CN111735921A - Multi-parameter observation instrument for marine acidification during ship-borne navigation - Google Patents
Multi-parameter observation instrument for marine acidification during ship-borne navigation Download PDFInfo
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Abstract
A ship-borne sailing seawater acidification multiparameter observation instrument relates to the technical field of ocean monitoring, wherein liquid outlets of a seawater filter and a standard liquid storage tank are respectively connected with a liquid inlet of a three-way valve, liquid outlets of the three-way valve are connected with a liquid inlet of a liquid separator, two liquid outlets of the liquid separator are respectively connected with liquid inlets of a first peristaltic pump and a second peristaltic pump, the liquid outlet of the first peristaltic pump is connected with a liquid inlet of a flow cell, and the liquid outlet of the second peristaltic pump is connected with a liquid inlet of a DIC detector; the water purifier is connected with a carrier liquid inlet of the DIC detector through a constant flow pump; the pH probe extends into the flow cell; the automatic sample introduction and detection of the instrument are controlled by a data acquisition and control chip. The device can realize high-precision automatic detection of seawater acidification parameters, can perform automatic measurement of standard samples and adjustment and calibration of instruments, needs a small amount of samples, does not need additional reagent consumption, and is particularly suitable for long-time continuous automatic observation of shipborne sea water pH and DIC or long-term unattended online observation in the field.
Description
Technical Field
The invention relates to the technical field of ocean monitoring, in particular to a ship-borne sailing seawater acidification multi-parameter observation instrument.
Background
pH and DIC in seawater are important parameters for characterizing seawater acidification, have important indication significance in marine acidification research, become basic parameters of marine acidification research, and are important parameters for understanding the activity process of marine organisms and extremely responding to marine environment. The method is accurate, rapid and convenient, and measures the space-time distribution and variability of the pH and DIC concentration of the seawater with high space-time resolution, is an indispensable key parameter for researching the geochemical process of marine organisms for understanding the marine acidification and the activity of the marine organisms, and plays an important role in the research of global marine ecosystem.
The seawater acidification is mainly made of CO2Dissolution causes, so the dissolved inorganic carbon DIC in seawater is a key parameter for studying seawater acidification. At present, coulometry is the main analysis method for DIC determination, and because current and time parameters can be accurately controlled, the method can achieve high accuracy and precision, the analysis error is about 0.05%, and the method is often used as the standard method for DIC determination. However, the whole analysis system is large in size due to long measuring time consumption, and is only suitable for laboratory operation and cannot be used for offshore field analysis and determination. Recently, with the development of technology, new methods and analysis techniques based on new principles have emerged in recent years around the determination of DIC, TA and pH in seawater. Sayles et al acidified seawater samples for CO2After escaping through a silicone semi-permeable membrane, the solution is absorbed by dilute NaOH solution, and a three-electrode conductivity detector is adopted for detecting and carrying out DIC measurement. In order to ensure the measurement precision, a multi-point standard sample is adopted for calibration, the measurement precision of DIC concentration is +/-5 mu M at 1.6-2.8 mM, and the analysis time of a single sample is about 70 min. The main disadvantages of this method are the long time and the high consumption of chemical reagents. Pencharee et al developed a DIC measurement device using a flow injection gas diffusion technique and a non-contact conductivity detector. The measurement precision is 0.48%, and the linear range of the concentration is 0.2-10 mM. The detector adopted by the method has large power consumption and volume, the measurement accuracy of 0.48 percent is obtained under the concentration of 6mMDIC, the average concentration level range of the existing ocean DIC is 1.8-2.3 mM, and the local area with high DIC, such as the black sea, is only 3.8-4.3 mM. At present, the measurement of seawater pH and DIC is mostly independent measurement, and a multi-parameter synchronous observation instrument is not available. Because the 4 parameters of the seawater acidification parameters of pH, DIC, alkalinity, Ca ions and the like have correlation, the rest 2 parameters can be obtained by calculation after any 2 parameters are obtained.
At present, the instrument and equipment for seawater acidification observation mainly depend on import, and a large amount of accurate field observation data cannot be obtained due to the laggard field measurement technology. In order to improve the overall level of the research on ocean carbon cycle and ocean acidification in China, the urgent need is to improve the ocean acidification site determination technology in China and establish a set of multi-parameter ocean acidification automatic observation system with high precision, low cost and in-situ measurement of multi-parameter (DIC, pH, temperature and salinity).
