CN114414431A - Distillation and absorption method and distillation and absorption device for soil ammonium nitrogen - Google Patents
Distillation and absorption method and distillation and absorption device for soil ammonium nitrogen Download PDFInfo
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- CN114414431A CN114414431A CN202210093245.8A CN202210093245A CN114414431A CN 114414431 A CN114414431 A CN 114414431A CN 202210093245 A CN202210093245 A CN 202210093245A CN 114414431 A CN114414431 A CN 114414431A
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- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
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Abstract
The invention discloses a distillation and absorption method and a distillation and absorption device for soil ammonium nitrogen, which comprise the following steps: putting the solution containing ammonium nitrogen and an ammonia reactant into a plurality of distillation absorption devices; placing a plurality of distillation absorption devices at 80 ℃, 100 ℃ and 120 ℃ respectively, distilling for 5min, 10min and 30min at set temperature respectively, and taking out NH contained in the distillation absorption devices3A fiber filter sheet; a plurality of distillation absorption devices are filled with NH3Taking out the fiber filter disc and respectively placing the fiber filter disc in an environment of 70 ℃ for drying for 2 hours; taking out a plurality of fiber filter discs and detecting the nitrogen content to obtain that the absorption efficiency of ammonium nitrogen distilled for 30min at the temperature of 120 ℃ reaches 100%; according to the invention, a plurality of groups of different distillation times are set at different temperatures, so that the temperature and the distillation time with the highest ammonium nitrogen absorption efficiency are obtained, and the purpose of improving the extraction efficiency and the extraction quality of ammonium nitrogen is further achieved.
Description
Technical Field
The invention relates to the technical field of test devices, in particular to a distillation and absorption method and a distillation and absorption device for soil ammonium nitrogen.
Background
Nitrogen is one of essential nutrient elements for plant growth and development, is also the most mineral element and the most exhaustible nutrient element absorbed from soil, and plays an important role in soil fertility. Ammonium ions (NH 4) form ammonium nitrogen in soil+) The existing form is the final product of mineralization and transformation of organic nitrogen compounds in soil, and is one of the most main forms of plant absorption and environmental pollution. The stable isotope tracer technology comprises N natural abundance technology and enrichment marking technology, is widely applied to researches on mineralization of organic nitrogen in soil, transformation of inorganic nitrogen, use efficiency of nitrogen fertilizer, biological effectiveness and the like, and relates to accurate determination of NH4+-N isotope ratio.
After the soil ammonium nitrogen is extracted, because the soluble nitrogen component in the extracting solution is complex, the ammonium nitrogen needs to be separated firstly and then prepared into a sample for the isotope mass spectrometer to detect, so the accuracy of the pretreatment method has great influence on the accuracy of the mass spectrometry result. At present, the main methods for separating soil ammonium nitrogen for stable isotope mass spectrometry are as follows: steam distillation and microdiffusion. The former method is the traditional method for separating and converting inorganic nitrogen in soil (Lurueyun, 1990), the separated and concentrated ammonium salt can be used for detecting 15N abundance by combining an element analyzer and a stable isotope mass spectrometer or converting trace ammonium into N2O gas by a chemical method, and then an isotope ratio mass spectrometer with an automatic preconcentration device is used for measuring N2The method for measuring the abundance of 15N in O, such as the ammonium nitrogen and nitrate nitrogen in soil with the publication number of CN1725008 and a special device thereof are used for measuring, and the device is complicated and has high cost. The diffusion method is NH4 in the soil extract+Conversion to NH under catalytic diffusion of MgO3Then absorbed by a filter disc containing potassium bisulfate, and the filter disc can be used for 15N abundance detection through the combination of an element analyzer and a stable isotope mass spectrometer. Wherein, the traditional distillation method has short processing time of a single sample and higher efficiency, but the experimental process has a plurality of operation steps and the sample is steamedCross contamination can be generated among the distillates, and batch processing of samples cannot be realized; the diffusion method instrument is simple to operate, can realize batch processing of samples, but the diffusion culture consumes long time (generally requiring 48 hours or more).
In order to solve the above problems, the present invention provides a distillation and absorption method and a distillation and absorption apparatus for soil ammonium nitrogen, which solve the problems of low extraction efficiency and poor extraction quality of ammonium nitrogen in the conventional soil ammonium nitrogen extraction method and apparatus.
Disclosure of Invention
The invention aims to provide a distillation absorption method and a distillation absorption device for soil ammonium nitrogen, and the purpose of improving the extraction efficiency and the extraction quality of the ammonium nitrogen is achieved.
