CN113532961A - U-shaped layered soil nitrous oxide gas collection method and device - Google Patents
U-shaped layered soil nitrous oxide gas collection method and device Download PDFInfo
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- CN113532961A CN113532961A CN202110954248.1A CN202110954248A CN113532961A CN 113532961 A CN113532961 A CN 113532961A CN 202110954248 A CN202110954248 A CN 202110954248A CN 113532961 A CN113532961 A CN 113532961A
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- 239000002689 soil Substances 0.000 title claims abstract description 154
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 239000001272 nitrous oxide Substances 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 24
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 63
- 239000010935 stainless steel Substances 0.000 claims abstract description 63
- 230000004907 flux Effects 0.000 claims abstract description 43
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000741 silica gel Substances 0.000 claims abstract description 35
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 35
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 claims abstract description 22
- 239000004202 carbamide Substances 0.000 claims abstract description 11
- 238000012258 culturing Methods 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 157
- 239000010410 layer Substances 0.000 claims description 28
- 229920001296 polysiloxane Polymers 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000005070 sampling Methods 0.000 claims description 15
- 238000007789 sealing Methods 0.000 claims description 13
- 235000013877 carbamide Nutrition 0.000 claims description 10
- 239000002344 surface layer Substances 0.000 claims description 10
- 235000007164 Oryza sativa Nutrition 0.000 claims description 7
- 235000009566 rice Nutrition 0.000 claims description 7
- 238000002474 experimental method Methods 0.000 claims description 4
- 230000004720 fertilization Effects 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 4
- 239000003755 preservative agent Substances 0.000 claims description 4
- 230000002335 preservative effect Effects 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000000499 gel Substances 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 238000005553 drilling Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 7
- 239000002680 soil gas Substances 0.000 description 8
- 241000209094 Oryza Species 0.000 description 6
- 230000007547 defect Effects 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 229920002379 silicone rubber Polymers 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2294—Sampling soil gases or the like
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/26—Devices for withdrawing samples in the gaseous state with provision for intake from several spaces
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N2001/1006—Dispersed solids
- G01N2001/1012—Suspensions
- G01N2001/1025—Liquid suspensions; Slurries; Mud; Sludge
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Abstract
The invention discloses a method and a device for collecting U-shaped layered soil nitrous oxide gas, comprising the following steps of: A. manufacturing a soil sample collecting device; B. manufacturing a U-shaped gas collecting pipe; C. collecting an undisturbed soil column; D. the U-shaped gas collecting pipes are arranged in the preformed holes of each soil layer, and the soil sample culture devices are assembled and installed; E. manufacturing a gas flux collecting device; F. adding urea to the soil surface of each soil column to be treated, performing submerged culture, performing drying treatment, and continuously culturing; G. and collecting a nitrous oxide emission flux gas sample of the cultured soil column on time during the culture period, collecting a volume gas sample from top to bottom from the layered silica gel tube, and determining the concentration of the nitrous oxide gas. Comprises a soil sample culture device, a gas flux acquisition device and a stainless steel square plate base. The PVC bottom plate sets up in the device's bottommost, and the PVC pipe is located the PVC bottom plate top, and the two links up department and seals with the silica gel. The method is easy to implement and convenient to operate. Simple structure, low cost, strong operability, convenient carrying, transportation, disassembly and assembly and convenient observation.
Description
Technical Field
The invention belongs to the technical field of simulating the nitrous oxide gas in the paddy soil under the flooding and dry falling conditions (emission), and particularly relates to a U-shaped layered soil nitrous oxide gas collecting method and a U-shaped layered soil nitrous oxide gas collecting device.
Background
Nitrous oxide (N)2O) is an important greenhouse gas, with a contribution rate of up to 6% to global warming, with a global warming potential of 300 times that of carbon dioxide over 100 years. Atmospheric nitrous oxide (N)2O) concentration is increasing at a rate of about 0.3% per year, nitrous oxide (N)2O) also contribute to depletion of the ozone layer (braiker, 2011). The paddy soil is one of the main farmland soil types in China, and is more important nitrous oxide (N)2O) emission source of nitrous oxide (N)2O) emission of 22% of total land (Bairenpo, 2013). Research shows that measures such as field baking, alternation of dry and wet and the like in a water-saving irrigation management mode of the rice field can cause nitrous oxide (N) in the soil of the rice field2O) (Cai et al, 1997).
