CN215115462U - Device for separating krypton and xenon in rock sample - Google Patents
Device for separating krypton and xenon in rock sample Download PDFInfo
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- CN215115462U CN215115462U CN202121635913.2U CN202121635913U CN215115462U CN 215115462 U CN215115462 U CN 215115462U CN 202121635913 U CN202121635913 U CN 202121635913U CN 215115462 U CN215115462 U CN 215115462U
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- 229910052724 xenon Inorganic materials 0.000 title claims abstract description 35
- 229910052743 krypton Inorganic materials 0.000 title claims abstract description 34
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000011435 rock Substances 0.000 title claims abstract description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 350
- 239000007788 liquid Substances 0.000 claims abstract description 175
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 175
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 42
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 238000002474 experimental method Methods 0.000 claims abstract description 23
- 239000007789 gas Substances 0.000 claims description 24
- 238000007789 sealing Methods 0.000 claims description 10
- 230000001502 supplementing effect Effects 0.000 claims description 6
- VFWCMGCRMGJXDK-UHFFFAOYSA-N 1-chlorobutane Chemical compound CCCCCl VFWCMGCRMGJXDK-UHFFFAOYSA-N 0.000 claims description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N methyl pentane Natural products CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 10
- 238000000926 separation method Methods 0.000 abstract description 10
- 229910052756 noble gas Inorganic materials 0.000 abstract description 8
- 239000003595 mist Substances 0.000 abstract description 6
- 238000004949 mass spectrometry Methods 0.000 abstract description 4
- 239000011261 inert gas Substances 0.000 abstract description 3
- 238000012545 processing Methods 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052734 helium Inorganic materials 0.000 description 5
- 238000007872 degassing Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052754 neon Inorganic materials 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000295 complement effect Effects 0.000 description 2
- 239000003673 groundwater Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- DNXNYEBMOSARMM-UHFFFAOYSA-N alumane;zirconium Chemical compound [AlH3].[Zr] DNXNYEBMOSARMM-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 150000002835 noble gases Chemical class 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
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Abstract
The utility model discloses a device for separating krypton and xenon in rock sample, including barrel and upper cover, include liquid nitrogen layer and heat-conducting agent layer in the barrel, liquid nitrogen layer suit is in the outside on heat-conducting agent layer, evacuation treatment can be done to the cavity between the outer wall on liquid nitrogen layer and the barrel, the inner chamber on liquid nitrogen layer can hold the liquid nitrogen, be provided with cold finger in the inner chamber on heat-conducting agent layer, can hold the heat-conducting agent between the inner wall on heat-conducting agent layer and the cold finger, cold finger is connected with heating element, cold finger is connected with temperature element, cold finger still is connected with the experiment chamber, the inner chamber and the experiment chamber of cold finger are linked together, the experiment chamber can be linked together with outside mist. The utility model is used for among the pretreatment process of mass spectrometry inert gas sample, easy operation is convenient, can high-quality high-efficient separation noble gas, shortens the experimental time, reduces the background, improves noble gas's purity simultaneously.
Description
Technical Field
The utility model relates to a geological sample analysis technical field especially relates to a device that is arranged in separating krypton and xenon in the rock sample.
Background
Rare gases are low in element abundance and inactive in chemical properties in the earth and the planets. In the geological history evolution process, the composition and isotope thereof are not easily influenced by the actions of complex chemical reaction, biological activity and the like, but only depend on physical processes such as mixing, diffusion, dissolution, adsorption, nuclear reaction and the like. Therefore, rare gas elements (i.e., helium He, neon Ne, argon Ar, krypton Kr, and xenon Xe) are widely used in research on material sources in the field of earth science and tracing and isotope-dating of geochemical processes, etc.
