AU2021105146A4 - Method for on-orbit calibrating basic parameters of a mass spectrometer - Google Patents
Method for on-orbit calibrating basic parameters of a mass spectrometer Download PDFInfo
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- AU2021105146A4 AU2021105146A4 AU2021105146A AU2021105146A AU2021105146A4 AU 2021105146 A4 AU2021105146 A4 AU 2021105146A4 AU 2021105146 A AU2021105146 A AU 2021105146A AU 2021105146 A AU2021105146 A AU 2021105146A AU 2021105146 A4 AU2021105146 A4 AU 2021105146A4
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- mass spectrometer
- orbit
- silicate mineral
- gas
- standard sample
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910052604 silicate mineral Inorganic materials 0.000 claims abstract description 53
- 238000001179 sorption measurement Methods 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims description 74
- 238000010438 heat treatment Methods 0.000 claims description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 22
- 229910052742 iron Inorganic materials 0.000 claims description 11
- 229910052609 olivine Inorganic materials 0.000 claims description 11
- 239000010450 olivine Substances 0.000 claims description 11
- 230000035945 sensitivity Effects 0.000 claims description 10
- 229910052724 xenon Inorganic materials 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052734 helium Inorganic materials 0.000 claims description 7
- 239000001307 helium Substances 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 229910052611 pyroxene Inorganic materials 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 3
- 238000001819 mass spectrum Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- -1 and more preferably Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000013024 troubleshooting Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/0009—Calibration of the apparatus
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/0027—Methods for using particle spectrometers
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
OF THE DISCLOSURE
The present disclosure relates to the technical field of calibration of basic
parameters of a mass spectrometer, and provides a method for on-orbit calibrating basic
parameters of a mass spectrometer, which, by using the feature that silicate mineral in a
molten state can adsorb gas in the environment, heats the silicate mineral to obtain
molten silicate mineral in a vacuum condition; places it in a standard gas environment
for adsorption, and cools rapidly to obtain a standard sample, and then pre-installs the
standard sample in a thermal control device of the mass spectrometer. After the mass
spectrometer enters a predetermined orbit, when it needs to use the mass spectrometer
for substance testing, the standard sample is heated on orbit to release the adsorbed
standard gas into the mass spectrometer to realize the calibration of the basic parameters
of the mass spectrometer. Since the silicate mineral will not release gas before being
heated, the risk of gas leakage caused by the use of standard gas cylinder is avoided, and
valves matching with the gas cylinder are not required, which reduces the weight of the
mass spectrometer, thus reducing the rocket launch cost.
17954468_1 (GHMatters) P116966.AU
Description
[01] The present disclosure relates to the technical field of calibration of basic parameters of mass spectrometer, and more particularly, to a method for on-orbit calibrating basic parameters of a mass spectrometer.
[02] The mass spectrometer is a common scientific analysis instrument in the deep space exploration process. Before scientific analysis, it is necessary to calibrate indicators of the mass spectrometer like mass axis, resolution, sensitivity. The traditional method generally carries a standard gas cylinder, which is connected to the mass spectrometer through two valves, so that the performance parameters of the mass spectrometer can be calibrated.
[03] The above calibration method has two disadvantages. Firstly, there is a risk of on-orbit gas leakage of the gas cylinder. If the gas cylinder leaks, the calibration cannot be completed. In addition, in order to increase the reliability of the instrument, the valve and the gas cylinder are designed to be heavier. The mass spectrometer needs to be sent to a predetermined orbit by the rocket, which undoubtedly increases the cost of rocket launch.
[04] Therefore, there is an urgent need to provide a low-cost method that can also achieve on-orbit calibration of basic parameters of the mass spectrometer.
[05] In view of this, the objective of the present disclosure is to provide a method for on-orbit calibrating basic parameters of a mass spectrometer. The calibration method provided by the present disclosure does not need to be equipped with a standard gas cylinder and matching valves, which avoids the presence of on-orbit gas leakage of the gas cylinder. Meanwhile, it reduces the weight of the mass spectrometer of on-orbit calibration, thereby reducing the cost of rocket launch.
[06] In order to realize the above objective, the present disclosure provides the following technical solutions:
[07] The present disclosure provides a method for on-orbit calibrating basic parameters of a mass spectrometer, comprising the following steps:
[08] (1) in a vacuum condition with a vacuum degree under 0.00001Pa, heating silicate mineral to get a molten silicate mineral;
[09] (2) placing the molten silicate mineral obtained at step (1) in an environment with rare gas for adsorption, and then cooling rapidly to obtain a standard sample;
[10] a rate of rapidly cooling in step (2) is 50200°C/min;
[11] (3) pre-installing the standard sample obtained at step (2) in a thermal control device of the mass spectrometer to perform on-orbit heating; a temperature of the on-orbit heating is not less than 600°C, and time of the on-orbit heating is not less than mins, to release the adsorbed rare gas into the mass spectrometer, to perform on-orbit
1 17954468_1(GHMtters) P116966.AU calibration of a mass axis, resolution and sensitivity of the mass spectrometer.