Due to nitrous oxide (N)2O) emission flux mainly measures nitrous oxide (N) on soil-gas interface2O) release dynamics, reflected by nitrous oxide (N) per unit area2O) total gas amount, but lack of nitrous oxide (N) at different cross-sectional areas of the soil2O) production, conversion and nitrous oxide (N)2O) emissions. In-situ collection of nitrous oxide (N) from soil profile2O) gas is used for accurately measuring and calculating soil nitrous oxide (N)2O) key technology for emission flux. Therefore, the method is to collect the soil column (0-20cm) of the original soil of the rice and place the soil column in a roomCulturing at constant temperature, adding urea to soil from external source, flooding, and drying by using U-shaped layered soil nitrous oxide (N)2O) gas collection device system for monitoring nitrous oxide (N) in different soil layers2O) emission, exploration of nitrous oxide (N)2O) emission and soil profile nitrous oxide (N)2O) intrinsic relation law of concentration.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to provide a U-shaped layered soil nitrous oxide (N)2O) gas collection method, the method is easy to implement and convenient to operate. Is favorable for simulating the nitrous oxide (N) of the undisturbed rice soil in the field2O), overcomes the defect that the conventional static box gas collection method has deviation of measurement results due to the influence of factors such as temperature, box body size and the like, and also overcomes the defect that the soil gas cannot be collected at any time and any place when the positioning embedded sampling bottle method is adopted to collect the soil gas. The method can realize the nitrogen protoxide (N) at different section parts of the soil body under the condition of constant temperature without embedding2O) production, conversion and nitrous oxide (N)2O) emission, ensuring that the subsequent gas chromatograph can realize accurate measurement of nitrous oxide (N)2O) is discharged.
The invention also aims to provide a U-shaped layered soil nitrous oxide (N)2O) gas acquisition's device, it is not good to have overcome the thermal-insulated effect of general static case, easily arouse measuring error, and most equipment volume is great, the quality is heavier, carry, the inconvenient defect of transportation and installation, open dynamic case has also been overcome when using, airflow pressure is difficult to control, the operation difficulty, thereby probably lead to the undulant defect of data, whole system precision requirement has also been overcome simultaneously, and is expensive, the difficult defect of developing large tracts of land monitoring, the device simple structure, it is small and light, therefore, the carrier wave prepaid electric energy meter is low in cost, and is suitable for extensively, the strong operability, carry, the transportation, easy dismounting and observation convenience.
In order to achieve the purpose, the invention adopts the following technical scheme:
u-shaped layered soil nitrous oxide (N)2O) gas collection method, comprising the steps of:
A. manufacturing a soil sample collecting device: a soil sample collecting device is manufactured by a PVC pipe barrel with the outer diameter (De) of 16cm, the inner diameter (D) of 15cm and the height (H) of 25cm, a 20 cm-depth scribed line and a direction arrow line are marked on the pipe wall, a matched barrel bottom plate is manufactured by a PVC plate, and the PVC plate is not sealed before sampling.
B. Manufacturing a U-shaped gas collecting pipe: cutting the inlet silicone tubes (De 14mm, D10 mm, air-permeable and waterproof) to a plurality of (2-8) tubes with the length of 15cm (according to the dosage) (sealing the two ends of the tubes by using matched silicone plugs for standby application) for collecting gas samples of various soil layers of the cultured soil columns. Every two sections of silica gel tubes are connected with one end of a U-shaped stainless steel capillary tube (D3 mm) for standby.
C. Collecting an original soil column: the prepared PVC sampling barrel is used for collecting undisturbed soil columns (0-20cm) of the rice, the integrity of the soil columns is guaranteed to the greatest extent, the soil samples are collected, and then the soil samples are covered by a prepared PVC bottom plate, wrapped by preservative films and transported back to a laboratory.
D. The U-shaped gas collecting pipes are arranged in reserved orifices of all soil layers, and the soil sample culture device is assembled and installed: two parallel holes (D14 mm) are drilled at the positions of the pipe wall 2.5 cm, 7.5cm, 12.5 cm and 17.5cm away from the soil surface layer along the horizontal direction, the connected U-shaped gas collecting pipes are installed in reserved orifices of each soil layer, and finally, a stainless steel needle of 2mm connected with a three-way valve is inserted into one side of a silicone tube externally, and the device is used for collecting gas samples of each soil layer (sealed by using 704 silica gel externally to keep the whole air tightness of the PVC pipe).