Noble gases find numerous applications in the field of geochemical research, for example: kr is mainly applied to researches such as groundwater dating, universal exposure age of meteorite, tracing of earth volatile sources, atmosphere origin, early evolution of solar system and the like. Scientific problems that Xe can solve include the estimation of the paleoclimate from groundwater and secondary sediment studies, air-ocean gas exchange, valance degassing, loss of earth volatiles, and the origin and evolution of the atmosphere, among others.
At present, the domestic test method for the He, Ne and Ar isotope composition in geological samples is mature, the rare gas analysis technology has been greatly developed in the aspects of precision and accuracy along with the introduction of a batch of high-precision rare gas mass spectrometers in recent years, and the He, Ne and Ar isotopes have been equivalent to the advanced international level. However, most of domestic laboratories do not carry out Kr and Xe tests, and the only test level has a large gap with the international advanced laboratories.
All studies on rare gases are based on mass spectrometry techniques with low background, high purity, high sensitivity, and high resolution. However, even if the same sample has different amounts of rare gases, the amount of rare gases may vary greatly or even by several orders of magnitude, and these differences may have an effect on the determination of the amount. Therefore, the separation and purification of rare gases are particularly important. The general purification scheme is roughly:
the separation and purification of He, Ne and Ar are relatively simple, the adsorption temperature of He is very low and is about 4K, the adsorption temperature of Ne is below 20K, and the adsorption temperature of Ar is below 80K. Therefore, the separation process generally employed is:
(1) and (3) purification: firstly, the gas released by the experimental sample is roughly purified to remove CO2Most of miscellaneous gases such as alkane and the like are further purified by equipment such as a zirconium-aluminum pump and the like;
(2) respectively adsorbing: immersing a cryogenic trap filled with activated carbon into liquid nitrogen at the periphery to adsorb most of Ar, and setting a commercial cryogenic pump at 10K to adsorb Ne, Kr, Xe and a small amount of residual Ar;
(3) respectively releasing: then the gas (He) at this time is diffused into the mass spectrometer for measurement; then setting a commercial low-temperature pump at 30K, releasing Ne, and diffusing into a mass spectrometer for measurement; if the detection of Kr and Xe is carried out, Ne is released, then the temperature is raised step by step (110K and 135K) to release the Ne respectively, and the Ne is diffused into a mass spectrometer for measurement; and finally, completely heating the liquid nitrogen low-temperature cold trap filled with the activated carbon, releasing Ar, and diffusing the Ar into a mass spectrometer for measurement.
The commercial apparatus used above requires a refrigerant such as high-purity helium gas to be used, and the temperature is reduced by volume compression, which consumes a lot of time, and also has problems that the matrix effect is difficult to remove and the background of the experiment is high because the residual Ar partially overlaps with the release temperature curves of Kr and Xe.
Therefore, how to reduce the experimental time, reduce the background, and improve the purity of the rare gas in the pretreatment process of the inert gas sample in mass spectrometry is a problem to be solved urgently by those skilled in the art.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a device for separating krypton and xenon in rock sample to solve the problem that above-mentioned prior art exists, shorten the experimental time, improve sample noble gas's purity.
In order to achieve the above object, the utility model provides a following scheme: the utility model provides a device for separating krypton and xenon in rock sample, including barrel and upper cover, the barrel with the upper cover can be dismantled and be connected, set up sealing element between barrel and the upper cover, include liquid nitrogen layer and heat-conducting agent layer in the barrel, the liquid nitrogen layer suit is in the outside of heat-conducting agent layer, the outer wall of liquid nitrogen layer with the cavity between the barrel can be done the evacuation and is handled, the inner chamber of liquid nitrogen layer can hold the liquid nitrogen, be provided with the cold finger in the inner chamber of heat-conducting agent layer, the inner wall of heat-conducting agent layer with can hold the heat-conducting agent between the cold finger, the cold finger is connected with heating element, heating element can be to the cold finger heating, the cold finger is connected with temperature measuring element, temperature measuring element can monitor the temperature in the cold finger, the cold finger still is connected with the experiment chamber, the inner chamber of cold finger with the experiment chamber is linked together, the experimental cavity can be communicated with external mixed gas.
