CN111579318B - Sampling device and sampling method applied to determination of ammonium nitrogen isotope - Google Patents
Sampling device and sampling method applied to determination of ammonium nitrogen isotope Download PDFInfo
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- CN111579318B CN111579318B CN202010516541.5A CN202010516541A CN111579318B CN 111579318 B CN111579318 B CN 111579318B CN 202010516541 A CN202010516541 A CN 202010516541A CN 111579318 B CN111579318 B CN 111579318B
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- G01N1/00—Sampling; Preparing specimens for investigation
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Abstract
The invention discloses a sampling device applied to determination of ammonium nitrogen isotopes, which comprises an isolation cover, wherein an air inlet hole and an air outlet hole are arranged on the isolation cover, an air inlet pipe is arranged on the air inlet hole, the air outlet hole is connected with an exhaust pipe, the exhaust pipe is connected with a gas sampling device, the air inlet pipe is connected with an air filtering device, the air filtering device comprises a first vacuum pump, a first gas washing bottle and a drying bottle which are connected in series, the air filtering device is arranged in a cooling device, a first temperature and humidity sensor which is arranged towards the ground direction is arranged in the isolation cover, and a second temperature and humidity sensor which is arranged towards the ground direction is arranged outside the isolation cover.
Description
Technical Field
The invention relates to the field of detection instruments, in particular to a sampling device and a sampling method applied to determination of ammonium nitrogen isotopes.
Background
Ammonia (NH) 3 ) As the most important alkaline gas in the atmosphere, it has an important influence on the environment. NH (NH) 3 With acid gases (SO) in the air 2 ，NO x ) The reaction forms ammonium salt, is PM 2，5 The important constituent components of (1). At the same time, NH 3 And NH 4 + Entering the surface ecosystem through dry and wet settlement is an important form of nitrogen settlement. NH in the atmosphere 3 There are many sources of contribution, the most important being agricultural sources. Previous researchIt was shown that NH in the atmosphere 3 The majority of the fertilizer is from agricultural production and life, and nearly 23% of the fertilizer is volatilized after the farmland is fertilized.
Determination of NH 3 The source contribution of (2) is correspondingly controlled, and NH can be effectively reduced 3 Is discharged. At present, two methods for tracing the source of pollutants in the air are a diffusion model method and a receptor model method. Isotopic tracing technology has gained a number of applications in recent years as a receptor model method, in NH 3 The source tracing method has good prospect. Isotopic tracing techniques require accurate source profiles, but agricultural sources are the major NH 3 The sources of contribution are very broad in their source spectrum and need further refinement.
The refined source spectrum needs to carry out refined in-situ measurement on a source, and an active method and a passive method are adopted for the sampling device for soil ammonia volatilization at present. The passive method can damage the soil structure, and the measurement of the ammonium nitrogen isotope has the requirement of detection limit, so that the passive method needs longer time for sampling, which is not beneficial to the improvement of time resolution. The active method is mainly aeration method, as shown in figure 1, the soil is provided with a transparent cover which is provided with two openings, one end is provided with a long pipe, and the other end is connected with NH in the transparent cover 3 The collection system is connected with the atmosphere through a long pipe, and the air extracting pump extracts the volatile NH from the atmosphere and the soil 3 Are collected into a gas washing bottle together; setting background NH at the same height as the long tube 3 The collecting device collects background NH 3 The two are buckled to obtain the volatile NH of the soil 3 . However, this is not suitable for the determination of ammonium nitrogen isotopes, which are not simple subtractive processes and therefore require NH that is volatile to the soil 3 And (4) independently sampling. Replacing the long tube with a gas washing device to remove background NH 3 Is an effective way, but is found in the actual test process because of soil NH 3 The volatilization is strongly influenced by the light, a transparent cover is needed, the temperature of the cover can be increased by over 10 ℃ in a few minutes, particularly in the noon with strong light, the water vapor in the soil can be quickly evaporated to be condensed into water drops on the inner wall of the cover, and NH 3 Is water-soluble, soil-volatile NH 3 Can be adsorbed in a large amount in water drops, which can affect the absorption efficiency of the gas washing bottle,and causes the ammonium nitrogen isotope to produce fractionation influence results; while too high a temperature may affect NH 3 Volatilization of [4] Resulting in testing of the resulting NH 3 The concentration deviates from the actual. There is therefore a need for improvements to existing devices.
