CN109632412B - A auxiliary device for trace nitrogen conversion N2O - Google Patents
A auxiliary device for trace nitrogen conversion N2O Download PDFInfo
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- CN109632412B CN109632412B CN201811479637.8A CN201811479637A CN109632412B CN 109632412 B CN109632412 B CN 109632412B CN 201811479637 A CN201811479637 A CN 201811479637A CN 109632412 B CN109632412 B CN 109632412B
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- bottle
- shell
- sample
- rotating shaft
- way valve
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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
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Abstract
The invention discloses a method for converting trace nitrogen into N2The auxiliary device of O comprises a shell, a rotating shaft is vertical, the bottom of the rotating shaft is positioned in the shell, and a sample disc which is coaxial with the rotating shaft and used for placing a sample bottle is fixedly arranged at the top of the rotating shaft; one side of the shell is rotatably connected with a side shaft, the top of the side shaft is provided with a supporting arm, an air cylinder is fixedly arranged on the supporting arm, a piston of the air cylinder is fixedly provided with a needle tube, and the air cylinder can drive the needle tube to be inserted into a sample bottle on the sample plate; the side wall of the shell is provided with at least two channels, the helium bottle, the multi-channel knob, one channel, the three-way valve and the needle tube are sequentially communicated, the compressed air bottle, the liquid reagent bottle, the multi-channel knob, the other channel, the three-way valve and the needle tube are sequentially communicated, the compressed air bottle is further communicated with a needle inserting electromagnetic valve of the air cylinder, and the vacuum pump, the two-way valve and the needle tube are sequentially communicated. The invention is used for converting the trace nitrogen into the N2The auxiliary device of O can realize the automatic liquid feeding, automatic vacuum replacement and automatic gas injection process of sample bottle among the nitrogen conversion process.
Description
Technical Field
The invention relates to the technical field of environmental detection equipment, in particular to a method for converting trace nitrogen into N2And (4) auxiliary devices of O.
Background
The earth surface layer is a source or sink of greenhouse gases, and researches on dynamic change and circulation characteristics of nitrogen in a land ecosystem are common hotspots of current ecological, biological geochemical and environmental scientific researches. The input, conversion and output of nitrogen in soil become leading edge and hot spot of current research in the field of soil nitrogen circulation and global climate change. The cycle of nitrogen can be roughly divided into 3 processes by human: nitrogen import (primarily biological nitrogen fixation); the transformation of nitrogen in the soil ecosystem (mainly including decomposition, mineralization and nitrification); nitrogen output (mainly denitrification and gas volatilization). Scientifically knows the dynamic change process and the regulation and control mechanism of the soil-plant nitrogen of the land ecosystem, fully knows the turnover mode, time and speed of the nitrogen in the ecosystem, and has important significance for improving the nitrogen fixation capacity of the land ecosystem.
Nitrogen stable isotope ratio (delta)15N) analysis method is one of the most scientific and effective methods for researching nitrogen circulation of water body and soil in land ecosystem, and is used for evaluating mineralization degree of biological nitrogen fixation and organic nitrogen and evaluating NO3 － /N2The method is widely applied to the fields of O source discussion and the like. Performing nitrogen stable isotope ratio (delta)15N) analysis requires NH in soil extract4 +、NO3 －And NO2 －Are all converted into N2O, and NH in the soil extract4 +、NO3 －And NO2 －Are all converted into N2The O process needs operations such as reagent injection, vacuum pumping, inert gas injection and the like, which are performed manually by operators at present, so that the efficiency is low, and operation errors are easily caused, thereby causing the defects of15N-N2The results of the O abundance test are inaccurate.
Disclosure of Invention
The invention aims to provide a method for converting N by trace nitrogen2O auxiliary device to solve the problems in the prior art and improve the content of the extracting solution15N-N2And the abundance of O tests the accuracy of the result, and avoids errors caused by manual operation.