Preferably, the cylinder comprises a bottom plate, a shell and a vacuum flange, the shell is of a hollow structure, the bottom plate is connected with one end of the shell, the vacuum flange is connected with the other end of the shell, the vacuum flange is detachably connected with the upper cover, and the sealing element is arranged between the vacuum flange and the upper cover; the liquid nitrogen layer is positioned in a cavity defined by the bottom plate, the shell and the vacuum flange, the upper cover is connected with a vacuum valve, and the vacuum valve can be used for vacuumizing the cavity defined by the barrel and the upper cover.
Preferably, the liquid nitrogen layer comprises a liquid nitrogen outer cylinder, a liquid nitrogen inner cylinder, a liquid nitrogen lower bottom plate and a liquid nitrogen upper bottom plate, the liquid nitrogen outer cylinder is sleeved outside the liquid nitrogen inner cylinder, a gap is formed between the liquid nitrogen outer cylinder and the liquid nitrogen inner cylinder, the liquid nitrogen upper bottom plate and the liquid nitrogen lower bottom plate are respectively arranged at two ends of the liquid nitrogen inner cylinder and the liquid nitrogen outer cylinder, a cavity defined by the liquid nitrogen outer cylinder, the liquid nitrogen inner cylinder, the liquid nitrogen upper bottom plate and the liquid nitrogen lower bottom plate can contain liquid nitrogen, and the liquid nitrogen inner cylinder is sleeved outside the cold finger.
Preferably, the liquid nitrogen upper bottom plate is connected with a liquid nitrogen hanging pipe, the liquid nitrogen hanging pipe is communicated with a cavity between the liquid nitrogen outer cylinder and the liquid nitrogen inner cylinder, the upper cover is connected with a liquid nitrogen outer pipe, the liquid nitrogen outer pipe is sleeved outside the liquid nitrogen hanging pipe, a gap is formed between the liquid nitrogen outer pipe and the liquid nitrogen hanging pipe, and the liquid nitrogen outer pipe is communicated with the cavity defined by the shell and the bottom plate.
Preferably, a hanging pipe supplementing core is arranged between the liquid nitrogen hanging pipe and the liquid nitrogen outer pipe, and the hanging pipe supplementing core can fix the relative position between the liquid nitrogen hanging pipe and the liquid nitrogen outer pipe.
Preferably, the upper cover is connected with a pipe joint, one end of the pipe joint, which is far away from the upper cover, is connected with a core seat, the pipe joint can be connected with a controller by using the core seat, and the heating element and the temperature measuring element are both connected with the controller.
Preferably, the inner cavity of the cold finger is located in the inner cavity of the heat conducting agent layer, the other end of the cold finger extends out of the liquid nitrogen layer, the temperature measuring element is located at one end of the cold finger extending out of the liquid nitrogen layer, and the temperature measuring element is located in the cylinder.
Preferably, the upper cover is connected with a middle pipe, the middle pipe is communicated with the heat conducting agent layer, and one end of the experiment cavity, which is far away from the cold finger, extends out of the middle pipe.
Preferably, the heating element is a thermal resistor or a thermocouple; the heat conducting agent is alcohol, methyl pentane or chlorobutane.
Preferably, the vacuum flange is bolted to the upper cover.