E. Manufacturing a gas flux collecting device: the gas flux acquisition device is characterized in that PVC pipes (De 16cm, D15 cm and H25 cm) with the same size are used for the gas flux acquisition device, one end of a PVC plate (De 20.6cm, D20 cm and H29.5 cm) is sealed to serve as the top, a fan is installed inwards on the top of a cover, a power supply and a three-way valve are connected outwards to be used for gas acquisition, and the PVC pipe serves as the gas flux acquisition device (various interfaces are sealed by using Nanda 704 silica gel externally). A stainless steel square plate capable of fixing a gas flux collecting device is arranged at the upper part of the soil sample culture device, and water is used for sealing before sampling (deionized water is added into the stainless steel square plate, and the water layer is kept unchanged at about 2cm depth).
F. The experimental facility is started after the barrel wall is completely sealedPlacing and treating: the fertilization standard is 200kg of N.h < -2 >, and the fertilization mode is that urea { CO (NH) (added from an external source) is added2)2And (Urea-15N2), wherein the Urea addition of each treatment soil column is as follows: each soil column was wetted (with a water layer appearing slightly on the surface of each soil layer) at 10:00 am on 13 am of 4.8.2018, and 7.58 g.L-1 of carbamide { CO (NH) (Co:. RTM.)2)2Solution 100mL of carbamide { CO (NH) at 9:00 am, 4/27/20182)2Slowly and uniformly adding the solution into the soil surface layer of each soil column, and keeping the soil surface at a free water depth of 2 cm. Then, gas in the silica gel tubes of all soil layers is immediately replaced by high-purity helium gas: the replacement was repeated 3 times in succession. Starting timing, representing the 1 st d flooded by 24h of flooded water, and then 1d every 24 h; after 28d of flooding, the dropping drying treatment is carried out at 21:00 of the day, the dropping drying time is 12h for 1d, and then the culture is continuously carried out for 63d every 24h for 1 d.
G. Nitrous oxide (N)2O) Collection nitrous oxide (N) was collected at 1 st, 4 th, 7 th, 9 th, 11 th, 14 th, 16 th, 19 th, 21 th, 24 th, 28 th, 30 th, 32 th, 35 th, 38 th, 40 th, 42 th, 44 th, 46 th, 48 th, 50 th, 53 th, 55 th, 58 th, 61 th, and 63 th d of the culture procedure2O) gas. Each gas collection time was 9 a.m.: 00 Initially, each treatment was carried out for 1h of nitrous oxide (N)2O) collecting a discharged flux gas sample, placing a gas flux collecting device on a groove of a culture earth pillar for gas sampling during gas collection, sealing the gas flux collecting device with water, switching on a power supply to enable a top fan to rotate so as to fully mix gas in the gas flux collecting device, and then connecting a top three-way valve of the device with an injector to collect gas. Gas samples were taken once each at 0min and 60min, respectively, 30mL of gas sample was collected each time, and the gas samples taken were measured over 48 h. Then, 5mL volume of gas sample (30 mL supplemented with high purity He gas) was collected from the layered silicone tube from top to bottom by syringe to measure nitrous oxide (N)2O) concentration. Can monitor nitrous oxide (N) in different soil layers2O) emissions.
Through the technical measures of the seven steps, the most critical steps are as follows:
step C, step D and step G of the present invention: the undisturbed soil column is collected, so that the simulation of the paddy field soil under the flooding and dry-falling condition is facilitated; in a laboratoryThe gas collection experiment avoids the influence of temperature on the gas discharge amount; adopts U-shaped layered soil nitrous oxide (N)2O) the gas collection method can collect the soil gas at any time and any place without damaging the original structure of the soil.
