CN106556598B - Automatic in-situ nutritive salt analysis device for seawater monitoring - Google Patents
Automatic in-situ nutritive salt analysis device for seawater monitoring Download PDFInfo
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- CN106556598B CN106556598B CN201610979456.6A CN201610979456A CN106556598B CN 106556598 B CN106556598 B CN 106556598B CN 201610979456 A CN201610979456 A CN 201610979456A CN 106556598 B CN106556598 B CN 106556598B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/00584—Control arrangements for automatic analysers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
Abstract
The invention discloses an in-situ nutritive salt automatic analysis device for seawater monitoring, which comprises a first colorimetric structure (4.1) for detecting ammonia nitrogen, a second colorimetric structure (4.2) for detecting phosphate, a third colorimetric structure (4.3) for detecting nitrite and a fourth colorimetric structure (4.4) for detecting nitrate; one branch of the sample injection and liquid discharge channel (1) is connected with a multi-way valve (2), and an injector (3) is connected with the multi-way valve (2) and is arranged in a bidirectional way; also comprises a reagent unit comprising a plurality of reagent bags (5) connected with the multi-way valve (2); the other branch of the sample injection and liquid discharge channel (1) is connected with a fourth colorimetric structure (4.4), and a peristaltic pump (7) is arranged at the inlet of the fourth colorimetric structure (4.4); a xenon lamp (8) and a spectrometer (9) are arranged beside the fourth colorimetric structure (4.4), and an outlet of the fourth colorimetric structure (4.4) is connected with the sample injection and liquid drainage channel (1). The invention is easy to clean and accurate in detection.
Description
Technical Field
The invention relates to the field of environmental monitoring, in particular to an in-situ nutrient salt automatic analysis device for seawater monitoring.
Background
The seawater nutrient salt is an important parameter for monitoring the quality of seawater, and is used for measuring the concentration and distribution of the nutrient salt in the seawater, and has important significance for red tide early warning and research on marine organism geochemical circulation.
The method for measuring the nutrient salt in the seawater is based on an on-site sampling-laboratory measuring method of a survey ship, has the defects of poor real-time performance, waste of manpower, financial resources, time and the like, can not obtain timely continuous data, can not effectively reflect the long-term change trend of the seawater, analyzes the water quality change and early warns of marine environment accidents. The automatic analyzer for in-situ monitoring of nutritive salt is paid attention to, and the detection method of the analyzer is generally based on spectrophotometry, adopts a peristaltic pump to control sample injection, mixes a water sample with a color reagent, and calculates the concentration of the water sample through a built-in standard curve. Because the environment of ocean on-line monitoring is complex, on-site conditions such as salinity, waves, turbidity and the like have higher requirements on the waterproof performance and corrosion resistance of monitoring instruments and the stability of reagents. The general material performance is difficult to meet the requirement of long-time on-line monitoring. The peristaltic pump has larger error in water sample and reagent quantification, and is easy to cause larger deviation of detection results.
Disclosure of Invention
The invention aims to provide an in-situ nutrient salt automatic analysis device for seawater monitoring so as to solve the problems in the prior art.
The technical scheme provided by the invention is as follows:
an automatic analysis device of in-situ nutrient salt for sea water monitoring, which is characterized in that: the device comprises a first colorimetric structure (4.1) for detecting ammonia nitrogen, a second colorimetric structure (4.2) for detecting phosphate, a third colorimetric structure (4.3) for detecting nitrite and a fourth colorimetric structure (4.4) for detecting nitrate;
one branch of the sample injection and liquid discharge channel (1) is connected with a multi-way valve (2), and an injector (3) is connected with the multi-way valve (2) and is arranged in a bidirectional way; also comprises a reagent unit comprising a plurality of reagent bags (5) connected with the multi-way valve (2); the inlets of the first colorimetric structure (4.1), the second colorimetric structure (4.2) and the third colorimetric structure (4.3) are respectively connected with the multi-way valve (2) directly or indirectly, and the outlets of the first colorimetric structure (4.1), the second colorimetric structure (4.2) and the third colorimetric structure (4.3) are respectively connected with the sample injection and liquid drainage channel (1) directly or indirectly;
the other branch of the sample injection and liquid discharge channel (1) is connected with a fourth colorimetric structure (4.4), and a peristaltic pump (7) is arranged at the inlet of the fourth colorimetric structure (4.4); a xenon lamp (8) and a spectrometer (9) are arranged beside the fourth colorimetric structure (4.4), and an outlet of the fourth colorimetric structure (4.4) is connected with the sample injection and liquid drainage channel (1).
