CN117191924B - Molecular pollutant in-situ analysis detection device with high-efficiency separation and dynamic characterization - Google Patents
Molecular pollutant in-situ analysis detection device with high-efficiency separation and dynamic characterization Download PDFInfo
- Publication number
- CN117191924B CN117191924B CN202310969383.2A CN202310969383A CN117191924B CN 117191924 B CN117191924 B CN 117191924B CN 202310969383 A CN202310969383 A CN 202310969383A CN 117191924 B CN117191924 B CN 117191924B
- Authority
- CN
- China
- Prior art keywords
- pollutant
- molecular
- vacuum
- bin body
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000003344 environmental pollutant Substances 0.000 title claims abstract description 137
- 231100000719 pollutant Toxicity 0.000 title claims abstract description 137
- 238000001514 detection method Methods 0.000 title claims abstract description 30
- 238000000926 separation method Methods 0.000 title claims abstract description 30
- 238000010249 in-situ analysis Methods 0.000 title claims abstract description 24
- 238000012512 characterization method Methods 0.000 title claims abstract description 21
- 238000003380 quartz crystal microbalance Methods 0.000 claims abstract description 87
- 238000010438 heat treatment Methods 0.000 claims abstract description 77
- 230000005855 radiation Effects 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000011065 in-situ storage Methods 0.000 claims abstract description 9
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- 239000000356 contaminant Substances 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 15
- 238000007872 degassing Methods 0.000 claims description 12
- 239000013049 sediment Substances 0.000 claims description 8
- 238000005137 deposition process Methods 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 8
- 238000012360 testing method Methods 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 4
- 229920001721 polyimide Polymers 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000009434 installation Methods 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 108010085603 SFLLRNPND Proteins 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VMESOKCXSYNAKD-UHFFFAOYSA-N n,n-dimethylhydroxylamine Chemical compound CN(C)O VMESOKCXSYNAKD-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
An in-situ analysis and detection device for molecular pollutants with high-efficiency separation and dynamic characterization belongs to the technical field of molecular pollutant analysis and detection. The invention solves the problem that the existing method for researching the composition of the space molecular pollutants can not realize in-situ separation and real-time dynamic analysis. The heating radiation plate is installed in the inside wall of the vacuum bin body, the mounting frame is rotatably installed on the upper portion of the vacuum bin body, the number of pollutant collecting plates is multiple and is paved at the bottom end of the mounting frame, the number of quartz crystal microbalances is at least two and is embedded between the multiple pollutant collecting plates, the quartz crystal microbalances, the heat protection cover and the molecular pollutant heating table are arranged from top to bottom in a right opposite mode, the quartz crystal microbalances are electrically connected with the QCM temperature controller, the mass spectrometer is fixedly installed outside the vacuum bin body, the mounting frame is in the horizontal state, the quartz crystal microbalances, the pollutant collecting plates and the mass spectrometer are arranged at equal heights, the vacuum pump is arranged outside the vacuum bin body, and the vacuum degree in the vacuum bin body is controlled through the vacuum pump.
Description
Technical Field
The invention relates to a molecular pollutant in-situ analysis and detection device with high-efficiency separation and dynamic characterization, and belongs to the technical field of molecular pollutant analysis and detection.
Background
In recent years, china completes important aerospace engineering represented by lunar exploration, mars exploration and space station construction, and China aerospace technology continuously reaches a new height. During the on-orbit of spaceflight, molecular pollutants released by organic materials in a high-vacuum environment are deposited on the surface of a sensitive load, which constitutes a great threat to the efficiency and the service life of precise electronic and optical instruments of the spacecraft, so that the spacecraft can encounter a difficult challenge in stability. With the development of space load of China towards high precision and high stability, the realization of on-orbit molecular pollution protection and control of a spacecraft is one of important problems to be solved by the spacecraft. Wherein the precise determination of the composition of the pollutant components and the analysis of the volatilization behavior are of great importance for the research of the prevention and control of the spatial molecular pollutants.
At present, composition studies on molecular contaminants often use Quartz Crystal Microbalances (QCM), mass Spectrometers (MS) and Gas Chromatography (GC). Wherein QCM can only study the composition and volatilization behaviour of the total contaminated mixture and cannot determine the individual contributions of the actually different contaminant composition components. Although gas chromatography-mass spectrometry (GC/MS) can achieve a degree of separation of mixed contaminants, in situ separation and real-time dynamic analysis cannot be achieved. Therefore, the method has great significance in realizing in-situ separation and detection of different pollutant molecules.
There are many but not all methods of studying the composition of spatial molecular contaminants. Quartz crystal microbalances have the advantage of multi-temperature step data fitting, but they can only conduct component studies of the total contamination mixture and cannot determine individual contributions of actually different kinds of contaminants. Gas-mass spectrometry (GC/MS) is widely used for the separation and identification of complex components, but cannot be performed in situ and in real time, regardless of the efficiency of GC/MS material separation.