U-shaped layered soil nitrous oxide (N)2O) a gas collection device: the device consists of three main structures, including a soil sample culture device, a gas flux acquisition device and a stainless steel square disc base (8). The contact area of the PVC pipe in the stainless steel square plate and the soil sample culture device is sealed by 704 glue, the gas flux collection device covers the stainless steel square plate base before collecting a gas sample, and the joint is sealed by water. The soil sample culture device comprises a PVC bottom plate, PVC pipes, four groups of U-shaped gas collecting pipes, a stainless steel needle head and a three-way valve; the soil sample culture device is characterized in that: the PVC bottom plate set up in the device's bottommost, the PVC pipe be located directly over the PVC bottom plate, the two junction is sealed with big 704 silica gel in south. Four groups of U-shaped gas collecting pipes are vertically arranged in the PVC pipe, the four groups of U-shaped gas collecting pipes are respectively inserted into the reserved holes at the positions of the pipe wall at the heights of 2.5, 7.5, 12.5 and 17.5cm away from the soil surface layer and connected with the pipe wall, and the joints are sealed by 704 southern large silica gel. The U-shaped gas collecting tube consists of a silica gel plug, a silica gel tube and a U-shaped stainless steel capillary tube. Two ends of each section of the silicone tube are respectively sealed by a silicone rubber plug, and each two sections of the silicone tubes are horizontally arranged in parallel in the left-right direction. The U-shaped stainless steel capillary is respectively connected with the outward ports of the left and right silicone tubes. The sealing barrel wall and the interfaces and joints of all parts are sealed by using south large 704 silica gel. And a 2mm stainless steel needle is inserted into the right silica gel plug and connected to the right silica gel tube. The three-way valve is connected with the outer end of the stainless steel needle head. The U-shaped gas collecting pipe is used for collecting gas samples of various soil layers (all joints outside are sealed by south large 704 silica gel so as to keep the whole air tightness of the PVC pipe). The stainless steel square plate base covers the top of the soil sample culture device, a circle (with the diameter of 10cm) is dug out in the middle of the stainless steel square plate base (8), the soil sample culture device is placed into the circle, the bottom of the soil sample culture device is supported by a PVC pipe of the soil sample culture device, and the contact area of the stainless steel square plate and the PVC pipe is sealed by 704 glue. The gas flux collecting device comprises a PVC pipe, a three-way valve, a stainless steel capillary pipe and a PVC plateThe gas flux collecting device uses PVC pipes with the same size as the bottom, and seals one end of a PVC plate as the top; one end of the stainless steel capillary tube penetrates through the small hole at the top of the cover and extends inwards, and the other end of the stainless steel capillary tube is outwards connected with the three-way valve and used for collecting nitrous oxide (N)2O) gas emission flux. An electric fan is arranged inwards on the top of the cover, and an electric wire is connected with the outside of the cover and used for uniformly mixing gas before gas production (the interfaces are sealed by using south large 704 silica gel outside). The gas flux collecting device is covered on a stainless steel square disc base before collecting a gas sample, and the joint is sealed by water to form a closed system.
The U-shaped gas collecting pipe in the other part is a key part. The U-shaped gas collecting pipes are arranged in reserved orifices of all soil layers, and finally, a three-way valve is connected to the outside to simulate the original state of the field of the nitrous oxide (N) in the paddy soil2O) a discharge process, and the U-shaped gas collecting pipe is used for collecting gas samples of all soil layers. The device overcomes the defect that the nitrogen monoxide (N) in unit soil area can be detected only in the past2O) the net discharge amount of the gas, and the problem that the original structure of the soil needs to be damaged and the soil gas can not be collected anytime and anywhere when the former method of collecting the soil gas by adopting a positioning embedded sampling bottle. The device can conveniently and accurately detect nitrous oxide (N) at different section parts of the soil body2O) production, conversion and nitrous oxide (N)2O) emissions, to explore the relationship between the two.
Compared with the prior art, the invention has the following advantages and effects
1. Nitrous oxide (N) in soil2O) is soil nitrous oxide (N)2O) production and consumption effects. The traditional soil gas collection mode is based on the soil surface, and only nitrous oxide (N) discharged from the soil surface can be collected2O) gas, is soil nitrous oxide (N)2O) net emission. The invention adopts the U-shaped gas collecting pipe to be arranged in the reserved hole of each soil layer, and finally, the three-way valve is externally connected to facilitate layered collection of gas samples with different depths.
2. The utility model discloses a novel gas collection system of practicality, simple structure, reasonable in design arranges 4 groups of U type collecting pipes from top to bottom in soil sample culture apparatus's PVC intraductal, has low cost, application scope extensively, advantage that maneuverability is strong.
In a word, the method can accurately collect nitrous oxide (N2O) generated by the undisturbed soil column at different soil depths, the device is simple, and the operation method is easy to implement.
Drawings
FIG. 1 shows a U-shaped layered soil nitrous oxide (N)2O) a schematic structural diagram of the gas collecting device.
Fig. 2 is a schematic diagram of a U-shaped gas collecting tube.
