CN114280247A - Gaseous nitric acid generating device and method for monitoring environmental atmosphere - Google Patents
Gaseous nitric acid generating device and method for monitoring environmental atmosphere Download PDFInfo
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- CN114280247A CN114280247A CN202111635575.7A CN202111635575A CN114280247A CN 114280247 A CN114280247 A CN 114280247A CN 202111635575 A CN202111635575 A CN 202111635575A CN 114280247 A CN114280247 A CN 114280247A
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Abstract
The invention discloses a gaseous nitric acid generating device and a gaseous nitric acid generating method for monitoring environmental atmosphere, wherein the device at least comprises synthetic air, a spiral diffusion pipe, a mass flow controller, a water suction pump, an electromagnetic drive micro pump, a standard gas generating solution, a water cooling tank, constant temperature water, a waste liquid barrel and a plurality of tetrafluoride pipes; the nitrate and the spiral diffusion pipe are used, the mixed liquid of sodium nitrate and 1% sulfuric acid solution is pumped into the spiral diffusion pipe by using an electromagnetic drive micro pump, gas-liquid mixing is carried out on the mixed liquid and the blown synthetic air in the spiral diffusion pipe, and then gas-liquid separation is carried out, so that gaseous nitric acid gas is obtained. The spiral diffusion pipe is adopted for gas-liquid mixing, so that the concentration of nitric acid in the discharged gas can be stabilized while the gas and the liquid are fully mixed; the full-automatic sample introduction and waste liquid collection are realized; effectively improve gaseous HNO in environmental atmosphere monitoring3The accuracy of the measurement; and the concentration of the directly generated gas containing nitric acid is flexible and adjustable, the sensitivity is high, the solution is easy to obtain, and the starting and the maintenance are simple and convenient.
Description
Technical Field
The invention belongs to the technical field of environmental atmosphere monitoring, relates to a gaseous nitric acid generation technology, and particularly relates to a device and a method for generating gaseous nitric acid based on a wet chemical method.
Background
Gaseous nitric acid (HNO)3) Is one of the most important trace reactive odd-nitrogen compounds in the atmosphere and plays an important role in both tropospheric and stratospheric atmospheric chemistry. With the increasing proportion of nitrate content in particulate matters in winter in recent years, gaseous nitric acid is used as an important precursor of nitrate, the level of the nitric acid in the ambient atmosphere and the chemical reaction path need to be researched urgently, and a reliable gaseous nitric acid source is urgently needed to assist the research work of a laboratory and the observation work of an external field.
Since gaseous nitric acid can react or adsorb on various surfaces, conventional gas preparation methods such as permeation tube and diffusion tube techniques often used in volatile organic compounds are difficult to apply to the preparation of gaseous nitric acid. In the reported laboratory work, the reaction of sulfuric acid and fuming nitric acid is commonly used for preparing gaseous nitric acid on site, although the method can obtain nitric acid with a certain concentration, the operation condition is harsh, and the final gaseous nitric acid product can be obtained only through the continuous cycle process of freezing and unfreezing, so that the complicated preparation mode is difficult to develop in a common laboratory, the calibration of an online monitoring gaseous nitric acid instrument in an external field is impossible, and in addition, the requirements of calibration of different gradients in the calibration of an environmental atmosphere monitoring instrument are difficult to realize.
Therefore, the existing device and process for preparing gaseous nitric acid are complex in preparation process and harsh in preparation conditions, and cannot solve the problems of concentration control and adjustment, and a generation device which can generate gaseous nitric acid under laboratory and external field observation conditions more easily needs to be provided for overcoming the defects.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a gaseous nitric acid generating device and a gaseous nitric acid generating method for monitoring environmental atmosphere, which can be used for monitoring environmental atmosphereReflect the collection and measurement accuracy of the environmental atmosphere monitoring instrument for gaseous nitrous acid more truly, and effectively improve the gaseous HNO in the environmental atmosphere monitoring3The accuracy of the measurement.
