Greenhouse gas collecting device for frozen sample

By designing a temperature-controlled water bath frozen sample thawing acquisition device for frozen samples, the problem of complex and small capacity of ice core sealed gas collection device in the prior art is solved, and efficient greenhouse gas collection of large-volume frozen environment samples is achieved, providing new data and perspectives for climate change research.

CN119804040APending Publication Date: 2025-04-11INST OF URBAN ENVIRONMENT CHINESE ACAD OF SCI
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Patent Information

Application Number
CN202411911844.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-24
Publication Date
2025-04-11

AI Technical Summary

Technical Problem

The existing ice core sealing gas collection device is complex and has a small capacity, and is not suitable for trace greenhouse gas collection in large-volume frozen environment samples.

Method used

A frozen sample greenhouse gas collection device including the main body of the in-situ collector and the top cover is designed. The principle of melting frozen samples from the temperature-controlled water bath to release sealed gas is adopted, and the precise collection of gas is achieved through helium cleaning and negative pressure collection.

Benefits of technology

It realizes efficient collection of frozen samples for sealing greenhouse gases, suitable for large-volume frozen environmental samples, and provides new methods and data for in-depth research on global climate change.

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Abstract

The invention provides a frozen sample greenhouse gas collecting device. The method comprises the following steps: replacing headspace by using helium, indirectly unfreezing a frozen sample by using a temperature control water bath interlayer so as to release sealed greenhouse gas, and collecting headspace gas to analyze the greenhouse gas and other original design ideas, and a physicochemical collection device thereof. The collecting device comprises a main body and a top cover, the main body comprises an inner bin, a water bath clamping bin, inner and outer bin fixing columns, a water inlet and a water outlet and the like, the top cover is provided with an inflating and gas discharging / collecting port and is in threaded connection with the upper portion of the main body, and the air tightness is guaranteed through double silica gel ring pads. The device can systematically collect environment sample sealed greenhouse gas such as land ice cover or ocean ice cover ice core, frozen soil layer or sediment and soil collected by artificial freezing. A new method, new data and a new view angle are provided for related research on the composition of the frozen and sealed greenhouse gas, and the device has the characteristics of high-value commercial scientific research new equipment.
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Description

Technical Field

[0001] The present invention relates to a collection technology for sealing greenhouse gases from ice cores of land ice sheets or ocean ice sheets, frozen soil layers, or sediments and soils that are collected due to artificial freezing. Specifically, it is a device for collecting layered frozen samples to seal trace greenhouse gases. Background Art

[0002] Greenhouse gases are key factors in global climate change. The atmosphere of geological times can be reconstructed by collecting greenhouse gases frozen in ice cores and frozen soil layers. At the same time, global wetland ecosystems are the main source of modern key greenhouse gases (such as CH4 and N2O). Since wetland sediment profiles develop into different redox systems with the depth of water cover, such as oxygen system, nitrogen system, manganese system, iron system, sulfur system and CO2-methane system, etc., redox stratification from the surface to the bottom can dominate different processes and pathways of greenhouse gas (such as CO2, N2O, CH4, etc.) generation and consumption. Refined research on the biogeochemical processes and pathways of greenhouse gas production and consumption in wetland sediment profiles can be carried out by in-situ freezing and collecting wetland sediment cores, sealing greenhouse gases in different oxidation-reduction soil layers ("an in-situ frozen wetland sediment core collection device" has been applied for), and after stratification, the greenhouse gases sealed in frozen samples are collected using the present invention. Based on the research idea of ​​using a temperature-controlled water bath to melt frozen samples to release the greenhouse gases generated by the historical atmospheric components or biogeochemical processes they have sealed, the present invention is specially proposed. Summary of the invention

[0003] A first object of the present invention is to collect greenhouse gases sealed in frozen samples for analyzing their concentrations.