Disclosure of Invention
In order to solve the problems, the invention provides a detection device capable of preventing condensation water drops of air in an isolation cover and taking out ammonia gas in the air, and the specific scheme is as follows:
the utility model provides a be applied to sampling device of ammonium nitrogen isotope survey, includes isolated cover, and isolated cover is last to install inlet port and venthole, install the intake pipe on the inlet port, the venthole is connected with the exhaust tube, and the exhaust tube is connected with gaseous sampling device, the intake pipe is connected with air filter, air filter includes first vacuum pump, first gas washing bottle and the drying bottle that concatenates in proper order, air filter sets up in cooling device, installs the first temperature and humidity sensor that sets up towards the ground direction in the isolated cover, and the outside of isolated cover is provided with the second temperature and humidity sensor that sets up towards the ground direction.
Furthermore, the inlet end of the first gas washing bottle is connected with a first vacuum pump through a guide pipe, a first rotor flowmeter is installed on the guide pipe, the outlet end of the first gas washing bottle is connected with the drying bottle through the guide pipe, and the outlet end of the drying bottle is connected with an air inlet pipe.
Further, the gas sampling device comprises a second gas washing bottle and a second vacuum pump, the inlet end of the second gas washing bottle is connected with an exhaust pipe, the outlet end of the second gas washing bottle is connected with the second vacuum pump through a guide pipe, a second rotameter is mounted on the guide pipe, and the gas sampling device is arranged in another cooling device.
Further, first gas washing bottle and second gas washing bottle are round bottom absorption bottle, and the bottle height of round bottom absorption bottle is 15cm, and solid quartz bubbling ball is installed to the absorption tube tip in the round bottom absorption bottle, and the radius difference of solid quartz bubbling ball and round bottom absorption bottle is 0.5cm.
Further, cooling device includes the heat preservation groove, is provided with semiconductor refrigeration piece and fan on the inside wall of heat preservation groove, air filter and gaseous sampling device place respectively in the heat preservation groove that corresponds, semiconductor refrigeration piece and fan all pass through the wire electricity with temperature controller and are connected.
Furthermore, two heat preservation grooves are all installed on the base, a power module is installed in the base, the power module is respectively electrically connected with the time controller, the temperature controller and the thermometer, the semiconductor refrigeration piece and the fan are respectively electrically connected with the temperature controller through leads, and the first vacuum pump and the second vacuum pump are respectively electrically connected with the time controller through leads.
Further, first temperature and humidity sensor and second temperature and humidity sensor pass through the wire electricity with the warm and humid acidimeter respectively and are connected, and isolated covering is seted up the wire guide through the wire, and the warm and humid acidimeter passes through the wire electricity with temperature controller and power module respectively and is connected.
Further, the outside of tubes parcel of intake pipe has insulation material, and the intake pipe extends to the bottom position in the isolated cover from isolated cover outside, and the exit end of intake pipe is provided with the shower nozzle that is conical structure, the bottom surface of shower nozzle is airtight structure, has seted up a plurality of exhaust holes on the conical surface of shower nozzle.
Further, a sampling method of the sampling device applied to the determination of the ammonium nitrogen isotope is characterized by comprising the following specific sampling steps:
step 2, judging whether temperature difference exists between the inside and the outside of the isolation cover according to the temperatures detected by the first temperature and humidity sensor and the second temperature and humidity sensor, if so, adjusting the temperature of a cooling device where the air filtering device is located to enable the temperature in the cooling device to be lower than the temperature outside the isolation cover, then opening a first vacuum pump to extract air, filtering and drying the air through the air filtering device, cooling the air through the cooling device, and then mixing and diluting the air with water vapor volatilized by soil in the isolation cover;
and 3, when the temperature in the isolation cover is close to the external temperature, carrying out gas sampling work through a gas sampling device.