Gaseous HNO in ambient atmosphere3In order to more truly reflect the collecting and measuring accuracy of the whole instrument for the gaseous nitrous acid, the gaseous HNO is used3The generating device calibrates the accuracy of the instrument. The invention realizes a device which is suitable for external field observation and can be simply built and can generate gaseous nitric acid gas with a certain concentration range (detection limit of-10 ppbv), thereby ensuring that gaseous HNO can be detected in the external field observation3The on-line calibration of the overall performance of the detecting instrument can meet the requirements of portability and simplicity of the generating device in external field observation.
The technical scheme provided by the invention is as follows:
a method for generating gaseous nitric acid (nitric acid gas) for monitoring environmental atmosphere is characterized in that a suitable spiral diffusion tube is designed, the existing gaseous nitric acid generation method combining fuming nitric acid and a freezing and thawing technology is replaced by a method combining nitrate and the spiral diffusion tube, and gaseous nitric acid is finally generated by a technology of gas-liquid mixing and then separation. The technical scheme of the invention is that a mixed solution of sodium nitrate and 1% sulfuric acid solution is pumped into a spiral diffusion tube by using an electromagnetic drive micro pump, gas-liquid mixing is carried out on the mixed solution and blown synthetic air in the spiral diffusion tube, and then gas-liquid separation is carried out, so that gas containing gaseous nitric acid with the concentration detection limit of-10 ppbv is finally obtained.
The method for generating the gaseous nitric acid comprises the following steps:
1) designing a spiral diffusion pipe, and sequentially connecting a synthetic air container, a mass flow meter and the spiral diffusion pipe, so that synthetic air in the synthetic air container enters the spiral diffusion pipe after being controlled by the mass flow meter;
2) placing the standard gas generation solution container in a water cooling tank (the temperature is 4 ℃); connecting the standard gas generation solution container and the first electromagnetic driving micro pump, so that the solution (sodium nitrate and 1% sulfuric acid solution) in the standard gas generation solution container can be pumped into the spiral diffusion tube through the first electromagnetic driving micro pump;
3) the synthetic air and the standard gas generating solution react in the spiral diffusion tube; the gas discharged from the gas outlet of the spiral diffusion tube is the gas containing gaseous nitric acid (nitric acid gas); and pumping waste liquid generated by the reaction into a waste liquid barrel through a second electromagnetic drive micro pump for treatment.
Through the operating condition who controls first electromagnetic drive micropump and mass flowmeter, take place the speed of solution pump income spiral diffusion tube and synthetic air inflow spiral pipe's velocity of flow through adjusting the mark gas, change the state that the gas-liquid combines to can adjust the concentration of output gaseous state nitric acid, the gas that contains gaseous state nitric acid that finally produces can let in online gaseous state nitric acid detection device.
The invention also provides a gaseous nitric acid (nitric acid gas) generating device for monitoring the ambient atmosphere, which at least comprises synthetic air (a container), a spiral diffusion tube, a mass flow controller, a water pump, an electromagnetic drive micro pump, a water cooling tank, a standard gas generating solution (sodium nitrate and 1% sulfuric acid solution) (the container), constant temperature water (the container), a water cooling tank, a waste liquid barrel and a plurality of 1/4-inch and 1/16-inch tetrafluoro pipes.