Wherein: the novel electric heating wire comprises a 1-PVC bottom plate, a 2A-first PVC pipe, a 2B-second PVC pipe, a 3-silica gel plug, a 4-silica gel pipe, a 5-U-shaped stainless steel capillary pipe, a 6-stainless steel needle head, a 7A-first three-way valve (purchased in the market), a 7B-second three-way valve (purchased in the market), an 8-stainless steel square plate, a 9-stainless steel capillary pipe, a 10-PVC plate (top), an 11-electric fan (common) and a 12-electric wire.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The experiment described in the embodiment is to determine nitrous oxide (N) in different soil layers of undisturbed paddy soil with different soil matrixes in south China during flooding and drying2O) emission dynamics of the gas.
Example 1:
u-shaped layered soil nitrous oxide (N)2O) gas collection method, comprising the steps of:
A. manufacturing a soil sample collecting device: a soil sample collecting device is manufactured by a PVC pipe barrel with the outer diameter (De) of 16cm, the inner diameter (D) of 15cm and the height (H) of 25cm, a 20 cm-depth scribed line and a direction arrow line are marked on the pipe wall, a matched barrel bottom plate is manufactured by a PVC plate, and the PVC plate is not sealed before sampling.
B. Manufacturing a U-shaped gas collecting pipe: the method comprises the steps of cutting a plurality of (2-8) inlet silicone tubes (De 14mm and D10 mm which are air-permeable and waterproof and have the length of 15cm to be a plurality of, and sealing two ends of the tubes by using matched silicone plugs for standby application, wherein the silicone tubes are used for collecting gas samples of various soil layers of the cultured soil columns, and connecting one end of each two sections of the silicone tubes with a U-shaped stainless steel capillary tube (D3 mm) for standby application.
C. Collecting an original soil column: the prepared PVC sampling barrel is used for collecting undisturbed soil columns (0-20cm) of the rice, the integrity of the soil columns is guaranteed to the greatest extent, the soil samples are collected, and then the soil samples are covered by a prepared PVC bottom plate, wrapped by preservative films and transported back to a laboratory.
D. The U-shaped gas collecting pipes are arranged in reserved orifices of all soil layers, and the soil sample culture device is assembled and installed: two holes (D14 mm) are respectively drilled in parallel along the horizontal direction at the positions of the pipe wall at the heights of 2.5, 7.5, 12.5 and 17.5cm away from the soil surface layer, the connected U-shaped gas collecting pipes are arranged in reserved orifices of each soil layer, and finally, a 2mm stainless steel needle connected with a three-way valve is inserted into one side of a silicone tube from the outside. The device is used for collecting soil gas samples of different depths in a layering mode (the south is externally sealed by 704 silica gels so as to keep the whole air tightness of the PVC pipe).
E. Manufacturing a gas flux collecting device: the gas flux collection device is characterized in that PVC pipes (De 16cm, D15 cm and H25 cm) with the same size are used for the gas flux collection device, one end of a PVC plate (De 20.6cm, D20 cm and H29.5 cm) is sealed to serve as the top, a fan is installed inwards on the top of a cover, a power supply and a three-way valve are connected outwards to collect gas, and the purpose is to uniformly mix gas samples before gas collection (the interfaces are sealed by south large 704 silica gel for external use). A stainless steel square plate capable of fixing a gas flux collecting device is arranged at the upper part of the soil sample culture device, and is sealed by water before sampling (deionized water is added into the stainless steel square plate, and the depth of a water layer is kept unchanged at about 2 cm), so that a closed system is formed.
F. Starting experiment setting treatment after the barrel wall is completely sealed: the fertilization standard is 200kg N.h-2The fertilizing mode is that urea { CO (NH) is added from an external source2)2}(Urea-15N2) The urea addition of each processing soil column is as follows: wetting each soil column (making each soil surface layer to be in a micro water layer state) at 10:00 am on 13 am of 4 and 13 months in 2018, and arranging 7.58 g.L-1Carbonyldiamides { CO (NH) }2)2Solution 100mL of carbamide { CO (NH) at 9:00 am, 4/27/20182)2Slowly and uniformly adding the solution into the soil surface layer of each soil column, and keeping the soil surface at a free water depth of 2 cm. Then, the gas in the silicone tube of each soil layer is immediately replaced by high-purity helium (continuously and repeatedly replaced for 3 times) so as to eliminate the residual air in the silicone tube from actually generatingNitrous oxide (N)2O) contamination and disturbance of the gas. Starting timing, representing the 1 st d flooded by 24h of flooded water, and then 1d every 24 h; after 28d of flooding, the dropping drying treatment is carried out at 21:00 of the day, the dropping drying time is 12h for 1d, and then the culture is continuously carried out for 63d every 24h for 1 d.