Further, in the step 2, the air flow rate transmitted by the first vacuum pump is controlled by adjusting the first rotor flowmeter, so that the humidity in the isolation cover is prevented from reaching a water vapor saturation state of 100%, and water vapor condensation is avoided;
and 3, when the gas sampling device samples in the step 3, setting a second rotor flow meter to control the flow rate of the second vacuum pump to be consistent with the flow rate of the first vacuum pump.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the air filtering device is arranged at the exhaust pipe, the actual nitrogen content in the cover is obtained without subtracting the nitrogen content in the air from the nitrogen content collected in the cover, an accurate value can be directly measured from the gas sampling device, and the error is reduced;
2. in the invention, the first gas washing bottle is connected with the drying bottle in series and is placed in the cooling device to keep a lower temperature. The atmosphere is dried by ammonia removal and cooled down via this treatment unit. Let in isolated cover, with the volatile steam of soil in, with the air intensification that sunshine irradiation leads to in, prevent the steam condensate and completely cover in the high temperature, the effectual efficiency that improves the sampling, avoided the fractionation of ammonium nitrogen isotope.
3. The first vacuum pump that the isolated cover was sent into to the extraction air and the second vacuum pump that extracts the interior air of isolated cover work simultaneously, and the flow is the same, maintains the interior ordinary pressure of cover, avoids taking outside air out from soil hole, has improved the sampling accuracy.
4. The gas washing bottle is a round bottom absorption bottle, and a small amount of liquid can achieve the effect of complete absorption by combining a solid quartz bubble forming ball with the radius difference within 0.5cm. The gas washing bottle is higher than 15cm and is also placed in the cooling device, and the absorption liquid is condensed and falls into the absorption liquid again before evaporating to the gas outlet, so that the water loss is effectively inhibited. Compared with the existing method, the time resolution of sampling is improved.
Drawings
FIG. 1 is a schematic diagram of a conventional aeration measuring apparatus;
FIG. 2 is a view showing the construction of the detecting instrument of the present invention;
fig. 3 is a structural view of the head.
Reference numerals are as follows:
1. an air exhaust pipe; 2. a first rotor flowmeter; 3. a second rotameter; 4. a first vacuum pump; 5. a second vacuum pump; 6. a time controller; 7. a temperature controller; 8. a thermo-hygrometer; 9. a power supply module; 10. a first gas washing bottle; 11. a second gas washing bottle; 12. drying the bottle; 13. a heat preservation groove; 14. a semiconductor refrigerating sheet; 141. a fan; 15. an air inlet pipe; 16. an isolation shield; 17. a sealing plate; 18. a first temperature and humidity sensor; 19. a second temperature and humidity sensor; 20. fixing the frame plate; 21. a spray head; 22. a conical surface; 23. an exhaust hole; 24. a base; 25. NH in the transparent cover 3 A collection device; 26. background NH 3 And (4) a collecting device.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
As shown in fig. 2, a be applied to sampling device of ammonium nitrogen isotope survey, including isolated cover 16, isolated cover 16 is transparent organic glass material, and isolated cover 16 is the cylinder structure, installs inlet port and venthole on the isolated cover 16, install intake pipe 15 on the inlet port, intake pipe 15 is connected with air filter, and air filter sets up in the cooling device that corresponds, the venthole is connected with exhaust tube 1, and exhaust tube 1 is connected with gaseous sampling device, and gaseous sampling device sets up in the cooling device that corresponds.