The utility model discloses for prior art gain following technological effect: the utility model discloses a device for separating krypton and xenon in rock sample, including barrel and upper cover, the barrel can be dismantled with the upper cover and be connected, set up sealing element between barrel and the upper cover, include liquid nitrogen layer and heat-conducting agent layer in the barrel, liquid nitrogen layer suit is in the outside on heat-conducting agent layer, evacuation processing can be done to cavity between the outer wall on liquid nitrogen layer and the barrel, the inner chamber on liquid nitrogen layer can hold the liquid nitrogen, be provided with the cold finger in the inner chamber on heat-conducting agent layer, can hold the heat-conducting agent between the inner wall on heat-conducting agent layer and the cold finger, the cold finger is connected with heating element, heating element can indicate to cold and heat, the cold finger is connected with temperature measuring element, temperature measuring element can monitor the temperature in the cold finger, the cold finger still is connected with the experiment chamber, the inner chamber and the experiment chamber of cold finger are linked together, the experiment chamber can be linked together with outside mist. The utility model discloses a device for separating krypton and xenon in rock sample is applicable to Ar, Kr, Xe mixed gas and separates, in noble gas's separation work, at first uses the cryogenic cold trap device that is equipped with the active carbon to adsorb most Ar, then uses the utility model discloses a separation of remaining Ar and Kr and Xe is carried out to the device, still uses commercial cold trap adsorption separation Ne at last.
The utility model discloses a device for separating krypton and xenon in rock sample, in operation, at first with the cavity evacuation processing between liquid nitrogen layer outer wall and the barrel, link to each other foretell device and sample pretreatment system, add the liquid nitrogen in the liquid nitrogen layer and carry out the precooling, the heat-conducting agent is added to the heat-conducting agent layer, let in cold finger through the experiment chamber with the mist, the mist carries out condensation adsorption in cold finger, adsorb the mist of Kr, Xe and a small amount of remaining Ar completely, then isolating device, make heating element work, temperature measuring element can monitor cold finger internal temperature, at first set the temperature between 80K-100K (for example 85K), in order to guarantee cold finger in still adsorbing the circumstances of Kr, Xe, release remaining Ar, vacuum bleed 2 min; and then setting the temperature to 155K by an isolating device, setting the temperature to 100K-135K (for example 103K) after 2min, enabling Xe in the cold finger to adsorb again without being influenced, and releasing Kr, finally setting the temperature to be higher than 135K (for example 155K), and releasing Xe, and after the experiment is finished, enabling the heating element of the cold finger to work, so as to achieve the purpose of rapid degassing. It should be noted here that the method for separating krypton and xenon from a rock sample of the present invention provides a temperature range, and a specific temperature value needs to be determined according to a specific experimental operation.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required 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 for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic cut-away view of an apparatus for separating krypton and xenon from a rock sample according to the present invention;
FIG. 2 is a schematic diagram of a portion of the structure of an apparatus for separating krypton and xenon from a rock sample according to the present invention;
FIG. 3 is a cross-sectional view taken along the direction C-C of FIG. 2;
the device comprises a shell, a vacuum flange, a vacuum valve, a liquid nitrogen outer cylinder, a liquid nitrogen inner cylinder, a liquid nitrogen lower bottom plate, a liquid nitrogen upper bottom plate, a liquid nitrogen hanging pipe, a liquid nitrogen outer tube, a liquid nitrogen inner cylinder, a liquid nitrogen lower bottom plate, a liquid nitrogen upper bottom plate, a liquid nitrogen hanging pipe, a liquid nitrogen outer tube, a hanging pipe, a pipe joint, a pipe socket and a middle pipe, wherein 100 is a device for separating krypton and xenon in a rock sample, 1 is a cylinder, 2 is an upper cover, 3 is a sealing element, 4 is a liquid nitrogen layer, 5 is a heat conducting agent layer, 6 is a cold finger, 7 is an experiment cavity, 8 is a bottom plate, 9 is a shell, 10 is a vacuum flange, 11 is a vacuum valve, 12 is a liquid nitrogen outer cylinder, 13 is a liquid nitrogen lower bottom plate, 15 is a liquid nitrogen upper bottom plate, 16 is a liquid nitrogen hanging pipe, 17 is a liquid nitrogen outer pipe, 18 is a hanging pipe complement core, 19 is a pipe complement, 20 is a pipe joint, and 21 is a middle pipe.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
The utility model aims at providing a device for separating krypton and xenon in rock sample to solve the problem that above-mentioned prior art exists, shorten the experimental time, improve sample noble gas's purity.