In order to achieve the purpose, the invention provides the following scheme: the invention provides a method for converting trace nitrogen into N2The auxiliary device of the O comprises a shell, a rotating shaft, a helium bottle, a compressed air bottle, a vacuum pump and a liquid reagent bottle; the rotating shaft is vertical, the bottom of the rotating shaft is positioned in the shell, and a sample disc which is coaxial with the rotating shaft and used for placing a sample bottle is fixedly arranged at the top of the rotating shaft; one side of the shell is rotatably connected with a paraxial shaft, and the top of the paraxial shaftThe sample bottle taking device is provided with a supporting arm, one end of the supporting arm, which is far away from the paraxial shaft, extends to the sample disc and is fixedly provided with an air cylinder, a needle tube is fixedly arranged on a piston of the air cylinder, the air cylinder is positioned above the sample bottle, and the air cylinder can drive the needle tube to be inserted into the sample bottle on the sample disc; the multi-channel needle valve is characterized in that at least two channels are arranged on the side wall of the shell, a multi-channel knob used for switching the channels is further arranged on the outer wall of the shell, the helium bottle, the multi-channel knob, one channel, the three-way valve and the needle tube are sequentially communicated, the compressed air bottle, the liquid reagent bottle, the multi-channel knob, the other channel, the three-way valve and the needle tube are sequentially communicated, the compressed air bottle is further communicated with a needle inlet electromagnetic valve of the air cylinder, and the vacuum pump, the two-way valve and the needle tube are sequentially communicated.
Preferably, the shell is internally provided with a driving motor, a gear and a positioning disc which is coaxial and fixedly connected with the rotating shaft, the gear is fixedly connected with an output shaft of the driving motor, and teeth which can be meshed with the gear are uniformly distributed on the bottom surface of the positioning disc in the circumferential direction.
Preferably, a guide arm is fixedly arranged at the bottom of the paraxial shaft and comprises an upper layer sheet body and a lower layer sheet body, and the positioning disc is clamped between the upper layer sheet body and the lower layer sheet body; a guide head is fixedly arranged on the upper layer sheet body, a spiral guide groove is formed in the top surface of the positioning disc, and the guide head is in sliding fit with the guide groove; the guide arm is provided with a photoelectric sensing device, a photoelectric receiving tube of the photoelectric sensing device is embedded in the guide head, a photoelectric emitting tube of the photoelectric sensing device is arranged at the position of the lower layer sheet body corresponding to the guide head, and a detection signal of the photoelectric sensing device is input into the controller circuit board through a circuit.
Preferably, the starting position and the ending position of the guide groove are respectively provided with a magnetic steel, the guide arm is further provided with two Hall switches for respectively detecting the two magnetic steels, and the Hall switches are electrically connected with the controller circuit board.
Preferably, the center of the guide groove is equidistantly provided with positioning holes corresponding to the sample bottles, and the upper disc of the sample disc is provided with insertion holes corresponding to the positioning holes.
Preferably, a controller circuit board is arranged in the shell, a display screen electrically connected with the controller circuit board is arranged on the outer wall of the shell, and the three-way valve, the two-way valve, the driving motor, the needle withdrawing electromagnetic valve of the cylinder and the needle inserting electromagnetic valve are respectively electrically connected with the controller circuit board.
Preferably, a gas pressure controller and a gas pressure gauge are arranged on a connecting pipe between the helium bottle and the multi-channel knob, a connecting pipe between the compressed air bottle and the liquid reagent bottle and a connecting pipe between the compressed air bottle and the needle inserting electromagnetic valve.
Preferably, the gas pressure controllers are electrically connected with the controller circuit board, and the gas pressure controllers and the gas pressure gauge are fixedly arranged on the outer wall of the shell.
The invention is used for converting the trace nitrogen into the N2Compared with the prior art, the auxiliary device of the O has the following technical effects:
the invention is used for converting the trace nitrogen into the N2The auxiliary device of O can realize trace inorganic nitrogen NH in soil leaching liquor (or water)4 +、NO3 －And NO2 －Conversion to N2Automatic liquid feeding, automatic vacuum replacement and automatic gas injection in the chemical reaction of O. Generated N2O gas is subjected to the determination of NO by the combination of a trace gas preconcentration device and isotope mass spectrometry (PreCon-IRMS)2In15The N abundance realizes mass spectrum detection of stable nitrogen isotopes in inorganic nitrogen under low sample quantity; the test error possibly introduced by complicated manual operation is avoided, the operation method of the device is simple, and the measurement result is accurate. The invention is used for converting the trace nitrogen into the N2The auxiliary device of O is made of cheap materials and has low manufacturing cost; the invention is used for converting the trace nitrogen into the N2The auxiliary device of O adopts stainless steel material and aluminum alloy material, and the outward appearance is pleasing to the eye, and durable.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 shows the trace nitrogen conversion of N according to the present invention2A schematic structural diagram of an auxiliary device of O;
