CN210742119U - Quantitative analysis device for ammonia nitrogen in seawater - Google Patents

Quantitative analysis device for ammonia nitrogen in seawater Download PDF

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CN210742119U
CN210742119U CN201921710686.8U CN201921710686U CN210742119U CN 210742119 U CN210742119 U CN 210742119U CN 201921710686 U CN201921710686 U CN 201921710686U CN 210742119 U CN210742119 U CN 210742119U
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ammonia nitrogen
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ammonia
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冯巍巍
孙冰
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Yantai Institute of Coastal Zone Research of CAS
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Yantai Institute of Coastal Zone Research of CAS
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Abstract

The utility model discloses an ammonia nitrogen quantitative analysis device in sea water for prepare the ammonia nitrogen that dissolves in the sea water and carry out quantitative determination through this device to the ammonia concentration who prepares out. The device comprises a preparation unit, a measurement unit and a data processing and control unit. The data processing and control unit can control the operation sequence of each part of the device and process the acquired spectrum signals so as to obtain the concentration of ammonia nitrogen. The device prepares ammonia gas from seawater by adding an alkaline reagent, obtains the absorbance of the gas by adopting an ultraviolet-visible absorption spectrum method, and analyzes the concentration of the gas by adopting a fast Fourier transform method. Compared with the traditional measuring method, the utility model has the advantages of simple operation, short measuring time, high automation degree, and is not easily interfered by pigment and particulate matter in water, thus improving the accuracy of system measurement; the monitoring level of the environmental protection department on the ammonia nitrogen in the seawater body is improved, and powerful technical support is provided for effectively preventing and controlling the ammonia nitrogen pollution of the water body.