The air filtering device comprises a first gas washing bottle 10, an air inlet pipe 15 is installed on the air inlet hole, a heat insulating material wraps the outside of the air inlet pipe 15, the air inlet pipe 15 extends to the bottom position inside the isolation cover 16 from the outside of the isolation cover 16, as shown in fig. 2, a spray head 21 in a conical structure is arranged at the outlet end of the air inlet pipe 15, the bottom surface of the spray head 21 is in a closed structure, and a plurality of exhaust holes 23 are formed in a conical surface 22 of the spray head 21. The function is to scatter the cold dry air upwards and mix the cold dry air with the air in the isolation cover 16, thereby avoiding the influence of the too low soil temperature on the volatilization of the ammonia caused by the direct spraying into the ground.
The air filtering device comprises a first gas washing bottle 10, wherein the inlet end of the first gas washing bottle 10 is connected with a first vacuum pump 4 through a guide pipe, a first rotor flowmeter 2 is installed on the guide pipe, the outlet end of the first gas washing bottle 10 is connected with a drying bottle 12, and the outlet end of the drying bottle 12 is connected with an air inlet pipe 15.
The gas sampling device comprises a second gas washing bottle 11, the inlet end of the second gas washing bottle 11 is connected with an exhaust pipe 1, the outlet end of the second gas washing bottle 11 is connected with a second vacuum pump 5 through a guide pipe, and a second rotameter 3 is installed on the guide pipe. In order to meet the requirement of detection limit of the ammonium nitrogen isotope, complete absorption cannot be guaranteed by using a mode of connecting two absorption bottles in series, so that the second gas washing bottle 11 uses a circular quartz foaming ball with a higher foaming effect to improve the absorption rate, the radius difference between the circular quartz foaming ball and the gas washing bottle (comprising the first gas washing bottle 10 and the second gas washing bottle 11) is within 0.5cm, the amount of solution is reduced as much as possible by using a round bottom absorption bottle, the detection limit of the ammonium nitrogen isotope can be reached within shorter sampling time, and the time resolution is improved. Too high foaming effect makes many tiny water droplets taken away by the air current, can carry away ammonium ion simultaneously, also can lead to the fractionation of ammonium nitrogen isotope when influencing absorption solution ammonium ion concentration. The addition of glycerol is an effective method for keeping moisture, but a large amount of glycerol has great influence on the measurement of ammonium ion concentration and ammonium nitrogen isotopes, so that the second gas washing bottle 11 is placed in a cooling device to reduce the temperature of absorption liquid in the gas washing bottle through the cooling device and inhibit the volatilization of the absorption liquid, and when the height of the second gas washing bottle exceeds 15cm, water vapor is condensed and flows back before reaching a gas outlet, and the loss of moisture can be effectively inhibited by adding a small amount of glycerol.
The first gas washing bottle 10, the second gas washing bottle 11 and the drying bottle 12 are made of aluminum materials, heat conduction is facilitated, teflon coatings are coated inside, and absorption solution inside the first gas washing bottle 10 and the second gas washing bottle 11 is 2% phosphoric acid.
Cooling device includes heat-preserving container 13, is provided with semiconductor refrigeration piece 14 and fan 141 on heat-preserving container 13's the inside wall, air filter and gas sampling device place respectively in the heat-preserving container 13 that corresponds, semiconductor refrigeration piece 14 and fan 141 all are connected through the wire electricity with temperature controller 7, and two heat-preserving containers 13 are all installed on base 24, install power module 9 in the base 24, and power module 9 makes the 24 centrobaries of base move down when providing electric power for the large capacity battery, play stable effect. The power module 9 is respectively electrically connected with the time controller 6, the temperature controller 7 and the thermometer, the semiconductor refrigerating sheet 14 and the fan 141 are respectively electrically connected with the temperature controller 7 through a lead, the first vacuum pump 4 and the second vacuum pump 5 are respectively electrically connected with the time controller 6 through leads, the time controller 6 can be set to be automatic and manual, the automatic gear switch is controlled to be started, and the manual gear can be set to be long and start time. Install first temperature and humidity sensor 18 towards the setting of ground direction in isolated cover 16, isolated cover 16 top is equipped with fixed frame plate 20, fixed frame plate 20 extends to the outside of isolated cover 16, fixed mounting has second temperature and humidity sensor 19 towards the setting of ground direction on the fixed frame plate 20, first temperature and humidity sensor 18 and second temperature and humidity sensor 19 pass through the wire electricity with warm and humid acidimeter 8 respectively and are connected, set up the wire guide through the wire on the isolated cover 16, warm and humid acidimeter 8 passes through the wire electricity with temperature controller 7 and power module 9 respectively and is connected, first temperature and humidity sensor 18 and second temperature and humidity sensor 19 all arrange near ground position in.