Disclosure of Invention
The invention aims to solve the problems that the sea water acidification observation parameter is single, multi-parameter synchronous observation cannot be carried out, the analysis method is complex, and a large amount of manpower and material resources are consumed in the prior art, and provides a ship-borne sea water acidification multi-parameter observation instrument which can automatically observe acidification parameters such as pH and DIC of sea water for a long time.
In order to achieve the purpose, the invention adopts the following technical scheme:
a ship-borne navigation seawater acidification multi-parameter observer comprises a seawater filter, a standard solution storage tank, a three-way valve, a liquid distributor, a first peristaltic pump, a flow cell, a pH probe detection circuit, a second peristaltic pump, a DIC detector, a constant flow pump, a water purifier, a data acquisition and control chip and a computer;
the seawater filter and the liquid outlet of the standard liquid storage tank are respectively connected with a liquid inlet of a three-way valve, the liquid outlet of the three-way valve is connected with a liquid inlet of a liquid separator, two liquid outlets of the liquid separator are respectively connected with liquid inlets of a first peristaltic pump and a second peristaltic pump, the liquid outlet of the first peristaltic pump is connected with a liquid inlet of the flow cell, and the liquid outlet of the second peristaltic pump is connected with a liquid inlet of the DIC detector; the water purifier is connected with a carrier liquid inlet of the DIC detector through a constant flow pump;
the pH probe extends into the flow cell and is electrically connected with the pH probe detection circuit; the three-way valve, the first peristaltic pump, the second peristaltic pump, the pH probe detection circuit, the DIC detector, the constant flow pump and the water purifier are all connected with the data acquisition and control chip, and the data acquisition and control chip is connected with the computer to control the automatic sample introduction and detection of the instrument through the data acquisition and control chip.
And a carrier liquid outlet of the DIC detector is connected with a water purifier to recycle the measured carrier waste liquid.
The parameter measurement method of the ship-borne sailing seawater acidification multi-parameter observation instrument comprises the following steps: when the seawater sample is measured, the valve position of a three-way valve is switched to a seawater sample inlet, sample introduction is started, firstly, the seawater sample removes seawater suspended particles through a filter, the seawater sample is divided into two paths through a liquid divider, one path is conveyed to a flow cell by a first peristaltic pump, parameters such as pH, temperature and salinity of the sample are measured by a pH probe, and the other path is conveyed to a DIC detector by a second peristaltic pump to measure the DIC concentration of the sample; and setting the detection time interval of the pH probe and the DIC detector according to requirements, and realizing synchronous measurement of different parameters.
Before the seawater sample is measured, the standard curve is manufactured and the instrument is calibrated.
In the invention, the standard curve manufacturing and instrument adjusting method comprises the following steps: firstly, a control system switches a valve position of a three-way valve to a sample injection port of a standard sample, standard solution enters the three-way valve through a standard solution storage tank and then is divided into two paths through a liquid divider, wherein one path enters a flow cell through a first peristaltic pump, a pH probe detects parameters such as pH, temperature, salinity and the like of the standard sample, the other path enters a DIC detector through a second peristaltic pump to measure the DIC concentration of the standard sample, a series of standard solutions with different concentrations are configured from low to high according to needs and measured, a standard curve is automatically generated according to the measurement result, and automatic adjustment and calibration of an instrument are completed.
The invention can carry out continuous sample feeding measurement according to the requirement and can also be set as intermittent standard sample feeding measurement.
The intermittent standard sample adding measurement steps are as follows: after measuring a certain amount of samples through program control, through switching the three-way valve, switch over the valve position to the sample introduction port of the standard sample by the sea water introduction port, realize the appearance of introduction of standard sample, accomplish the standard sample and measure the back, the automatic measure of sea water continues to be carried out to the valve position of automatic switch-over three-way valve to the sea water introduction port, thereby realize the automatic switch-over detection of sample and standard sample.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
the invention utilizes the liquid separator and the low-flow pH and DIC detection technology to realize the synchronous on-line detection of multiple parameters of seawater acidification, and realize the automatic measurement of a standard curve and the automatic adjustment and calibration of an instrument, thereby solving the problems of single measurement, complex system and low automation degree of the traditional seawater acidification parameter; the invention realizes high-precision and automatic detection of multi-parameter pH, DIC, temperature, salinity and the like of seawater acidification, and is particularly suitable for long-time automatic observation of multi-parameter seawater acidification during shipborne navigation.
The pure water required by the DIC detector is provided by the water purifier through the constant flow pump, and the wastewater generated by the DIC detector is recycled through the water purifier, so that extra reagent consumption is not required, and the device is energy-saving and environment-friendly.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Reference numerals: the device comprises a seawater filter 1, a standard solution storage tank 2, a three-way valve 3, a standard sample injection port 3A, a seawater injection port 3B, a liquid separator 4, a first peristaltic pump 5, a flow cell 6, a pH probe 7, a pH probe detection circuit 8, a second peristaltic pump 9, a DIC detector 10, a constant flow pump 11, a water purifier 12, a data acquisition and control chip 13 and a computer 14.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects of the present invention clearer and clearer, the present invention is further described in detail below with reference to the accompanying drawings and embodiments.
As shown in fig. 1, the present embodiment includes a seawater filter 1, a standard solution storage tank 2, a three-way valve 3, a liquid separator 4, a first peristaltic pump 5, a flow cell 6, a pH probe 7, a pH probe detection circuit 8, a second peristaltic pump 9, a DIC detector 10, a constant flow pump 11, a water purifier 12, a data acquisition and control chip 13, and a computer 14;
liquid outlets of the seawater filter 1 and the standard liquid storage tank 2 are respectively connected with a liquid inlet of a three-way valve 3, a liquid outlet of the three-way valve 3 is connected with a liquid inlet of a liquid distributor 4, two liquid outlets of the liquid distributor 4 are respectively connected with liquid inlets of a first peristaltic pump 5 and a second peristaltic pump 9, a liquid outlet of the first peristaltic pump 5 is connected with a liquid inlet of a flow cell 6, and a liquid outlet of the second peristaltic pump 9 is connected with a liquid inlet of a DIC detector 10; the water purifier 12 is connected with the carrier liquid inlet of the DIC detector 10 through the constant flow pump 11, and the carrier liquid outlet of the DIC detector 10 is connected with the water purifier 12, so that pure water generated by the water purifier 12 is used as a carrier for detecting DIC, and measured carrier waste liquid is recycled by the water purifier 12.
The pH probe 7 extends into the flow cell 6, and the pH probe 7 is electrically connected with the pH probe detection circuit 8; the three-way valve 3, the first peristaltic pump 5, the second peristaltic pump 9, the pH probe detection circuit 8, the DIC detector 10, the constant flow pump 11 and the water purifier 12 are all connected with a data acquisition and control chip 13, the data acquisition and control chip 13 is connected with a computer 14, and automatic sample introduction and detection of the instrument are controlled through the data acquisition and control chip 13.
The parameter measurement method of the ship-borne sailing seawater acidification multi-parameter observation instrument comprises the following steps:
1) before the measurement of the seawater sample is started, the preparation of a standard curve and the calibration of an instrument are carried out: firstly, a control system switches a valve position of a three-way valve 3 to a standard sample injection port 3A, standard solution enters the three-way valve 3 through a standard solution storage tank 2, then the standard sample is divided into two paths through a liquid divider 4, wherein one path enters a flow cell 6 through a first peristaltic pump 5, parameters such as pH, temperature and salinity of the standard sample are detected through a pH probe 7, meanwhile, the other path enters a DIC detector 10 through a second peristaltic pump 9 to measure the DIC concentration of the standard sample, a series of standard solutions with different concentrations are configured from low to high according to needs and measured, a standard curve is automatically generated according to the measurement result, and automatic adjustment and calibration of an instrument are completed;
2) after the automatic measurement of the standard curve is completed, the seawater sample measurement is started: switching the valve position of a three-way valve 3 to a seawater sample inlet 3B, starting sample introduction, firstly removing seawater suspended particles from a seawater sample through a filter, dividing the seawater sample into two paths through a liquid divider 4, wherein one path is conveyed to a flow cell 6 by a first peristaltic pump 5, parameters such as pH, temperature and salinity of the seawater sample are measured by a pH probe 7, and the other path is conveyed to a DIC detector 10 by a second peristaltic pump 9 to measure the DIC concentration of the seawater sample; the detection time intervals of the pH probe 7 and the DIC detector 10 are set according to requirements, and synchronous measurement of different parameters is achieved.
The invention can carry out continuous sample feeding measurement according to the requirement and can also be set as intermittent standard sample feeding measurement.
The intermittent standard sample adding measurement steps are as follows: after measuring a certain amount of samples through program control, through switching three-way valve 3, switch over the valve position to standard sample introduction port 3A by sea water introduction port 3B, realize the appearance of advancing of standard sample, accomplish standard sample and measure the back, automatic switch over three-way valve 3's valve position to sea water introduction port 3B, continue to carry out the automatic measure of sea water to realize the automatic switch over detection of sample and standard sample.
The pure water is automatically generated by the water purifier, the measurement process is automatically controlled, the high-precision automatic detection of seawater acidification parameters can be realized, the automatic measurement of a standard sample and the adjustment and calibration of an instrument can be simultaneously carried out, the required sample amount is small, the extra reagent consumption is not needed, the unattended automatic operation of seawater acidification parameters is really realized, the long-time stable operation in the complex shipborne sailing observation is ensured, and the device is particularly suitable for the long-time continuous automatic observation of the pH and DIC of shipborne sailing seawater or the long-term unattended online observation in the field.
Claims (7)
1. On-board sea water acidification multi-parameter visulizer that walks to navigate, its characterized in that: the device comprises a seawater filter, a standard solution storage tank, a three-way valve, a liquid separator, a first peristaltic pump, a flow cell, a pH probe detection circuit, a second peristaltic pump, a DIC detector, a constant flow pump, a water purifier, a data acquisition and control chip and a computer;
the seawater filter and the liquid outlet of the standard liquid storage tank are respectively connected with a liquid inlet of a three-way valve, the liquid outlet of the three-way valve is connected with a liquid inlet of a liquid separator, two liquid outlets of the liquid separator are respectively connected with liquid inlets of a first peristaltic pump and a second peristaltic pump, the liquid outlet of the first peristaltic pump is connected with a liquid inlet of the flow cell, and the liquid outlet of the second peristaltic pump is connected with a liquid inlet of the DIC detector; the water purifier is connected with a carrier liquid inlet of the DIC detector through a constant flow pump;
the pH probe extends into the flow cell and is electrically connected with the pH probe detection circuit; the three-way valve, the first peristaltic pump, the second peristaltic pump, the pH probe detection circuit, the DIC detector, the constant flow pump and the water purifier are all connected with the data acquisition and control chip, and the data acquisition and control chip is connected with the computer to control the automatic sample introduction and detection of the instrument through the data acquisition and control chip.
2. The on-board marine acidification multiparameter observation instrument of claim 1, wherein: and a carrier liquid outlet of the DIC detector is connected with a water purifier to recycle the measured carrier waste liquid.
3. The parameter measurement method adopting the ship-borne sailing seawater acidification multi-parameter observation instrument of any one of claims 1-2 is characterized by comprising the following steps: when the seawater sample is measured, the valve position of a three-way valve is switched to a seawater sample inlet, sample introduction is started, firstly, the seawater sample removes seawater suspended particles through a filter, the seawater sample is divided into two paths through a liquid divider, one path is conveyed to a flow cell by a first peristaltic pump, the pH probe measures the pH, temperature and salinity parameters of the sample, and the other path is conveyed to a DIC detector by a second peristaltic pump to measure the DIC concentration of the sample; and setting the detection time interval of the pH probe and the DIC detector according to requirements, and realizing synchronous measurement of different parameters.
4. A parameter measurement method according to claim 3, characterized in that: before the seawater sample is measured, the standard curve is made and the instrument is calibrated.
5. The method of claim 4, wherein the standard curve is prepared and the instrument is calibrated by the following steps: firstly, a control system switches a valve position of a three-way valve to a sample injection port of a standard sample, standard solution enters the three-way valve through a standard solution storage tank and then is divided into two paths through a liquid divider, wherein one path enters a flow cell through a first peristaltic pump, a pH probe detects pH, temperature and salinity parameters of the standard sample, the other path enters a DIC detector through a second peristaltic pump to measure the DIC concentration of the standard sample, a series of standard solutions with different concentrations are configured from low to high according to needs and measured, a standard curve is automatically generated according to the measurement result, and automatic adjustment and calibration of an instrument are completed.
6. A parameter measurement method according to claim 3, characterized in that: continuous sample feeding measurement can be carried out according to the requirement, and intermittent standard sample feeding measurement can also be set.
7. The parameter measurement method of claim 6, wherein the step of intermittently adding the standard sample comprises: after measuring a certain amount of samples through program control, through switching the three-way valve, switch over the valve position to the sample introduction port of the standard sample by the sea water introduction port, realize the appearance of introduction of standard sample, accomplish the standard sample and measure the back, the automatic measure of sea water continues to be carried out to the valve position of automatic switch-over three-way valve to the sea water introduction port, thereby realize the automatic switch-over detection of sample and standard sample.
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