In order to make the above objects, features and advantages of the present invention more comprehensible, the present invention is described in detail with reference to the accompanying drawings and the detailed description.
Please refer to fig. 1-3, wherein fig. 1 is a schematic sectional view of the apparatus for separating krypton and xenon from a rock sample according to the present invention, fig. 2 is a schematic partial structural view of the apparatus for separating krypton and xenon from a rock sample according to the present invention, and fig. 3 is a schematic sectional view of fig. 2 along the direction C-C.
The utility model provides a device 100 for krypton and xenon in separation rock sample, including barrel 1 and upper cover 2, barrel 1 can be dismantled with upper cover 2 and be connected, set up sealing element 3 between barrel 1 and the upper cover 2, include liquid nitrogen layer 4 and heat-conducting agent layer 5 in the barrel 1, liquid nitrogen layer 4 suit is in the outside of heat-conducting agent layer 5, evacuation processing can be done to the cavity between the outer wall of liquid nitrogen layer 4 and the barrel 1, liquid nitrogen layer 4's inner chamber can hold the liquid nitrogen, be provided with cold finger 6 in the inner chamber of heat-conducting agent layer 5, can hold the heat-conducting agent between the inner wall of heat-conducting agent layer 5 and the cold finger 6, cold finger 6 is connected with heating element, heating element can indicate 6 heating to cold, cold finger 6 is connected with temperature measuring element, temperature measuring element can monitor the temperature in the cold finger 6, cold finger 6 still is connected with experiment chamber 7, the inner chamber of cold finger 6 is linked together with experiment chamber 7, experiment chamber 7 can be linked together with outside mist.
Use the utility model discloses a during device 100 for separating krypton and xenon in rock sample, at first with the cavity evacuation processing between 4 outer walls in liquid nitrogen layer and the barrel 1, will the utility model discloses a device links to each other with sample pretreatment system, adds liquid nitrogen in liquid nitrogen layer 4 and carries out the precooling, and heat-conducting agent layer 5 adds the heat-conducting agent, lets in the cold finger 6 with gas mixture through experiment chamber 7, and gas mixture carries out the condensation in cold finger 6 and adsorbs, adsorbs the mixed gas of Kr, Xe and a small amount of remaining Ar completely, then makes heating element work, and temperature measuring element can monitor the temperature in the cold finger 6, at first sets the temperature between 80K-100K to guarantee in the cold finger 6 still adsorb under the condition of Kr, Xe, completely release Ar; and then setting the temperature between 100K and 135K to enable Xe in the cold finger 6 not to be influenced and release Kr, finally setting the temperature to be higher than 135K to release Xe, and after the experiment is finished, enabling the heating element of the cold finger 6 to work to achieve the purpose of rapid degassing. The utility model discloses a device 100 for separating krypton and xenon in rock sample for among the pretreatment process of mass spectrometry inert gas sample, easy operation is convenient, can high-quality high-efficient separation noble gas, shortens the experimental time, reduces the background, improves noble gas's purity simultaneously.
The cylinder body 1 comprises a bottom plate 8, a shell 9 and a vacuum flange 10, the shell 9 is of a hollow structure, the bottom plate 8 is connected with one end of the shell 9, the vacuum flange 10 is connected with the other end of the shell 9, the vacuum flange 10 is detachably connected with the upper cover 2, so that other parts in the cylinder body 1 can be conveniently disassembled and assembled, the sealing element 3 is arranged between the vacuum flange 10 and the upper cover 2, leakage is avoided, and the vacuum degree of the cylinder body 1 after vacuum-pumping treatment is ensured; liquid nitrogen layer 4 is located the cavity that bottom plate 8, shell 9, vacuum flange 10 enclose, and upper cover 2 is connected with vacuum valve 11, utilizes vacuum valve 11 to do the evacuation processing to the cavity that barrel 1 and upper cover 2 enclose, utilizes vacuum valve 11 to carry out the evacuation processing to the inner chamber of barrel 1, reduces the influence of external environment temperature to cold finger 6.