G. Nitrous oxide (N)2O) Collection nitrous oxide (N) was collected at 1 st, 4 th, 7 th, 9 th, 11 th, 14 th, 16 th, 19 th, 21 th, 24 th, 28 th, 30 th, 32 th, 35 th, 38 th, 40 th, 42 th, 44 th, 46 th, 48 th, 50 th, 53 th, 55 th, 58 th, 61 th, and 63 th d of the culture procedure2O) gas. Each gas collection time was 9 a.m.: 00 Initially, each treatment was carried out for 1h of nitrous oxide (N)2O) collecting a flux gas sample, placing the gas flux collecting device on a groove of a culture earth pillar for gas sampling (the upper part of the soil sample culture device is contacted with a stainless steel square disc base) during gas collection, sealing the gas flux collecting device with water, switching on a power supply to enable a top fan to rotate to enable the top fan to fully mix gas in the gas flux collecting device, and then connecting a three-way valve at the top of the device with an injector to collect gas. Gas samples were taken once each at 0min and 60min, respectively, 30mL of gas sample was collected each time, and the gas samples taken were measured over 48 h. Then, 5mL volume of gas sample (30 mL supplemented with high purity He gas) was collected from the layered silicone tube from top to bottom by syringe to measure nitrous oxide (N)2O) concentration.
Through the specific implementation, the nitrous oxide (N) at different section parts of the soil body can be realized under the condition of constant temperature and without embedding2O) production, conversion and nitrous oxide (N)2O) emission, ensuring accurate measurement of nitrous oxide (N) by a subsequent gas chromatograph2O) emissions.
Example 2:
as can be seen from FIGS. 1 and 2, a U-shaped layered soil nitrous oxide (N)2O) gaseous collection system, the device include soil sample culture apparatus, gaseous flux collection system, stainless steel square plate base (8), and the PVC pipe contact area in stainless steel square plate base (8) and the soil sample culture apparatus is glued with 704 and is sealed, gathers gaseous sample front shroud on stainless steel square plate base (8), and the joint is sealed with the water. The method is characterized in that: soil sample culture apparatus packageDraw PVC bottom plate (1), first PVC pipe (2A), four groups U type gas collecting pipes, stainless steel needle (6), first three-way valve (7A), PVC bottom plate (1) set up in the device's bottommost, first PVC pipe (2A) are located PVC bottom plate (1) top, the two department of linking is sealed with big 704 silica gel in south. Four groups of U-shaped gas collecting pipes are vertically arranged in the first PVC pipe (2A), the four groups of U-shaped gas collecting pipes are respectively inserted into the reserved holes at the positions of the pipe wall at the heights of 2.5, 7.5, 12.5 and 17.5cm from the soil surface layer to be connected with the pipe wall, and the joints are sealed by using south large 704 silica gel. The stainless steel square disc base (8) covers the top of the soil sample culture device, the stainless steel square disc base (8) is 18cm by 3cm (length by width by height), a circle (with the diameter of 10cm) is dug out of the middle of the stainless steel square disc base (8), the soil sample culture device is placed in the circle, the bottom of the circle is supported by a second PVC pipe (2B) of the soil sample culture device, the contact area of the stainless steel square disc (8) and a first PVC (2A) and a second PVC pipe (2B) is sealed by 704 glue, the gas flux collection device uses the first PVC pipe (2A) and the second PVC pipe (2B) (De 16cm, D15 cm and H25 cm) with the same size as the bottom, and uses a PVC plate (10) with the size of 20.6cm D20 cm and H29.5 cm as the top after one end of the plate is sealed; one end of the stainless steel capillary tube (9) penetrates through the small hole in the top of the cover and extends inwards, and the other end of the stainless steel capillary tube (9) is outwards connected with a second three-way valve (7B) and used for collecting the emission flux of nitrous oxide (N2O) gas. An electric fan (11) is arranged inwards on the top of the cover, an electric wire (12) is connected with the outside of the cover, and the U-shaped gas collecting tube consists of a silica gel plug (3), a silica gel tube (4) and a U-shaped stainless steel capillary tube (5). Two ends of each section of the silicone tube (4) are respectively sealed by a silicone rubber plug (3), and each two sections of the silicone tubes (4) are horizontally arranged in parallel in the left-right direction. The U-shaped stainless steel capillary tube (5) is respectively connected with the outward ports of the left and right silicone tubes (4). The joint of the sealing barrel wall and each component is sealed by using south large 704 silica gel. And the U-shaped gas collecting pipe is connected to the right silicone tube (4) by inserting a 2mm stainless steel needle (6) into the right silicone plug (3) outside the U-shaped gas collecting pipe. The first three-way valve (7A) is connected with the outer end of the stainless steel needle (6). The U-shaped gas collecting pipe is used for collecting gas samples of various soil layers (all joints outside are sealed by south large 704 silica gel so as to keep the whole air tightness of the PVC pipe). The gas flux collecting device comprises a second PVC pipe (2B), a second three-way valve (7B), a stainless steel capillary tube (9), a top PVC plate (10) and an electric fan(11) And an electric wire (12). Used for mixing gas before gas production (the interface is sealed by south large 704 silica gel for external use). The gas flux collecting device covers the stainless steel square disc base (8) before collecting a gas sample, and the joint is sealed by water to form a closed system.