[12] Preferably, the silicate mineral in step (1) comprises pyroxene and/or iron olivine.
[13] Preferably, the silicate mineral is iron olivine.
[14] Preferably, a particle size of the silicate mineral in step (1) is not less than 50 meshes.
[15] Preferably, the rear gas is Helium and Xenon.
[16] The present disclosure provides a method for on-orbit calibrating basic parameters of a mass spectrometer on orbit, comprising the following steps: heating silicate mineral in a vacuum condition to get a molten silicate mineral; placing the molten silicate mineral in an environment with rare gas for adsorption, and then cooling rapidly to obtain a standard sample; pre-installing the obtained standard sample obtained in a thermal control device of the mass spectrometer to perform on-orbit heating, to release the adsorbed rare gas into the mass spectrometer, so as to perform on-orbit calibration of the basic parameters of the mass spectrometer. The present disclosure, by using the feature that silicate mineral in a molten state can adsorb gas in the environment, heats the silicate mineral to obtain molten silicate mineral in a vacuum condition; places it in a standard gas environment for adsorption, and cools rapidly to obtain a standard sample, and then pre-install the standard sample in a thermal control device of the mass spectrometer. After the mass spectrometer enters a predetermined orbit, when it needs to use the mass spectrometer for substance testing, the standard sample is heated on-orbit to release the adsorbed rear gas into the mass spectrometer to realize the calibration of the basic parameters of the mass spectrometer. Since the silicate mineral will not release gas before being heated, the risk of gas leakage caused by the use of standard gas cylinder is avoided, and valves matching with the gas cylinder are not required, which reduces the weight of the mass spectrometer, thus reducing the rocket launch cost.
[17] The present disclosure provides a method for on-orbit calibrating basic parameters of a mass spectrometer on orbit, comprising the following steps:
[18] (1) in a vacuum condition with a vacuum degree under 0.00001Pa, heating silicate mineral to get a molten silicate mineral;
[19] (2) placing the molten silicate mineral obtained at step (1) in an environment with rare gas for adsorption, and then cooling rapidly to obtain a standard sample;
[20] rate of rapidly cooling down in step (2) is 50200°C/min;
[21] (3) pre-installing the standard sample obtained at step (2) in a thermal control device of the mass spectrometer to perform on-orbit heating; a temperature of the on-orbit heating is not less than 600°C, and time of the on-orbit heating is not less than mins, to release the adsorbed rare gas into the mass spectrometer, to perform on-orbit calibration of a mass axis, resolution and sensitivity of the mass spectrometer.
[22] The present disclosure heats the silicate mineral in a vacuum condition to obtain a molten silicate mineral.
[23] In the present disclosure, the silicate mineral preferably comprises pyroxene
2 17954468_1 (GHMatters) P116966.AU and/or iron olivine, and more preferably, iron olivine. The present discloses, by using the feature that silicate mineral in a molten state can adsorb gas in the environment, uses the silicate mineral as the carrier of the rear gas; in the present disclosure, iron olivine with relatively low melting point is used as the carrier of the rear gas.
[24] In the present disclosure, the particle size of the silicate mineral is preferably not less than 50 mesh. The present disclosure limits the particle size of the silicate mineral in the above range, which is beneficial to increase the melting rate of the silicate mineral.
[25] In the present disclosure, the vacuum degree of the vacuum environment is preferably less than 0.00001Pa. The present disclosure performs heating in a vacuum condition, so as to prevent the silicate mineral in the molten state from adsorbing other gases in the environment; controlling the vacuum degree in the above degree is beneficial for the adsorption effect of the rear gas.
[26] The present disclosure does not have special requirements for the heating temperature, as long as it can melt the silicate mineral. The present disclosure controls the heating temperature to melt the silicate mineral, and uses the feature that the silicate mineral can adsorb the gas in the environment, and uses the silicate mineral as the carrier of the rear gas.
[27] The present disclosure has no special regulations on the heating device, as long as it can provide the required heating temperature and vacuum degree. The present disclosure has no special regulations on the amount of the silicate mineral, and it depends on the amount allowed by the selected heating device.
[28] After the molten silicate mineral is obtained, the molten silicate mineral is placed in a rare gas environment for adsorption, and then is rapidly cooled to obtain a standard sample; the rapid cooling rate is 50-200°C/min. In the present disclosure, the cooling rate is controlled within the above-mentioned range, which can better load the rare gas in the silicate mineral.