In the preferred embodiment of the invention, the first color comparison structure (4.1) is connected with an outlet of the multi-way valve (2), and the outlet of the first color comparison structure (4.1) is connected with the sample injection and liquid discharge channel (1);
the second colorimetric structure (4.2) is connected with the other outlet of the multi-way valve (2), and the outlet of the second colorimetric structure (4.2) is connected with the inlet of the third colorimetric structure (4.3); the outlet of the third colorimetric structure (4.3) is connected to the sample and liquid drainage channel 1.
In the preferred embodiment of the invention, a three-way valve (6) is arranged on the branch connected with the fourth colorimetric structure (4.4) for detecting nitrate, and the three-way valve (6) is connected with the inlet of a peristaltic pump (7).
In a preferred embodiment of the invention, the reagent unit comprises a plurality of exchangeable reagent bags (5), each connected by a pipeline to a multi-way valve (2).
In the preferred embodiment of the invention, the colorimetric mechanism adopts a Z-type cuvette and is fixed in a manner of tilting 40-60 degrees.
In a preferred embodiment of the invention, different reagent bags (5) are filled with different detection reagents, wherein one of the reagent bags (5) is filled with pure water.
In a preferred embodiment of the invention, the reagent bag (5) is replaceable.
From the above description, the present invention provides an in-situ automatic analyzer for nutrient salts for seawater monitoring, which has the following advantages compared with the existing automatic analyzers for nutrient salts on the market:
(1) The quantitative injection pump is adopted in the water sample in the detection process, and compared with other quantitative modes such as peristaltic pumps, the quantitative injection pump has the advantages of being higher in accuracy and good in stability, meanwhile, the mixing of the sample and the reagent can be realized in the syringe, the whole colorimetric system is simplified, the structure is prevented from being too complex, liquid leakage or dead angles are prevented, and the detection is not affected by cleaning finally.
(2) On one hand, due to different absorption wavelengths adopted by each parameter of the colorimetric structure, the stability of the monochromatic lamp with different wavelengths is better, and the deviation of a detection result caused by the drift of a light source is prevented. In addition, the separation of the colorimetric structure can avoid interference caused by different detection reagents to influence detection. The diameter of the colorimetric structure can be smaller than 2mm, the use amount of the reagent is reduced, and the maintenance period is prolonged.
(3) The instrument realizes reagent replacement modularization: all reagent bags can realize that whole module is changed, change the reagent frame, will correspond the serial number and connect with reagent bag serial number correspond can, convenient field maintenance.
(4) The invention uses the injection pump as a driver, can simultaneously detect a plurality of parameters, realizes automatic online continuous monitoring of ammonia nitrogen, nitrite nitrogen, nitrate nitrogen and phosphate, can carry a buoy monitoring system for in-situ online water quality monitoring of marine environment, and combines the power supply, data acquisition and wireless communication technology to send monitoring data to a terminal receiving device in real time so as to achieve the aim of real-time monitoring.
Drawings
Fig. 1 is a schematic structural view of an in-situ nutrient salt automatic analysis device for seawater monitoring according to the present invention.