[0004] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are particularly adopted:

[0005] A greenhouse gas collection device for frozen samples includes an in-situ collector body and a top cover; the in-situ collector body consists of four parts: an inner chamber, a water bath clamp chamber, inner and outer chamber fixing columns, and a water inlet and outlet. The inner chamber wall and the outer wall of the main body are fully closed and nested at the mouth and bottom of the main body to form a water bath clamp chamber (with a fixing column inside), and the outer wall of the main body is opposite (180 o )Open the water inlet and drain port of the water bath clamp. The top cover has a helium inlet and a drain / collection port, which are connected to the inner chamber. A silicone groove is set on the inner side of the top, which is connected to the collector body through a threaded airtight connection.

[0006] Preferably, the device body is made of stainless steel or lightweight aluminum alloy.

[0007] Preferably, the upper port of the device body and the inside of the top cover are fitted with threads, and a silicone groove is designed on the inner side of the top cover, and a silicone ring gasket is embedded to ensure sealing.

[0008] Preferably, the top cover of the device has two air holes, which are sealed with replaceable T-shaped silicone plugs; helium inflation and exhaust as well as greenhouse gas sample collection are all connected to the inner chamber by a syringe needle with a three-way valve piercing the silicone; the helium hole needle is connected to the gas cylinder with a silicone tube, which is adjusted by a flow regulating valve at the gas cylinder mouth; the exhaust / gas collection needle is connected to the three-way valve, which is used to exhaust the atmosphere (during helium cleaning before water bath melting) and collect gas samples (after melting equilibrium).

[0009] Preferably, the size of each component of the device can be adjusted in proportion according to actual needs, and the material can be selected according to actual needs.

[0010] Therefore, the present invention adopts a frozen sample greenhouse gas collection device with the above structure, which can realize the collection of greenhouse gases sealed in frozen samples; it is simple to operate, and can also be applied to the collection of greenhouse gases sealed in environmental samples such as ice cores of land ice sheets or ocean ice sheets, permafrost layers, or sediments and soil collected by artificial freezing. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings used in the technical description of the embodiments.

[0012] Figure 1 This is a schematic diagram of the overall structure of a frozen sample greenhouse gas collection device of the present invention;

[0013] Figure 2 This is a partially detailed structural cross-sectional view of a frozen sample greenhouse gas collection device of the present invention. DETAILED DESCRIPTION

[0014] The embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings, but those skilled in the art will appreciate that the following examples are only used to illustrate the present invention and should not be construed as limiting the scope of application of the present invention. If the specific conditions and specifications are not specified in the examples, they shall be carried out under conventional conditions or conditions recommended by the manufacturer. The materials used, which do not specify the manufacturer and specifications, are all conventional products that can be purchased commercially. The dimensions of each component can be adjusted in proportion according to actual needs, and the material can be selected according to actual needs. Secondly, the technical solution of the present invention can be modified or equivalently replaced, and these modifications or equivalent replacements cannot deviate from the connotation and scope of the technical solution of the present invention after modification.

[0015] Greenhouse gases are a key factor in global climate change. The atmosphere of geological times can be reconstructed by collecting greenhouse gases frozen in ice cores and frozen soil layers. At the same time, detailed research on the biogeochemical processes and pathways of greenhouse gas production and consumption in wetland sediment profiles can be carried out by collecting wetland sediment cores through in-situ freezing, and using the present invention to collect greenhouse gases sealed in frozen samples after stratification. In view of the fact that the current ice core sealed gas collection device is complex and has a small capacity, it is not suitable for trace greenhouse gas collection devices for large-volume frozen environment samples. The present invention provides a simple collection device for greenhouse gases from large-capacity frozen samples.

[0016] The method of the present invention is based on the principle of releasing sealed gases by melting frozen samples in a temperature-controlled water bath. A frozen sample thawing device with a water bath clamp is specially designed. The gas in the headspace of the collection device is purged and replaced with helium before thawing, and the greenhouse gases released by the thawing of the frozen samples are collected for analyzing the greenhouse gas components sealed in the frozen samples.

