CN109742010B - Vacuum sample feeding and changing method for vacuum instrument - Google Patents
Vacuum sample feeding and changing method for vacuum instrument Download PDFInfo
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- CN109742010B CN109742010B CN201811404484.0A CN201811404484A CN109742010B CN 109742010 B CN109742010 B CN 109742010B CN 201811404484 A CN201811404484 A CN 201811404484A CN 109742010 B CN109742010 B CN 109742010B
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Abstract
The invention discloses a vacuum sample feeding and changing method for a vacuum instrument. The vacuum sample feeding and changing method comprises the following steps: the vacuum cavity is pumped by a molecular pump to keep a vacuum state; the driving assembly drives the target holder assembly to move to the opening on the inner side of the sample inlet hole so as to seal the opening on the inner side of the sample inlet hole, a transition cavity is formed between the target holder assembly and the sealing cover, air is introduced into the transition cavity so that the transition cavity is in a normal pressure state, and the sealing cover is opened; when the sample target with sample is placed on the target seat component; closing the sealing cover, and pumping the transition cavity through the backing pump; detecting molecular pump power by a power detector; judging whether the pressure in the transition cavity reaches a preset pressure value according to the molecular pump power detected by the power detector; the power detector is used for detecting the power of the molecular pump to judge whether the vacuum cavity reaches a vacuum state. The vacuum sample feeding and changing method is high in sample feeding and changing efficiency and can accurately detect the vacuum states in the vacuum cavity and the transition cavity.
Description
Technical Field
The invention relates to a vacuum sample feeding and changing method for a vacuum instrument.
Background
At present, when a matrix assisted laser desorption time of flight mass spectrometer (MALDI-TOF MS) analyzes a sample, a sample substance to be analyzed and a matrix are required to be mixed or sequentially spotted on a sample target, and a cocrystal is generated after drying and can be sent into a vacuum cavity for analysis. The vacuum environment of the vacuum chamber is provided by a molecular pump and a backing pump, and the pressure of the vacuum chamber is usually less than 10- 4pa, the placing of the sample target into the vacuum chamber is typically accomplished using a transition chamber. The sample target is firstly put into the transition cavity, the transition cavity is pre-pumped to rough vacuum so as to meet the working vacuum degree of the molecular pump, and the sample target can enter the vacuum cavity.
The detection method of the vacuum state in the transition cavity and the high vacuum state of the vacuum cavity is still realized by the traditional vacuum gauge. The vacuum state in the transition cavity is judged by a low vacuum gauge, and the target can be accessed only when the transition cavity reaches a preset vacuum degree. The use of low vacuum gauges is detrimental to instrument design and increases cost.
Disclosure of Invention
Therefore, it is necessary to provide a vacuum sample feeding and changing method which has high sample feeding and changing efficiency and can accurately detect the vacuum state in the transition cavity.
A vacuum sample feeding and changing method for a vacuum instrument, comprising the steps of:
closing a sealing cover of a vacuum instrument, and sucking a vacuum cavity of the vacuum instrument through a backing pump and a molecular pump to keep the vacuum cavity in a vacuum state;
the driving assembly drives the target holder assembly to move to an opening on the inner side of a sample inlet of the vacuum instrument so as to seal the opening on the inner side of the sample inlet, the target holder assembly and the sealing cover seal the sample inlet to form a transition cavity, air is supplied to the transition cavity so that the transition cavity is in a normal pressure state, and the sealing cover is opened;
placing a sample target with a sample spotted on the target seat assembly, closing the sealing cover, and pumping the transition cavity through the backing pump;
detecting the molecular pump power by a power detector;
and judging whether the pressure in the transition cavity reaches a preset pressure value or not according to the molecular pump power detected by the power detector.
In one embodiment, when the pressure in the vacuum chamber is less than 1 × 10-3And Pa, the vacuum cavity reaches a vacuum state.
In one embodiment, the preset pressure is 10Pa-1000 Pa.