[29] The present disclosure preferably injects rare gas into the vacuum environment where the molten silicate mineral is located in the condition of preparing the molten silicate mineral, so that the molten silicate mineral is placed in the rare gas environment for adsorption, and then is rapidly cooled down to obtain a standard sample.
[30] In the present disclosure, there is no special regulation on the injection method, and technical solution for introducing gas which is well known to those skilled in the art can be adopted. The present disclosure does not specifically limit the amount of the standard gas, as long as the molten silicate mineral is in a rare gas atmosphere. In the present disclosure, the molten silicate mineral in the rare gas atmosphere can realize adsorption of the standard gas.
[31] In the present disclosure, the rear gas is preferably Helium and Xenon. The present disclosure selects the rear gas with stable performance, which does not react easily during the calibration, and thus enhances stability of the calibration.
[32] In the present disclosure, the helium gas is preferably helium gas with a mass number of 4. In the present disclosure, the xenon gas is preferably xenon gas with a mass number of 132 and xenon gas with a mass number of 129. The present disclosure uses helium gas with a mass number of 4 and xenon gas with a mass number of 132 to
3 17954468_1 (GHMatters) P116966.AU realize calibration in the range of 4-132; xenon gas with a mass number of 129 is used as a reference to measure the accuracy of the calibration.
[33] After the standard sample is obtained, the present disclosure pre-installs the standard sample in the thermal control device of the mass spectrometer, performs on-orbit heating, releases the adsorbed rare gas into the mass spectrometer, and performs on-orbit calibration of the basic parameters of the mass spectrometer.
[34] In the present disclosure, the on-orbit heating temperature is preferably not less than 600°C, and the on-orbit heating time is preferably not less than 10 mins. The present disclosure uses a thermal control device that comes with the mass spectrometer to heat the prepared standard sample on-orbit within the above-defined temperature and time range. The rare gas in the standard sample can be fully released, and the released rare gas directly enters the mass spectrometer directly uses the released rare gas to realize the calibration of the basic parameters of the mass spectrometer.
[35] The present disclosure does not have special regulations on the calibration method of the mass axis, resolution and sensitivity, and calibration can be carried out by using the method of calibrating the mass axis, resolution and sensitivity of the mass spectrometer using rare gases, which is well known to those skilled in the art. The present disclosure, by using the feature that silicate mineral in a molten state can adsorb gas in the environment, heats the silicate mineral to obtain molten silicate mineral in a vacuum condition; places it in a standard gas environment for adsorption, and cools rapidly to obtain a standard sample, and then pre-installs the standard sample in a thermal control device of the mass spectrometer; after the mass spectrometer enters a predetermined orbit, when it needs to use the mass spectrometer for substance testing, the standard sample is heated on-orbit to release the adsorbed standard gas into the mass spectrometer to realize the calibration of the basic parameters of the mass spectrometer. Since the silicate mineral will not release gas before being heated, the risk of gas leakage caused by the use of standard gas cylinder is avoided, and valves matching with the gas cylinder are not required, which reduces the weight of the mass spectrometer, thus reducing the rocket launch cost.
[36] The technical solutions of the present disclosure will be described clearly and completely in the following in conjunction with the examples of the present disclosure. Obviously, the described examples are merely a part of the examples of the present invention, rather than all the examples. Based on the examples of the present invention, all other examples obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present disclosure.
[37] Example 1
[38] Iron olivine powder is added in a vacuum high temperature furnace (the weight of the iron olivine powder is 1.5g, with an average particle size of 60 mesh), and the vacuum degree in the furnace is controlled to be less than 0.00001Pa, and heating is performed until the iron olivine powder is melted at 1300°C. Under this temperature and pressure, a mixture of 4He, 13 2 Xe, and 129Xe is injected into the high-temperature furnace cavity, and then the temperature of the furnace cavity is rapidly cooled (with a temperature rate is 180°C/min) to form solid iron olivine, and a standard sample containing standard gas is obtained. The standard sample is evenly divided into several
4 17954468_1 (GHMatters) P116966.AU parts, one of which is used to analyze and test the content of He and Xe in the standard sample, and the other samples are used for the calibration of mass axis, resolution and sensitivity of the mass spectrometer.
[39] Calibration of mass axis:
[40] Take 0.25g of the prepared standard sample and put it into the thermal control device of the mass spectrometer. After the thermal control device is heated to 600 degrees Celsius and maintained for 30 minutes, 4He, 13 2 Xe and 129Xe gases are released, and the released gases are analyzed by using the mass spectrometer. The analysis process uses low-speed scanning, scanning from the lowest mass number to the highest mass number. Three peaks appear on the mass spectrum obtained by the analysis. When these three peaks appear in positions with mass-to-charge ratios of 4, 129, and 132, respectively, calibration is not required; if the three peaks do not appear in the corresponding positions, the actual mass number of the standard gases 4He and 13 2 Xe and the measured corresponding mass number are substituted into the correction formula y=ax+b (X represents the actual mass of a certain standard gas, y represents the mass of the corresponding standard gas measured on the mass spectrum, and a and b represent the correction factors) to calculate a and b, and the mass axis is corrected by using the obtained correction formula; the test result of 129Xe is used to measure the accuracy of the quality axis after calibration.