[0017] Specifically, the full diagram of the device of the present invention is shown in Figure 1 , the top view of the substructure is shown in Figure 2 .like Figure 1 As shown, the present invention provides a frozen sample greenhouse gas collection device, including a collector "main body 1" and a "top cover 2", the collector main body is a double-layer hollow clamp structure, the 20 mm portion of the main body top opening is the "main body mouth 3", and its external thread is used to screw and seal with the top cover; the "mouth 3" and the "headspace gas and sediment bin 4" together constitute an "inner bin 5", the inner bin has a diameter of 146 mm and a height of 90 mm; the inner bin wall and the outer wall of the main body are double-nested and closed to form a "water bath clamp 6" with a thickness of 17 mm, and the water bath clamp is provided with a "water bath water inlet 7" and a "water outlet 8" opposite to each other on the outside of the main body. The water inlet and outlet of the temperature-controlled water bath are connected to the water bath clamp chamber, and are connected to the water bath pot, peristaltic pump, etc. through the "silicone tube 9" on the outside; a "fixed column 10" with a diameter of 20 mm and a height of 10 mm is set between the center of the bottom of the inner chamber wall and the outer wall, and is welded to the bottom inner wall of the "main outer chamber 11" (diameter 180 mm, height 80 mm); a "silicone ring gasket 12" with a diameter of 5 mm is set on the upper part of the "main outer chamber 11" to seal with the "top cover 2".

[0018] The device "top cover 2" is 30 mm high and 180 mm in diameter. The solid side wall is 17 mm thick and has an arched thread. The solid top is 10 mm thick and has a 2.5 mm deep and 5 mm wide annular "silicone pad groove 13" milled. The silicone ring gasket is filled in and sealed with the "main body mouth 3" through threads, and a double-layer silicone seal is achieved with the above-mentioned "main body mouth silicone gasket 12" to ensure the airtightness of the device; "helium filling hole 14" and "exhaust / gas collection hole 15" are set on both sides of the center of the "top cover 2", and a commercially available T-shaped silicone bottle stopper (diameter 20 The air pipe connected to the needle is connected to the "single-vent valve 16" and the "three-way valve 17". The other end of the "single-vent valve 16" is connected to the helium cylinder through the "trachea 18", and the air pressure is adjusted by the cylinder pressure valve. One end of the "three-way valve 17" can be connected to the "gas collection bag / bottle 19", and the other end is emptied for helium cleaning of the "main body inner chamber 5" to discharge the air.

[0019] The operation steps of the embodiment of the present invention are as follows:

[0020] (a) Place the frozen sample into the "inner chamber 5", open the "helium filling hole 14" and "exhaust / gas collection hole 15" of the "top cover 2", screw them together with the "main body 1" until they are tight, cover with a T-shaped silicone plug, insert the syringe needle to connect the helium "single-vent valve 16" and "three-vent valve 17", screw the "three-vent valve 17" until it is emptied, open the helium bottle pressure valve to clean the "inner chamber 5" with helium, after cleaning for a certain period of time, close the "single-vent valve 16" and "three-vent valve 17" at the same time, after balancing for an appropriate period of time, open the "single-vent valve 16" and "three-vent valve 17" again to empty, and clean the headspace of the "inner chamber 5" with helium. This can be repeated 2-3 times to ensure that the headspace air is completely replaced by helium.