Specifically, the liquid nitrogen layer 4 comprises a liquid nitrogen outer cylinder 12, a liquid nitrogen inner cylinder 13, a liquid nitrogen lower bottom plate 14 and a liquid nitrogen upper bottom plate 15, the liquid nitrogen outer cylinder 12 is sleeved outside the liquid nitrogen inner cylinder 13, a gap is formed between the liquid nitrogen inner cylinder 13 and the liquid nitrogen lower bottom plate 15, the liquid nitrogen upper bottom plate 15 and the liquid nitrogen lower bottom plate 14 are respectively arranged at two ends of the liquid nitrogen inner cylinder 13 and the liquid nitrogen outer cylinder 12, a cavity surrounded by the liquid nitrogen outer cylinder 12, the liquid nitrogen inner cylinder 13, the liquid nitrogen upper bottom plate 15 and the liquid nitrogen lower bottom plate 14 can contain liquid nitrogen, and the liquid nitrogen inner cylinder 13 is sleeved outside the cold finger 6. When using the utility model discloses a during the device, to the liquid nitrogen layer 4 flush into liquid nitrogen, cool down to the liquid nitrogen temperature in advance.
In the present embodiment, because the liquid nitrogen inner cylinder 13 and the liquid nitrogen outer cylinder 12, the liquid nitrogen upper bottom plate 15 is connected with the liquid nitrogen hanging pipe 16, the liquid nitrogen hanging pipe 16 is communicated with the cavity between the liquid nitrogen outer cylinder 12 and the liquid nitrogen inner cylinder 13, the liquid nitrogen can be input to the liquid nitrogen layer 4 by using the liquid nitrogen hanging pipe 16, the upper cover 2 is connected with the liquid nitrogen outer pipe 17, the liquid nitrogen outer pipe 17 is sleeved outside the liquid nitrogen hanging pipe 16, a gap is formed between the liquid nitrogen outer pipe 17 and the liquid nitrogen hanging pipe 16, and the liquid nitrogen outer pipe 17 is communicated with the cavity enclosed by the housing 9 and the bottom plate 8.
In order to support the liquid nitrogen hanging pipe 16, a hanging pipe supplementing core 18 is arranged between the liquid nitrogen hanging pipe 16 and the liquid nitrogen outer pipe 17, and the hanging pipe supplementing core 18 can fix the relative position between the liquid nitrogen hanging pipe 16 and the liquid nitrogen outer pipe 17, so that the stability and the reliability of the device are improved.
More specifically, the upper cover 2 is connected with a pipe joint 19, one end of the pipe joint 19, which is far away from the upper cover 2, is connected with a core print 20, the pipe joint 19 can be connected with a controller by using the core print 20, the heating element and the temperature measuring element are both connected with the controller, and the controller can control the heating temperature of the heating element on the cold finger 6, so that the rare gas can be separated conveniently.
It should also be noted that the inner cavity of the cold finger 6 is located in the inner cavity of the heat conducting agent layer 5, the other end of the cold finger 6 is extended out from the liquid nitrogen layer 4, the temperature measuring element is located at one end of the cold finger 6 extended out from the liquid nitrogen layer 4, the temperature measuring element is located in the cylinder 1, the temperature measuring element is prevented from being affected by the liquid nitrogen and the heat conducting agent, and the monitoring accuracy of the temperature in the cold finger 6 is improved.
Furthermore, the upper cover 2 is connected with a middle pipe 21, the middle pipe 21 is communicated with the heat conducting agent layer 5, and one end of the experiment cavity 7, which is far away from the cold finger 6, extends out of the middle pipe 21, so that the experiment cavity is conveniently connected with a sample pretreatment system.