In one embodiment, the step of determining, by the controller, whether the pressure in the transition chamber reaches the preset pressure value specifically includes the following steps:
when the molecular pump power detected by the power detector rises to be greater than or equal to a preset power value and smaller than the rated power in a first preset time period, and is greater than the initial running power and smaller than the preset power value in a second preset time period, the pressure in the transition cavity reaches a preset pressure value, wherein the rated power is greater than the preset power value and the initial running power is greater than the preset power value.
In one embodiment, the first preset time period is 10s to 50 s.
In one embodiment, the second preset time period is 10s to 50 s.
In one embodiment, the preset power value is 10-250W.
In one embodiment, whether the vacuum chamber reaches a preset vacuum degree is judged through a vacuum gauge.
In one embodiment, when the power of the molecular pump gradually decreases to zero within a third preset time period, the molecular pump stops running, and the third preset time period is 0.5min-2 min.
In one embodiment, the rated power is 150W, the preset power value is 80W, and the initial running power is 55W.
The vacuum sample feeding and changing method for the vacuum instrument is high in sample feeding and changing efficiency and can accurately detect whether the vacuum state in the transition cavity meets the sample feeding and changing requirement. When changing a kind in the vacuum box, it is right through the molecular pump the vacuum cavity suction makes the vacuum cavity keeps the vacuum state, will advance the sample hole through backing plate subassembly and sealed lid and seal and form the transition chamber, admit air to the transition intracavity and make the transition chamber be in the ordinary pressure state, open sealed lid, after sample application in the sample target, place the sample target on the backing plate subassembly, the sample on the sample target is in non-dry state this moment, close sealed lid after through the pressure that pumps to the transition chamber in reaching the default, power detector connects the molecular pump in order to obtain molecular pump power, can judge whether the vacuum state of transition chamber reaches the requirement through the detection to molecular pump power, detection sensitivity is high, fast and the accuracy is good. Compared with the problems of low accuracy and poor sensitivity when the traditional low-vacuum gauge is used for detecting the vacuum state of the transition cavity, the vacuum sample feeding and changing method provided by the invention has the advantages that the sensitivity and accuracy of the retrieval of the vacuum state of the transition cavity are improved, the sample introduction time is indirectly shortened, the sample drying time is shortened, when the pressure in the transition cavity is gradually reduced, the sample on the sample target is gradually dried, the vacuum drying can enable sample crystals on the sample target to be more uniform, the high-throughput rapid detection is facilitated, the vacuum sample feeding and changing method can be applied to equipment such as a mass spectrometer, the application range is wide, the analysis speed of an analysis instrument such as the mass spectrometer can be effectively improved, and the accuracy, the sensitivity, the resolution and the reproducibility of sample analysis are. In addition, the vacuum sample feeding and changing method reduces the use of the traditional low vacuum gauge and greatly reduces the cost.
Drawings
FIG. 1 is a schematic structural diagram of a mass spectrometer with a function of rapid drying of mass spectrum samples according to an embodiment;
FIG. 2 is a schematic diagram of a vacuum sample feeding and changing device for a vacuum instrument according to an embodiment;
FIG. 3 is a schematic diagram of the vacuum sample feeding and changing device for the vacuum instrument shown in FIG. 2;
FIG. 4 is a flow chart of a mass spectrometry method using the mass spectrometer with rapid drying of mass spectrometry samples shown in FIG. 1;
FIG. 5 is a flow chart illustrating the determination of whether the power of the molecular pump of the vacuum sample inlet and changing apparatus shown in FIG. 2 satisfies the requirement of the curve;
FIG. 6 is a graph of molecular pump power at a preset pressure in the transition chamber;
FIG. 7 is a graph illustrating the power of the molecular pump during a first predetermined time period without increasing to a predetermined power value;
FIG. 8 is a graph of molecular pump power rising above a preset power value for a first preset time period, but not falling for a second preset time period;
FIG. 9 is a graph of the molecular pump power continuously ramping up to its rated power for a first predetermined period of time and holding the rated power for a second predetermined period of time;
FIG. 10 is a schematic view showing a vacuum state during the target entering process in the vacuum chamber;
FIG. 11 is a graph comparing the crystallization effects of 3-HPA matrix in natural drying with drying in a vacuum loading and changing apparatus;
FIG. 12 is a graph comparing the crystallization effect of CHCA matrix in natural drying versus drying in a vacuum loading device.
