixing and reacting the reagent and the sample; the first optical-fluid coupler 24 and the second optical-fluid coupler 25 are connection ports for introducing the mixed liquid and the light into and out of the liquid core waveguide 23 at the same time. The optical fiber transmits light emitted from the light source and light emitted into the detector; all tubes were of FEP Teflon (Teflon) material with an outer diameter of 1.58mm (1/16 ") and an inner diameter of 0.57mm (0.03").
Claims (1)
1. An in-situ detection system for deep sea trace ion concentration is characterized by comprising a liquid path system and a control system; wherein, the liquid way system includes: seven reagent bags, eight filter screens, eight electromagnetic valves, an electromagnetic valve seat (17), three metering pumps, two chemical reaction coils, two light-liquid couplers, a liquid core waveguide (23), a detector (26), a light source (27) and the like; wherein, the first reagent bag 1 is connected with the inlet of a first electromagnetic valve (9), the second reagent bag (2) is connected with the inlet of a second electromagnetic valve (10), the third reagent bag (3) is connected with the inlet of a third electromagnetic valve (11), the fourth reagent bag (4) is connected with the inlet of a fifth electromagnetic valve (13), the fifth reagent bag (5) is connected with the inlet of a sixth electromagnetic valve (14), the sixth reagent bag (6) is connected with the inlet of a seventh electromagnetic valve (15), the seventh reagent bag (7) is connected with the inlet of an eighth electromagnetic valve (16), a filter screen (8) is arranged at the inlet of each electromagnetic valve, the outlets of the first electromagnetic valve (9) and the second electromagnetic valve (10) are connected with the inlet of a first metering pump (18), the outlet of the third electromagnetic valve (11) is connected with the inlet of a second metering pump (19), the fourth electromagnetic valve (12), the fifth electromagnetic valve (13), Outlets of a sixth electromagnetic valve (14), a seventh electromagnetic valve (15) and an eighth electromagnetic valve (16) are all connected with an inlet of a third metering pump (20), and the eight electromagnetic valves are all arranged on an electromagnetic valve seat (17); outlets of a second metering pump (19) and a third metering pump (20) are connected with one end of a first chemical reaction coil (21), the other end of the first chemical reaction coil (21) and an outlet of a first metering pump (18) are connected with one end of a second chemical reaction coil (22), the other end of the second chemical reaction coil (22) is sequentially connected with a first light-liquid coupler (24), a liquid core waveguide tube (23) and a second light-liquid coupler (25), the first light-liquid coupler (24) is connected with a light source (27) through an optical fiber, and the second light-liquid coupler (25) is connected with a detector (26) through an optical fiber; the control system includes: the system comprises a controller unit, a real-time clock, a memory card, a digital acquisition card, an energy supply module, a power supply conversion module, a pump valve control panel and the like; the energy supply module supplies power to the controller unit and the pump valve control panel through the power supply conversion module, the real-time clock and the storage card are all connected with the controller unit, the light source, the eight electromagnetic valves and the three metering pumps of the liquid path system are all connected with the pump valve control panel, the pump valve control panel is connected with the digital acquisition card, and the digital acquisition card and the detector of the liquid path system are all connected with the controller unit through the USB interface.
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| CN2012100335805A CN102590540A (en) | 2012-02-15 | 2012-02-15 | In-situ detection system for concentration of deep sea micro-ions |
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| CN2012100335805A CN102590540A (en) | 2012-02-15 | 2012-02-15 | In-situ detection system for concentration of deep sea micro-ions |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107907698A (en) * | 2017-12-14 | 2018-04-13 | 中国科学院深海科学与工程研究所 | A kind of Biogeochemistry original position experimental provision for deep-sea |
| CN109490563A (en) * | 2018-10-18 | 2019-03-19 | 中国海洋大学 | A kind of sampling device for solubilised state divalent Fe and Ti in seawater |
| CN109752375A (en) * | 2019-03-18 | 2019-05-14 | 天津市环境保护科学研究院 | A kind of device and method of real-time detection ferrous ion concentration |
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| CN107907698A (en) * | 2017-12-14 | 2018-04-13 | 中国科学院深海科学与工程研究所 | A kind of Biogeochemistry original position experimental provision for deep-sea |
| CN109490563A (en) * | 2018-10-18 | 2019-03-19 | 中国海洋大学 | A kind of sampling device for solubilised state divalent Fe and Ti in seawater |
| CN109752375A (en) * | 2019-03-18 | 2019-05-14 | 天津市环境保护科学研究院 | A kind of device and method of real-time detection ferrous ion concentration |
| CN111664887A (en) * | 2020-05-05 | 2020-09-15 | 中国海洋大学 | Resistivity probe rod-based seabed floating mud layer dynamic change in-situ observation method |
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