1. Sample injection and liquid drainage channel
2. Multi-way valve
3. Injection syringe
Colorimetric Structure 4.1 first colorimetric Structure 4.2 second colorimetric Structure 4.3 third colorimetric Structure 4.4 fourth colorimetric Structure
5. Reagent bag
6. Three-way valve
7. Peristaltic pump
8. Xenon lamp
9. Spectrometer
Detailed Description
The structure of the invention is as follows:
an in-situ nutrient salt automatic analysis device for seawater monitoring comprises a first colorimetric structure 4.1 for ammonia nitrogen detection, a second colorimetric structure 4.2 for phosphate detection, a third colorimetric structure 4.3 for nitrite detection and a fourth colorimetric structure 4.4 for nitrate detection;
one branch of the sample injection and liquid discharge channel 1 is connected with the multi-way valve 2, and one injector 3 is connected with the multi-way valve 2, and the two are arranged in a bidirectional way. Also included is a reagent unit comprising a plurality of replaceable reagent bags 5, each connected to a different line inlet of the multi-way valve 2. Different reagent bags 5 are filled with different detection reagents, and one of the reagent bags 5 is filled with pure water.
The first color comparison structure 4.1 is connected with an outlet of the multi-way valve 2, and the outlet of the first color comparison structure 4.1 is connected to the sample injection and liquid discharge channel 1.
The second colorimetric structure 4.2 is connected to the other outlet of the multiway valve 2 and the outlet of the second colorimetric structure 4.2 is connected to the inlet of the third colorimetric structure 4.3. The outlet of the third colorimetric structure 4.3 is connected to the sample and drain channel 1.
The other branch of the sample introduction and liquid discharge channel 1 is connected with a fourth colorimetric structure 4.4 for detecting nitrate; the branch is provided with a three-way valve 6, and the three-way valve 6 is connected with an inlet of a peristaltic pump 7. The outlet of the peristaltic pump 7 is connected with the fourth colorimetric structure 4.4. A xenon lamp 8 and a spectrometer 9 are arranged beside the fourth colorimetric structure 4.4. The outlet of the fourth colorimetric structure 4.4 is connected to the sample and drain channel 1.
The invention is used as follows:
the detection principle of ammonia nitrogen, nitrite nitrogen, nitrate nitrogen and phosphate is based on spectrophotometry.
Ammonia nitrogen detection: a certain volume of water sample is driven by the injector 3, a sample inlet is controlled by the multi-way valve 2, the water sample enters from the sample inlet and drain channel 1, then enters the multi-way valve 2, and then enters the injector 3. Then, the multi-way valve 2 switches other ammonia nitrogen detection reagent interfaces, a certain volume of color reagent in the reagent bag 5 is injected into the injector 3, a water sample is mixed with the color reagent and then developed, developed liquid is discharged from the injector 3 after the development is completed, enters the colorimetric structure 4.1 through the multi-way valve 2, a 520nm wavelength led lamp is used as a detection light source, a photocell is used as a detector to detect the absorbance, the concentration of the water sample is calculated through a built-in standard curve, and the reaction liquid is discharged from the outside of the instrument through the sample injection and liquid discharge channel 1 after the detection is completed.
Detection of phosphate and nitrite: the mode is consistent with ammonia nitrogen, the multi-way valve 2 is used for controlling the switching of the sample inlet, a certain volume of reagent types corresponding to different detection parameters are added, after mixed color development is carried out in the injector 3, the reagent types finally enter the colorimetric mechanisms 4.2 and 4.3 respectively, then led light sources with wavelengths of 700nm and 520nm are used for detection, and a detection result is obtained through a built-in standard curve after the detection flow is finished.
The detection method of the nitrate is based on an ultraviolet absorption spectrophotometry, a water sample enters from a sample injection and drainage channel 1, is directly switched into a colorimetric mechanism 4.4 by a peristaltic pump 7 through a three-way valve 6, takes a full-band xenon lamp as a light source, takes a spectrometer (the wavelength detection range is 200-1100 nm) as a detector, and calculates the concentration of the water sample through a built-in nitrate detection model. As no external color reagent is needed for nitrate detection, the sample injection amount does not influence the detection result, the peristaltic pump is adopted to control the flow, the power consumption is lower, and the cost is correspondingly reduced. The nitrate detection pipeline is separated from other parameter detection pipelines, so that other parameter color developing agents and the color developing solution after reaction can be prevented from interfering with the absorption peak of nitrate, and the detection result is more accurate.