Disclosure of Invention
The invention aims to solve the technical problems, and further provides an in-situ analysis and detection device for molecular pollutants with high efficiency in separation and dynamic characterization.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the utility model provides a high-efficient separation and dynamic characterization's molecular contaminant normal position analysis detection device, includes the vacuum storehouse body, mass spectrometer, temperature controller, vacuum pump and sets up heating radiation board, molecular contaminant heating platform, heat shield, quartz crystal microbalance, pollutant collecting plate, QCM temperature controller and mounting bracket in the vacuum storehouse body, wherein, heating radiation board installs the inside wall at the vacuum storehouse body, the mounting bracket rotates the upper portion of installing at the vacuum storehouse body, and the quantity of pollutant collecting plate is a plurality of and lays in the bottom of mounting bracket, the quantity of quartz crystal microbalance is two at least and all inlays between a plurality of pollutant collecting plates, and quartz crystal microbalance, heat shield and molecular contaminant heating platform are just arranged from top to bottom, quartz crystal microbalance with QCM temperature controller electricity is connected, mass spectrometer installs quartz crystal microbalance, pollutant collecting plate and mass spectrometer etc. high setting under the mounting bracket horizontality in the vacuum storehouse body outside, heating radiation board connection is provided with the temperature controller, through the vacuum pump of vacuum control storehouse body internal vacuum pump is connected to the vacuum.
Further, the horizontal distance between the quartz crystal microbalance and the mass spectrometer is less than 10cm.
Further, an arc-shaped through groove is processed on the top end surface of the molecular pollutant heating table.
Further, the vacuum bin body is connected with a vacuum gauge.
Further, the vacuum pump includes a mechanical pump and a molecular pump.
Further, the number of the heating radiation plates is four, and the heating radiation plates are respectively attached to the four inner side walls of the vacuum bin body.
Further, a fixed plate is fixedly arranged in the vacuum bin body, and the mounting frame is rotatably arranged on the fixed plate.
Further, a bin gate and a gas release valve are arranged on the vacuum bin body.
The molecular pollutant in-situ analysis and detection method adopting the device comprises the following steps:
step one, placing a pollutant source on a molecular pollutant heating table;
step two, vacuumizing the vacuum bin body by adopting a vacuum pump until the vacuum degree is 1 multiplied by 10 -5 Pa；
Step three, heating the heating radiation plate to raise the temperature, and controlling the temperature in the vacuum bin body to reach the room temperature to 400-500K through a temperature controller;
controlling the temperature of the quartz crystal microbalance to be 150-280K through a QCM temperature controller, and keeping a relatively low temperature state compared with a heating radiation plate;
step five, starting a molecular pollutant heating table to release molecular pollutants, wherein the temperature of the molecular pollutant heating table is the same as that of a heating radiation plate or the temperature difference between the molecular pollutant heating table and the heating radiation plate is 0-5 ℃, the degassing time is 4-6 days, and pollutant molecules are deposited on a quartz crystal microbalance and a pollutant collecting plate;
step six, after the deposition process is finished, closing the heating radiation plate and the molecular pollutant heating table, and closing the vacuum pump after the temperature displayed by the temperature controller approaches to the room temperature;
step seven, opening the air release valve until the vacuum degree in the vacuum bin body is normal pressure, closing the air release valve, and taking out pollutant materials;
step eight, rotating the mounting frame to enable the quartz crystal microbalance and the pollutant collecting plate to face the mass spectrometer;
step nine, after determining an initial temperature and a final temperature according to the properties of the selected pollutant source, re-discharging the sediment through temperature programming of a QCM temperature controller, and releasing the deposited pollutant to a mass spectrometer;
step ten, quantitatively determining contributions of different types of pollutants by analyzing mass spectrometer data and quartz crystal microbalance data collected in the sediment re-emission process, and carrying out molecular recognition in a chemical database; the detected total mass is divided into different categories by analyzing the mass spectrometer data collected during the gradient heating phase, the released molecules are qualitatively identified by comparing the records of the mass spectrometer with the existing spectrum database, and the process of re-releasing the pollutants and analyzing is completed.
Further, in the step nine, the temperature programming speed of the QCM temperature controller is 1-3K/min.
Compared with the prior art, the invention has the following effects:
in order to ensure that the deposition amount of pollutants on a quartz crystal microbalance is as much as possible in the test process, the high-efficiency separation and dynamic characterization molecular pollutant in-situ analysis and detection device mainly adopts two measures, namely, a mounting frame, a heat shield and a molecular pollutant heating table are arranged from top to bottom in a right opposite way, and the quartz crystal microbalance and a pollutant collecting plate are arranged on the mounting frame in parallel, so that the quartz crystal microbalance faces a pollutant source in the air release process, and the direct flux of the pollutants in release is collected; secondly, through setting up the heat protection casing for gaseous pollutant transmission process's loss rate reduces by a wide margin in the degasification process, provides the restriction to gaseous pollutant transmission route through the heat protection casing on the one hand, and on the other hand in the pollutant source degasification process, the heat protection casing remains fairly high temperature throughout, makes any pollutant can not adsorb and causes transmission loss on its surface.