[0021] (b) Turn on the water bath and heat the water to the appropriate temperature. Use the "silicone tube 9" to connect the water bath and the "water inlet 7", "drain outlet 8" and the water bath to form a circulating water bath, and connect the silicone tube between the "drain outlet 8" and the water bath to a peristaltic pump to ensure that the hot water in the water bath in the "silicone tube 9" continues to flow. Open the water outlet of the water bath, and inject hot water from the "water inlet 7" into the "water clamp chamber 6" and discharge it from the "drain outlet 8". This step takes a certain amount of time to ensure that the frozen samples in the "inner chamber 5" are thawed;

[0022] (c) During the thawing process, reopen the "three-way air valve 17" to the gas collection end, connect the "vacuum gas collection bag / bottle 19" to collect the sealed greenhouse gases released during the thawing process of the frozen samples in the "inner chamber 5" of the collector by negative pressure.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] The method provided by the present invention is a method for thawing and collecting frozen samples in a temperature-controlled water bath. Through the thawing operation, the system collects greenhouse gases sealed in the frozen samples, providing new methods, new data and new perspectives for in-depth research on key greenhouse gases in global climate change.

Claims

1. A frozen sample greenhouse gas collection device, characterized in that: The original design idea is to release and collect greenhouse gases sealed in frozen samples (ice cores, frozen soil or artificially frozen samples, etc.) by using a temperature-controlled water bath. The materialized collection device includes a collector body and a top cover. The collector body is a double-layer hollow sandwich structure, consisting of four parts: an inner chamber, a water bath sandwich, inner and outer chamber fixed columns, and a water inlet and outlet. The inner chamber wall and the outer wall of the main body are fully closed and nested at the mouth and bottom of the main body to form a water bath sandwich (with fixed columns inside), and the outside of the main body is opposite (180 o ) Open the water bath clamping chamber water inlet (upper edge) and drain outlet (lower edge); the top cover is provided with an air inlet and an exhaust port (gas collection port), which are closed with a T-shaped silicone plug; a groove is made on the inner side of the top of the top cover to bury a silicone ring gasket, and the inner wall has threads to achieve an airtight connection with the collector body through the threads; before heating and thawing, helium is used to replace the gas in the headspace through the air inlet and exhaust hole of the top cover.

2. A frozen sample greenhouse gas collection device according to claim 1, characterized in that: An original design idea to use a temperature-controlled water bath to seal and collect greenhouse gas release from frozen samples.

3. A frozen sample greenhouse gas collection device according to claim 1, characterized in that: The collector body is a double-layer hollow sandwich structure, which consists of four parts: an inner chamber, a water bath sandwich, inner and outer chamber fixing columns, and a water inlet and outlet, as shown in FIG1 .

4. A frozen sample greenhouse gas collection device according to claim 1, characterized in that: The double-layer hollow clamp structure of the collector body is a water bath clamp, and a fixed column is set between the outer wall of the body and the inner wall of the clamp to improve the strength of the collector, and a water inlet (upper edge) and a drain outlet (lower edge) are set opposite (180°) to the outer wall of the body, as shown in Figure 1-1.

5. The frozen sample greenhouse gas collection device according to claim 1, characterized in that: The inside of the top cover and the mouth of the main body are matched with threads. A silicone groove is designed in the top cover to embed a silicone ring gasket, and a silicone ring gasket is provided at the mouth of the main body to achieve a double airtight connection between the top cover and the main body, as shown in the top view of the cross-section of Figure 2B-B.

6. The frozen sample greenhouse gas collection device according to claim 1, characterized in that: In order to collect frozen samples and seal greenhouse gases, the helium filling port and the exhaust / gas collection port of the top cover are sealed by replaceable T-shaped silicone plugs. The replaceable silicone plugs can be pierced by a syringe needle with a three-way valve and connected to the inner chamber gas chamber. Before freezing, the head space of the inner chamber is cleaned with helium through the system and replaced with helium to collect trace greenhouse gases released during the melting process of the frozen samples, as shown in Figure 1-2, the top view of the section of Figure 2-BB and the front view of the section of Figure 2-DD.

7. The frozen sample greenhouse gas collection device according to claim 1, characterized in that: The collection device can be applied to the collection of greenhouse gases stored in environmental samples such as ice cores of land ice sheets or ocean ice sheets, frozen soil layers, or sediments and soil collected through artificial freezing.