Description

Quantitative analysis device for ammonia nitrogen in seawater
Technical Field
The utility model relates to a sea water environmental pollution on-line monitoring field especially relates to environmental optical monitoring technical field, specifically is a quantitative analysis device of ammonia nitrogen in sea water.
Background
Seawater resources are important resources for survival and development of human beings, seawater pollution can have important influence on the stability of marine ecology, so that the diversity of marine organisms is damaged, and great loss can be caused to marine fishery and marine culture, so that the detection of the quality of seawater is particularly important.
With the development of economic society of China, the seawater pollution is more and more serious. The contents of ammonia nitrogen and hydrogen sulfide in seawater are increased by marine culture in various places of coastal areas, domestic sewage in coastal cities, industrial wastewater discharge and the like. The ammonia nitrogen is an important factor for limiting the growth and total yield of plants in seawater, when the content of the ammonia nitrogen is too high, seawater is eutrophicated, and algae in the ocean can propagate and grow in a large quantity, so that red tide occurs, a large amount of marine organisms die, and great loss is caused to marine fishery.
According to the marine survey standards and the marine monitoring standards of China, the main methods for detecting the content of ammonia nitrogen in seawater in China are a sodium hypobromite oxidation method and an indophenol blue method. The sodium hypobromite oxidation method needs a large amount of chemical reagents and is complex in operation process, a seawater sample can be tested after being filtered by an oil film, the seawater sample needs to be tested immediately after being collected, otherwise the seawater sample needs to be refrigerated and stored, and in addition, ammonia gas in air in the measurement process can also influence the accuracy of the result. The indophenol blue method is easily affected by metal ions in seawater, uses more chemical reagents and toxic reagents, is complex to operate, has long analysis time, and also needs oil film filtration to prevent ammonia in air from being affected. In addition, methods for detecting ammonia nitrogen in water bodies include a Nashin reagent photometry, a salicylic acid-hypochlorous acid photometry and the like, but the methods are not suitable for measuring ammonia nitrogen in seawater. The method adopts a xenon lamp to irradiate ammonia gas to obtain an ultraviolet spectrum, and the concentration is calculated by analyzing the absorbance. The method only needs to add the alkaline reagent, and compared with the method, the method has the advantages of less reagent consumption, simple operation and no influence of pigment and pollutants in the seawater. The system can directly detect seawater after sampling without water sample pretreatment, has high detection speed, avoids complex steps and can carry out real-time monitoring.
SUMMERY OF THE UTILITY MODEL
In order to solve the technical problem, the utility model provides a need not artifical on duty, easy operation, degree of automation height and can realize real-time continuous detection's device. The device is composed of a preparation unit, a circulation unit, a measurement unit and a data processing and control unit, and achieves the purpose of measuring ammonia nitrogen rapidly and accurately in real time. The measuring method adopted by the device is different from the traditional method for measuring the content of ammonia nitrogen in seawater, the traditional method is abandoned, and a new device is built, so that the detection of ammonia nitrogen is completed in a gaseous state. The specific technical scheme is as follows:
a quantitative analysis device for ammonia nitrogen in seawater comprises a preparation unit, a measurement unit and a data processing and control unit;
the preparation unit consists of a sample introduction part and a reaction container; the sample introduction part comprises a water sample inlet device and a reagent inlet device; the reaction vessel is of a cylindrical structure, the side surface of the reaction vessel is provided with an air inlet, a sampling port, a reagent port and a water inlet from top to bottom in sequence, the bottom of the reaction vessel is provided with a waste liquid outlet, and the upper part of the reaction vessel is provided with a gas outlet;
the water inlet device comprises a sampling pump, the water inlet end of the sampling pump is connected with the water sample pool, and the water outlet end of the sampling pump is connected with the reaction container;
the reagent feeding device comprises a peristaltic pump, the output end of the peristaltic pump is connected with the reagent port, and the inlet end of the peristaltic pump is connected with the reagent bottle;
the air inlet is connected with an air-ammonia conversion valve;
the waste liquid outlet is connected with a drain valve; the gas outlet is connected with an exhaust valve;
the measuring unit comprises an absorption cell, a xenon lamp light source and a spectrometer, wherein lenses are arranged at the upper end and the lower end of the absorption cell; the xenon lamp light source is arranged at the bottom of the absorption cell, a first lens is arranged between the xenon lamp light source and the bottom of the absorption cell, the upper part of the absorption cell is provided with a spectrometer, and a second lens is arranged between the spectrometer and the absorption cell; light emitted by a xenon lamp light source sequentially passes through the bottom end of the absorption cell, the first lens, gas in the absorption cell and the second lens and then reaches the spectrometer through the optical fiber;
the upper part of the absorption pool is a gas inlet, the lower end of the absorption pool is a gas outlet, the gas inlet is connected with a sampling port of the reaction container, the gas outlet is connected with an air pump, and the air pump is connected with the bottom of the reaction container;