In specific implementation, the structure of the spiral diffusion pipe is designed, and the spiral diffusion pipe is provided with an air inlet, an air outlet, a liquid inlet, a liquid outlet and a constant-temperature water inlet and outlet; wherein the outer diameters of the air inlet and the air outlet are the same (both are 6 mm); the outer diameters of the liquid inlet and the liquid outlet are the same (both 4mm), and the inner diameters are the same (both 2 mm); the winding diameter of the spiral diffusion pipe is 2cm, 5 turns of winding are performed, and the inner diameter of the pipe of the spiral diffusion pipe is 2 mm. The synthetic air outlet is connected with a gas inlet of the mass flow meter through an 1/4-inch tetrafluoride pipe; the mass flow meter gas outlet is connected with the spiral diffusion pipe gas inlet through an 1/4-inch tetrafluoride pipe; a water outlet of constant temperature water (20 ℃) is connected with a liquid inlet of a water pump through a 1/4-inch tetrafluoride pipe; a liquid outlet of the water suction pump is connected with a constant-temperature water inlet of the spiral diffusion pipe through an 1/4-inch tetrafluoro pipe; the constant-temperature water outlet of the spiral diffusion pipe is connected with the constant-temperature water (20 ℃) inlet through an 1/4-inch tetrafluoride pipe; the standard gas generating solution (sodium nitrate and 1% sulfuric acid solution) is placed in the water cooling tank; the standard gas generating solution is connected with a liquid inlet of a first electromagnetic driving micro pump through 1/16 tetrafluoride tubes, a liquid outlet of the first electromagnetic driving micro pump is connected with a liquid inlet of a spiral diffusion tube through 1/16 tetrafluoride tubes, a liquid outlet of the spiral diffusion tube is connected with a liquid inlet of a second electromagnetic driving micro pump through 1/16 tetrafluoride tubes, and a liquid outlet of the second electromagnetic driving micro pump is connected with a waste liquid barrel through 1/16 tetrafluoride tubes.
When the gaseous nitric acid gas generating device works, synthetic air enters the mass flow meter, gas (1-2L/min) controlled by the mass flow meter enters the spiral diffusion tube, solution in standard gas generating solution (sodium nitrate and 1% sulfuric acid solution) placed in a water cooling tank (with the temperature of 4 ℃) is pumped into the spiral diffusion tube through the first electromagnetic driving micro-pump, waste liquid is pumped into the waste liquid barrel through the second electromagnetic driving micro-pump for treatment, and gas discharged from the gas outlet in the spiral diffusion tube is gas containing gaseous nitric acid. Through the operating condition who controls first electromagnetic drive micropump and mass flowmeter, take place the speed of solution pump income spiral diffusion tube and synthetic air inflow spiral pipe's velocity of flow through adjusting the mark gas, change the state that the gas-liquid combines to can adjust the concentration of output gaseous state nitric acid, the gas that contains gaseous state nitric acid that finally produces can let in online gaseous state nitric acid detection device.
Compared with the prior art, the technical scheme of the invention has the following technical advantages:
firstly, the invention adopts the spiral diffusion tube to mix gas and liquid, ensures the gas and liquid to be fully mixed and can stabilize the concentration of nitric acid in the discharged gas.
Secondly, the invention combines the spiral diffusion tube and the electromagnetic drive micro pump to realize full-automatic sample introduction and waste liquid collection.
The invention can directly generate gas containing nitric acid, and has the advantages of flexible and adjustable concentration, high sensitivity, easy solution acquisition, and simple and convenient start and maintenance.
Drawings
FIG. 1 is a block diagram of an apparatus for generating gaseous nitric acid in accordance with an embodiment of the present invention;
wherein, 1-synthetic air (container); 1-2-mass flow controller; 1-3-a helical diffuser tube; 1-4-1 and 1-4-2 are all electromagnetic drive micro pumps; 1-5-standard gas generating solution (sodium nitrate and 1% sulfuric acid solution) container; 1-6-waste liquid barrel; 1-7-a water pump; 1-8-constant temperature water (container); 1-9-water cooling tank.
FIG. 2 is a block diagram of a spiral diffuser designed in accordance with the present invention;
wherein the outer diameter of the 1-3-1-air inlet and the outer diameter of the 1-3-air outlet are both 6 mm; 1-3-2-the liquid inlet and 1-3-4-the liquid outlet are both 4mm in outer diameter and 2mm in inner diameter; 1-3-5-constant temperature water inlet and outlet; the standard of the spiral diffusion tube is that the winding diameter is 2cm, the winding is 5 circles, and the inner diameter of the spiral diffusion tube is 2 mm.
Detailed Description
The invention will be further described by way of examples, without in any way limiting the scope of the invention, with reference to the accompanying drawings.