Example 2
A sampling method of a sampling device applied to determination of ammonium nitrogen isotopes comprises the following specific sampling steps:
step 2, judging whether temperature difference exists between the inside and the outside of the isolation cover 16 according to the temperatures detected by the first temperature and humidity sensor 18 and the second temperature and humidity sensor 19, if the temperature difference exists, adjusting the temperature of a cooling device where an air filtering device is located to enable the temperature in the cooling device to be lower than the temperature outside the isolation cover, then opening the first vacuum pump 4 to extract air, filtering and drying the air through the air filtering device, and enabling the air after being cooled by the cooling device to enter the isolation cover 16 to be mixed with water vapor volatilized from soil for dilution; and controlling the air flow rate transmitted by the first vacuum pump 4 by adjusting the first rotor flowmeter 2, and changing the dilution speed so as to prevent the humidity in the isolation cover 16 from reaching a water vapor saturation state of 100 percent and avoid water vapor condensation;
in the experiment process, the temperature of the heat preservation tank 13 in which the air filtering device is arranged is 0 ℃, for example, the external temperature is 5 ℃, the temperature in the isolation cover 16 is 10 ℃, and the temperature in the isolation cover 16 is reduced to a value close to the external temperature, namely, close to 5 ℃ by inputting dry and cold air with the temperature of 0 ℃ into the isolation cover 16.
And 3, when the temperature in the isolation cover 16 is close to the external temperature, turning on a second vacuum pump 5 in the gas sampling device, controlling the flow rate of the second vacuum pump 5 by arranging a second rotameter 3 to keep the same as the air supply flow rate of the first vacuum pump 4, and simultaneously adjusting a time controller 6 to a manual mode to set sampling time to perform gas sampling.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. A sampling device applied to determination of ammonium nitrogen isotopes comprises an isolation cover, wherein an air inlet hole and an air outlet hole are formed in the isolation cover, an air inlet pipe is arranged on the air inlet hole, the air outlet hole is connected with an exhaust pipe, and the exhaust pipe is connected with a gas sampling device;
the inlet end of the first gas washing bottle is connected with a first vacuum pump through a guide pipe, a first rotor flowmeter is arranged on the guide pipe, the outlet end of the first gas washing bottle is connected with a drying bottle through the guide pipe, and the outlet end of the drying bottle is connected with a gas inlet pipe;
the gas sampling device comprises a second gas washing bottle and a second vacuum pump, the inlet end of the second gas washing bottle is connected with an exhaust pipe, the outlet end of the second gas washing bottle is connected with the second vacuum pump through a guide pipe, a second rotameter is installed on the guide pipe, and the gas sampling device is arranged in the other cooling device;
absorption solution is filled in the first gas washing bottle and the second gas washing bottle, and the absorption solution is 2% phosphoric acid.
2. The sampling device applied to the determination of the ammonium nitrogen isotope is characterized in that the first gas washing bottle and the second gas washing bottle are both round-bottom absorption bottles, the height of each round-bottom absorption bottle is 15cm, a solid quartz bubbling ball is mounted at the end part of an absorption tube in each round-bottom absorption bottle, and the radius difference between the solid quartz bubbling ball and the round-bottom absorption bottle is 0.5cm.