Description of the reference numerals
10: the mass spectrometer has a function of quickly drying a mass spectrum sample; 100: a vacuum sample feeding and changing device; 110: a vacuum sample introduction mechanism; 111: a vacuum box; 1111: a vacuum chamber; 1112: a sample inlet hole; 112: a sealing cover; 113: a target holder assembly; 114: a drive assembly; 115: a seal member; 116: a transition chamber; 120: a vacuum pump assembly; 121: a molecular pump; 122: a backing pump; 123: a pre-pumping valve; 124: an air return valve; 125: an air return pipe; 126: pre-pumping a pipe; 127: a vacuum tube; 128: a suction nozzle; 129: a gas return nozzle; 200: an ion source; 300: a mass analyzer; 400: a controller; 20: a sample target.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. When an element is referred to as being "on" another element, it can be directly connected to the other element or intervening elements may also be present.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, an embodiment of the present invention provides a mass spectrometer 10 with a function of fast drying a mass spectrum sample, which includes a vacuum sample exchange device 100 for a vacuum instrument, an ion source 200, a mass analyzer 300, an ion detector, and a controller 400. Referring to fig. 2, the vacuum sample inlet and changing device 100 for a vacuum instrument specifically includes a vacuum sample inlet mechanism 110, a vacuum pump assembly 120 and a power detector.
Referring to fig. 3, the vacuum sample injection mechanism 110 includes a vacuum box 111, a sealing cover 112 located outside the vacuum box 111, and a backing plate assembly 113 and a driving assembly 114 disposed inside the vacuum box 111.
The vacuum chamber 111 has a vacuum chamber 1111 and a sample inlet 1112 connected to the vacuum chamber 1111, the sealing cap 112 is used for opening or closing the outer opening of the sample inlet 1112, the backing plate assembly 113 is mounted on the driving assembly 114, the driving assembly 114 is electrically connected to the controller 400 for driving the backing plate assembly 113 to move, and when the backing plate assembly 113 moves to seal the inner opening of the sample inlet 1112, a transition chamber 116 is formed between the backing plate assembly 113 and the sealing cap 112.
The vacuum pump assembly 120 includes a molecular pump 121 and a backing pump 122. The molecular pump 121 is connected to the vacuum chamber 1111, the molecular pump 121 is also connected to the backing pump 122, and the backing pump 122 is connected to the sample inlet 1112. The controller 400 is electrically connected to the molecular pump 121 and the backing pump 122.
Referring to fig. 3, the vacuum pump assembly 120 includes a pre-pump valve 123, an air return valve 124, an air return pipe 125, and a pre-pump pipe 126, and the pre-pump 122 is connected to the sample inlet 1112 through the pre-pump pipe 126; the pre-pumping valve 123 is disposed on the pre-pumping pipe 126, the air return pipe 125 is connected to the sample inlet 1112, and the air return valve 124 is disposed on the air return pipe 125. The muffler 125 is not shown in fig. 3.
The power detector is connected with the molecular pump 121 for obtaining the power of the molecular pump to obtain the power of the molecular pump. The power detector is not shown in any of fig. 1-12.
The ion source 200 is installed in the vacuum chamber 111 for ionizing and accelerating the sample on the sample target 20 into ions.
The mass analyser 300 communicates with the vacuum chamber 111 for distinguishing between different mass numbers of ions in time of flight.
An ion detector is used to detect the intensity of the ions per mass number.