the spectrometer is connected with the data processing and control unit;
the data processing and control unit is connected with various pumps, valves, xenon light sources and spectrometers in the device.
The air pump is connected to the bottom of the reaction vessel through a check valve.
The air-ammonia gas conversion valve is connected with the activated carbon gas source processor.
The inlet end of the peristaltic pump is connected with the output end of the three-way electromagnetic valve, two inlet ends of the three-way electromagnetic valve are respectively connected with two container bottles, and the two container bottles are respectively filled with a reaction reagent concentrated sodium hydroxide solution and a cleaning reagent diluted sulfuric acid solution.
The utility model has the advantages that:
1. the ammonia nitrogen is measured by adopting an ultraviolet-visible absorption spectrum method, so that the use of a large amount of chemical reagents in the traditional method is avoided.
2. The ammonia nitrogen concentration is measured in the gas phase, so that the influence of pigments and particles in water on measurement can be avoided, and the measurement accuracy is improved.
3. The water sample acquisition, the reagent addition, the liquid and gas discharge after the test and the like realize automation, and the complicated manual operation steps are avoided.
4. The device can realize the automatic acquisition of seawater sample, need not artifical sample, and one-time measuring time is very short, and one-time sampling can carry out a lot of measurements, makes equipment can realize real-time, continuous detection.
5. The device adds few reagents during measurement, does not need manual configuration and is nontoxic, waste liquid after measurement is nontoxic, and the device can be directly discharged by adding a proper amount of acid without polluting the environment.
6. After every measurement, the peristaltic pump can pump the washing liquid and wash the device, makes reaction vessel keep clean, and the solenoid valve of business turn over air also can open, makes the air in the device circulate with the external world, guarantees the accuracy of next measurement.
Drawings
FIG. 1 is a schematic structural view of the present patent;
FIG. 1, activated carbon source processor 1; 2. an air-ammonia conversion valve; 3. a reaction vessel; 4. a sampling pump; 5. a three-way electromagnetic valve; 6. a peristaltic pump; 7. a drain valve; 8. a check valve; 9. an air pump; 10. a xenon light source; 11. a first lens; 12. an absorption tank; 13. a second lens; 14. an optical fiber; 15. a spectrometer; 16. a data processing and control unit; 17. and (4) exhausting the valve.
FIG. 2 is a flow chart of the detection of the present patent;
FIG. 3 is a schematic view of a reagent inlet port connection.
Detailed Description
The structure of the utility model is shown in figure 1, which comprises a preparation unit, a measurement unit, a data processing and control unit;
the preparation unit consists of a sample introduction part and a reaction container; the sample introduction part comprises a water sample inlet device and a reagent inlet device; the reaction container 3 is of a cylindrical structure, the side surface of the reaction container is provided with an air inlet 31, a sampling port 32, a reagent port 33 and a water inlet 34 from top to bottom in sequence, the bottom of the reaction container is provided with a waste liquid outlet 35, and the upper part of the reaction container is provided with a gas outlet 36;
the water inlet device comprises a sampling pump 4, the water inlet end of the sampling pump 4 is connected with the water sample pool, and the water outlet end is connected with the water inlet 34 of the reaction container 3;
the reagent feeding device comprises a peristaltic pump 6, the output end of the peristaltic pump 6 is connected with the reagent port 33, and the inlet end of the peristaltic pump is connected with the reagent bottle;
the air inlet 31 is connected with the air-ammonia gas conversion valve 2;
the waste liquid outlet 35 is connected with the drain valve 7; the gas outlet 36 is connected with the exhaust valve 17;
the measuring unit comprises an absorption cell 12, a xenon lamp light source 10 and a spectrometer 15, wherein lenses are arranged at the upper end and the lower end of the absorption cell 12; the xenon lamp light source 10 is arranged at the bottom of the absorption cell, a first lens 11 is arranged between the xenon lamp light source 10 and the bottom of the absorption cell 12, the spectrometer is arranged at the upper part of the absorption cell, and a second lens 13 is arranged between the spectrometer and the absorption cell; light emitted by the xenon lamp light source sequentially passes through the bottom end of the absorption cell, the first lens, gas in the absorption cell and the second lens and then reaches the spectrometer 15 through the optical fiber;
the upper part of the absorption cell is a gas inlet 121, the lower end is a gas outlet 122, the gas inlet 121 is connected with a sampling port 32 of the reaction container, the gas outlet 122 is connected with an air pump 9, and the air pump 9 is connected with the bottom of the reaction container 3;
the spectrometer is connected with a data processing and control unit 16;
the data processing and control unit is connected with various pumps, valves, xenon light sources and spectrometers in the device.
The air pump is connected to the bottom of the reaction vessel through a check valve 8.
The air-ammonia gas conversion valve is connected with the activated carbon gas source processor 1.
The inlet end of the peristaltic pump is connected with the output end of the three-way electromagnetic valve 5, two inlet ends of the three-way electromagnetic valve 5 are respectively connected with two container bottles, and the two container bottles are respectively filled with a reaction reagent concentrated sodium hydroxide solution and a cleaning reagent dilute sulfuric acid solution.
The device may be disposed within the housing 20.
The utility model discloses a prepare ammonia nitrogen with gaseous form in the sea water, acquire ammonia ultraviolet spectrum and analysis to this inversion gas concentration.
Principle of measurement
The measurement principle is based on the ultraviolet absorption spectrum of ammonia gas in equilibrium with dissolved ammonia in a water sample. The ammonia gas has a plurality of absorption peaks at the wavelength of 190-205 nm, the absorption peaks are analyzed by adopting a fast Fourier transform method, a characteristic signal of the ammonia gas is extracted, and then the concentration of the ammonia gas is obtained through inversion. Adding 10% sodium hydroxide reagent into seawater sample to make chemical reaction
Figure BDA0002232076530000061
Proceeding to the right to make ammonia nitrogen in seawaterCan be prepared in the form of ammonia, and when the pH of the solution is more than 12, NH4+ in the solution is negligible.
The operation of the whole apparatus will be described below
The device consists of a preparation unit, a circulation unit, a measurement unit and a data processing and control unit. Wherein the preparation unit consists of a sample introduction part and a reaction container. The sample introduction part comprises a water inlet sample and a reagent inlet. The sampling pump controls the water sample inflow, and the air-ammonia conversion valve can selectively control the air and ammonia. The reagent feeding portion container bottle 52 is used for containing a reaction reagent concentrated sodium hydroxide solution, and the container bottle 53 is used for containing a cleaning reagent diluted sulfuric acid solution. The capacity of the container bottle is about 1.5 liters, so that the reagent can meet the requirement of long-time measurement, and the frequent addition of the reagent is avoided. The three-way electromagnetic valve 5 is used for selecting the type of the added reagent, and the peristaltic pump 6 sucks the reagent into the reaction vessel. The reaction container 3 is a glass cylindrical structure with two circular ends, the bottom of the reaction container is provided with a waste liquid outlet, and the upper part of the reaction container is provided with a gas outlet. The circulating unit is a sealed whole formed by connecting a reaction container, an absorption pool, an air pump and the like by using a polyethylene pipe, and a check valve 8 is arranged at an air inlet section at the bottom end of the reaction pool and used for preventing liquid from flowing back.
Two outer containers in the device are used for containing reagent solution, both containers are larger than the reaction container, and the use amount of the reagent in the containers is strictly controlled by a peristaltic pump. The three-way electromagnetic valve can freely switch between extracting reaction reagent and cleaning liquid. The maximum lift of the sampling pump can reach 6 meters, and the sampling pump can directly extract a water sample from the ocean to enter the reaction container and also can extract the water sample from a container for containing the water sample. The gas communication between the gas inside the apparatus and the outside air and between the containers is controlled by the air-ammonia gas changeover valve 2, the exhaust valve 17 and the air pump 9. The reaction vessel provides a location for the production of gas, and the total amount of liquid added per time should be less than one third of the reaction vessel. The absorption cell 12 is the site of gas detection. Ultraviolet fused quartz lenses are arranged on the upper surface and the lower surface of the flow cell, and light is converged on the optical fiber head. The spectrometer 15 selects an instrument with high resolution and accuracy. The air pump 9 provides power for the circulation of gas in the system. The check valve prevents liquid at the bottom of the reaction vessel from flowing back into the flow cell.
When the ultraviolet spectrum of the air needs to be measured, the air-ammonia conversion electromagnetic valve 2 is controlled to allow the air to enter, the air circulates in the circulating unit under the action of the air pump, the air is discharged from the exhaust pipe opening controlled by the exhaust valve 17, after a period of time, the light of the xenon lamp passes through the quartz lens, the gas in the circulating pool, the quartz lens, and the optical fiber transmits an optical signal to the spectrometer.
When the ammonia ultraviolet spectrum needs to be measured, firstly, an air-ammonia conversion electromagnetic valve is adjusted to close an air inlet passage, a gas inlet passage in a reaction container is opened, and an electromagnetic valve of an exhaust port is closed to enable ammonia to circulate in a closed circulation unit. And adjusting the three-way electromagnetic valve to enable the concentrated sodium hydroxide solution to enter the reaction container under the pumping of the peristaltic pump, and enabling a seawater sample to enter the reaction container through the water pump to react with the reagent to prepare ammonia. The reagent inflow and the water sample inflow are strictly controlled by a peristaltic pump and a sampling pump respectively, and an air pump provides power for flowing ammonia; and after the concentration of the gas in the circulating unit is stable, controlling a xenon lamp, a photoelectric detector and a spectrometer to measure.
When the measurement is finished, the waste liquid and the exhaust gas are discharged. In addition, the device needs to be cleaned, and a three-way electromagnetic valve is adjusted to enable dilute sulfuric acid cleaning liquid in an external container to enter the reaction container for cleaning under the action of the peristaltic pump 6.
The utility model discloses in, the spectrum appearance model: ocean optics corporation QE65 Pro; air pump model: KJ-24V; the type of the water pump is as follows: OEM-UB 04; the data processing and control unit is commercially available product such as porphyry PCM3363 from violoxing technologies ltd, beijing.

Claims (4)

1. A quantitative analysis device for ammonia nitrogen in seawater is characterized in that: the device comprises a preparation unit, a measurement unit and a data processing and control unit;
the preparation unit consists of a sample introduction part and a reaction container; the sample introduction part comprises a water sample inlet device and a reagent inlet device; the reaction vessel is of a cylindrical structure, the side surface of the reaction vessel is provided with an air inlet, a sampling port, a reagent port and a water inlet from top to bottom in sequence, the bottom of the reaction vessel is provided with a waste liquid outlet, and the upper part of the reaction vessel is provided with a gas outlet;
the water inlet device comprises a sampling pump, the water inlet end of the sampling pump is connected with the water sample pool, and the water outlet end of the sampling pump is connected with the reaction container;
the reagent feeding device comprises a peristaltic pump, the output end of the peristaltic pump is connected with the reagent port, and the inlet end of the peristaltic pump is connected with the reagent bottle;
the air inlet is connected with an air-ammonia conversion valve;
the waste liquid outlet is connected with a drain valve; the gas outlet is connected with an exhaust valve;
the measuring unit comprises an absorption cell, a xenon lamp light source and a spectrometer, wherein lenses are arranged at the upper end and the lower end of the absorption cell; the xenon lamp light source is arranged at the bottom of the absorption cell, a first lens is arranged between the xenon lamp light source and the bottom of the absorption cell, the upper part of the absorption cell is provided with a spectrometer, and a second lens is arranged between the spectrometer and the absorption cell; light emitted by a xenon lamp light source sequentially passes through the bottom end of the absorption cell, the first lens, gas in the absorption cell and the second lens and then reaches the spectrometer through the optical fiber;
the upper part of the absorption pool is a gas inlet, the lower end of the absorption pool is a gas outlet, the gas inlet is connected with a sampling port of the reaction container, the gas outlet is connected with an air pump, and the air pump is connected with the bottom of the reaction container;
the spectrometer is connected with the data processing and control unit;
the data processing and control unit is connected with various pumps, valves, xenon light sources and spectrometers in the device.
2. The apparatus for quantitatively analyzing ammonia nitrogen in seawater according to claim 1, characterized in that: the air pump is connected to the bottom of the reaction vessel through a check valve.
3. The apparatus for quantitatively analyzing ammonia nitrogen in seawater according to claim 1, characterized in that: the air-ammonia gas conversion valve is connected with the activated carbon gas source processor.
4. The apparatus for quantitatively analyzing ammonia nitrogen in seawater according to claim 1, characterized in that: the inlet end of the peristaltic pump is connected with the output end of the three-way electromagnetic valve, two inlet ends of the three-way electromagnetic valve are respectively connected with two container bottles, and the two container bottles are respectively filled with a reaction reagent concentrated sodium hydroxide solution and a cleaning reagent diluted sulfuric acid solution.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110596031A (en) * 2019-10-14 2019-12-20 中国科学院烟台海岸带研究所 Quantitative analysis device for ammonia nitrogen in seawater

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110596031A (en) * 2019-10-14 2019-12-20 中国科学院烟台海岸带研究所 Quantitative analysis device for ammonia nitrogen in seawater

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