3. The sampling device applied to the determination of the ammonium nitrogen isotope as claimed in claim 2, wherein the cooling device comprises a heat-preserving tank, a semiconductor refrigeration sheet and a fan are arranged on the inner side wall of the heat-preserving tank, the air filtering device and the gas sampling device are respectively placed in the corresponding heat-preserving tank, and the semiconductor refrigeration sheet and the fan are both electrically connected with the temperature controller through leads.
4. The sampling device applied to the determination of the ammonium nitrogen isotope in accordance with claim 3, wherein the two heat preservation tanks are both installed on a base, a power module is installed in the base, the power module is electrically connected with the time controller, the temperature controller and the thermometer respectively, the semiconductor refrigeration sheet and the fan are electrically connected with the temperature controller respectively through wires, and the first vacuum pump and the second vacuum pump are electrically connected with the time controller respectively through wires.
5. The sampling device applied to the determination of the ammonium nitrogen isotope according to claim 4, wherein the first temperature and humidity sensor and the second temperature and humidity sensor are respectively and electrically connected with a temperature and humidity meter through a lead, the insulation cover is provided with a lead hole through which the lead passes, and the temperature and humidity meter is respectively and electrically connected with the temperature controller and the power module through leads.
6. The sampling device applied to the determination of the isotope of ammonium nitrogen as claimed in claim 5, wherein the outside of the tube of the inlet tube is wrapped with a thermal insulation material, the inlet tube extends from the outside of the insulation cover to the bottom position inside the insulation cover, the outlet end of the inlet tube is provided with a nozzle in a conical structure, the bottom surface of the nozzle is in a closed structure, and the conical surface of the nozzle is provided with a plurality of exhaust holes.
7. The sampling method of the sampling device for ammonium nitrogen isotope assay according to any one of claims 1 to 6, characterized in that the sampling steps are as follows:
step 1, covering soil to be measured by an isolation cover, and arranging a first temperature and humidity sensor and a second temperature and humidity sensor inside and outside the isolation cover;
step 2, judging whether temperature difference exists between the inside and the outside of the isolation cover according to the temperatures detected by the first temperature and humidity sensor and the second temperature and humidity sensor, if so, adjusting the temperature of a cooling device where an air filtering device is located to enable the temperature in the cooling device to be lower than the temperature outside the isolation cover, then, opening a first vacuum pump to extract air, filtering and drying the air through the air filtering device, and enabling the air to enter the isolation cover after being cooled by the cooling device to be mixed and diluted with water vapor volatilized by soil;
and 3, when the temperature in the isolation cover is close to the external temperature, carrying out gas sampling work by a gas sampling device.
8. The sampling method applied to the sampling device for ammonium nitrogen isotope determination of claim 7, wherein in the step 2, the air flow rate transmitted by the first vacuum pump is controlled by adjusting the first rotor flow meter, so as to prevent the humidity in the isolation cover from reaching a water vapor saturation state of 100%, and avoid water vapor condensation;
and (3) when the gas sampling device samples in the step (3), setting a second rotor flow meter to control the flow rate of the second vacuum pump to be consistent with the flow rate of the first vacuum pump.
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| CN205506826U (en) * | 2016-04-21 | 2016-08-24 | 黑龙江省森林工程与环境研究所 | Normal position monitoring devices of forest soil environmental factor carbon dioxide flux and volatility ammonia |
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| CN108709782A (en) * | 2018-07-12 | 2018-10-26 | 中国农业科学院农业环境与可持续发展研究所 | A kind of the soil ammonia volatilization capture device and computational methods of ridge tillage method planting site |
| CN109827917A (en) * | 2019-03-28 | 2019-05-31 | 中国三峡建设管理有限公司 | Ammonia burst size CONTINUOUS VISCOSITY MEASURING and method in a kind of concrete |
| CN110686942A (en) * | 2019-09-26 | 2020-01-14 | 沈阳大学 | Farmland and lawn soil ammonia collection device that volatilizees |
| CN111044472A (en) * | 2019-11-27 | 2020-04-21 | 北京农业智能装备技术研究中心 | Farmland mulching film volatile matter detection device and detection method |
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