According to the invention, the pollutant collecting plate is added on the quartz crystal microbalance, and the pollutant collecting plate and the quartz crystal microbalance keep the same temperature, but the surface area of the pollutant collecting plate is ten times that of the quartz crystal microbalance, so that the pollutant can be released up to ten times in the heating process of the flat gradient of the quartz crystal microbalance, thereby enhancing the signal in the mass spectrometer, increasing the signal to noise ratio of the mass spectrometer and improving the sensitivity of the test; in addition, through rotating the mounting bracket and installing in the vacuum bin body for before the deposition process is finished, gradient heating begins, quartz crystal microbalance and pollutant collecting plate can rotate and face the mass spectrometer, and the pollutant of deposit is direct to be released towards the mass spectrometer, further increases the signal to noise ratio of mass spectrometer, makes the sensitivity of test further improve.
The high-efficiency separation and dynamic characterization molecular pollutant in-situ analysis and detection device can perform high-efficiency separation and in-situ dynamic detection of molecular pollutants, identify each pollutant component type, quantitatively determine the content of each pollutant to supplement and analyze test data of total mass loss of the quartz crystal microbalance, and better understand the degassing process of different pollutant molecules by combining mass loss data of in-situ gradient heating of the high-sensitivity quartz crystal microbalance with mass spectrometer data.
Drawings
FIG. 1 is a schematic front view of an in situ analysis and detection apparatus for molecular contaminants with high efficiency of separation and dynamic characterization (under deposition process) according to the present invention;
FIG. 2 is a schematic front view of the in situ analysis and detection device for molecular contaminants with high efficiency of separation and dynamic characterization (under the process of re-release) according to the present invention.
Detailed Description
While the present embodiments have been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that the present invention is not limited to the embodiments described, and that various modifications and changes can be made without departing from the scope of the invention.
It should be noted that, the descriptions of the directions of "left", "right", "upper", "lower", "top", "bottom", and the like of the present invention are defined based on the relation of orientations or positions shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the structures must be constructed and operated in a specific orientation, and thus, the present invention should not be construed as being limited thereto. In the description of the present invention, the meaning of "plurality" is two or more unless specifically defined otherwise.
In the description of the present invention, unless explicitly stated and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
The first embodiment is as follows: the embodiment is described by combining fig. 1 and fig. 2, an in-situ analysis and detection device for efficiently separating and dynamically characterizing molecular pollutants, which comprises a vacuum bin body 1, a mass spectrometer 2, a temperature controller 3, a vacuum pump and a heating radiation plate 5, a molecular pollutant heating table 6, a heat protection cover 7, a quartz crystal microbalance 8, a pollutant collecting plate 9, a QCM temperature controller 10 and a mounting frame, wherein the heating radiation plate 5 is mounted on the inner side wall of the vacuum bin body 1, the mounting frame is rotatably mounted on the upper part of the vacuum bin body 1, the number of the pollutant collecting plates 9 is multiple and is paved at the bottom end of the mounting frame, the quartz crystal microbalance 8, the heat protection cover 7 and the molecular pollutant heating table 6 are arranged from top to bottom in a positive manner, the quartz crystal microbalance 8 is electrically connected with the QCM temperature controller 10, the mass spectrometer 2 is fixedly mounted on the outside of the vacuum bin body 1 and in a horizontal state, the vacuum pump is connected with the vacuum pump 3 through the vacuum bin body 1, the vacuum pump is arranged on the vacuum bin body 3, and the vacuum pump is connected with the vacuum bin body 1.
The invention provides a method for simulating high temperature of 400-600K and high vacuum degree of 1X 10 -4 ～1×10 -5 And under the Pa space environment condition, the in-situ analysis testing device for efficiently separating and dynamically characterizing the space molecular pollutants. Wherein the molecular contaminants include, but are not limited to, room temperature curable structural adhesives, silicone oils, pump oils, hydrocarbons, esters, and the like.
By adopting the molecular pollutant in-situ analysis and detection device with high-efficiency separation and dynamic characterization, in the degassing process, the high-temperature high-vacuum condition is set through the vacuum pump and the heating radiation plate 5, so that the simulation of the space environment where the polluted materials are located in the degassing process is more real.
The number of quartz crystal microbalances 8 is preferably more than two to take the average of a plurality of measurements.