In the specific embodiment, the heating element is a thermal resistor or a thermocouple, so that the heating is convenient and quick; the heat-conducting agent is alcohol, methyl pentane or chlorobutane, and can be selected according to actual conditions in production.
Besides, the vacuum flange 10 is connected with the upper cover 2 through bolts, so that the vacuum sealing device is convenient to disassemble and assemble, and can also compress the sealing element 3 to avoid leakage.
The utility model discloses a device 100 for separating krypton and xenon in rock sample, the during operation at first is through vacuum valve 11 with the cavity evacuation processing between liquid nitrogen layer 4 outer wall and the barrel 1, will the device of the utility model and sample pretreatment system link to each other, before gas separation, add the liquid nitrogen and carry out the pre-cooling between liquid nitrogen inner tube 13 and liquid nitrogen urceolus 12, heat-conducting agent layer 5 adds the heat-conducting agent, let in mixed gas in cold finger 6 through experiment chamber 7, mixed gas carries out the condensation absorption 20min in cold finger 6, adsorb the mixed gas of Kr, Xe and a small amount of remaining Ar completely, then isolating device, make heating element work, temperature measuring element can monitor the cold finger 6 internal temperature, at first with the temperature setting in certain temperature value (for example 85K) between 80K-100K, under the condition of still adsorbing Kr, Xe in order to guarantee that cold finger 6 is interior, release Ar completely, vacuum pumping for 2 min; and then the isolating device sets the temperature to 155K, after 2min, the temperature is set to a certain temperature value (for example 103K) between 100K and 135K again, Xe in the cold finger 6 is adsorbed again and is not influenced, Kr is released, finally, the temperature is set to a certain temperature value (for example 155K) higher than 135K, Xe is released, and after the experiment is finished, the heating element of the cold finger 6 is enabled to work, so that the purpose of rapid degassing is achieved. It should be noted here that the method for separating krypton and xenon from a rock sample of the present invention provides a temperature range, and a specific temperature value needs to be determined according to a specific experimental operation.
The utility model discloses a concrete example is applied to explain the principle and the implementation mode of the utility model, and the explanation of the above example is only used to help understand the method and the core idea of the utility model; meanwhile, for the general technical personnel in the field, according to the idea of the present invention, there are changes in the concrete implementation and the application scope. In summary, the content of the present specification should not be construed as a limitation of the present invention.
Claims (9)
1. An apparatus for separating krypton and xenon in a rock sample, characterized by: comprises a cylinder body and an upper cover, the cylinder body is detachably connected with the upper cover, a sealing element is arranged between the cylinder body and the upper cover, the cylinder body comprises a liquid nitrogen layer and a heat-conducting agent layer, the liquid nitrogen layer is sleeved outside the heat-conducting agent layer, the cavity between the outer wall of the liquid nitrogen layer and the cylinder body can be vacuumized, the inner cavity of the liquid nitrogen layer can contain liquid nitrogen, a cold finger is arranged in the inner cavity of the heat conducting agent layer, a heat conducting agent can be contained between the inner wall of the heat conducting agent layer and the cold finger, the cold finger is connected with a heating element which can heat the cold finger, the cold finger is connected with a temperature measuring element, the temperature measuring element can monitor the temperature in the cold finger, the cold finger is also connected with an experimental cavity, the inner cavity of the cold finger is communicated with the experimental cavity, and the experimental cavity can be communicated with external mixed gas.
2. The apparatus of claim 1, wherein the apparatus further comprises: the cylinder body comprises a bottom plate, a shell and a vacuum flange, the shell is of a hollow structure, the bottom plate is connected with one end of the shell, the vacuum flange is connected with the other end of the shell, the vacuum flange is detachably connected with the upper cover, and the sealing element is arranged between the vacuum flange and the upper cover; the liquid nitrogen layer is positioned in a cavity defined by the bottom plate, the shell and the vacuum flange, the upper cover is connected with a vacuum valve, and the vacuum valve can be used for vacuumizing the cavity defined by the barrel and the upper cover.