In order to achieve the purpose, the invention provides the following scheme:
a distillation absorption method of soil ammonium nitrogen comprises the following steps:
putting the solution containing ammonium nitrogen and an ammonia reactant into a plurality of distillation absorption devices;
placing a plurality of distillation absorption devices at the temperature of 80 ℃, 100 ℃ and 120 ℃ respectively, distilling 5min, 10min and 30min at the set temperature respectively, and taking out NH in the distillation absorption devices3A fiber filter sheet;
a plurality of distillation absorption devices are filled with NH3Taking out the fiber filter disc and respectively placing the fiber filter disc in an environment of 70 ℃ for drying for 2 hours;
and taking out a plurality of fiber filter discs and detecting the nitrogen content to obtain that the absorption efficiency of distilling 30min ammonium nitrogen at the temperature of 120 ℃ reaches 100%.
Preferably, the fiber filter is taken out of the distillation and absorption device by tweezers and is placed in a drying box for drying.
Preferably, the heating device is a dry thermostat with a temperature control range of 5 ℃ to 130 ℃.
Preferably, the thickness of the fibrous filter sheet is 6mm to 10 mm.
The distillation and absorption device applied to the distillation and absorption method of the soil ammonium nitrogen comprises a thermostat and a plurality of reactors arranged on the thermostat, wherein each reactor comprises a reaction bottle and an ammonia vapor absorber arranged at the bottle mouth of the reaction bottle, each ammonia vapor absorber comprises a composite PTFE (polytetrafluoroethylene) membrane, a fiber filter disc, a sleeve pipe and a sealing gasket, one end of each sleeve pipe is communicated with the bottle mouth in a sealing mode, the other end of each sleeve pipe is provided with the sealing gasket, the fiber filter disc and the composite PTFE membrane are sequentially arranged in the sleeve pipe from top to bottom, and potassium hydrogen sulfate is arranged on the fiber filter disc.
Preferably, the sealing device further comprises a threaded sealing cover, wherein the outer surface of the sleeve is provided with a first thread matched with the threaded sealing cover, and the threaded sealing cover is in meshed connection with the sleeve.
Preferably, an annular first groove is formed in one end, communicated with the bottle opening, of the sleeve, the width of the first groove is equal to the thickness of the side wall of the bottle opening, and the bottle opening is inserted into the first groove.
Preferably, a second groove is formed in the inner wall of the sleeve, and the fiber filter disc is clamped in the second groove.
Preferably, the composite PTFE membrane is in contact with the mouth of the bottle.
Preferably, the sealing gasket is nitrile rubber, the diameter is 13mm to 15mm, and the thickness is 1.5mm to 2 mm.
Compared with the prior art, the invention has the following technical effects:
1. according to the invention, a plurality of groups of different distillation times are set at different temperatures, so that the temperature and the distillation time with the highest ammonium nitrogen absorption efficiency are obtained, and the purpose of improving the extraction efficiency and the extraction quality of ammonium nitrogen is further achieved.
2. Taking the fiber filter disc out of the distillation and absorption device by using tweezers, and placing the fiber filter disc in a drying box for drying; the use of tweezers guarantees quick convenient taking out of fibre filter element, adopts the drying cabinet to carry out the drying simultaneously only to place into the drying cabinet with a plurality of distillation plant can.
3. The heating device is a dry thermostat, and the temperature control range of the dry thermostat is 5-130 ℃.
4. The invention discloses a distillation absorption device applied in a distillation absorption method of soil ammonium nitrogen, which comprises a thermostat and a plurality of reactors arranged on the thermostat, wherein each reactor comprises a reaction bottle and an ammonia vapor absorber arranged at the bottle mouth of the reaction bottle, each ammonia vapor absorber comprises a composite PTFE (polytetrafluoroethylene) membrane, a fiber filter disc, a sleeve pipe with one end hermetically communicated with the bottle mouth and a sealing gasket arranged at the other end of the sleeve pipe, the fiber filter disc and the composite PTFE membrane are sequentially arranged in the sleeve pipe from top to bottom, and potassium hydrogen sulfate is arranged on the fiber filter disc.