In order to ensure that the deposition amount of pollutants on the quartz crystal microbalance 8 is as much as possible in the test process, the high-efficiency separation and dynamic characterization molecular pollutant in-situ analysis and detection device mainly adopts two measures, namely, a mounting frame, a thermal protection cover 7 and a molecular pollutant heating table 6 are arranged right from top to bottom, the quartz crystal microbalance 8 and a pollutant collecting plate 9 are arranged on the mounting frame in parallel, so that the quartz crystal microbalance 8 faces a pollutant source in the air release process, and the direct flux when the pollutants are released is collected; secondly, through setting up thermal shield 7 for gaseous pollutant transmission process's loss rate reduces by a wide margin in the degasification process, provides the restriction to gaseous pollutant transmission route through thermal shield 7 on the one hand, and on the other hand in the pollutant source degasification process, thermal shield 7 remains fairly high temperature throughout for any pollutant can not adsorb and cause transmission loss on its surface.
According to the invention, the pollutant collecting plate 9 is added on the quartz crystal microbalance 8, and the pollutant collecting plate 9 and the quartz crystal microbalance 8 keep the same temperature, but the surface area of the pollutant collecting plate 9 is about ten times that of the quartz crystal microbalance 8, so that the pollutant can be released up to ten times in the process of heating the quartz crystal micro in a flat gradient manner, thereby enhancing the signal in the mass spectrometer 2, increasing the signal-to-noise ratio of the mass spectrometer 2 and improving the sensitivity of the test; in addition, through installing the mounting bracket rotation in vacuum storehouse body 1 for before the deposition process is finished, gradient heating begins, quartz crystal microbalance 8 and pollutant collecting plate 9 can rotate towards mass spectrometer 2, and the pollutant of deposit is directly released towards mass spectrometer 2, further increases mass spectrometer 2's SNR, makes the sensitivity of test further improve.
The high-efficiency separation and dynamic characterization molecular pollutant in-situ analysis and detection device can perform high-efficiency separation and in-situ dynamic detection of molecular pollutants, identify each pollutant component type, quantitatively determine the content of each pollutant to supplement and analyze the test data of the total mass loss of the quartz crystal microbalance 8, and better understand the degassing process of different pollutant molecules by combining the mass loss data of the high-sensitivity quartz crystal microbalance 8 in-situ gradient heating with the data of the mass spectrometer 2.
A mass spectrometer control valve 17 is arranged between the mass spectrometer and the vacuum bin body.
The horizontal distance between the quartz crystal microbalance 8 and the mass spectrometer 2 is less than 10cm. By such a design, the quartz crystal microbalance 8 and the mass spectrometer 2 are made very close to each other in space, and the loss caused by the turbulent diffusion of the gas is negligible by utilizing the space close enough to each other.
An arc through groove is processed on the top end surface of the molecular pollutant heating table 6. So designed, the pollutant source is convenient to place.
The vacuum bin body 1 is connected with a vacuum gauge 11.
The vacuum pump includes a mechanical pump 12 and a molecular pump 13. By the design, the vacuum degree in the vacuum bin body 1 can be conveniently adjusted by arranging the mechanical pump 12 and the molecular pump 13, and the requirement on higher vacuum conditions in experiments is met. Control valves are respectively arranged on the connecting pipelines between the mechanical pump 12 and the vacuum bin body 1 and the connecting pipelines between the molecular pump 13 and the vacuum bin body 1.
The number of the heating radiation plates 5 is four, and the heating radiation plates are respectively attached to the four inner side walls of the vacuum chamber body 1. By the design, the internal temperature of the vacuum bin body 1 is more uniform.
The vacuum bin body 1 is internally fixedly provided with a fixed plate 14, and the mounting frame is rotatably arranged on the fixed plate 14. Through the design, the rotary installation of the installation frame in the vacuum bin body 1 is realized through the fixing plate 14, and then the position rotation of the quartz crystal microbalance 8 and the pollutant collecting plate 9 on the installation frame is realized.
The vacuum bin body 1 is provided with a bin gate 15 and a gas release valve 16. By the design, the bin gate 15 is arranged, so that the pollutant source can be conveniently taken and placed.
The second embodiment is as follows: referring to fig. 1 and 2, a method for in situ analysis and detection of molecular contaminants using the above device according to the present embodiment includes the following steps:
step one, placing a pollutant source on a molecular pollutant heating table 6;
step two, vacuumizing the vacuum bin body 1 by adopting a vacuum pump until the vacuum degree is 1 multiplied by 10 -5 Pa; the mechanical pump 12 is adopted to carry out rough air suction on the vacuum bin body 1 until the vacuum degree is 1 multiplied by 10 -1 Pa, the process takes 20-40 min; the molecular pump 13 is adopted to carry out main air suction to the vacuum chamber body 1 until the vacuum degree is 1 multiplied by 10 -5 Pa, the process takes 2-4 hours;
step three, heating the heating radiation plate 5 to raise the temperature, and controlling the temperature in the vacuum bin body 1 to reach the room temperature to 400-500K through the temperature controller 3; the temperature settings within the vacuum chamber 1 vary widely depending on the molecular contamination being measured, the temperatures being set to match the temperatures experienced by the contaminated materials during the aerospace mission.