The vacuum sample inlet and changing device 100 is provided with the pre-pumping pipe 126 between the pre-pumping valve 123 and the transition chamber 116, during pre-pumping, the pre-pump 122 can only meet the pre-pumping requirement and the working requirement of the molecular pump 121, and the molecular pump 121 does not stop running, so that the vacuum state in the vacuum chamber 1111 can be ensured. When the transition chamber 116 is pre-pumped, the pre-pump 122 not only needs to satisfy the vacuum degree at the front end of the molecular pump 121, but also pre-pumps the gas in the transition chamber 116, so that the power of the molecular pump will be affected, and when the pre-pumping valve 123 is opened, the power of the molecular pump becomes large; pre-pumping for a period of time, and stabilizing the power of the molecular pump; after a period of pre-pumping, the gas in the transition chamber 116 is exhausted, and the molecular pump power is restored to normal. The whole pre-pumping process and the pre-pumping state can be judged by detecting the power of the molecular pump, the pre-pumping state of the transition cavity 116 can be judged without additionally increasing a low vacuum gauge, whether the sealing cover 112 on the vacuum box 111 is covered or not can also be judged by the power, and if the sealing cover is not covered, the power of the molecular pump is maintained to be in high-power operation.
In a specific example, the outer opening of the sample inlet 1112 is opened on the upper surface of the sample inlet box, and the inner opening of the sample inlet 1112 is opened on the inner wall of the sample inlet cavity at the top.
Further, the sealing cover 112 is rotatably connected to the vacuum box 111.
In a specific example, a sealing edge protrudes from the outer peripheral surface of the sealing cover 112, the sealing edge surrounds the periphery of the sealing cover 112, the size of the sealing cover 112 is matched with the size of the sample inlet 1112, and when the sealing cover 112 is matched with the outer opening of the sample inlet 1112 in an embedded mode, the sealing edge abuts against the outer wall of the sample inlet box.
In a specific example, the vacuum sampling mechanism 110 further includes a sealing ring surrounding the sealing cover 112 and connected to the sealing edge.
In a specific example, the volume of the transition chamber 116 is 1-600cm3。
Further, a control passage is provided on the vacuum box 111. One end of the control channel is connected to the sample inlet 1112, and the other end is open to the outer surface of the vacuum chamber 111, and the pre-pumping pipe 126 and the air return pipe 125 are both connected to the outer opening of the control channel.
In a specific example, referring to fig. 3, the vacuum sampling mechanism 110 further includes a sealing member 115, and the sealing member 115 is not shown in fig. 1 and 2. The sealing member 115 is located outside the vacuum chamber 111 and connected to the vacuum chamber 111 to seal the outer opening of the control channel, and the sealing member 115 is provided with an air suction hole and an air return hole, both of which are communicated with the sample inlet 1112 through the control channel. A pre-pump valve 123 is connected to the sealing member 115 for opening or closing the pump hole. An air return valve 124 is connected to the sealing member 115 for opening or closing the air return hole, a pre-suction pipe 126 is connected to the suction hole, and an air return pipe 125 is connected to the air return hole.
The vacuum pump assembly 120 further includes a return nozzle 129 and a suction nozzle 128, the return nozzle 125 is connected to the return nozzle 129, and the suction nozzle 128 is connected to the suction hole.
In one specific example, the power of the molecular pump 121 is 0W-300W, preferably 0W-150W, and the inner diameter of the end of the pre-pump tube 126 near the sample inlet is 0.01mm-2mm, preferably 0.18 mm. The power of the molecular pump 121 is set to be 0W-150W, the inner diameter of one end, close to the sample inlet, of the pre-pumping pipe 126 is set to be 0.01mm-2mm, the purposes of low cost and good pre-pumping effect are achieved, and the inner diameter of one end, close to the sample inlet, of the pre-pumping pipe 126 is not easy to be too large or too small. If the inner diameter of the end of the pre-pumping pipe 126 close to the sample inlet is too large, the pre-pump 122 with high pumping speed is required, which may cause problems of high cost and large volume noise, and if the inner diameter of the end of the pre-pumping pipe 126 close to the sample inlet is too small, the pre-pump 122 may take too long pumping time, which may affect the crystallization degree of the sample, and further affect the sensitivity and reproducibility of the instrument detection, and may cause a long sample inlet time, which may cause a low detection rate.
Further, the vacuum pump assembly 120 further includes a vacuum tube 127, the molecular pump 121 is connected to the backing pump 122 through the vacuum tube 127, and the inner diameter of the vacuum tube 127 is larger than that of the pre-pumping tube 126.
