CN209446521U - Vacuum for vacuum instrument is into varying device - Google Patents

Vacuum for vacuum instrument is into varying device Download PDF

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Publication number
CN209446521U
CN209446521U CN201821939535.5U CN201821939535U CN209446521U CN 209446521 U CN209446521 U CN 209446521U CN 201821939535 U CN201821939535 U CN 201821939535U CN 209446521 U CN209446521 U CN 209446521U
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vacuum
sample
pump
return
valve
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喻佳俊
朱星高
张业荣
覃斌
黄利勇
林利泉
刘平
代新
黄凯彬
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Guangzhou Hsin Kang Yuan Medical Technology Co Ltd
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Guangzhou Hsin Kang Yuan Medical Technology Co Ltd
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Abstract

The utility model discloses a kind of vacuum for vacuum instrument into varying device.The vacuum includes vacuum sample introduction mechanism, vacuum pump component and power detector into device is varied;Vacuum sample introduction mechanism includes vacuum tank, the sealing cover outside vacuum tank and the backing plate assemblies and driving assembly being located in vacuum tank;Vacuum tank has vacuum chamber and is connected to the sample holes of vacuum chamber, and for driving backing plate assemblies mobile, backing plate assemblies and sealing cover can seal sample holes to form adapter cavity driving assembly;Vacuum pump component includes molecular pump, fore pump, takes out valve, return-air valve, muffler and pre- pumping pipe in advance;Molecular pump is connected to vacuum chamber, and molecular pump is also connected to fore pump, and fore pump is connected to sample holes by taking out pipe in advance;Pre- valve of taking out is located on pre- pumping pipe, and muffler is connected to sample holes, and return-air valve is located on muffler;Power detector connection molecule pump.The vacuum into vary installation cost it is low, into varying high-efficient and can accurately detect vacuum state in adapter cavity.