Controlling the temperature of the quartz crystal microbalance 8 to be 150-280K through the QCM temperature controller 10, and keeping a relatively low temperature state compared with the heating radiation plate 5; the experiment selects different temperatures, at least three different quartz crystal microbalances 8 are used for collecting pollutants, and the optimal deposition temperature is selected according to the deposition amount of the pollutants. The temperature of QCM suitable for low temperature is tested, and the temperature with the largest pollutant deposition amount is selected as the optimal set temperature through multiple experiments
Step five, starting a molecular pollutant heating table 6 to release molecular pollutants, wherein the temperature of the molecular pollutant heating table 6 is the same as or different from the temperature of a heating radiation plate 5 by 0-5 ℃, the degassing time is 4-6 days, and pollutant molecules are deposited on a quartz crystal microbalance 8 and a pollutant collecting plate 9;
step six, after the deposition process is finished, closing the heating radiation plate 5 and the molecular pollutant heating table 6, and closing the vacuum pump after the temperature displayed by the temperature controller 3 is close to the room temperature; the vacuum pump shut-down sequence is to shut down the molecular pump 13 first and then the mechanical pump 12.
Step seven, opening the air release valve 16 until the vacuum degree in the vacuum bin body 1 is normal pressure, closing the air release valve 16, and taking out pollutant materials; the QCM and contaminant collecting plate 9 deposition contaminant step is completed as this step proceeds.
Step eight, rotating the mounting frame to enable the quartz crystal microbalance 8 and the pollutant collecting plate 9 to face the mass spectrometer 2; causing the deposited contaminants to be released directly towards the mass spectrometer 2.
Step nine, after determining the initial temperature and the final temperature according to the properties of the selected pollutant source, re-discharging the sediment through temperature programming of the QCM temperature controller 10, and releasing the deposited pollutant to the mass spectrometer 2; programming temperature: the set program continuously increases linearly or non-linearly with time. The starting and ending temperatures at which the material is re-released are determined by the nature of the source of the contaminant and the temperature of the space environment experienced by the material when in use. For example: the black polyimide film material has a long-term use temperature range of 73-573K, a boiling point higher than 180K and high temperature resistance up to 673K. The QCM controls the initial temperature to be 160-180K and the end temperature to be 340-360K; the 704 silicone rubber adhesive has a boiling point higher than 375K, the use temperature of high-temperature silicone oil is 288-588K, the density is 1.070g/mL, the temperature coefficient is 0.00053, the viscosity at 25 ℃ is 44-50 mpa.s, the QCM controls the initial temperature to 288-390K, and the end temperature to 580-600K; the J-133 room temperature curing structural adhesive does not need heating and pressurizing during curing, has high strength, is fatigue-resistant, vibration-resistant and wet heat aging-resistant when the thickness of the adhesive layer reaches 1.6mm, and has the use temperature of 193-373K, the QCM control initial temperature of 180-200K and the end temperature of 380-400K. The QCM and the contaminants deposited thereon during the temperature programming of the contaminant trap 9 are re-discharged by heating.
Step ten, quantitatively determining contributions of different types of pollutants by analyzing mass spectrometer 2 data and quartz crystal microbalance 8 data collected in the sediment re-emission process, and carrying out molecular recognition in a chemical database; the detected total mass is separated into different categories by analyzing the mass spectrometer 2 data collected during the gradient heating phase, the released molecules are qualitatively identified by comparing the records of the mass spectrometer 2 with an existing spectral database, and the process of re-releasing the contaminants and analyzing is completed. Once a single molecule is identified, it is easier to find a particular fragment in the MS data.
In step nine, the temperature programming speed of the QCM temperature controller 10 is 1-3K/min.
And a third specific embodiment: the present embodiment will be described with reference to fig. 1 and 2, in which the simulated vacuum degree is 1×10 -5 And (3) quantitatively and qualitatively analyzing the organic matter component degassed by the black polyimide film material under the conditions of Pa and 378K.
