CN115684053A - Sublimation water vapor and isotope fractionation online measuring device and measuring method thereof - Google Patents
Sublimation water vapor and isotope fractionation online measuring device and measuring method thereof Download PDFInfo
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- CN115684053A CN115684053A CN202211335971.2A CN202211335971A CN115684053A CN 115684053 A CN115684053 A CN 115684053A CN 202211335971 A CN202211335971 A CN 202211335971A CN 115684053 A CN115684053 A CN 115684053A
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Abstract
The invention discloses an online measuring device and method for distillation of sublimation water vapor and isotopes, and relates to a device and method for collecting water-containing simulated lunar soil low-temperature sublimation water vapor and measuring water vapor concentration and isotope composition online by adopting laser absorption spectrum. The device comprises a low-temperature sublimation unit, a cold trap collection unit, a temperature control unit, a laser spectrum measurement unit and a circuit control and signal acquisition unit. The method comprises the steps of simulating sublimation of lunar soil in different low-temperature environments with water, collecting sublimation water vapor by a cold trap, heating and extracting the water vapor by a hollow pipe, and measuring the water content and the isotope composition by laser spectroscopy. The online measurement of the water vapor and isotope composition before and after the water-containing simulated lunar soil sublimes under different low-temperature working conditions is realized.
Description
Technical Field
The invention relates to the technical field of laser absorption spectroscopy, in particular to an online measuring device and a measuring method for sublimation water vapor and isotope fractionation.
Background
In cosmic chemistry, the D/H ratio is commonly used to track the source of water in the solar planets or asteroids. The detection of the content and the source of the lunar water provides important support for future lunar bases and manned lunar exploration activities. However, the detection of the water ice of the moon is currently based on the steps of drilling, sample extraction/transfer and thermal analysis, and considering the ultra-high vacuum conditions existing on the surface of the moon and the procedures of temperature rise extraction and transfer, there is a risk that all the water ice content is lost during the sample extraction and transfer. Furthermore, if only a portion of the water ice is lost during the period, fractionation of hydrogen isotopes is introduced, thereby making the isotopic analysis of the residual ice sample uncertain. Therefore, the water-containing lunar soil needs to be studied for the change of water vapor content and isotope fractionation caused by sublimation under different low temperature environments. However, historically, the sublimed water vapor was collected internationally by a cold trap and then transferred to a mass spectrometer for off-line measurement. This is complicated to operate and expensive in terms of equipment, and may introduce unnecessary errors into the transfer process.
Disclosure of Invention
The invention aims to provide an online measuring device and an online measuring method for sublimation water vapor and isotope fractionation, which aim to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention discloses a sublimation water vapor and isotope fractionation online measuring device on one hand, which comprises:
a sample tube;
the low-temperature sublimation unit comprises a primary cold trap, a secondary cold trap and a three-way valve V1 for connecting the primary cold trap and the secondary cold trap;
the cold trap collection unit comprises a collection cold trap and a switch valve V2 which is connected with the collection cold trap and a three-way valve V1;
the spectrum measuring unit comprises a laser measuring mechanism for acquiring laser absorption spectrum data and an on-off valve V3; the laser measuring mechanism is connected between the switch valve V2 and the switch valve V3;
and the temperature control unit is used for adjusting the temperature of the low-temperature sublimation unit, the cold trap collection unit and the spectrum measurement unit.
As a further scheme of the invention: the collecting cold trap comprises a collecting chamber and a collecting pipe 312, wherein the collecting pipe 312 is arranged in the collecting chamber, and the collecting pipe 312 is connected with the inlet end of the switch valve V2.
As a further scheme of the invention: and liquid nitrogen is filled in the primary cold trap and the collection chamber.
As a further scheme of the invention: and the secondary cold trap is filled with absolute ethyl alcohol.
As a further scheme of the invention: the laser measurement mechanism comprises a vacuum tank, and an ICL laser, a spectrum cavity, a temperature measurement module and a pressure measurement module which are arranged in the vacuum tank.
As a further scheme of the invention: the pressure measurement module comprises a first vacuum gauge for monitoring the water vapor pressure in the spectrum cavity and a second vacuum gauge for monitoring the pressure in the vacuum tank.
As a further scheme of the invention: and the vacuum pump is connected with the switch valve V3.
The invention also discloses a measuring method of any one of the sublimation water vapor and isotope fractionation online measuring devices, which comprises the following steps:
step A: placing a sample tube filled with a sample in the primary cold trap, connecting the sample tube with a first inlet of a three-way valve V1, and simultaneously opening a switch valve V2 and a switch valve V3;
and B: starting a vacuum pump to vacuumize, and then closing the switch valve V2 and the switch valve V3;
and C: moving the sample tube into a secondary cold trap, so that the sample tube is connected with a second inlet of the three-way valve V1, the sample is subjected to low-temperature sublimation in the secondary cold trap, and water vapor generated by sublimation enters the collecting tube 312 to be collected;
step D: closing the three-way valve V1, opening the switch valve V2, removing the collecting chamber, heating the water ice in the collecting pipe 312 by the temperature control unit, introducing the generated water vapor into the spectrum measuring unit, and measuring the water vapor content and the isotope ratio R Sublimation ；
Step E: opening a switch valve V3, and vacuumizing the spectrum measuring unit and the cold trap collecting unit;
step F: close ooff valve V3, open three-way valve V1, heat the sample after sublimating in the unit to low temperature sublimation through the temperature control unit, during the steam that produces directly gets into the spectrum chamber, measure steam content and isotope ratio R Residue(s) of . The heating temperature is 200 deg.C, and the time is 2-3min. In practical operation, the heating can be stopped when the pressure in the spectrum cavity reaches the maximum value.
As a further scheme of the invention: the vacuum in step B and step E was 0.01Pa.
As a further scheme of the invention: the low-temperature sublimation temperature in the step C is 170K-240K.
As a further scheme of the invention: and D, heating at 200 ℃ for 1-3 minutes.
As a further scheme of the invention: the pressure in the spectral cavity in step F is not higher than 2000Pa. If the pressure exceeds 2000Pa, the spectral signal is distorted and cannot be measured.
As a further scheme of the invention: and D, measuring the water vapor content in the step F by the following formula:
P＝A/(S*L*X) (1)
wherein, P [ atm [ ]]For the calculated water vapor content, A cm -1 ]Is the integrated absorbance of the selected absorption peak, S [ cm ] -2 *atm -1 ]The absorption line of the selected absorption peak is strong, L cm]The effective path length of the Herriott multiple reflection cell, and X is the water vapor partial pressure ratio. Because pure water vapor measurement is adopted and no other gas is contained, the water vapor partial pressure ratio XIs 1.
As a further scheme of the invention: isotope ratio measurements were made in step D and step F by the following formulas:
wherein R is the calculated isotopic ratio, A HDO 、
Respectively selected HDO and H 2 16 Integral absorbance of O absorption peak, TK]In order to measure the temperature of the gas,
S(T) HDO respectively selected HDO and H 2 16 Linear intensity of O absorption peak at temperature T.
As a further scheme of the invention: further comprising the step G: calculating an isotope fractionation coefficient alpha; the isotopic fractionation coefficient α was calculated by the following formula:
α＝R residue of /R Sublimation 。 (3)
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for measuring the low-temperature sublimation water vapor content and isotope fractionation of the water-containing simulated lunar soil on line by using a laser absorption spectrum technology, has simple system operation and high sensitivity, provides important basis for detecting lunar water ice, realizes the on-line measurement of the water vapor and isotope composition before and after sublimation of the water-containing simulated lunar soil under different low-temperature working conditions, and also provides ideas for the measurement of the water vapor content and isotope in other types of soil.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a schematic diagram of the structure of a spectrum measuring unit and a circuit control signal acquisition unit according to the present invention;
in the figure: the system comprises a 1-sample tube, a 2-low temperature sublimation unit, a 21-primary cold trap, a 22-secondary cold trap, a 23-three-way valve V1, a 3-cold trap collection unit, a 31-collection cold trap, a 32-switching valve V2, a 311-collection chamber, a 312-collection tube, a 4-spectrum measurement unit, a 41-laser measurement mechanism, a 411-spectrum cavity, a 412-temperature measurement module, a 413-vacuum tank, a 42-switching valve V3, a 43-first vacuum gauge, a 44-second vacuum gauge, a 5-vacuum pump and a 6-circuit control and signal acquisition unit.
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.
In the description of the present invention, it should be noted that the terms "upper", "lower", "left", "right", "inner", "outer", and the like indicate orientations or positional relationships based on orientations or positional relationships shown in the drawings or orientations or positional relationships that are conventionally arranged when the products of the present invention are used, and are used for convenience of description and simplicity of description only, and do not indicate or imply that the devices or elements indicated 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. Furthermore, the terms "first," "second," and the like are used merely to distinguish one description from another, and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may be, for example, fixedly connected, detachably connected, or integrally connected; the connection can be mechanical connection or communication connection; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in a specific case to those of ordinary skill in the art.
Referring to fig. 1-2, in an embodiment of the present invention, an online measurement device for measuring sublimation water and isotope fractionation of lunar soil containing water based on spectroscopy includes a sample tube 1, a low temperature sublimation unit 2, a cold trap collection unit 3, a temperature control unit, a spectrum measurement unit 4, and a circuit control and signal acquisition unit 6.
Further, the low-temperature sublimation unit 2 comprises a primary cold trap 21 filled with liquid nitrogen and a secondary cold trap 22 filled with absolute ethyl alcohol and capable of realizing different gradient low-temperature environments, and the low-temperature sublimation of the sample can be realized by placing the sample tube 1 in the primary cold trap 21 or the secondary cold trap 22.
Further, the cold trap collecting unit 3 comprises a collecting cold trap 31 filled with liquid nitrogen and a switch valve V2 31, the collecting cold trap 31 comprises a collecting chamber 311 and a collecting pipe 312, the collecting chamber 311 is used for freezing the collecting pipe 312 and collecting water vapor generated when the water-containing simulated lunar soil is sublimated at low temperature.
Furthermore, the temperature control unit is provided with a temperature control device and a heating device, so that the water ice in the cold trap collecting unit 3 and the low-temperature sublimation unit 2 can be quickly sublimated at high temperature, and the temperature control unit also comprises a heating element for heating the pipeline.
Further, the spectrum measuring unit 4 includes a laser measuring mechanism 41 and an on-off valve V3, the laser measuring mechanism 41 is connected between the on-off valve V2 and the on-off valve V3 42; the laser measuring mechanism 41 comprises a vacuum tank 413, and an ICL laser, a spectrum cavity 411 (namely a Herriott multiple reflection cell), a collimating lens, a focusing lens, an InGaSn photodetector, a temperature measuring module 412 and a pressure measuring module 411 which are arranged in the vacuum tank 413. The ICL laser is arranged on the multiple absorption pool and used for emitting laser, the working wavelength of the ICL laser can simultaneously cover the light isotope molecular absorption peak and the heavy isotope molecular absorption peak of water, the interference of the light isotope molecular absorption peak and the heavy isotope molecular absorption peak by other molecular absorption peaks is small in the wavelength range, the ICL laser can simultaneously contain the absorption peaks of various water isotopes, and the HDO and other isotopes can be simultaneously measured by using one laser; the temperature measuring module 412 is used for monitoring the temperature in the spectrum cavity 411 in real time; the pressure measuring module comprises a first vacuum gauge 43 and a second vacuum gauge 44, wherein the first vacuum gauge 43 is used for monitoring the water vapor pressure in the spectrum cavity 411, and the second vacuum gauge 44 is used for monitoring the air pressure in the vacuum tank 413. The laser measuring mechanism 41 acquires laser absorption spectrum data and transmits the laser absorption spectrum data to the circuit control and signal acquisition unit 6.
Furthermore, the circuit control and signal acquisition unit 6 comprises a temperature control module, a laser driving module, a signal generator module, an A/D acquisition module, a signal amplification module, a data acquisition module and an upper computer. The circuit control and signal acquisition unit 6 is used for controlling the temperature in the optical cavity, modulating and locking the output wavelength of the laser light source, receiving the laser absorption spectrum data and processing the data to calculate the water vapor content and the isotope ratio; the A/D acquisition module, the signal amplification module, the data acquisition module and the upper computer are used for acquiring and processing the laser absorption spectrum data to obtain the water vapor content and the isotope ratio.
The water-containing simulated lunar soil sublimation water vapor and isotope fractionation online measurement method comprises the following specific steps:
step A: placing the sample tube 1 filled with the water-containing simulated lunar soil in a primary cold trap 21, connecting the sample tube into a main pipeline through a three-way valve V1, and opening a switch valve V2 and a switch valve V3;
and B: vacuumizing the measuring device to a preset vacuum degree of 0.01Pa; then closing the switch valve V2 and the switch valve V3, and placing the sample collecting pipe 312 in the collecting cold trap 31;
and C: placing the sample tube 1 in a secondary cold trap 22, opening V1, and sublimating the water-containing simulated lunar soil in a low-temperature environment of 170K-240K;
step D: closing the three-way valve V1, opening the switch valve V2, removing the collecting cold trap 31 in the cold trap collecting unit 3, immediately heating the water ice in the collecting pipe 312 by using a heating device of the temperature control unit, and allowing the water vapor generated by sublimation to enter the spectrum cavity 411 through the sample collecting main pipeline and the main pipeline for online measurement of the water vapor content and the isotope ratio; the heating temperature is 200 ℃, and the heating time is 1-3 minutes;
step E: opening a switch valve V3, and vacuumizing the laser spectrum measuring unit 4, the cold trap collecting unit 3 and a communicating pipeline thereof to a preset vacuum degree of 0.01Pa;
step F: and closing the switch valve V3, opening the three-way valve V1, heating the water-containing simulated lunar soil sublimated in the low-temperature sublimation assembly by using a heating device of the temperature control unit, and directly measuring the water vapor generated by sublimation in the spectrum cavity 411 on line to obtain the water vapor content and the isotope ratio. The heating temperature is 200 ℃ and the time is 1 to 3 minutes; the pressure of the water vapor generated by sublimation in the spectrum cavity is lower than 2000Pa.
And D, calculating the water vapor content and the isotope ratio through the following formulas in the steps F and D:
P＝A/(S*L*X) (1)
wherein P is the calculated water vapor content, A is the integral absorbance of the selected absorption peak, S is the absorption line intensity of the selected absorption peak, and L is the effective path length of the Herriott multiple reflection cell. R is the calculated isotopic ratio, A HDO 、
Respectively selected HDO and H 2 16 Integral absorbance of O absorption peak, TK]Is the temperature of the gas to be measured,
S(T) HDO respectively selected HDO and H 2 16 Linear intensity of O absorption peak at temperature T.
In order to quantify the influence of low-temperature sublimation on isotope fractionation, the water ice of the collecting pipe 312 and the sample pipe 1 is heated and then measured to respectively obtain the isotope ratio R of the sublimated water ice Sublimation And the residual isotope ratio R Residue of And calculating the isotopic fractionation coefficient from the formula:
α＝R residue of /R Sublimation (3)
Although the present description is described in terms of embodiments, not every embodiment includes only a single embodiment, and such description is for clarity only, and those skilled in the art should be able to integrate the description as a whole, and the embodiments can be appropriately combined to form other embodiments as will be understood by those skilled in the art.
Therefore, the above description is only a preferred embodiment of the present application, and is not intended to limit the scope of the present application; all the equivalent changes made within the scope of the claims of the present application are the protection scope of the claims of the present application.
Claims (15)
1. The utility model provides a sublimation steam and isotope fractionation on-line measuring device which characterized in that includes:
a sample tube (1);
a low-temperature sublimation unit (2) including a primary cold trap (21), a secondary cold trap (22), and a three-way valve V1 (23) connecting the primary cold trap (21) and the secondary cold trap (22);
a cold trap collection unit (3) including a collection cold trap (31), and an on-off valve V2 (32) connecting the collection cold trap (31) and a three-way valve V1 (23);
a spectrum measuring unit (4) including a laser measuring mechanism (41) for acquiring laser absorption spectrum data, an on-off valve V3 (42); the laser measuring mechanism (41) is connected between the switch valve V2 (32) and the switch valve V3 (42);
and the temperature control unit is used for adjusting the temperature of the low-temperature sublimation unit (2), the cold trap collection unit (3) and the spectrum measurement unit (4).
2. The on-line measuring device for sublimation water vapor and isotope fractionation according to claim 1, wherein the collecting cold trap (31) comprises a collecting chamber (311) and a collecting pipe 312 (312), wherein the collecting pipe 312 (312) is arranged in the collecting chamber (311), and the collecting pipe 312 (312) is connected with an inlet end of a switch valve V2 (32).
3. The device for on-line measurement of sublimation vapor and isotope fractionation according to claim 2, wherein the primary cold trap (21) and the collection chamber (31) are filled with liquid nitrogen.
4. The on-line measuring device for sublimation vapor and isotope fractionation as claimed in claim 2, wherein said secondary cold trap (22) is filled with absolute ethanol.
5. The device for on-line measurement of sublimated water vapor and isotope fractionation according to claim 1, wherein the laser measuring mechanism (41) comprises a vacuum tank (413), and a laser, a spectrum cavity (411), a temperature measuring module (412) and a pressure measuring module which are arranged in the vacuum tank.
6. The on-line measuring device for sublimation vapor and isotope fractionation according to claim 5, wherein the pressure measuring module comprises a first vacuum gauge (43) for monitoring vapor pressure in the spectrum cavity (411), and a second vacuum gauge (44) for monitoring pressure level in the vacuum tank (413).
7. The on-line measuring device for sublimation vapor and isotope fractionation according to claim 1, further comprising a vacuum pump (5) connected to the switching valve V3 (42).
8. The method for measuring the sublimation water vapor and isotope fractionation online measuring device as claimed in any one of claims 1 to 7, comprising the steps of:
step A: placing a sample tube filled with a sample in a primary cold trap, connecting the sample tube with a first inlet of a three-way valve V1, and simultaneously opening a switch valve V2 and a switch valve V3;
and B: starting a vacuum pump to vacuumize, and then closing the switch valve V2 and the switch valve V3;
step C: moving the sample tube into a secondary cold trap, so that the sample tube is connected with a second inlet of the three-way valve V1, the sample is subjected to low-temperature sublimation in the secondary cold trap, and water vapor generated by sublimation enters the collecting tube 312 to be collected;
step D: the three-way valve V1 is closed, the switch valve V2 is opened, the collecting chamber is removed, the water ice in the collecting pipe 312 is heated through the temperature control unit, and the sublimated water vapor enters the lightIn a spectrum measuring unit, the water vapor content and the isotope ratio R are measured Sublimation ；
Step E: opening the switch valve V3, and vacuumizing the spectral measurement unit and the collecting pipe 312;
step F: close ooff valve V3, open three-way valve V1, heat the sample after subliming in the temperature control unit to the low temperature sublimation unit, during sublimed steam directly gets into the spectrum chamber, measure steam content and isotope ratio R Residue(s) of 。
9. The method of claim 8, wherein the degree of vacuum in step B and step E is 0.01Pa.
10. The method according to claim 8, wherein the low temperature sublimation temperature in the step C is 170K to 240K.
11. The method according to claim 8, wherein the heating temperature in step D is 200 ℃ and the heating time is 1 to 3 minutes.
12. The method of claim 8, wherein the pressure in the spectral cavity in step F is not higher than 2000Pa.
13. The method of measurement according to claim 8, wherein the moisture content measurement in steps D and F is performed by the following formula:
P＝A/(S*L*X) (1)
wherein P [ is the calculated water vapor content, A is the integral absorbance of the selected absorption peak, S is the absorption line intensity of the selected absorption peak, L is the effective path length of the Herriott multiple reflection cell, and X is the water vapor partial pressure ratio.
14. The method of measurement according to claim 8, wherein the isotope ratio measurement is performed in step D and step F by the following formula:
wherein R is the calculated isotopic ratio, A HDO 、
Respectively selected HDO and H 2 16 The integral absorbance of the O absorption peak, T is the temperature of the gas to be measured,
S(T) HDO respectively selected HDO and H 2 16 Linear intensity of O absorption peak at temperature T.
15. The measurement method according to claim 8, further comprising a step G: calculating an isotope fractionation coefficient alpha; the isotopic fractionation coefficient α was calculated by the following formula:
α＝R residue of /R Sublimation 。 (3)。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116499980A (en) * | 2023-05-17 | 2023-07-28 | 中国科学院合肥物质科学研究院 | Lunar soil water ice content and oxyhydrogen isotope calibration system and measurement system |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116499980A (en) * | 2023-05-17 | 2023-07-28 | 中国科学院合肥物质科学研究院 | Lunar soil water ice content and oxyhydrogen isotope calibration system and measurement system |
| CN116499980B (en) * | 2023-05-17 | 2024-02-13 | 中国科学院合肥物质科学研究院 | Lunar soil water ice content and oxyhydrogen isotope calibration system and measurement system |
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