Drawings
In order to more clearly illustrate the present invention or 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 is a schematic structural diagram of a distillation and absorption device;
FIG. 2 is a schematic view of the gasket construction;
FIG. 3 is a schematic structural view of a fibrous filter sheet;
FIG. 4 is a schematic view of a sleeve structure;
FIG. 5 is a bottom view of the bushing;
wherein, 1, a thread sealing cover; 2. a sleeve; 3. a reaction bottle; 4. a solution containing ammonium nitrogen; 5. a dry thermostat; 6. a gasket; 7. potassium hydrogen sulfate; 8. a fiber filter sheet; 9. a sleeve; 10. a second groove; 11. a first groove.
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 distillation absorption method and a distillation absorption device for soil ammonium nitrogen, and the purpose of improving the extraction efficiency and the extraction quality of the ammonium nitrogen is achieved.
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.
A distillation absorption method of soil ammonium nitrogen comprises the following steps: putting the solution containing ammonium nitrogen and an ammonia reactant into a plurality of distillation absorption devices; placing a plurality of distillation absorption devices at the temperature of 80 ℃, 100 ℃ and 120 ℃ respectively, distilling 5min, 10min and 30min at the set temperature respectively, and taking out NH in the distillation absorption devices3A fiber filter sheet; the NH contained in a plurality of distillation absorption devices3Taking out the fiber filter disc and respectively placing the fiber filter disc in an environment of 70 ℃ for drying for 2 hours; taking out a plurality of fiber filter discs and detecting the nitrogen content to obtain that the absorption efficiency of distilling 30min ammonium nitrogen at the temperature of 120 ℃ reaches 100%; according to the invention, a plurality of groups of different distillation times are set at different temperatures, so that the temperature and the distillation time with the highest ammonium nitrogen absorption efficiency are obtained, and the purpose of improving the extraction efficiency and the extraction quality of ammonium nitrogen is further achieved. The recovery rate of the ammonium nitrogen produced by distillation is shown in the following table:
further, taking the fiber filter disc out of the distillation and absorption device by using tweezers, and placing the fiber filter disc in a drying box for drying; the use of tweezers guarantees quick convenient taking out of fibre filter element, adopts the drying cabinet to carry out the drying simultaneously only to place into the drying cabinet with a plurality of distillation plant can.
Further, the heating device is a dry thermostat, and the temperature control range of the dry thermostat is 5 ℃ to 130 ℃.
Further, the thickness of the fiber filter sheet is 6mm to 10 mm.
Referring to fig. 1 to 5, a distillation absorption device applied in a distillation absorption method of soil ammonium nitrogen, comprising a thermostat and a plurality of reactors arranged on the thermostat, wherein each reactor comprises a reaction bottle 3 and an ammonia vapor absorber arranged at the bottle mouth of the reaction bottle 3, the ammonia vapor absorber comprises a composite PTFE membrane, a fiber filter 8, a sleeve 2 with one end hermetically communicated with the bottle mouth, and a sealing gasket 6 arranged at the other end of the sleeve 2, the fiber filter 8 and the composite PTFE membrane are sequentially arranged in the sleeve 2 from top to bottom, and potassium hydrogen sulfate 7 is arranged on the fiber filter 8;
referring to fig. 1, the sealing device further comprises a threaded sealing cover 1, a first thread matched with the threaded sealing cover 1 is arranged on the outer surface of the sleeve 2, and the threaded sealing cover 1 is in meshed connection with the sleeve 2; the sealing screw cap 1 is additionally arranged on the sleeve 2, so that the sealing degree of the sleeve 2 and the reaction bottle 3 is further enhanced, and the dissipation of ammonia vapor is avoided.
Referring to fig. 5, an annular first groove 11 is formed in one end of the sleeve 2, which is communicated with the bottle mouth, the width of the first groove 11 is the same as the thickness of the side wall of the bottle mouth, and the bottle mouth is inserted into the first groove 11; the bottle mouth is inserted into the first groove 11 to ensure the sealing of the sleeve 2 and the bottle mouth, the connection mode covers the bottle mouth and the connection joint of the sleeve 2 in the groove of the sleeve 2, the sealing performance of the sleeve 2 and the bottle mouth is further enhanced, and the ammonia steam loss is reduced.
Referring to fig. 4, a second groove 10 is formed in the inner wall of the casing 2, and the fiber filter 8 is clamped in the second groove 10, so that the fiber filter 8 is stably arranged in the casing 2.
Further, the composite PTFE film is in contact with the bottle opening, the bottle opening is completely covered by the composite PTFE film, only ammonia steam is allowed to pass through, and water vapor cannot pass through, so that the ammonia steam and potassium hydrogen sulfate 7 are ensured to fully react, and the interference of the water vapor cannot be received.