Through the specific components, the U-shaped gas collecting tube can conveniently and accurately detect nitrous oxide (N) at different section parts of the soil body2O) production, conversion and nitrous oxide (N)2O) emissions, to explore the relationship between the two.
Claims (6)
1. A U-shaped layered soil nitrous oxide gas collection method comprises the following steps:
A. manufacturing a soil sample collecting device: a PVC pipe barrel is used for self-manufacturing a soil sample collecting device, a groove with the depth of 20cm and a direction arrow line are marked on the pipe wall, a PVC plate is used for manufacturing a pairing barrel bottom plate, and the barrel is not sealed before sampling;
B. manufacturing a U-shaped gas collecting pipe: cutting an inlet silicone tube to a length of 15cm, sealing two ends of the tube by using a matched silicone plug for standby application, and collecting gas samples of various soil layers of the cultured soil column, wherein each two sections of the silicone tube are connected with one end by using a U-shaped stainless steel capillary tube for standby application;
C. collecting an original soil column: collecting original soil columns of rice by 0-20cm by using the manufactured PVC sampling barrel, sealing the bottom by using a prepared matched PVC bottom plate after the soil samples are collected, wrapping a preservative film and transporting the preservative film to a laboratory;
D. the U-shaped gas collecting pipes are arranged in reserved orifices of all soil layers, and the soil sample culture device is installed in a combined mode: respectively drilling two holes in parallel along the horizontal direction at the positions of the pipe wall 2.5 cm, 7.5cm, 12.5 cm and 17.5cm away from the soil surface layer, arranging the connected U-shaped gas collecting pipes into reserved orifices of each soil layer, and finally inserting a 2mm stainless steel needle connected with a three-way valve into one side of a silicone tube externally for collecting gas samples of each soil layer;
E. manufacturing a gas flux collecting device: the gas flux collecting device is formed by using PVC pipes with the same size, one end of a PVC plate is sealed to serve as the top, a fan and a stainless steel needle head are installed inwards on the top of a cover, a power supply and a three-way valve are connected outwards to be used for gas collection, all interfaces are sealed by 704 silica gel outside, a stainless steel square disc for fixing the gas flux collecting device is installed on the upper portion of the soil sample culture device, and water is used for sealing before sampling;
F. starting experiment setting treatment after the barrel wall is completely sealed: the fertilization rate is 200kg N.h-2The fertilizing mode is that urea is added from an external source, and the urea in each soil column is added as follows: the soil columns were wetted at 10:00 am on day 1 after the start of cultivation, and the arrangement was 7.58 g.L-1Slowly and uniformly adding 100mL of carbamide solution into the soil surface layer of each soil column at 9:00 am after 4-6 days, and keeping the soil surface at a free water depth of 2 cm; replacing gas in the silicone tube of each soil layer with high-purity helium, and continuously and repeatedly replacing for 3 times; starting timing, representing the 1 st d flooded by 24h of flooded water, and then 1d every 24 h; performing falling dry treatment at 21:00 of the day after flooding for 28d, wherein the falling dry time is 12h for 1d, and continuously culturing for 63d every 24h for 1 d;
G. collection of nitrous oxide gas was collected at 1, 4, 7, 9, 11, 14, 16, 19, 21, 24, 28, 30, 32, 35, 38, 40, 42, 44, 46, 48, 50, 53, 55, 58, 61 and 63d of the culture process, respectively, each gas collection time being 9 a.m.: 00, firstly, collecting a nitrous oxide emission flux gas sample for 1 hour after treatment, placing a gas flux collection device on a groove of a culture earth pillar for gas sampling during gas collection, sealing the gas flux collection device with water, switching on a power supply to enable a top fan to rotate, fully mixing gas in the gas flux collection device, and connecting a top three-way valve of the device with an injector to collect gas; respectively sampling gas samples once in 0min and 60min, collecting 30mL gas samples each time, and measuring the sampled gas samples within 48 h; 5mL volume gas samples were collected from the layered silicone tube from top to bottom with a syringe, respectively, and the nitrous oxide concentration was determined.
2. The U-shaped layered soil nitrous oxide gas collecting device of claim 1, which comprises a soil sample culture device, a gas flux collecting device, a stainless steel square plate base (8), wherein the contact area between the stainless steel square plate base (8) and a PVC pipe in the soil sample culture device is sealed by using 704 glue, a gas sample collecting front cover is covered on the stainless steel square plate base (8), and the joint is sealed by using water, and is characterized in that: the soil sample culture device comprises a PVC bottom plate (1), a first PVC pipe (2A), four groups of U-shaped gas collecting pipes and a first three-way valve (7A), wherein the PVC bottom plate (1) is arranged at the bottommost end of the device, the first PVC pipe (2A) is positioned above the PVC bottom plate (1), the joint of the first PVC pipe and the PVC bottom plate is sealed by 704 silica gel, the four groups of U-shaped gas collecting pipes are vertically arranged in the first PVC pipe (2A), the four groups of U-shaped gas collecting pipes are respectively inserted into a reserved hole at the height of 2.5, 7.5, 12.5 and 17.5cm from the soil surface layer of the pipe wall to be connected with the pipe wall, the joint is sealed by 704 silica gel, a stainless steel square disc base (8) covers the top of the soil sample culture device, a circle is dug out in the middle of the stainless steel square disc base, the soil sample culture device is placed into the circle, the contact area of the stainless steel square disc base (8) with the first PVC pipe (2A) and the second PVC pipe (2B) is sealed by 704 gel, the gas flux collecting device comprises a second PVC pipe (2B), a second three-way valve (7B), a stainless steel capillary (9), a top PVC plate (10), an electric fan (11) and an electric wire (12), wherein the top is arranged at the back of one end of the PVC plate (10) in a sealing mode, one end of the stainless steel capillary (9) penetrates through a small hole in the top of the cover to extend inwards, the other end of the stainless steel capillary (9) is connected with the second three-way valve (7B) outwards, the electric fan (11) is installed inwards in the top of the cover, and the electric wire (12) is connected outside.
3. The U-shaped layered soil nitrous oxide gas collecting device according to claim 2, wherein: the U-shaped gas collecting tube consists of a silica gel plug (3), a silica gel tube (4) and a U-shaped stainless steel capillary tube (5), wherein the two ends of each cut silica gel tube (4) are respectively sealed by the silica gel plug (3), each two cut silica gel tubes (4) are arranged side by side in the horizontal direction, the U-shaped stainless steel capillary tube (5) is respectively connected with the outward ports of the left and right silica gel tubes (4), the sealing barrel wall and the interfaces of all parts, and the joint is sealed by 704 silica gel.
4. The U-shaped layered soil nitrous oxide gas collecting device according to claim 2, wherein: the outside of the U-shaped gas collecting tube is connected to the right silicone tube (4) by inserting a 2mm stainless steel needle (6) into the right silicone plug (3).
5. The U-shaped layered soil nitrous oxide gas collecting device according to claim 2, wherein: the gas flux collecting device is covered on a stainless steel square disc base (8) by using a first PVC pipe (2A) and a second PVC pipe (2B) with the same size as the bottom, and a joint is sealed by water to form a closed system.
6. The U-shaped layered soil nitrous oxide gas collecting device according to claim 2, wherein: the first three-way valve (7A) is connected with the outer end of the stainless steel needle (6).
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