the device comprises a cylinder 1, a sample bottle 2, a sample plate 3, a three-way valve 4, a two-way valve 5, a compressed air bottle 6, a guide arm 7, a vacuum pump 8, a needle insertion electromagnetic valve 9, a gas pressure gauge 10, a liquid reagent bottle 11, a display screen 12, a controller circuit board 13, a gas pressure controller 14, a gear 15, a multichannel knob 16, a positioning plate 17 and a helium bottle 18.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a method for converting N by trace nitrogen2O auxiliary device to solve the problems in the prior art and improve the extraction liquid15N-N2And the abundance of O tests the accuracy of the result, and avoids errors caused by manual operation.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
As shown in FIG. 1, this example is for trace nitrogen conversion of N2The auxiliary device of O comprises a shell, a rotating shaft, a helium bottle 18, a compressed air bottle 6, a vacuum pump 8 and a liquid reagent bottle 11; rotating shaftThe bottom of the rotating shaft is positioned in the shell, and the top of the rotating shaft is fixedly provided with a sample disc 3 which is coaxial with the rotating shaft and used for placing the sample bottle 2; one side of the shell is rotatably connected with a paraxial shaft, the top of the paraxial shaft is provided with a supporting arm, one end of the supporting arm, which is far away from the paraxial shaft, extends to the sample disc 3 and is fixedly provided with an air cylinder 1, a piston of the air cylinder 1 is fixedly provided with a needle tube, the air cylinder 1 is positioned above the sample bottles 2, and the air cylinder 1 can drive the needle tube to be inserted into the sample bottles 2 on the sample disc 3; the side wall of the shell is provided with at least two channels, the outer wall of the shell is further provided with a multi-channel knob 16 used for switching the channels, the helium bottle 18, the multi-channel knob 16, one channel (channel 1 for short), the three-way valve 4 and the needle tube are sequentially communicated, the compressed air bottle 6, the liquid reagent bottle 11, the multi-channel knob 16, the other channel (channel 2 for short), the three-way valve 4 and the needle tube are sequentially communicated, the compressed air bottle 6 is further communicated with the needle inlet electromagnetic valve 9 of the air cylinder 1, and the vacuum pump 8, the two-way valve 5 and the needle tube are sequentially communicated. The shell is also internally provided with a driving motor, a gear 15 and a positioning disk 17 which is coaxial and fixedly connected with the rotating shaft, the gear 15 is fixedly connected with an output shaft of the driving motor, and teeth which can be meshed with the gear 15 are uniformly distributed on the bottom surface of the positioning disk 17 in the circumferential direction.
A guide arm 7 is fixedly arranged at the bottom of the paraxial shaft, the guide arm 7 comprises an upper layer sheet body and a lower layer sheet body, and a positioning disc 17 is clamped between the upper layer sheet body and the lower layer sheet body; a guide head is fixedly arranged on the upper layer sheet body, a spiral guide groove is arranged on the top surface of the positioning disk 17, and the guide head is in sliding fit with the guide groove; the guide arm 7 is provided with a photoelectric sensing device, a photoelectric receiving tube of the photoelectric sensing device is embedded in the guide head, a photoelectric emitting tube of the photoelectric sensing device is arranged at the position of the lower layer sheet body corresponding to the guide head, and a detection signal of the photoelectric sensing device is input into the controller circuit board 13 through a circuit. The initial position and the end position of the guide groove are respectively provided with a magnetic steel, the guide arm 7 is also provided with two Hall switches for respectively detecting the two magnetic steels, and the Hall switches are electrically connected with the controller circuit board 13. The center of the guide groove is equidistantly provided with positioning holes corresponding to the sample bottles 2, and the upper disc of the sample disc 3 is provided with jacks corresponding to the positioning holes.
The inside controller circuit board 13 that is provided with of casing, be provided with the display screen 12 that is connected with controller circuit board 13 electricity on the casing outer wall, three-way valve 4, two-way valve 5, driving motor, the withdraw of the needle solenoid valve of cylinder 1 and the solenoid valve 9 of inserting the needle are connected with controller circuit board 13 electricity respectively. And a gas pressure controller 14 and a gas pressure gauge 10 are arranged on a connecting pipe between the helium bottle 18 and the multi-channel knob 16, a connecting pipe between the compressed air bottle 6 and the liquid reagent bottle 11 and a connecting pipe between the compressed air bottle 6 and the needle inserting electromagnetic valve 9. The gas pressure controllers 14 are electrically connected with the controller circuit board 13, and the gas pressure controllers 14 and the gas pressure meters 10 are fixedly arranged on the outer wall of the shell.