Preferably, the pre-pump valve 123 is a solenoid valve, the air return valve 124 is a solenoid valve, and the controller 400 is electrically connected to the pre-pump valve 123 and the air return valve 124. The vacuum sample feeding and changing device 100 for the vacuum instrument improves the automation degree by arranging the pre-pumping valve 123 and the air return valve 124 which are electromagnetic valves, and saves the sample feeding and changing time.
The vacuum sample feeding and changing device 100 composed of the vacuum sample feeding mechanism 110, the vacuum pump assembly 120 and the power detector is low in cost, high in sample feeding and changing efficiency and capable of accurately detecting the vacuum state in the transition cavity 116, and when the vacuum sample feeding and changing device is used for a mass spectrometer, the accuracy of mass spectrometry results of the mass spectrometer can be improved. When the vacuum box 111 is used for changing samples, the sample inlet 1112 is sealed by the target holder assembly 113 and the sealing cover 112 to form the transition cavity 116, air is introduced into the transition cavity 116 to enable the transition cavity 116 to be in a normal pressure state, the sealing cover 112 is opened, samples are applied to the sample target 20, the sample target 20 is placed on the target holder assembly 113, the sample on the sample target 20 is in a non-dry state at the moment, the pressure in the transition cavity 116 is pumped to a preset value by closing the sealing cover 112, the power detector is connected with the molecular pump 121 to obtain the power of the molecular pump, whether the vacuum state in the transition cavity 116 meets the requirement or not can be judged by detecting the power of the molecular pump, and the detection sensitivity is high, the speed is high, and the accuracy is good.
Compared with the problems of low accuracy and poor sensitivity when the traditional vacuum gauge is used for detection, the vacuum sample feeding and changing device 100 for the vacuum instrument greatly shortens the detection time, is beneficial to high-flux rapid detection, can be suitable for equipment such as a mass spectrometer, can effectively improve the analysis speed of the analysis instrument such as the mass spectrometer, and has a wide application range. In addition, the vacuum sample inlet and changing device 100 of the invention reduces the use of the traditional low vacuum gauge, the micro switch and the vacuum gauge, and greatly reduces the cost. Further, as the pressure within the transition chamber 116 gradually decreases, the sample on the sample target 20 is gradually dried, and the vacuum drying can make the sample crystals on the sample target 20 more uniform, thereby improving the accuracy, sensitivity, resolution and reproducibility of sample analysis.
The mass spectrometer 10 with the function of rapidly drying the mass spectrum sample has the advantages of low cost, high analysis speed, high detection sensitivity, high resolution and good reproducibility. The mass spectrometer 10 with the function of rapidly drying the mass spectrum sample can realize the integration of rapidly drying the mass spectrum sample and detecting the sample, the vacuum sample introduction mechanism 110 realizes the vacuum drying of the sample on the sample target 20 while realizing the sample introduction and exchange, when the sample exchange is carried out in the vacuum box 111, the sample introduction hole 1112 is sealed by the target seat assembly 113 and the sealing cover 112 to form the transition cavity 116, the transition cavity 116 is in a normal pressure state by introducing gas into the transition cavity 116, the sealing cover 112 is opened, the sample is spotted on the sample target 20, the sample target 20 is placed on the target seat assembly 113, the sample on the sample target 20 is in a non-drying state at the moment, the pressure in the transition cavity 116 is pumped to a preset value after the sealing cover 112 is closed, when the pressure in the transition cavity 116 is gradually reduced, the sample on the sample target 20 is gradually dried, the vacuum drying can make the sample crystal on the sample target 20 more uniform, thereby improving the accuracy of sample analysis, Sensitivity, resolution and reproducibility.
FIGS. 11 and 12 show comparative experiments of crystallization effects obtained by the conventional method and the method of the present invention, in which 1. mu.L of each of CHCA matrix and 3-HPA matrix was spotted on the sample target 20. The natural drying time depends on the environmental humidity, under the environmental humidity of 80%, the drying time of 1 mu L of sample is about 20min, and the mass spectrometer 10 with the mass spectrum sample rapid drying function only needs 2min by vacuum pre-pumping drying, so that the time is greatly saved. It can also be seen from fig. 11 and 12 that the vacuum drying method makes the crystallization of the sample more uniform and the crystallization particles smaller, and the mass spectrometer 10 with the function of rapid drying of mass spectrometry sample of the present invention is particularly suitable for mass spectrometry analysis of the sample with the agglomerated crystallization particles such as 3-HPA.
Referring to fig. 11 and 12, when the crystallization effect of the sample dried by using the mass spectrometer 10 with the function of rapidly drying the mass spectrum sample of the present invention is compared with the crystallization effect of the sample dried by the conventional natural drying method, it can be seen that the crystallization distribution of the 3-HPA matrix in the sample dried by the natural drying method is not uniform, and the crystallization distribution of the 3-HPA matrix in the vacuum sample exchanging device 100 of the mass spectrometer 10 with the function of rapidly drying the mass spectrum sample of the present invention is uniform; the crystal distribution of the CHCA matrix is not uniform in a dried sample by a natural drying method, and the crystal distribution of the CHCA matrix is uniform in vacuum drying in the vacuum sample exchange device 100 of the mass spectrometer 10 with the function of quickly drying the mass spectrum sample. Therefore, compared with the traditional method of drying and then feeding samples, the mass spectrometer provided by the invention completes drying work while feeding samples, greatly shortens the detection and analysis time, is beneficial to high-throughput rapid detection, and can effectively improve the analysis speed because the sample drying time influences the analysis speed.
The invention also relates to a mass spectrometry method of the mass spectrometer 10 with the function of quickly drying mass spectrometry samples, which is shown in figure 4 and comprises the following steps:
The driving assembly 114 drives the backing plate assembly 113 to move to the inner opening of the sample inlet 1112 to seal the inner opening of the sample inlet 1112, a transition cavity 116 is formed between the backing plate assembly 113 and the sealing cover 112, the air return valve 124 is opened, air is supplied to the transition cavity 116, so that the transition cavity 116 is in a normal pressure state, and the sealing cover 112 is opened.
After spotting the sample on the sample target 20, the sample target 20 is placed on the backing plate assembly 113; closing the sealing cover 112, closing the air return valve 124, opening the pre-pumping valve 123, and pumping the transition chamber 116 by the pre-pump 122 until the pressure in the transition chamber 116 reaches a preset value; the pre-set value of the pressure at which the transition chamber 116 is pumped into the transition chamber 116 by the backing pump 122 is 10Pa to 1000 Pa.
The controller controls the driving assembly 114 to drive the backing plate assembly 113 to move so as to drive the sample target 20 to move to the ion source 200, and the sample on the sample target 20 is ionized into ions by the ion source 200.
The power detector detects molecular pump power. And judging whether the pressure in the transition cavity 116 reaches a preset pressure value or not according to the molecular pump power detected by the power detector.
The vacuum gauge detects whether the vacuum chamber 1111 has reached a vacuum state.
The ion source 200 ionizes and accelerates the sample on the sample target 20 into ions.
The mass analyser 300 distinguishes between different mass numbers of ions by time of flight.
The ion detector detects the intensity of ions per mass number.
Referring to fig. 5, determining whether the pressure in the transition chamber 116 reaches the preset pressure value, that is, determining whether the power of the molecular pump meets the curve requirement, specifically includes the following steps:
judging whether the power of the molecular pump meets the curve requirement: when the power of the molecular pump detected by the power detector rises to be greater than or equal to the preset power value and less than the rated power thereof in the first preset time period, and is greater than the initial operating power thereof and less than the preset power value in the second preset time period, it indicates that the pressure in the transition chamber 116 reaches the preset pressure value, as shown in fig. 6. Wherein, the rated power is larger than the power preset value and is larger than the initial running power. Wherein the first preset time period is 10s-50s, for example 30 s. The second predetermined period of time is 10s-50s, for example 30 s. The power preset value can be 10W-250W. For example, the nominal power shown in FIGS. 6-10 is 150W, the power preset is 80W, and the initial operating power is 55W.
Judging whether the vacuum cavity reaches a preset vacuum degree or not through a vacuum gauge, wherein the pressure in the vacuum cavity is less than 1 multiplied by 10-3And Pa, the vacuum cavity reaches a vacuum state.
The molecular pump power state is shown in fig. 6 and 10 when the backing pump 122 is in the normal pre-pump state. Before the pre-pumping valve 123 is not opened, the molecular pump 121 operates at the initial operating power, after the pre-pumping valve 123 is opened, the molecular pump power increases and exceeds the power preset value but does not exceed the rated power of the molecular pump 121, and after several seconds, the gas in the transition cavity 116 is pumped, the molecular pump power decreases to a stable state, the pre-pumping valve 123 is closed, and the molecular pump power is restored to the initial operating power, thereby completing the whole pre-pumping process. Fig. 10 shows a graph of the change in the vacuum degree in the vacuum chamber 1111, and the change in the vacuum degree is performed in three stages, i.e., the replacement of the sample target 20 (target replacement), the preliminary evacuation (preliminary evacuation) of the transition chamber 1111, and the entry of the sample target 20 into the vacuum chamber (target entry).
The backing pump 122 is in an abnormal pre-pumping state, and there are three situations.
(1) When the molecular pump power detected by the power detector does not rise to the power preset value within the first preset time period, as shown in fig. 7, or the molecular pump power does not change. This may be due to the internal diameter of the pre-extraction tube 126 being too small, or the pre-extraction tube 126 being plugged, at which time the pre-extraction tube 126 needs to be replaced.
(2) The molecular pump power rises above the power preset value for a first preset time period, but does not drop for a second preset time period, as shown in fig. 8. This is because the sealing cover 112 of the vacuum chamber 111 is not covered or foreign materials block the sealing cover 112, and the sealing cover 112 should be repaired or replaced.
(3) The power of the molecular pump continuously increases to the rated power thereof in the first preset time period and keeps the rated power to the second preset time period, and the power of the molecular pump gradually decreases to zero in the third preset time period, which indicates that the molecular pump 121 stops operating, as shown in fig. 9. This is because the internal diameter of the pre-pumping tube 126 is too large, or the pre-pumping tube 126 is out of order due to a leak, which results in a failure of pre-pumping, and at this time, the pre-pumping tube 126 needs to be repaired or replaced.
The mass spectrometry method of the mass spectrometer 10 with the mass spectrometry sample rapid drying function can complete the drying work while feeding the sample, greatly shorten the detection and analysis time and facilitate high-throughput rapid detection. The mass spectrometry method is simple to operate, saves time and labor, and has high detection and analysis efficiency, high accuracy, high sensitivity, high resolution and good reproducibility.
The vacuum sample feeding and changing method for the vacuum instrument is high in sample feeding and changing efficiency and can accurately detect whether the vacuum states in the vacuum cavity 1111 and the transition cavity 116 meet the sample feeding and changing requirements. When the vacuum box 111 is used for changing samples, the vacuum chamber 1111 is pumped by the molecular pump 121 to be kept in a vacuum state, the sample inlet hole 1112 is sealed by the target holder assembly 113 and the sealing cover 112 to form the transition chamber 116, the transition chamber 116 is in a normal pressure state by introducing air into the transition chamber 116, the sealing cover 112 is opened, the sample is spotted on the sample target 20, the sample target 20 is placed on the target holder assembly 113, the sample on the sample target 20 is in a non-dry state, the pressure in the transition chamber 116 after the sealing cover 112 is closed reaches a preset value by pumping the transition chamber 116, the power detector is connected with the molecular pump 121 to obtain the power of the molecular pump, whether the vacuum state in the transition chamber 116 meets the requirement or not can be judged by detecting the power of the molecular pump, and the detection sensitivity is high, the speed is high, and the accuracy is good. Compared with the problems of low accuracy and poor sensitivity when the traditional low-vacuum gauge is used for detecting the vacuum state of the transition cavity, the vacuum sample feeding and changing method provided by the invention has the advantages that the sensitivity and accuracy of the retrieval