The invention provides a gaseous nitric acid (nitric acid gas) generating device and a generating method thereof for monitoring environmental atmosphere. The method for generating the gaseous nitric acid comprises the following steps:
1) the synthetic air container, the mass flow meter and the spiral diffusion pipe are connected in sequence, so that synthetic air in the synthetic air container enters the spiral diffusion pipe after being controlled by the mass flow meter;
2) placing the standard gas generation solution container in a water cooling tank (the temperature is 4 ℃); connecting the standard gas generation solution container and the first electromagnetic driving micro pump, so that the solution (sodium nitrate and 1% sulfuric acid solution) in the standard gas generation solution container can be pumped into the spiral diffusion tube through the first electromagnetic driving micro pump;
3) the synthetic air and the standard gas generating solution react in the spiral diffusion tube; the gas discharged from the gas outlet of the spiral diffusion tube is the gas containing gaseous nitric acid (nitric acid gas); and pumping waste liquid generated by the reaction into a waste liquid barrel through a second electromagnetic drive micro pump for treatment.
In specific implementation, the gaseous nitric acid generator at least comprises synthetic air (a container), a spiral diffusion tube, a mass flow controller, a water pump, an electromagnetic drive micro pump, a water cooling tank, a standard gas generating solution (sodium nitrate and 1% sulfuric acid solution) (the container), constant temperature water (the container), a waste liquid barrel and a plurality of 1/4-inch and 1/16-inch tetrafluoro tubes.
FIG. 1 is a view showing a device for generating gaseous nitric acid gas according to an embodiment of the present invention, as shown in FIG. 1, synthetic air 1-1 enters a 1-3 spiral diffusion tube after the flow rate is adjusted by a mass flow controller 1-2, a standard gas generating liquid 1-5 is placed in a water cooling tank 1-9 to keep the temperature of a solution in the standard gas generating liquid 1-5 at 4 ℃, the standard gas generating liquid 1-5 is connected to a liquid inlet of a first electromagnetically driven micro-pump 1-4-1, a liquid inlet of the spiral diffusion tube 1-3 is connected to a liquid outlet of the first electromagnetically driven micro-pump 1-4-1, a liquid outlet of the spiral diffusion tube 1-3 is connected to a liquid inlet of a second electromagnetically driven micro-pump 1-4-2, a liquid outlet of the second electromagnetically driven micro-pump 1-4-2 is connected to a waste liquid tank 1-6, the liquid inlet of the water pump 1-7 is connected with the constant temperature water 1-8, the liquid outlet of the water pump 1-7 is connected with the constant temperature water inlet of the spiral diffusion pipe 1-3, and the constant temperature water outlet of the spiral diffusion pipe 1-3 is connected with the constant temperature water 1-8.
FIG. 2 shows the structure of the spiral diffuser pipe designed by the present invention, which is provided with an air inlet 1-3-1, an air outlet 1-3-3, a liquid inlet 1-3-2, a liquid outlet 1-3-4, and a constant temperature water inlet and outlet 1-3-5. Wherein the outer diameters of the air inlet 1-3-1 and the air outlet 1-3-3 are both 6 mm; the outer diameters of the liquid inlet 1-3-2 and the liquid outlet 1-3-4 are both 4mm, and the inner diameters thereof are both 2 mm; the winding diameter of the spiral diffusion pipe is 2cm, 5 turns of winding are performed, and the inner diameter of the pipe of the spiral diffusion pipe is 2 mm.
The working process of the device during operation is concretely that the flow of the synthetic air in the synthetic air container 1-1 is regulated by a mass flow controller 1-2, the synthetic air regulated by the mass flow controller 1-2 enters a spiral diffusion pipe 1-3, simultaneously, a standard gas generating liquid (sodium nitrate and 1% sulfuric acid solution) 1-5 placed in a water cooling box 1-9 is pumped into the spiral diffusion pipe 1-3 by a first electromagnetic driving micro-pump 1-4-1, the liquid with nitrate ions in the spiral diffusion pipe 1-3 is mixed with the synthetic air in a gas-liquid mode, the gas discharged from an air outlet of the spiral diffusion pipe 1-3 is the gas containing gaseous nitric acid with a certain concentration (detection limit of-10 ppbv), and the waste liquid after gas-liquid mixing passes through a liquid outlet of the spiral diffusion pipe 1-3 and passes through a second electromagnetic driving micro-pump 1-4-2 pump And (3) entering a waste liquid barrel 1-6 for treatment, wherein in the running process of the device, constant-temperature water 1-8 is continuously and circularly pumped into the spiral diffusion pipe 1-3 through a water pump 1-7.