Step one, the bin gate is opened, and a black polyimide film material is placed on a molecular pollutant heating table, wherein the black kapton sample is a piece of single material with the thickness of 40.48cm multiplied by 30.88cm multiplied by 0.00198 cm. Folding the whole sheet of material with 4.02 cm wide folds, fixing the folded material with a pre-cleaned metal clip, and closing the bin gate;
step (a)2. Opening a mechanical pump valve, and vacuumizing the vacuum bin body by using a mechanical pump until the vacuum degree is 1 multiplied by 10 as shown by a vacuum gauge -1 Pa, this process takes 30 minutes; closing the mechanical pump valve and the mechanical pump, and opening the molecular pump and the molecular pump valve until the vacuum gauge shows that the vacuum degree reaches 1 multiplied by 10 -5 Pa, this process takes 4 hours;
step three, heating the heating radiation plate to raise the temperature, and controlling the temperature of the vacuum bin body to reach room temperature to 378K through a temperature controller;
controlling the temperature 150K by the QCM temperature controller 10, and keeping a relatively low temperature state compared with the heating radiation plate;
step five, starting a molecular pollutant heating table to release molecular pollutants, keeping the temperature of the molecular pollutant heating table around 378K as much as possible, and carrying out degassing for 6 days, wherein pollutant molecules are deposited on the QCM and the collecting plate;
step six, closing a heating radiation plate after the deposition process is finished, closing a molecular pollutant heating table, closing a molecular pump valve and a molecular pump after the temperature displayed by a temperature controller is close to the room temperature, and then closing a mechanical pump valve and a mechanical pump;
step seven, opening the air release valve until the vacuum gauge shows that the vacuum degree is normal pressure, closing the air release valve, opening the bin gate, taking out the black polyimide film material, and closing the bin gate;
step eight, rotating the mounting frame to enable the quartz crystal microbalance and the pollutant collecting plate to face the mass spectrometer;
step nine, programming the temperature to be 2K/min to 350K by using 180K as an initial temperature through a QCM temperature controller 10, re-discharging the sediment and then conveying the sediment to a mass spectrometer;
step ten, QCM data of pollutant re-release and data comprehensive analysis of mass spectrum show that two organic pollutants are re-released, namely N, N-dimethylhydroxylamine and possibly propane, and the temperatures are respectively 190K and 280K, which shows that the device successfully realizes separation and identification of two organic molecular pollutants.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. An in-situ analysis and detection device for molecular pollutants with high-efficiency separation and dynamic characterization is characterized in that: comprises a vacuum bin body (1), a mass spectrometer (2), a temperature controller (3), a vacuum pump and a heating radiation plate (5), a molecular pollutant heating table (6), a heat shield (7), a quartz crystal microbalance (8), a pollutant collecting plate (9), a QCM temperature controller (10) and a mounting frame, wherein the heating radiation plate (5) is arranged on the inner side wall of the vacuum bin body (1), the mounting frame is rotatably arranged on the upper part of the vacuum bin body (1), the pollutant collecting plates (9) are multiple and are paved at the bottom end of the mounting frame, the quartz crystal microbalance (8) are at least two and are embedded among the multiple pollutant collecting plates (9), the quartz crystal microbalance (8), the heat shield (7) and the molecular pollutant heating table (6) are arranged from top to bottom in a right direction, the quartz crystal microbalance (8) is electrically connected with the QCM temperature controller (10), the mass spectrometer (2) is fixedly arranged on the vacuum bin body (1) and is connected with the quartz crystal microbalance (3) in the vacuum bin body (3) through the temperature controller (3), the quartz crystal microbalance (8) is arranged in the vacuum bin body (1), the vacuum bin body (1) is externally connected with a vacuum pump, and the vacuum degree in the vacuum bin body (1) is controlled by the vacuum pump.
2. The high efficiency separation and dynamic characterization molecular contaminant in situ analysis and detection apparatus according to claim 1, wherein: the horizontal distance between the quartz crystal microbalance (8) and the mass spectrometer (2) is less than 10cm.
3. The high efficiency separation and dynamic characterization molecular contaminant in situ analysis and detection apparatus according to claim 1 or 2, wherein: an arc-shaped through groove is processed on the top end surface of the molecular pollutant heating table (6).
4. The high efficiency separation and dynamic characterization molecular contaminant in situ analysis and detection apparatus according to claim 1, wherein: the vacuum bin body (1) is connected with a vacuum gauge (11).
5. The high efficiency separation and dynamic characterization molecular contaminant in situ analysis and detection apparatus according to claim 1, wherein: the vacuum pump comprises a mechanical pump (12) and a molecular pump (13).
6. The high efficiency separation and dynamic characterization molecular contaminant in situ analysis and detection apparatus according to claim 1, wherein: the number of the heating radiation plates (5) is four, and the heating radiation plates are respectively stuck to the four inner side walls of the vacuum bin body (1).
7. The high efficiency separation and dynamic characterization molecular contaminant in situ analysis and detection apparatus according to claim 1, wherein: the vacuum bin body (1) is internally and fixedly provided with a fixed plate (14), and the mounting frame is rotatably arranged on the fixed plate (14).
8. The high efficiency separation and dynamic characterization molecular contaminant in situ analysis and detection apparatus according to claim 1, wherein: the vacuum bin body (1) is provided with a bin gate (15) and a gas release valve (16).