of the vacuum state of the transition cavity are improved, the sample introduction time is indirectly shortened, the sample drying time is shortened, when the pressure in the transition cavity 116 is gradually reduced, the sample on the sample target 20 is gradually dried, the vacuum drying can enable sample crystals on the sample target 20 to be more uniform, the high-throughput rapid detection is facilitated, the method can be applied to equipment such as a mass spectrometer, the application range is wide, the analysis speed of an analysis instrument such as the mass spectrometer can be effectively improved, and the accuracy, the sensitivity, the resolution and the reproducibility of the sample analysis are improved. In addition, the method of the invention reduces the use of the traditional target cover micro switch, the traditional low vacuum gauge and the traditional vacuum gauge, and greatly reduces the cost.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A vacuum sample feeding and changing method for a vacuum instrument is characterized by comprising the following steps:
closing a sealing cover of a vacuum instrument, and sucking a vacuum cavity of the vacuum instrument through a backing pump and a molecular pump to keep the vacuum cavity in a vacuum state;
the driving assembly drives the target holder assembly to move to an opening on the inner side of a sample inlet of the vacuum instrument so as to seal the opening on the inner side of the sample inlet, the target holder assembly and the sealing cover seal the sample inlet to form a transition cavity, air is supplied to the transition cavity so that the transition cavity is in a normal pressure state, and the sealing cover is opened;
placing a sample target with a sample spotted on the target seat assembly, closing the sealing cover, and pumping the transition cavity through the backing pump;
detecting molecular pump power by a power detector;
judging whether the pressure in the transition cavity reaches a preset pressure value or not according to the molecular pump power detected by the power detector; the step of judging whether the pressure in the transition cavity reaches the preset pressure value specifically comprises the following steps: when the molecular pump power detected by the power detector rises to be greater than or equal to a preset power value and smaller than the rated power in a first preset time period, and is greater than the initial running power and smaller than the preset power value in a second preset time period, the pressure in the transition cavity reaches a preset pressure value, wherein the rated power is greater than the preset power value and the initial running power is greater than the preset power value.
2. The vacuum sample exchange method for vacuum instrument as claimed in claim 1, wherein when the pressure in the vacuum chamber is less than 1 x 10-3And Pa, the vacuum cavity reaches a vacuum state.
3. Vacuum sample exchange method for a vacuum instrument according to claim 1 or 2, characterized in that said preset pressure value is comprised between 10Pa and 1000 Pa.
4. Vacuum sample exchange method for a vacuum instrument according to claim 1 or 2, characterized in that the volume of the transition chamberThe product is 1-600cm3。
5. The vacuum sample inlet and changing method for a vacuum instrument as claimed in claim 4, wherein the first preset time period is 10s-50 s.
6. The vacuum sample inlet and changing method for a vacuum instrument as claimed in claim 4, wherein the second preset time period is 10s-50 s.
7. The vacuum sample inlet and changing method for the vacuum instrument as claimed in claim 4, wherein the preset power value is 10W-250W.
8. The vacuum inlet changing method for a vacuum instrument as claimed in claim 4, wherein it is judged whether the vacuum chamber reaches a preset vacuum degree by a vacuum gauge.
9. The vacuum sample changing method for the vacuum instrument as claimed in claim 1, wherein the molecular pump stops running when the power of the molecular pump gradually decreases to zero in a third preset time period, and the third preset time period is 0.5min-5 min.
10. The vacuum sample exchange method for the vacuum instrument as claimed in claim 9, wherein the rated power is 150W, the preset power value is 80W, and the initial operation power is 55W.
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| CN110864959A (en) * | 2019-10-28 | 2020-03-06 | 散裂中子源科学中心 | Sample changing method and system for low-temperature environment equipment and application |
| CN111852280A (en) * | 2020-06-22 | 2020-10-30 | 上海集成电路研发中心有限公司 | Device and method for replacing device in vacuum cavity |
| CN112582250B (en) * | 2020-11-15 | 2021-09-17 | 复旦大学 | Matrix-assisted laser desorption ion source device |
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