This example is for trace nitrogen conversion to N2In the O auxiliary device, a gear 15 on a driving motor drives a positioning disc 17 to rotate when the O auxiliary device works, the positioning disc 17 drives a sample disc 3 fixed on a rotating shaft to rotate together, meanwhile, a guide head on a guide arm 7 moves in a guide groove, the position of the positioning hole is detected and a side shaft is driven to rotate together, when the guide head moves and detects the positioning hole in the corresponding guide groove, the driving motor stops moving, and at the moment, the guide arm 7 also drives a cylinder 1 and a needle tube on the side shaft to rotate above a corresponding sample bottle 2 in the sample disc 3 to prepare for needle insertion. While this example was used for trace nitrogen conversion to N2The automatic vacuum pumping, automatic liquid adding, automatic vacuum replacement and automatic gas injection of the auxiliary device of O comprise the following specific working processes:
(1) automatic vacuum pumping: the needle tube is positioned above the sample bottle 2, a rapid vacuum-pumping program is selected on the display screen 12, the needle tube is driven by the cylinder 1 to enter the sample bottle 2, the two-way valve 5 is opened, the vacuum pump 8 is communicated with the needle head, the gas sample is pumped away by the vacuum pump 8, the optimal pumping time is 20 seconds, then the two-way valve 5 is closed, the needle is retreated, the next bottle position is moved, and the next vacuum-pumping is prepared.
(2) Automatic cleaning: the multichannel knob 16 is turned to the I position, so that the channel No. 1 is communicated with the multichannel knob 16, an automatic cleaning program is selected on the display screen 12, the needle tube is positioned above the sample bottle 2, the vacuum pump 8 is preheated, the needle is inserted, the two-way valve 5 is opened for quick vacuum pumping, the two-way valve 5 is closed, the three-way valve 4 is opened for filling high-purity helium, the three-way valve 4 is closed, and one-time filling and cleaning is completed; then opening a two-way valve 5 to quickly vacuumize, closing the two-way valve 5, opening a three-way valve 4 to fill high-purity helium, and closing the three-way valve 4; finally, the two-way valve 5 is opened to allow the vacuum pump 8 to evacuate the gas in the bottle for a long time (about 20 seconds).
(3) Automatic gas injection: the multichannel knob 16 turns to the position I, so that the channel 1 is communicated with the multichannel knob 16, an automatic dilution program is selected on the display screen 12, and the device automatically completes the following processes: the needle tube is positioned above the bottle, the three-way valve 4 is opened, gas is released for a period of time to wash the helium pipe and the threshold, then gas is released for about 0.5 second to wash the sample gas during each dilution, the needle is inserted and filled with helium, the three-way valve 4 is closed, the needle is withdrawn, and the needle is positioned to the next bottle level for dilution.
(4) Automatic liquid adding: connect liquid pipeline and injector, turn multichannel knob 16 to No. II position, make No. 2 passageway and multichannel knob 16 communicate with each other, select automatic liquid feeding procedure on display screen 12 to set the cleaning time to 0, the following process will be accomplished automatically to the device: the needle tube is positioned above the bottle, the three-way valve 4 is opened, the needle is inserted for filling, the three-way valve 4 is closed, the needle is withdrawn, and the needle tube is positioned to the next bottle level for filling.