It is noted that the disclosed embodiments are intended to aid in further understanding of the invention, but those skilled in the art will appreciate that: various alternatives and modifications are possible without departing from the invention and scope of the appended claims. Therefore, the invention should not be limited to the embodiments disclosed, but the scope of the invention is defined by the appended claims.
Claims (10)
1. A gaseous nitric acid generation method for environmental atmosphere monitoring is characterized in that nitrate and a spiral diffusion tube are used, a mixed solution of sodium nitrate and 1% sulfuric acid solution is pumped into the spiral diffusion tube by using an electromagnetic drive micro pump, gas-liquid mixing is carried out on the mixed solution and blown synthetic air in the spiral diffusion tube, and then gas-liquid separation is carried out, so that gaseous nitric acid gas is obtained; the method comprises the following steps:
1) designing a spiral diffusion tube; the synthetic air container, the mass flow meter and the spiral diffusion pipe are connected in sequence, so that synthetic air in the synthetic air container enters the spiral diffusion pipe after being controlled by the mass flow meter;
the spiral diffusion pipe is provided with an air inlet, an air outlet, a liquid inlet, a liquid outlet and a constant-temperature water inlet and outlet; wherein, the outer diameters of the air inlet and the air outlet are the same; the outer diameters of the liquid inlet and the liquid outlet are the same, and the inner diameters of the liquid inlet and the liquid outlet are the same; the winding diameter of the spiral diffusion pipe is 2cm, the spiral diffusion pipe is wound for a plurality of circles, and the inner diameter of the pipe of the spiral diffusion pipe is 2 mm;
2) placing the standard gas generating solution container in a water cooling box; connecting the standard gas generation solution container and the first electromagnetic drive micro pump, so that the solution in the standard gas generation solution container can be pumped into the spiral diffusion tube through the first electromagnetic drive micro pump; the solution in the standard gas generation solution container is sodium nitrate and 1 percent sulfuric acid solution;
3) the synthetic air and the standard gas generating solution react in the spiral diffusion tube; the gas discharged from the gas outlet of the spiral diffusion tube is the gas containing gaseous nitric acid;
the speed of the standard gas generation solution pumped into the spiral diffusion tube and the flow rate of the synthetic air flowing into the spiral tube are adjusted by controlling the first electromagnetic drive micro pump and the mass flow meter, and the gas-liquid combination state is changed, so that the concentration of the output gaseous nitric acid is adjusted.
2. The method of claim 1, wherein the waste liquid from the reaction is pumped into a waste liquid tank by a second electromagnetically driven micro pump; the finally generated gas containing gaseous nitric acid can be introduced into an online gaseous nitric acid detection device for detection.