Description

Vacuum for vacuum instrument is into varying device
Technical field
The utility model relates to a kind of vacuum for vacuum instrument into varying device.
Background technique
In recent years, substance assistant laser desorpted time of-flight mass spectrometer (MALDI-TOF MS) be increasingly becoming protein, The important means of the large biological molecules such as polypeptide, nucleic acid analysis.And in microbial identification and field of nucleic acid detection, move towards to face The bed application stage.The sample material being analysed to is needed to mix with matrix by MALDI-TOF MS or successively point is done on sample target Co-crystal thereof is generated after dry, is allowed for access in vacuum chamber and is analyzed.The vacuum environment of vacuum chamber is by molecular pump and fore pump It provides, the pressure of vacuum chamber usually need to be less than 10-4Pa, sample target are put into vacuum chamber and adapter cavity completion are usually used.Sample target It is first put into adapter cavity, adapter cavity is evacuated to black vacuum in advance to reach the working vacuum degree for meeting molecular pump, and sample target can just enter In vacuum chamber.
The mode of traditional realization vacuum switching is as follows: target platform is moved at the inside opening of sample holes to close sample holes Inside opening, to adapter cavity air inlet make transition chamber thereof air pressure and it is extraneous balance, open the sealing cover on vacuum tank, carry out sample The replacement of product.After the completion of sample replacement, sealing cover is covered, sample target touches microswitch, shows to have covered, but can not sentence Whether disconnected sealing ring is normal;Adapter cavity is aspirated, after pre- pumping a period of time, the vacuum taken out in advance is judged by forevacuum ga(u)ge Degree, until adapter cavity reaches predetermined vacuum level, Cai Kejin target, at this point, the pressure due to transition chamber thereof is less than the pressure of vacuum chamber, After target platform is removed and opens the inside opening of sample holes, transition chamber thereof and vacuum chamber perforation, vacuum chamber is by high vacuum moment Become black vacuum environment, needs again to carry out vacuum chamber by vacuum pump at this time to be evacuated to the high vacuum shape for meeting detection environment State, and detected by vacuum gauge.The pre- pumping situation of adapter cavity judges that the vacuum state of vacuum chamber passes through by forevacuum ga(u)ge Vacuum gauge judgement, so increases the complexity and cost of design.
Utility model content
Based on this, it is necessary to provide it is a kind of it is at low cost, into varying high-efficient and can accurately detect vacuum shape in adapter cavity The vacuum for vacuum instrument of state is into varying device.
A kind of vacuum for vacuum instrument is into varying device, including vacuum sample introduction mechanism, vacuum pump component and power Detector;
The vacuum sample introduction mechanism includes vacuum tank, the sealing cover outside the vacuum tank and is located at the vacuum tank Interior backing plate assemblies and driving assembly, the vacuum tank has the sample holes of vacuum chamber and the connection vacuum chamber, described close Capping is used to open or closes the outer openings of the sample holes, and the backing plate assemblies are mounted in the driving component, institute Driving assembly is stated for driving the backing plate assemblies mobile, is opened when the backing plate assemblies are moved on the inside of the sealing sample holes When mouth, the sample holes are sealed to form adapter cavity by the backing plate assemblies and the sealing cover;
The vacuum pump component includes molecular pump, fore pump, takes out valve, return-air valve, muffler in advance and take out pipe in advance, and described point Son pump is connected to the vacuum chamber, and the molecular pump is also connected to the fore pump, and the fore pump is connected to institute by the pre- pumping pipe State sample holes;The pre- pumping valve is located on the pre- pumping pipe, and the muffler is connected to the sample holes, and the return-air valve is located at institute It states on muffler;
The power detector connects the molecular pump for obtaining the power of molecular pump to obtain molecule pump power.
The vacuum tank is equipped with control channel in one of the embodiments, and one end of the control channel is connected to institute Sample holes are stated, the other end is opened on the outer surface of the vacuum tank, and the pre- pumping pipe is connected to the control with the muffler The outer openings in channel.
The vacuum sample introduction mechanism further includes sealing element in one of the embodiments,;The sealing element is located at described true The outside of empty van and the outer openings that the control channel is sealed on the vacuum tank are connected to, the sealing element, which is equipped with, to be taken out Stomata and return-air hole, the aspirating hole and the return-air hole are connected to by the control channel with the sample holes, institute It states pre- pumping valve to be connected on the sealing element to be used to open or close the aspirating hole, the return-air valve is connected to described close To be used to open or close the return-air hole on sealing, the pre- pumping pipe is connected to the aspirating hole, and the muffler is connected to institute State return-air hole.
The power of the molecular pump is 0W-300W in one of the embodiments, and the pre- pumping is managed close to the sample holes One end internal diameter be 0.01mm-2mm.
The pre- internal diameter managed close to one end of the sample holes of taking out is 0.18mm in one of the embodiments, described The power of molecular pump is 0W-150W.
The vacuum pump component further includes vacuum tube in one of the embodiments, and the molecular pump passes through the vacuum Pipe is connected to the fore pump, and the internal diameter of the vacuum tube is greater than the pre- internal diameter for taking out pipe.
The pre- pumping valve is solenoid valve in one of the embodiments,.
The return-air valve is solenoid valve in one of the embodiments,.