In the description of the present invention, it should be noted that the terms "top", "bottom", "vertical", "inside", "outside", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
The principle and the implementation mode of the invention are explained by applying a specific example, and the description of the embodiment is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (1)
1. N for trace nitrogen conversion2O auxiliary device, characterized by: comprises a shell, a rotating shaft,A helium bottle, a compressed air bottle, a vacuum pump and a liquid reagent bottle; the rotating shaft is vertical, the bottom of the rotating shaft is positioned in the shell, and a sample disc which is coaxial with the rotating shaft and used for placing a sample bottle is fixedly arranged at the top of the rotating shaft; a side shaft is rotatably connected to one side of the shell, a supporting arm is arranged at the top of the side shaft, one end, far away from the side shaft, of the supporting arm extends to the sample disc and is fixedly provided with an air cylinder, a needle tube is fixedly arranged on a piston of the air cylinder, the air cylinder is positioned above the sample bottle, and the air cylinder can drive the needle tube to be inserted into the sample bottle on the sample disc; the side wall of the shell is provided with at least two channels, the outer wall of the shell is also provided with a multi-channel knob for switching the channels, the helium bottle, the multi-channel knob, one channel, a three-way valve and the needle tube are sequentially communicated, the compressed air bottle, the liquid reagent bottle, the multi-channel knob, the other channel, the three-way valve and the needle tube are sequentially communicated, the compressed air bottle is also communicated with a needle inserting electromagnetic valve of the air cylinder, and the vacuum pump, the two-way valve and the needle tube are sequentially communicated; a driving motor, a gear and a positioning disc which is coaxial and fixedly connected with the rotating shaft are further arranged in the shell, the gear is fixedly connected with an output shaft of the driving motor, and teeth which can be meshed with the gear are circumferentially and uniformly distributed on the bottom surface of the positioning disc; a guide arm is fixedly arranged at the bottom of the paraxial shaft and comprises an upper layer sheet body and a lower layer sheet body, and the positioning disc is clamped between the upper layer sheet body and the lower layer sheet body; a guide head is fixedly arranged on the upper layer sheet body, a spiral guide groove is formed in the top surface of the positioning disc, and the guide head is in sliding fit with the guide groove; a photoelectric sensing device is arranged on the guide arm, a photoelectric receiving tube of the photoelectric sensing device is embedded in the guide head, a photoelectric emitting tube of the photoelectric sensing device is arranged at the position of the lower layer sheet body corresponding to the guide head, and a detection signal of the photoelectric sensing device is input into a controller circuit board through a circuit; the starting position and the ending position of the guide groove are respectively provided with a magnetic steel, and the guide arm is also provided with two Hall sensors which respectively detect the two magnetic steelsThe Hall switch is electrically connected with the controller circuit board; positioning holes corresponding to the sample bottles are equidistantly formed in the center of the guide groove, and inserting holes corresponding to the positioning holes are formed in the upper disc of the sample disc; a controller circuit board is arranged in the shell, a display screen electrically connected with the controller circuit board is arranged on the outer wall of the shell, and the three-way valve, the two-way valve, the driving motor, the needle withdrawing electromagnetic valve of the air cylinder and the needle inserting electromagnetic valve are respectively and electrically connected with the controller circuit board; a gas pressure controller and a gas pressure gauge are arranged on a connecting pipe between the helium bottle and the multi-channel knob, a connecting pipe between the compressed air bottle and the liquid reagent bottle and a connecting pipe between the compressed air bottle and the needle inserting electromagnetic valve; the gas pressure controller is electrically connected with the controller circuit board, and the gas pressure controller and the gas pressure gauge are fixedly arranged on the outer wall of the shell.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811479637.8A CN109632412B (en) | 2018-12-05 | 2018-12-05 | A auxiliary device for trace nitrogen conversion N2O |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811479637.8A CN109632412B (en) | 2018-12-05 | 2018-12-05 | A auxiliary device for trace nitrogen conversion N2O |
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| Publication Number | Publication Date |
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| CN109632412A CN109632412A (en) | 2019-04-16 |
| CN109632412B true CN109632412B (en) | 2021-07-27 |
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Citations (4)
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| WO2009007042A2 (en) * | 2007-07-06 | 2009-01-15 | Thermo Fisher Scientific (Bremen) Gmbh | Device for providing gases, in particular for isotopic ratio analysis |
| CN201522479U (en) * | 2009-10-23 | 2010-07-07 | 万运帆 | Automatic gas sample injector |
| CN103776674A (en) * | 2014-01-20 | 2014-05-07 | 西华大学 | Nitrogen extracting and purifying device of nitrogen isotope sample in water |
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2018
- 2018-12-05 CN CN201811479637.8A patent/CN109632412B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2706764Y (en) * | 2004-05-29 | 2005-06-29 | 徐滋秋 | Portable overall organic carbon tester |
| WO2009007042A2 (en) * | 2007-07-06 | 2009-01-15 | Thermo Fisher Scientific (Bremen) Gmbh | Device for providing gases, in particular for isotopic ratio analysis |
| CN201522479U (en) * | 2009-10-23 | 2010-07-07 | 万运帆 | Automatic gas sample injector |
| CN103776674A (en) * | 2014-01-20 | 2014-05-07 | 西华大学 | Nitrogen extracting and purifying device of nitrogen isotope sample in water |
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| Title |
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| "N2O产生法测定土壤无机态氮15N丰度";曹亚澄 等;《土壤学报》;20130131;第113-119页 * |
| "微扩散法测定铵态氮、硝态氮的15N稳定同位素研究综述";温腾 等;《土壤》;20160831;全文 * |
| "扩散法测定土壤无机氮15N丰度方法优化研究";张珮仪 等;《土壤学报》;20170731;全文 * |
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