After the detection of each parameter is finished, the parameter is switched to a pure water pipeline for cleaning through a multi-way valve 2, so that the follow-up detection is not interfered after the detection of the previous parameter is finished.
Preferably, the colorimetric mechanism adopts a Z-type cuvette, and the fixing mode is inclined by 50 degrees, so that the influence of bubbles on a detection light path can be effectively prevented.
The instrument realizes reagent replacement modularization, all reagent bags can realize whole module replacement, the reagent frame is replaced, the corresponding serial number connector corresponds to the reagent bag number, and the field maintenance is convenient.
The foregoing is merely an embodiment of the present invention, but the design concept of the present invention is not limited thereto, and any insubstantial modification of the present invention by using the concept shall belong to the behavior of infringement of the protection scope of the present invention.
Claims (6)
1. An automatic analysis device of in-situ nutrient salt for sea water monitoring, which is characterized in that: the device comprises a first colorimetric structure (4.1) for detecting ammonia nitrogen, a second colorimetric structure (4.2) for detecting phosphate, a third colorimetric structure (4.3) for detecting nitrite and a fourth colorimetric structure (4.4) for detecting nitrate;
one branch of the sample injection and liquid discharge channel (1) is connected with a multi-way valve (2), and an injector (3) is connected with the multi-way valve (2) and is arranged in a bidirectional way; also comprises a reagent unit comprising a plurality of reagent bags (5) connected with the multi-way valve (2); the inlets of the first colorimetric structure (4.1), the second colorimetric structure (4.2) and the third colorimetric structure (4.3) are respectively connected with the multi-way valve (2) directly or indirectly, and the outlets of the first colorimetric structure (4.1), the second colorimetric structure (4.2) and the third colorimetric structure (4.3) are respectively connected with the sample injection and liquid drainage channel (1) directly or indirectly;
the other branch of the sample injection and liquid discharge channel (1) is connected with a fourth colorimetric structure (4.4), and a peristaltic pump (7) is arranged at the inlet of the fourth colorimetric structure (4.4); a xenon lamp (8) and a spectrometer (9) are arranged beside the fourth colorimetric structure (4.4), and an outlet of the fourth colorimetric structure (4.4) is connected with a sample injection and liquid drainage channel (1);
the colorimetric mechanism adopts a Z-type cuvette, and the fixing mode is inclined by 40-60 degrees;
the first color comparison structure (4.1) is connected with an outlet of the multi-way valve (2), and the outlet of the first color comparison structure (4.1) is connected to the sample injection and liquid drainage channel (1);
the second colorimetric structure (4.2) is connected with the other outlet of the multi-way valve (2), and the outlet of the second colorimetric structure (4.2) is connected with the inlet of the third colorimetric structure (4.3); the outlet of the third colorimetric structure (4.3) is connected to the sample injection and liquid drainage channel (1).
2. An in situ nutrient salt automatic analysis device for seawater monitoring as claimed in claim 1, wherein: the branch of the fourth colorimetric structure (4.4) for detecting nitrate is also provided with a three-way valve (6), and the three-way valve (6) is connected with the inlet of the peristaltic pump (7).
3. An in situ nutrient salt automatic analysis device for seawater monitoring as claimed in claim 1, wherein: by a means of
The reagent unit comprises a plurality of replaceable reagent bags (5), and each reagent bag is connected to the multi-way valve (2) through a pipeline.
4. An in situ nutrient salt automatic analysis device for seawater monitoring as claimed in claim 1, wherein: different reagent bags (5) are filled with different detection reagents, and one of the reagent bags (5) is filled with pure water.
5. An in situ nutrient salt automatic analysis device for seawater monitoring as claimed in claim 1, wherein:
the reagent bag (5) is replaceable.