9. An in situ analytical detection method of molecular contaminants using the device of any one of claims 1 to 8, characterized in that: the method comprises the following steps:
step one, placing a pollutant source on a molecular pollutant heating table (6);
step two, vacuumizing the vacuum bin body (1) by adopting a vacuum pump until the vacuum degree is 1 multiplied by 10 -5 Pa；
Step three, heating the heating radiation plate (5) to raise the temperature, and controlling the temperature in the vacuum bin body (1) to reach the room temperature to 400-500K through the temperature controller (3);
controlling the temperature of the quartz crystal microbalance (8) to be 150-280K through a QCM temperature controller (10), and keeping a relatively low temperature state compared with the heating radiation plate (5);
step five, starting a molecular pollutant heating table (6) to release molecular pollutants, wherein the temperature of the molecular pollutant heating table (6) is the same as that of a heating radiation plate (5) or the temperature difference between the molecular pollutant heating table and the heating radiation plate is 0-5 ℃, the degassing time is 4-6 days, and pollutant molecules are deposited on a quartz crystal microbalance (8) and a pollutant collecting plate (9);
step six, after the deposition process is finished, closing the heating radiation plate (5) and the molecular pollutant heating table (6), and closing the vacuum pump after the temperature displayed by the temperature controller (3) is close to the room temperature;
step seven, opening the air release valve (16) until the vacuum degree in the vacuum bin body (1) is normal pressure, closing the air release valve (16), and taking out pollutant materials;
step eight, rotating the mounting frame to enable the quartz crystal microbalance (8) and the pollutant collecting plate (9) to face the mass spectrometer (2);
step nine, after determining an initial temperature and a final temperature according to the properties of the selected pollutant source, re-discharging the sediment through temperature programming of a QCM temperature controller (10), and releasing the deposited pollutant to a mass spectrometer (2);
step ten, quantitatively determining contributions of different types of pollutants by analyzing mass spectrometer (2) data and quartz crystal microbalance (8) data collected in the sediment re-emission process, and carrying out molecular recognition in a chemical database; the detected total mass is divided into different types by analyzing the mass spectrometer (2) data collected in the gradient heating stage, the released molecules are qualitatively identified by comparing the record of the mass spectrometer (2) with the existing spectrum database, and the pollutant is released again and the analysis process is completed.
10. The method according to claim 9, wherein: in the step nine, the temperature programming speed of the QCM temperature controller (10) is 1-3K/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310969383.2A CN117191924B (en) | 2023-08-03 | 2023-08-03 | Molecular pollutant in-situ analysis detection device with high-efficiency separation and dynamic characterization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310969383.2A CN117191924B (en) | 2023-08-03 | 2023-08-03 | Molecular pollutant in-situ analysis detection device with high-efficiency separation and dynamic characterization |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN117191924A CN117191924A (en) | 2023-12-08 |
| CN117191924B true CN117191924B (en) | 2024-04-05 |
Family
ID=88991426
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310969383.2A Active CN117191924B (en) | 2023-08-03 | 2023-08-03 | Molecular pollutant in-situ analysis detection device with high-efficiency separation and dynamic characterization |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117191924B (en) |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004014981A (en) * | 2002-06-11 | 2004-01-15 | Hitachi Kokusai Electric Inc | Substrate processing apparatus |
| CN101776557A (en) * | 2009-12-17 | 2010-07-14 | 中国航天科技集团公司第五研究院第五一○研究所 | Device for testing grease evaporation rate in vacuum environment |
| CN101852707A (en) * | 2010-05-20 | 2010-10-06 | 中国科学院化学研究所 | Quartz crystal microbalance signal amplification method taking polystyrene spheres as template |
| CN101876613A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | Method for monitoring sensitive low-temperature surface pollution of spacecrafts |
| CN101876614A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | In-situ monitoring device for non-metal material outgassing pollution of optical surfaces of spacecrafts |
| CN101876612A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | In-situ monitoring method for outgasing contamination of nonmetallic materials on optical surface of spacecraft |
| DE102013021489A1 (en) * | 2013-12-13 | 2015-01-08 | Carl Zeiss Sms Gmbh | Contamination determination in a vacuum chamber |
| CN108717029A (en) * | 2018-05-31 | 2018-10-30 | 北京航空航天大学 | Low-temperature control system and control method for vacuum QCM |
| CN113758947A (en) * | 2021-08-11 | 2021-12-07 | 中国科学院上海光学精密机械研究所 | Test device and method for inducing molecular pollution in spacecraft cabin by total ionization dose |
| CN114112308A (en) * | 2021-11-01 | 2022-03-01 | 中国科学院上海光学精密机械研究所 | Device and method for measuring pollutants on surface of optical piece |
| CN114112774A (en) * | 2021-11-16 | 2022-03-01 | 哈尔滨工业大学 | Device and method for analyzing and testing adsorption and desorption performances of molecular pollutants |