[41] Calibration of the resolution:
[42] After the three peaks appearing on the mass spectrum are calibrated on the mass axis, the peak width at 50% of the peak height of any one of them indicates the resolution of the mass spectrometer; select any one of the three peaks and use the formula R=M /AM (M represents a mass number displayed on the standard gas mass spectrum; AM represents the peak width at 50% of the peak height) to calculate value R; when value R is not less than the actual mass number of the standard gas corresponding to the selected peak, it means that the instrument is working normally; otherwise, it means that the instrument has fault or needs to be adjusted, and the subsequent test should be performed after troubleshooting or after it is adjusted to be normal.
[43] Calibration of sensitivity
[44] The sensitivity calibration of the mass spectrometer is realized by the formula p=IV/CB*m,; wherein p represents sensitivity, I represents the current corresponding to the mass number corresponding to 4He, 13 2 Xe or 129Xe in the standard sample obtained by analysis; V represents the volume of the analysis chamber of the calibrated mass spectrometer; CB represents the contents of 4 He, 13 2 Xe and 129Xe in the standard sample obtained by using any method of the prior art for determining the contentsof 4 He, 13 2 Xe and 129Xe in the same standard sample in the thermal control device pre-installed in the mass spectrometer; m denotes the mass of the standard sample pre-installed in the thermal control device of the mass spectrometer.
[45] To sum up, the technical solution provided by the present disclosure fixes the standard gas into the silicate mineral, so there is no need to use the standard gas cylinder and matching valves, avoiding the risk of on-orbit leakage of the gas cylinder, and reducing the weight of the mass spectrometer, which in turn reduces the cost of rocket
5 17954468_1 (GHMatters) P116966.AU launches.
[46] The above are only the preferred examples of the present disclosure. It should be pointed out that for those of ordinary skill in the art, several improvements and modifications can be made without departing from the principles of the present disclosure, and these improvements and modifications should be regarded as the protection scope of the present disclosure.
[47] It is to be understood that, if any prior art publication is referred to herein, such reference does not constitute an admission that the publication forms a part of the common general knowledge in the art, in Australia or any other country.
[48] In the claims which follow and in the preceding description of the invention, except where the context requires otherwise due to express language or necessary implication, the word "comprise" or variations such as "comprises" or "comprising" is used in an inclusive sense, i.e. to specify the presence of the stated features but not to preclude the presence or addition of further features in various embodiments of the invention.
6 17954468_1 (GHMatters) P116966.AU
Claims (5)
1. A method for on-orbit calibrating basic parameters of a mass spectrometer, comprising the following steps: (1) in a vacuum condition with a vacuum degree under 0.00OOlPa, heating silicate minerals to get a molten silicate mineral; (2) placing the molten silicate mineral obtained at step (1) in an environment with rare gas for adsorption, and then cooled rapidly to obtain a standard sample; a rate of rapid cooling in step (2) is 50200°C/min; (3) pre-installing the standard sample obtained at step (2) in a thermal control device of the mass spectrometer to perform on-orbit heating; a temperature of the on-orbit heating is not less than 600°C, and time of the on-orbit heating is not less than mins, to release the adsorbed rare gas into the mass spectrometer, to perform on-orbit calibration of a mass axis, resolution and sensitivity of the mass spectrometer.
2. The method of claim 1, wherein the silicate mineral in step (1) comprises pyroxene and/or iron olivine.
3. The method of claim 2, wherein the silicate mineral is iron olivine.
4. The method of claim 1 or 2, wherein a particle size of the silicate mineral in step (1) is not less than 50 meshes.
5. The method of claim 1, wherein the rear gas is Helium and Xenon.
7 17954468_1(GHMtters) P116966.AU
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2021105146A AU2021105146A4 (en) | 2021-08-09 | 2021-08-09 | Method for on-orbit calibrating basic parameters of a mass spectrometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2021105146A AU2021105146A4 (en) | 2021-08-09 | 2021-08-09 | Method for on-orbit calibrating basic parameters of a mass spectrometer |
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| Publication Number | Publication Date |
|---|---|
| AU2021105146A4 true AU2021105146A4 (en) | 2021-10-07 |
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| AU2021105146A Ceased AU2021105146A4 (en) | 2021-08-09 | 2021-08-09 | Method for on-orbit calibrating basic parameters of a mass spectrometer |
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2021
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