3. The method of claim 1, wherein in step 2), the temperature of the water cooling tank is 4 ℃.
4. The method of claim 1, wherein the gas from step 1) is fed into the spiral diffuser at a flow rate of 1-2L/min.
5. A gaseous nitric acid generating device for monitoring ambient atmosphere is characterized by at least comprising synthetic air, a spiral diffusion tube, a mass flow controller, a water suction pump, an electromagnetic drive micro pump, a standard gas generating solution, constant temperature water, a water cooling tank, a waste liquid barrel and a plurality of tetrafluoride tubes; the standard gas generating solution adopts a mixed solution of sodium nitrate and 1% sulfuric acid solution; wherein:
the spiral diffusion pipe is provided with an air inlet, an air outlet, a liquid inlet, a liquid outlet and a constant-temperature water inlet and outlet; wherein, the outer diameters of the air inlet and the air outlet are the same; the outer diameters of the liquid inlet and the liquid outlet are the same, and the inner diameters of the liquid inlet and the liquid outlet are the same; the winding diameter of the spiral diffusion pipe is set to be 2cm, the spiral diffusion pipe is wound for 5 circles, and the inner diameter of the spiral diffusion pipe is set to be 2 mm;
the synthetic air outlet is connected with a gas inlet of the mass flow meter; the gas outlet of the mass flow meter is connected with the gas inlet of the spiral diffusion pipe; the constant-temperature water outlet is connected with the liquid inlet of the water pump; a liquid outlet of the water suction pump is connected with a constant-temperature water inlet of the spiral diffusion pipe; the constant-temperature water outlet of the spiral diffusion pipe is connected with the constant-temperature water inlet; the standard gas generating solution is placed in the water cooling box; the standard gas generating solution is connected with a first electromagnetic drive micro-pump liquid inlet, a first electromagnetic drive micro-pump liquid outlet is connected with the spiral pipe liquid inlet, a spiral diffusion pipe liquid outlet is connected with a second electromagnetic drive micro-pump liquid inlet, and a second electromagnetic drive micro-pump liquid outlet is connected with the waste liquid barrel; the phases are connected through a tetrafluoride pipe;
when the gaseous nitric acid gas generating device works, synthetic air enters the mass flow meter, the gas controlled by the mass flow meter enters the spiral diffusion tube, standard gas generating solution placed in the water cooling tank is pumped into the spiral diffusion tube through the first electromagnetic driving micro pump, waste liquid is pumped into the waste liquid barrel through the second electromagnetic driving micro pump for treatment, and gas discharged from the gas outlet of the spiral diffusion tube is the gas containing gaseous nitric acid.
6. The apparatus of claim 5 wherein the tetrafluoride tube comprises 1/4 inches tetrafluoride tube and 1/16 inches tetrafluoride tube; the outer diameters of the air inlet and the air outlet of the spiral diffusion pipe are both 6 mm; the outer diameter of the liquid inlet and the outer diameter of the liquid outlet are both 4mm, and the inner diameter is both 2 mm).
7. A gaseous nitric acid generating apparatus for ambient atmosphere monitoring according to claim 6, wherein:
the synthetic air outlet is connected with a gas inlet of the mass flow meter through an 1/4-inch tetrafluoride pipe; a mass flow meter gas outlet is connected with the spiral diffusion pipe gas inlet through an 1/4-inch tetrafluoride pipe; the constant-temperature water is connected with a liquid inlet of a water pump through an 1/4-inch tetrafluoro pipe; a liquid outlet of the water suction pump is connected with a constant-temperature water inlet of the spiral diffusion pipe through an 1/4-inch tetrafluoro pipe; a constant-temperature water outlet of the spiral diffusion pipe is connected with constant-temperature water through an 1/4-inch tetrafluoride pipe; the standard gas generating solution is connected with a liquid inlet of a first electromagnetic driving micro pump through a 1/16 tetrafluoride tube, a liquid outlet of the first electromagnetic driving micro pump is connected with a liquid inlet of a spiral diffusion tube through a 1/16 tetrafluoride tube, a liquid outlet of the spiral diffusion tube is connected with a liquid inlet of a second electromagnetic driving micro pump through a 1/16 tetrafluoride tube, and a liquid outlet of the second electromagnetic driving micro pump is connected with a waste liquid barrel through a 1/16 tetrafluoride tube.
8. The gaseous nitric acid generator for environmental atmospheric monitoring of claim 6, wherein the gas controlled by the mass flow meter enters the spiral diffuser at 1-2L/min.
9. The gaseous nitric acid generator of claim 6, wherein the water cooled tank is set at a temperature of 4 degrees celsius.
10. The gaseous nitric acid generating apparatus for ambient atmosphere monitoring of claim 6, wherein the constant temperature water temperature is set to 20 degrees celsius.
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Citations (1)
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| CN107228923A (en) * | 2017-06-27 | 2017-10-03 | 中国科学院化学研究所 | A kind of preparation method of standard gaseous nitrous acid and generation system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107228923A (en) * | 2017-06-27 | 2017-10-03 | 中国科学院化学研究所 | A kind of preparation method of standard gaseous nitrous acid and generation system |
Non-Patent Citations (1)
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| 杨闻达等: "一种气态亚硝酸制备技术的研发", 《环境化学》 * |
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