| CN115698374A (en) * | 2020-05-01 | 2023-02-03 | 应用材料公司 | Quartz crystal microbalance concentration monitoring |
| CN115683291A (en) * | 2022-11-16 | 2023-02-03 | 兰州空间技术物理研究所 | Integrated type difference frequency quartz crystal microbalance |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060090232A (en) * | 2003-09-26 | 2006-08-10 | 더 비오씨 그룹 피엘씨 | Detection of contaminants within fluid pumped by a vacuum pump |
| EP2490006A4 (en) * | 2009-10-14 | 2018-05-02 | Nippon Paper Industries Co., Ltd. | Method for measuring degree of contaminant deposition |
-
2023
- 2023-08-03 CN CN202310969383.2A patent/CN117191924B/en active Active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004014981A (en) * | 2002-06-11 | 2004-01-15 | Hitachi Kokusai Electric Inc | Substrate processing apparatus |
| CN101776557A (en) * | 2009-12-17 | 2010-07-14 | 中国航天科技集团公司第五研究院第五一○研究所 | Device for testing grease evaporation rate in vacuum environment |
| CN101876613A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | Method for monitoring sensitive low-temperature surface pollution of spacecrafts |
| CN101876614A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | In-situ monitoring device for non-metal material outgassing pollution of optical surfaces of spacecrafts |
| CN101876612A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | In-situ monitoring method for outgasing contamination of nonmetallic materials on optical surface of spacecraft |
| CN101852707A (en) * | 2010-05-20 | 2010-10-06 | 中国科学院化学研究所 | Quartz crystal microbalance signal amplification method taking polystyrene spheres as template |
| DE102013021489A1 (en) * | 2013-12-13 | 2015-01-08 | Carl Zeiss Sms Gmbh | Contamination determination in a vacuum chamber |
| CN108717029A (en) * | 2018-05-31 | 2018-10-30 | 北京航空航天大学 | Low-temperature control system and control method for vacuum QCM |
| CN115698374A (en) * | 2020-05-01 | 2023-02-03 | 应用材料公司 | Quartz crystal microbalance concentration monitoring |
| CN113758947A (en) * | 2021-08-11 | 2021-12-07 | 中国科学院上海光学精密机械研究所 | Test device and method for inducing molecular pollution in spacecraft cabin by total ionization dose |
| CN114112308A (en) * | 2021-11-01 | 2022-03-01 | 中国科学院上海光学精密机械研究所 | Device and method for measuring pollutants on surface of optical piece |
| CN114112774A (en) * | 2021-11-16 | 2022-03-01 | 哈尔滨工业大学 | Device and method for analyzing and testing adsorption and desorption performances of molecular pollutants |
| CN115683291A (en) * | 2022-11-16 | 2023-02-03 | 兰州空间技术物理研究所 | Integrated type difference frequency quartz crystal microbalance |
Also Published As
| Publication number | Publication date |
|---|---|
| CN117191924A (en) | 2023-12-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5773707A (en) | Calibration method for multisample dynamic headspace sampler | |
| CN103415908A (en) | Evacuating a sample chamber | |
| CN104459053B (en) | A kind of gas sample injection device and apply its air-channel system and method | |
| Wang et al. | A new method for determining the initial mobile formaldehyde concentrations, partition coefficients, and diffusion coefficients of dry building materials | |
| CN110618077B (en) | Device and method for measuring dynamic air filtering and isolating efficiency of fabric and application | |
| CN117191924B (en) | Molecular pollutant in-situ analysis detection device with high-efficiency separation and dynamic characterization | |
| CN104678062A (en) | VOC (volatile organic compound) gas and non-methane total hydrocarbon gas sampling and detecting system | |
| US8388742B2 (en) | Apparatus to measure permeation of a gas through a membrane | |
| CN114112774A (en) | Device and method for analyzing and testing adsorption and desorption performances of molecular pollutants | |
| Kotchetova et al. | Rapid assessment of soil pollution with kerosene using a carbon-nanotube-based piezosensor | |
| CN106596871A (en) | Method and device for detecting performance reliability of air quality monitor | |
| CN112067751A (en) | Emission detection device | |
| KR20060110153A (en) | Devices and a method for measuring emission substances from construction materials | |
| CN109085027B (en) | Sampling device and concentration determination method for semi-volatile organic compounds in ambient air | |
| Sefa et al. | Gas uptake of 3D printed acrylonitrile butadiene styrene using a vacuum apparatus designed for absorption and desorption studies | |
| Glassford et al. | Characterization of contamination generation characteristics of satellite materials | |
| Barhate et al. | Effect of aerosol sampling conditions on PM2. 5 sampling accuracy | |
| CN110187018A (en) | The detection method of volatile organic compounds in indoor air concentration based on passive sampling | |
| CN101858902A (en) | Soil alteration carbonate measuring method integrating carbon isotope ratio | |
| US20220082478A1 (en) | System and method for monitoring for the presence of elements | |
| CN102749302A (en) | Portable Fourier infrared spectrum detection device and detection method thereof | |
| CN113311093A (en) | Laboratory pyrolysis and flue gas collection device and analysis method for fireproof plugging material | |
| CN210465351U (en) | VOCs on-site rapid detection device in wooden furniture | |
| CN118168864A (en) | Passive atmosphere sampler, sampling method and application thereof in rapid detection of organic chlorine pesticide in ambient air | |
| CN110286171A (en) | VOCs spot sampling system and rapid detection method in a kind of soft furniture |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |