CN104198538A - Shipborne cruising dissolved inorganic carbon observation device and method - Google Patents
Shipborne cruising dissolved inorganic carbon observation device and method Download PDFInfo
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- CN104198538A CN104198538A CN201410492373.5A CN201410492373A CN104198538A CN 104198538 A CN104198538 A CN 104198538A CN 201410492373 A CN201410492373 A CN 201410492373A CN 104198538 A CN104198538 A CN 104198538A
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- carbonate
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Abstract
The invention discloses a shipborne cruising dissolved inorganic carbon observation device and method, and relates to marine monitoring. The observation device comprises a seawater sampling device, a three-way valve, acid adding pipes, an acidification device, a CO2 exchange device, an electrical conductivity detector, a carbonate and alkali liquor leacheate generator, a methanesulfonic acid leacheate generator and a data collecting and controlling device. The method comprises the steps as follows: the carbonate and alkali liquor leacheate generator is started, alkali liquor enters the electrical conductivity detector through the CO2 exchange device, data of the electrical conductivity detector is collected after stabilization, and the measured data is a background value; the sampling device is started, the methanesulfonic acid leacheate generator is started simultaneously, a seawater sample and a methanesulfonic acid solution enter the acidification device through the acid adding pipes for acidification reaction, the sample after the acidification reaction enters a selective permeable membrane pipe of the CO2 exchange device, CO2 is permeated outside the pipe and absorbed by the alkali liquor, and the concentration of the alkali liquor after absorption is measured by the electrical conductivity detector; and sampling is stopped after measurement is performed for a period of time, and the measurement is finished when the electrical conductivity detector is restored to the background value.
Description
Technical field
The present invention relates to marine monitoring, especially relate to a kind of device and method that is applicable to boat-carrying and walks the long-time automatic Observation of dissolved inorganic carbon in navigation water.
Background technology
Seawater dissolved inorganic carbon (Dissolved Inorganic Carbon, DIC) is the summation of the concentration of carbon of various inorganic carbonates, supercarbonate, carbonic acid and carbon dioxide in ocean, accounts for seawater total carbon more than 95%.DIC has become the basic parameter of Ocean acidification research, is the important parameter of understanding sea life production run.Accurately, fast and convenient and high time-space resolution ground measure spatial and temporal distributions and the variability of seawater DIC concentration, for understanding Ocean acidification and ocean to CO
2absorption, conversion and transition process most important, be research marine biogeochemistry process indispensable key parameter, in global ocean carbon cycle, play an important role.
At present, seawater DIC observation technology mainly contains coulometric titration and NDIR (Non-Dispersive Infrared) CO
2analytic approach, these methods have higher degree of accuracy, are current internationally recognized DIC analytical approachs.But due to complicated, the bulky and inconvenient operation of device, and high to analyst's technical ability requirement, therefore can only be used for lab analysis, be difficult to use in on-the-spot boat-carrying and walk boat observation.At present mainly to preserve after sampling at the scene to the measurement of seawater DIC, take back experimental determination, but in Sample storage process, due to the variation of environment cause DIC measurement result and actual variance larger, therefore exploitation be suitable for boat-carrying walk boat ocean DIC observation technology become urgent problem.Along with the development of technology, the detection method of seawater DIC is developed, and has occurred colourimetry, gravimetric method, equilibrium pressure force method, alkalimeter algorithm, thermal conductance class electrochemical process etc.Chinese patent CN203287283U discloses a kind of dissolved inorganic carbon and dissolved organic carbon of high-speed and high-efficiency and has surveyed altogether device, this device can be measured dissolved inorganic carbon and the dissolved organic carbon in water body simultaneously, but this apparatus structure complexity, the sample measurement time is long, temporal resolution is low, is not suitable for boat-carrying and walks boat.CN101806789B discloses analyzer for analyzing concentration of inorganic carbon in a kind of water body, and CN103913553A discloses a kind of seawater dissolved inorganic carbon measurement mechanism of walking to navigate, and these 2 kinds of public technologies have all adopted the dissolved inorganic carbon in water body is converted into CO
2, then pass through CO
2detecting device Analysis for CO
2concentration, DIC is converted into CO by the method
2, need gas-liquid separation device and air lift process and add carrier gas process to make operation complicated; Meanwhile, gas is subject to impact that the environmental parameter such as temperature, humidity and pressure changes very greatly, and when rig-site utilization, the stability of device is difficult to ensure, accuracy of detection is also affected.Need first the carbonate in seawater to be changed into CO for DIC detection technique
2and carry out separating and measuring, and need in this course to add acid solution and inert carrier gas or alkali absorption liquid, therefore, be badly in need of wanting a kind of online reagent generation technique, required various reagent when producing DIC and measuring, to meet long-time boat-carrying walk the to navigate demand of automatic Observation.
Summary of the invention
The object of the invention is the device complexity, the automaticity that exist for current DIC field observation technology low, add material carry with preserve difficulty, standard specimen is difficult to the problems such as acquisition, provide leacheate generation technique and DIC measuring technique and up-to-date CO
2permeable membrane technology combines, and can realize the automatic generation of the bronsted lowry acids and bases bronsted lowry liquid of standard specimen and required interpolation, the automatic measurement of typical curve and the Self-regulation track of making and instrument, and the boat-carrying that precision and automaticity are higher is walked navigation water dissolved inorganic carbon observation device and method.
Described boat-carrying is walked navigation water dissolved inorganic carbon observation device and is provided with seawater sampling device, T-valve, adds acid tube, acidizing device, CO
2switch, electric conductivity detector, carbonate and alkali lye leacheate generator, pyrovinic acid leacheate generator, data acquisition and controller;
Described seawater sampling device is provided with water sample injection port, seawater sampling device, carbonate are connected with T-valve respectively with the carbonate standard specimen outlet of alkali lye leacheate generator, between T-valve, acidizing device entrance and pyrovinic acid leacheate generator, be provided with and add acid tube, CO
2the acidified sample entrance of switch is connected with acidizing device outlet, CO
2switch alkali absorption liquid entrance is connected with the outlet of alkali lye leacheate generator alkali lye with carbonate, CO
2the outlet of switch alkali absorption liquid is connected with electric conductivity detector; CO
2switch is provided with CO
2selectivity permeable membrane pipe, CO
2acidifying solution discard solution discharge port is established in the outlet of selectivity permeable membrane pipe, and electric conductivity detector is provided with alkali absorption liquid discard solution discharge port; Seawater sampling device, T-valve, carbonate are all connected with controller with data acquisition with pyrovinic acid leacheate generator and electric conductivity detector with alkali lye leacheate generator, and data acquisition and controller are provided with data connecting line.
Carbonate and alkali lye leacheate generator produce required carbonate standard specimen and alkali lye by the mode of ionization, and the solubility of carbonate standard specimen and alkali lye is by electric current and the Control of Voltage of carbonate and the input of alkali lye leacheate generator.The required acid solution of described acidifying is pyrovinic acid, is produced by pyrovinic acid leacheate generator.
Described seawater sampling device is provided with sampling valve and constant-flux pump.
Described electric conductivity detector can adopt contact electric conductivity detector.
Described boat-carrying is walked navigation water dissolved inorganic carbon observation procedure, adopts described boat-carrying to walk navigation water dissolved inorganic carbon observation device, comprises the following steps:
1) in the time carrying out seawater sample measurement, first open carbonate and alkali lye leacheate generator, allow alkali lye pass through CO
2switch, enters electric conductivity detector, gathers the data of electric conductivity detector after stable, and the data of now measuring are background value;
2) open sampling device, open pyrovinic acid leacheate generator simultaneously, seawater sample and pyrovinic acid solution enter acidizing device and carry out acidification reaction by adding acid tube, and the sample after acidification reaction enters CO
2in the selectivity permeable membrane pipe of switch, CO
2infiltrate into pipe outer by alkali liquor absorption, the concentration of lye after absorption changes to be measured by electric conductivity detector;
3) measure after a period of time, stop sample introduction, in the time that electric conductivity detector returns to background value, measuring process finishes.
In step 1) in, described in carry out seawater sample measure time, can select continuous sample introduction measure or intermittent sample introduction measure; Described in the time carrying out seawater sample measurement, can first production standard curve and instrument adjustment, the method for making of described typical curve can be: according to the concentration of required a series of carbonate standard specimen solution, calculate carbonate and the corresponding excitation current of alkali lye leacheate generator and voltage, set corresponding input current and magnitude of voltage by data acquisition and controller, carbonate and alkali lye leacheate generator are according to setting value, concentration produces a series of carbonate titers from low to high successively, and successively by acidizing device and CO
2switch transforms, and the absorption liquid after conversion enters electric conductivity detector and measures, and obtains a series of standard specimen concentration, automatically generates typical curve, and complete instrument adjustment according to measurement result.
In step 3) in, described a period of time can be chosen in 1～10min as required.
Described boat-carrying is walked in navigation water dissolved inorganic carbon observation device, carbonate standard specimen and absorption alkali lye are produced by carbonate and alkali lye leacheate generator, the concentration that input current by Non-leaching liquid generator and voltage obtain needed carbonate standard specimen and alkali lye, realizes automatic generation and the interpolation of multiple carbonate standard specimen.The acid solution that described acid adding device adds is pyrovinic acid, and is produced by pyrovinic acid leacheate generator.
Beneficial effect of the present invention is as follows:
The boat-carrying the present invention relates to is walked navigation water dissolved inorganic carbon observation device, leacheate generator is measured for DIC, realize carbonate standard specimen, the acid of required interpolation and the automatic generation of absorption alkali lye, realized the automatic measurement of typical curve and the Self-regulation track of instrument.Overcome field observation complicated operation, the low problem that obtains of automaticity.Adopt CO
2film transformation technology, directly by CO
2be converted into carbonate solution and measure, overcome CO
2the problem that air lift and detection exist, the conditions such as environment temperature, humidity, pressure that greatly reduced change the impact on testing result, realized the high precision of seawater DIC, automatically detected.The present invention can automatically produce and measure required standard specimen, sample acidifying and CO
2absorb needed bronsted lowry acids and bases bronsted lowry solution, Self-regulation track and measurement, the boat-carrying that is particularly suitable for seawater dissolved inorganic carbon in long-time ocean expedition walk the to navigate observation of dissolved inorganic carbon in the long-term unattended water of Continuous Observation or field.
Brief description of the drawings
Fig. 1 is the structural representation that boat-carrying of the present invention is walked navigation water dissolved inorganic carbon observation device device embodiment.
Embodiment
Referring to Fig. 1, described boat-carrying walks that navigation water dissolved inorganic carbon observation device embodiment is provided with seawater sampling device 1, T-valve 2, adds acid tube 3, acidizing device 4, CO
2switch 5, electric conductivity detector 7, carbonate and alkali lye leacheate generator 8, pyrovinic acid leacheate generator 9, data acquisition and controller 10;
Described seawater sampling device 1 is provided with water sample injection port 11, seawater sampling device 1, carbonate are connected with T-valve 2 respectively with the carbonate standard specimen outlet 15 of alkali lye leacheate generator 8, between T-valve 2, acidizing device entrance 19 and pyrovinic acid leacheate generator 9, be provided with and add acid tube 3, CO
2the acidified sample entrance 21 of switch 5 is connected with acidizing device outlet 20, CO
2switch alkali absorption liquid entrance 17 is connected with alkali lye leacheate generator alkali lye outlet 16 with carbonate, CO
2switch alkali absorption liquid outlet 18 is connected with electric conductivity detector 7; CO
2switch 5 is provided with CO
2selectivity permeable membrane pipe 6, CO
2acidifying solution discard solution discharge port 12 is established in the outlet of selectivity permeable membrane pipe 6, and electric conductivity detector 7 is provided with alkali absorption liquid discard solution discharge port 13; Seawater sampling device 1, T-valve 2, carbonate are all connected with controller 10 with data acquisition with pyrovinic acid leacheate generator 9 and electric conductivity detector 7 with alkali lye leacheate generator 8, and data acquisition and controller 10 are provided with data connecting line 14.
Carbonate and alkali lye leacheate generator 8 produce required carbonate standard specimen and alkali lye, electric current and Control of Voltage that the solubility of carbonate standard specimen and alkali lye is inputted by carbonate and alkali lye leacheate generator 8 by the mode of ionization.The required acid solution of described acidifying is pyrovinic acid, is produced by pyrovinic acid leacheate generator 9.
Described seawater sampling device 1 is provided with sampling valve and constant-flux pump.
Described electric conductivity detector 7 can adopt contact electric conductivity detector.
Described boat-carrying is walked navigation water dissolved inorganic carbon observation procedure, adopts described boat-carrying to walk navigation water dissolved inorganic carbon observation device, comprises the following steps:
1) in the time carrying out seawater sample measurement, first open carbonate and alkali lye leacheate generator, allow alkali lye pass through CO
2switch, enters electric conductivity detector, gathers the data of electric conductivity detector after stable, and the data of now measuring are background value; While carrying out seawater sample measurement, can select continuous sample introduction to measure or the measurement of intermittent sample introduction; Described in the time carrying out seawater sample measurement, can first production standard curve and instrument adjustment, the method for making of described typical curve can be: according to the concentration of required a series of carbonate standard specimen solution, calculate carbonate and the corresponding excitation current of alkali lye leacheate generator and voltage, set corresponding input current and magnitude of voltage by data acquisition and controller, carbonate and alkali lye leacheate generator are according to setting value, concentration produces a series of carbonate titers from low to high successively, and successively by acidizing device and CO
2switch transforms, and the absorption liquid after conversion enters electric conductivity detector and measures, and obtains a series of standard specimen concentration, automatically generates typical curve, and complete instrument adjustment according to measurement result.
2) open sampling device, open pyrovinic acid leacheate generator simultaneously, seawater sample and pyrovinic acid solution enter acidizing device and carry out acidification reaction by adding acid tube, and the sample after acidification reaction enters CO
2in the selectivity permeable membrane pipe of switch, CO
2infiltrate into pipe outer by alkali liquor absorption, the concentration of lye after absorption changes to be measured by electric conductivity detector;
3) measure after a period of time, stop sample introduction, in the time that electric conductivity detector returns to background value, measuring process finishes; Described a period of time can be chosen in 1～10min as required.
Below in conjunction with Fig. 1, a concrete application of the present invention is described.Before starting to measure seawater sample, the making of advanced column criterion curve and the adjustment of instrument.Select as required a series of carbonate standard specimen concentration, calculate carbonate and alkali lye leacheate generator 8 corresponding excitation current and voltages, set corresponding input current and magnitude of voltage by data acquisition and controller 10, carbonate and alkali lye leacheate generator 8 are according to electric current and the magnitude of voltage set, and concentration produces a series of carbonate titers from low to high successively.The valve position of T-valve 2 is switched to and leacheate generator carbonate standard specimen outlet 15 valve position that are connected, start the pyrovinic acid that pyrovinic acid leacheate generator 9 produces required concentration simultaneously, the concentration of pyrovinic acid is adjusted by electric current and the voltage of input, carbonate standard specimen and pyrovinic acid solution are after adding acid tube 3 and mixing, successively by acidizing device 4 and CO
2switch 5 transforms, and the absorption liquid after conversion enters electric conductivity detector 7 and measures, and obtains a series of standard specimen concentration, automatically generates typical curve according to measurement result, completes the Self-regulation track of instrument.
Complete after the automatic measurement of typical curve, start to carry out seawater sample measurement, the valve position of T-valve 2 is switched to the valve position being connected with sampling device 1, open carbonate and alkali lye leacheate generator 8 generation alkali lye automatically, alkali lye passes through CO
2switch 5 enters electric conductivity detector 7, gathers the data of electric conductivity detector 7 after stable, and the data of now measuring are background value; Treat after a period of stabilisation, open sampling device, open pyrovinic acid leacheate generator 9 simultaneously, seawater sample and pyrovinic acid solution mix by adding acid tube 3, enter acidizing device 4 and carry out acidification reaction after mixing, and the sample after acidifying enters CO
2in the selectivity permeable membrane pipe 6 of switch 5, CO
2diffuse to pipe outward by alkali liquor absorption by permeable membrane, the acidified sample waste liquid after exchange is discharged by waste liquid mouth 12, and the concentration of lye after absorption changes to be measured by electric conductivity detector 7, and absorption liquid waste liquid is discharged by discard solution discharge port 13.Measure after a period of time, stop sample introduction, in the time that electric conductivity detector returns to background value, measuring process finishes.Measure next time, start seawater sampling device 1 and carry out sample introduction, complete automatic measurement by above-mentioned steps.
As required, seawater sampling device 1 can carry out continuous sample introduction measurement, also can be set to intermittent sample introduction and measure.While measuring standard specimen, only T-valve 2 need be switched to standard specimen entrance valve position, carbonate and alkali lye leacheate generator 8 produce required carbonate standard specimen automatically, automatically measure by above-mentioned steps.In the time measuring seawater sample, can automatically carry out as required the measurement of standard specimen.Carbonate standard solution of the present invention, alkali absorption liquid and souring soln all produce automatically, measuring process is controlled automatically by controller, the unmanned of truly having realized DIC measurement moves automatically, guarantees to walk long-time steady operation in boat observation at complicated boat-carrying.
Claims (10)
1. boat-carrying is walked navigation water dissolved inorganic carbon observation device, it is characterized in that being provided with seawater sampling device, T-valve, adds acid tube, acidizing device, CO
2switch, electric conductivity detector, carbonate and alkali lye leacheate generator, pyrovinic acid leacheate generator, data acquisition and controller;
Described seawater sampling device is provided with water sample injection port, seawater sampling device, carbonate are connected with T-valve respectively with the carbonate standard specimen outlet of alkali lye leacheate generator, between T-valve, acidizing device entrance and pyrovinic acid leacheate generator, be provided with and add acid tube, CO
2the acidified sample entrance of switch is connected with acidizing device outlet, CO
2switch alkali absorption liquid entrance is connected with the outlet of alkali lye leacheate generator alkali lye with carbonate, CO
2the outlet of switch alkali absorption liquid is connected with electric conductivity detector; CO
2switch is provided with CO
2selectivity permeable membrane pipe, CO
2acidifying solution discard solution discharge port is established in the outlet of selectivity permeable membrane pipe, and electric conductivity detector is provided with alkali absorption liquid discard solution discharge port; Seawater sampling device, T-valve, carbonate are all connected with controller with data acquisition with pyrovinic acid leacheate generator and electric conductivity detector with alkali lye leacheate generator, and data acquisition and controller are provided with data connecting line.
2. boat-carrying is walked navigation water dissolved inorganic carbon observation device as claimed in claim 1, it is characterized in that described carbonate and alkali lye leacheate generator produce required carbonate standard specimen and alkali lye by the mode of ionization, the solubility of carbonate standard specimen and alkali lye is by electric current and the Control of Voltage of carbonate and the input of alkali lye leacheate generator.
3. boat-carrying is walked navigation water dissolved inorganic carbon observation device as claimed in claim 1, it is characterized in that the required acid solution of described acidifying is pyrovinic acid, is produced by pyrovinic acid leacheate generator.
4. boat-carrying is walked navigation water dissolved inorganic carbon observation device as claimed in claim 1, it is characterized in that described seawater sampling device is provided with sampling valve and constant-flux pump.
5. boat-carrying is walked navigation water dissolved inorganic carbon observation device as claimed in claim 1, it is characterized in that described electric conductivity detector adopts contact electric conductivity detector.
6. boat-carrying is walked navigation water dissolved inorganic carbon observation procedure, it is characterized in that adopt as arbitrary in claim 1～5 as described in boat-carrying walk navigation water dissolved inorganic carbon observation device, described observation procedure comprises the following steps:
1) in the time carrying out seawater sample measurement, first open carbonate and alkali lye leacheate generator, allow alkali lye pass through CO
2switch, enters electric conductivity detector, gathers the data of electric conductivity detector after stable, and the data of now measuring are background value;
2) open sampling device, open pyrovinic acid leacheate generator simultaneously, seawater sample and pyrovinic acid solution enter acidizing device and carry out acidification reaction by adding acid tube, and the sample after acidification reaction enters CO
2in the selectivity permeable membrane pipe of switch, CO
2infiltrate into pipe outer by alkali liquor absorption, the concentration of lye after absorption changes to be measured by electric conductivity detector;
3) measure after a period of time, stop sample introduction, in the time that electric conductivity detector returns to background value, measuring process finishes.
7. boat-carrying is walked navigation water dissolved inorganic carbon observation procedure as claimed in claim 6, it is characterized in that in step 1) in, described in carry out seawater sample measure time, can select continuous sample introduction measure or intermittent sample introduction measure.
8. boat-carrying is walked navigation water dissolved inorganic carbon observation procedure as claimed in claim 6, it is characterized in that in step 1) in, described in the time carrying out seawater sample measurement, first production standard curve and instrument adjustment.
9. boat-carrying is walked navigation water dissolved inorganic carbon observation procedure as claimed in claim 8, the method for making that it is characterized in that described typical curve is: according to the concentration of required a series of carbonate standard specimen solution, calculate carbonate and the corresponding excitation current of alkali lye leacheate generator and voltage, set corresponding input current and magnitude of voltage by data acquisition and controller, carbonate and alkali lye leacheate generator are according to setting value, concentration produces a series of carbonate titers from low to high successively, and successively by acidizing device and CO
2switch transforms, and the absorption liquid after conversion enters electric conductivity detector and measures, and obtains a series of standard specimen concentration, automatically generates typical curve, and complete instrument adjustment according to measurement result.
10. boat-carrying is walked navigation water dissolved inorganic carbon observation procedure as claimed in claim 6, it is characterized in that in step 3) in, described a period of time is chosen in 1～10min as required.
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Cited By (3)
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| CN106771027A (en) * | 2016-12-09 | 2017-05-31 | 国家海洋局第三海洋研究所 | Ocean dissolved inorganic carbon in site measurement instrument |
| CN108195995A (en) * | 2017-12-26 | 2018-06-22 | 中国科学院海洋研究所 | The measuring device of carbonate content in a kind of marine sediment |
| CN111735921A (en) * | 2020-06-12 | 2020-10-02 | 自然资源部第三海洋研究所 | Multi-parameter observation instrument for marine acidification during ship-borne navigation |
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| CN104198538B (en) | 2016-06-29 |
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