3. The apparatus of claim 2, wherein the apparatus further comprises: the liquid nitrogen layer comprises a liquid nitrogen outer cylinder, a liquid nitrogen inner cylinder, a liquid nitrogen lower bottom plate and a liquid nitrogen upper bottom plate, the liquid nitrogen outer cylinder is sleeved outside the liquid nitrogen inner cylinder, a gap is formed between the liquid nitrogen outer cylinder and the liquid nitrogen inner cylinder, the liquid nitrogen upper bottom plate and the liquid nitrogen lower bottom plate are respectively arranged at two ends of the liquid nitrogen inner cylinder and the liquid nitrogen outer cylinder, a cavity formed by the liquid nitrogen outer cylinder, the liquid nitrogen inner cylinder, the liquid nitrogen upper bottom plate and the liquid nitrogen lower bottom plate can contain liquid nitrogen, and the liquid nitrogen inner cylinder is sleeved outside the cold finger.
4. The apparatus of claim 3, wherein the apparatus further comprises: the liquid nitrogen upper bottom plate is connected with a liquid nitrogen hanging pipe, the liquid nitrogen hanging pipe is communicated with a cavity between the liquid nitrogen outer barrel and the liquid nitrogen inner barrel, the upper cover is connected with a liquid nitrogen outer pipe, the liquid nitrogen outer pipe is sleeved outside the liquid nitrogen hanging pipe, a gap is formed between the liquid nitrogen outer pipe and the liquid nitrogen hanging pipe, and the liquid nitrogen outer pipe is communicated with the cavity defined by the shell and the bottom plate.
5. The apparatus of claim 4, wherein the apparatus further comprises: and a hanging pipe supplementing core is arranged between the liquid nitrogen hanging pipe and the liquid nitrogen outer pipe, and the hanging pipe supplementing core can fix the relative position between the liquid nitrogen hanging pipe and the liquid nitrogen outer pipe.
6. The apparatus of claim 1, wherein the apparatus further comprises: the upper cover is connected with a pipe joint, one end of the pipe joint, far away from the upper cover, is connected with a core seat, the pipe joint can be connected with a controller by using the core seat, and the heating element and the temperature measuring element are both connected with the controller.
7. The apparatus of claim 6, wherein the apparatus further comprises: the inner cavity of the cold finger is positioned in the inner cavity of the heat conducting agent layer, the other end of the cold finger extends out of the liquid nitrogen layer, the temperature measuring element is positioned at one end of the cold finger extending out of the liquid nitrogen layer, and the temperature measuring element is positioned in the cylinder body.
8. The apparatus of claim 1, wherein the apparatus further comprises: the upper cover is connected with a middle pipe, the middle pipe is communicated with the heat conducting agent layer, and one end of the experiment cavity, which is far away from the cold finger, extends out of the middle pipe.
9. The apparatus of claim 1, wherein the apparatus further comprises: the heating element is a thermal resistor or a thermocouple; the heat conducting agent is alcohol, methyl pentane or chlorobutane.
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| Application Number | Priority Date | Filing Date | Title |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115561123A (en) * | 2022-09-19 | 2023-01-03 | 北京科技大学 | Hydrogen permeation experimental device and method for metal pipe under gas-phase hydrogen environment |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115561123A (en) * | 2022-09-19 | 2023-01-03 | 北京科技大学 | Hydrogen permeation experimental device and method for metal pipe under gas-phase hydrogen environment |
| CN115561123B (en) * | 2022-09-19 | 2024-05-14 | 北京科技大学 | Hydrogen permeation experimental device and experimental method for metal pipe in gas phase hydrogen environment |
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