Further, the sealing gasket 6 is nitrile rubber with the diameter of 13mm to 15mm and the thickness of 1.5mm to 2 mm.
The use method of the distillation absorption device in the invention is as follows:
sucking 1mL of solution 4 containing ammonium nitrogen, placing the solution in a reaction bottle 3, weighing 3mg of MgO, adding the MgO into the reaction bottle 3, quickly adding an ammonia vapor absorber, and then covering a sleeve 2 and a threaded sealing cover; the reaction flask 3 is placed on a dry thermostat 5 and distilled at 120 ℃ for 30 min; and after the distillation is finished and the reaction bottle 3 is cooled, taking out the filter disc by using tweezers, drying the filter disc in a drying oven at 70 ℃ for 2 hours, and detecting the nitrogen content.
The adaptation according to the actual needs is within the scope of the invention.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. The distillation absorption method for the soil ammonium nitrogen is characterized by comprising the following steps:
putting the solution containing ammonium nitrogen and an ammonia reactant into a plurality of distillation absorption devices;
placing a plurality of distillation absorption devices at 80 ℃, 100 ℃ and 120 ℃ respectively, distilling for 5min, 10min and 30min at set temperature respectively, and taking out NH contained in the distillation absorption devices3A fiber filter sheet;
a plurality of distillation absorption devices are filled with NH3Taking out the fiber filter disc and respectively placing the fiber filter disc in an environment of 70 ℃ for drying for 2 hours;
and taking out a plurality of fiber filter discs and detecting the nitrogen content to obtain that the absorption efficiency of distilling 30min of ammonium nitrogen at the temperature of 120 ℃ reaches 100%.
2. The method for distilling and absorbing soil ammonium nitrogen according to claim 1, wherein the fibrous filter sheet is taken out of the distilling and absorbing device by tweezers and is placed in a drying box for drying.
3. The method for distilling and absorbing soil ammonium nitrogen according to claim 1, wherein the heating device is a dry thermostat, and the temperature of the dry thermostat is controlled within a range of 5 ℃ to 130 ℃.
4. The distillation absorption device according to claim 1, wherein the thickness of the fiber filter sheet is 6mm to 10 mm.
5. The distillation and absorption device applied to the distillation and absorption method of the soil ammonium nitrogen is characterized by comprising a thermostat and a plurality of reactors arranged on the thermostat, wherein each reactor comprises a reaction bottle and an ammonia vapor absorber arranged at the bottle mouth of the reaction bottle, each ammonia vapor absorber comprises a composite PTFE (polytetrafluoroethylene) membrane, a fiber filter disc, a sleeve pipe and a sealing gasket, one end of each sleeve pipe is communicated with the bottle mouth in a sealing mode, the other end of each sleeve pipe is provided with the sealing gasket, the fiber filter disc and the composite PTFE membrane are sequentially arranged in the sleeve pipe from top to bottom, and the fiber filter disc is provided with potassium hydrogen sulfate.
6. The distillation absorption device as claimed in claim 5, further comprising a screw sealing cover, wherein the outer surface of the sleeve is provided with a first screw thread matching with the screw sealing cover, and the screw sealing cover is engaged with the sleeve.
7. A distillation absorption device as claimed in claim 5, wherein an annular first groove is formed in one end of the sleeve communicating with the bottle mouth, the width of the first groove is the same as the thickness of the side wall of the bottle mouth, and the bottle mouth is inserted into the first groove.
8. The distillation and absorption device as claimed in claim 7, wherein a second groove is formed in the inner wall of the sleeve, and the fiber filter is clamped in the second groove.
9. A distillation absorption device according to claim 5, wherein said composite PTFE membrane is in contact with said spout.
10. A distillation absorbing device according to claim 5, wherein the sealing pad is nitrile rubber with a diameter of 13mm to 15mm and a thickness of 1.5mm to 2 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210093245.8A CN114414431A (en) | 2022-01-26 | 2022-01-26 | Distillation and absorption method and distillation and absorption device for soil ammonium nitrogen |
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| CN202210093245.8A CN114414431A (en) | 2022-01-26 | 2022-01-26 | Distillation and absorption method and distillation and absorption device for soil ammonium nitrogen |
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| CN112666245A (en) * | 2020-12-18 | 2021-04-16 | 中国科学院地球环境研究所 | Preparation method of ammonium nitrogen adsorption bag in natural water and detection method of isotope thereof |
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2022
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| US5022967A (en) * | 1989-09-18 | 1991-06-11 | Lachat Instruments | Microdistillation apparatus |
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