6. An automatic analysis method of in-situ nutrient salt for seawater monitoring, which is characterized in that the automatic analysis device of in-situ nutrient salt for seawater monitoring is adopted, and the method comprises the following steps:
1) Ammonia nitrogen detection: a certain volume of water sample is driven by an injector (3), a sampling port is controlled by a multi-way valve (2), after the water sample enters the injector (3), the multi-way valve (2) switches other ammonia nitrogen detection reagent interfaces, a certain volume of color reagent in a reagent bag (5) is injected into the injector (3), the water sample and the color reagent are mixed and then developed, developed liquid is discharged from the injector (3) after the development is completed, enters the first color comparison structure (4.1) through the multi-way valve (2), a 520nm wavelength led lamp is used as a detection light source, a photocell is used as a detector to detect the absorbance of the water sample, the concentration of the water sample is calculated through a built-in standard curve, and the reaction liquid is discharged from the sampling liquid discharge channel (1) to the outside of the instrument after the detection is completed;
2) Detection of phosphate and nitrite: a certain volume of water sample is driven by an injector (3), a sampling port is controlled by a multi-way valve (2), after the water sample enters the injector (3), the multi-way valve (2) switches other ammonia nitrogen detection reagent interfaces, a certain volume of color reagent in a reagent bag (5) is injected into the injector (3), the water sample is mixed with the color reagent and then developed, after the development is completed, the developed color liquid is discharged by the injector (3), and finally the water sample enters a second colorimetric mechanism (4.2) and a third colorimetric mechanism (4.3) respectively, then the water sample is detected by led light sources with wavelengths of 700nm and 520nm respectively, and a detection result is obtained by a built-in standard curve after the detection flow is completed;
3) Detection of nitrate: the water sample is directly switched into a fourth colorimetric mechanism (4.4) by a peristaltic pump (7) through a three-way valve (6), a full-wave-band xenon lamp is used as a light source, a spectrometer with the wavelength detection range of 200-1100nm is used as a detector, and the concentration of the water sample is calculated through a built-in nitrate detection model.
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| CN107782724A (en) * | 2017-12-04 | 2018-03-09 | 深圳市朗诚科技股份有限公司 | A kind of nutritive salt in-situ analyzer and nutrient concentrations analysis method |
| CN112444487B (en) * | 2020-10-13 | 2023-02-21 | 南京南瑞水利水电科技有限公司 | Water quality multi-parameter analysis method and system |
| CN112903414A (en) * | 2021-02-08 | 2021-06-04 | 杭州帆昂环保科技有限公司 | Multi-parameter automatic water quality analysis method and system |
| CN114235730A (en) * | 2022-02-21 | 2022-03-25 | 中国科学院烟台海岸带研究所 | Seawater nutrient salt online monitoring system and seawater nutrient salt detection method |
| CN115078678A (en) * | 2022-08-01 | 2022-09-20 | 中国长江三峡集团有限公司 | System and method for monitoring ammonia nitrogen release flux in lake nutrient salt |
| CN116519610B (en) * | 2023-05-11 | 2023-11-03 | 原生代(青岛)科技有限公司 | Nutritive salt in-situ analysis device |
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| JP2000266677A (en) * | 1999-01-14 | 2000-09-29 | Shimadzu Corp | Analyzer for nitrogen compound, phosphorus compound and organic contaminant |
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| CN102375068B (en) * | 2010-08-20 | 2013-10-16 | 北京吉天仪器有限公司 | Full-automatic nutrient salt analyzer and analysis method thereof |
| CN206177825U (en) * | 2016-11-08 | 2017-05-17 | 厦门斯坦道科学仪器股份有限公司 | A normal position nutritive salt autoanalysis device for sea water monitoring |
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| JP2006047323A (en) * | 2000-05-26 | 2006-02-16 | Shimadzu Corp | Measurement/liquid feed mechanism for aqueous solution for analysis and water quality analyzer using it |
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