The above-mentioned vacuum for vacuum instrument into vary installation cost it is low, into varying high-efficient and can accurately detect adapter cavity Interior vacuum state can be improved mass spectrometric detection accuracy when it is used for mass spectrograph.When being varied in vacuum tank, lead to It crosses backing plate assemblies and sealing cover closes sample holes to form adapter cavity, air inlet makes adapter cavity be in normal pressure shape into adapter cavity State opens sealing cover and sample target is placed on backing plate assemblies by sample point sample after sample target, at this time the sample on sample target Product are in non-dry state, close after sealing cover and reach preset value by the pressure for be pumped in adapter cavity to adapter cavity, Power detector connection molecule is pumped to obtain molecule pump power, may determine that the true of adapter cavity by the detection to molecule pump power Whether dummy status reaches requirement, and detection sensitivity is high, speed is fast and accuracy is good.Compared to traditional vacuum gauge come when detecting The problem of accuracy is low, poor sensitivity, the vacuum for vacuum instrument of the utility model substantially reduces inspection into device is varied The time is surveyed, is conducive to high-throughput quickly detection, can be adapted for using in the equipment such as mass spectrograph, analysis instrument can be effectively improved such as Mass spectrometric analysis speed, use scope are wide.In addition the vacuum of the utility model reduces traditional low vacuum into device is varied The use of rule and microswitch, substantially reduces cost.Further, when the pressure in adapter cavity is gradually reduced, on sample target Sample it is gradual drying, vacuum drying can make sample crystallization body on sample target more evenly to improve the accurate of sample analysis Property, sensitivity, resolution ratio and reproducibility.
The above-mentioned vacuum for vacuum instrument is taking out the pre- pumping pipe of installation between valve and adapter cavity into device is varied in advance, pre- to take out When, fore pump is only able to satisfy the pre- work requirements taken out and require and be able to satisfy molecular pump, and molecular pump is unlikely to shut down, such energy Enough guarantee the vacuum state in vacuum chamber.When being taken out in advance to adapter cavity, since not only to meet molecular pump front end true for fore pump Reciprocal of duty cycle will also be pumped through in advance and cross intracavitary gas, therefore molecule pump power will be affected, when opening pre- pumping valve, molecule pump power Become larger;Pre- take out stablizes a period of time, molecular pump power stability;After pre- pumping a period of time, the gas in adapter cavity is taken out to the greatest extent, molecule Pump power just restores normal.By detection molecules pump power, it can judge entirely to be pumped through journey in advance and take out state in advance, not need volume The outer pre- pumping state for increasing forevacuum ga(u)ge and judging adapter cavity, and whether the sealing cover on vacuum tank also can determine whether by power Through covering, molecule pump power will be maintained at high power operation if not covering.
The above-mentioned vacuum for vacuum instrument is 0W-150W, takes out in pipe in advance into the power for varying device setting fore pump Diameter is 0.05mm-2mm, realizes the good purpose of at low cost, pre- pumping effect, and the pre- internal diameter for taking out pipe is not easy to excessive be also not susceptible to It is small.If the pre- internal diameter for taking out pipe is excessive, then high-power fore pump is needed, problem at high cost can be so brought, smoked pipe as pre- Internal diameter is too small, then the overlong time of fore pump suction, causes sample injection time long, and sample injection time length can then bring detection sensitivity Low, the problem of detection accuracy is poor, poor reproducibility.
The above-mentioned vacuum for vacuum instrument is that solenoid valve improves certainly into device is varied by the way that pumping valve, return-air valve in advance is arranged Dynamicization degree is saved into varying the time.
Detailed description of the invention
Fig. 1 is the mass spectrometer configuration schematic diagram described in an embodiment with mass spectrum sample rapid draing function;
Fig. 2 is vacuum described in an embodiment for vacuum instrument into varying apparatus structure schematic diagram;
Fig. 3 is the vacuum shown in Fig. 2 for vacuum instrument into varying apparatus structure schematic diagram;
Fig. 4 is to use the mass spectrometric mass spectrometric analysis method process shown in FIG. 1 with mass spectrum sample rapid draing function Figure;
Fig. 5 is to judge whether vacuum shown in Fig. 2 meets the flow chart of curve requirement into the molecule pump power for varying device;
Fig. 6 reaches molecular pump power graph when pressure preset value for the pressure in adapter cavity;
Fig. 7 is curve graph when molecule pump power does not rise to power preset value in the first preset time period;
It is more than power preset value that Fig. 8 goes up in the first preset time period for molecule pump power, but in the second preset time Curve graph when not declining in section;
Fig. 9 is that molecule pump power continuous rise in the first preset time period to its rated power and keeps rated power extremely Curve graph when the second preset time period;
Figure 10 is in vacuum chamber into the vacuum state schematic diagram during target;
Figure 11 is 3-HPA matrix in natural drying and vacuum into varying crystallization effect comparison diagram dry in device;
Figure 12 is CHCA matrix in natural drying and vacuum into varying crystallization effect comparison diagram dry in device.
Description of symbols
10: the mass spectrograph with mass spectrum sample rapid draing function;100: vacuum is into varying device;110: vacuum sample introduction machine Structure;111: vacuum tank;1111: vacuum chamber;1112: sample holes;112: sealing cover;113: backing plate assemblies;114: driving assembly; 115: sealing element;116: adapter cavity;120: vacuum pump component;121: molecular pump;122: fore pump;123: taking out valve in advance;124: returning Air valve;125: muffler;126: pre- to take out pipe;127: vacuum tube;128: air exhaust nozzle;129: return-air mouth;200: ion source;300: matter Contents analyzer;400: controller;20: sample target.
Specific embodiment
The utility model is more fully retouched below with reference to relevant drawings for the ease of understanding the utility model, It states.The preferred embodiment of the utility model is given in attached drawing.But the utility model can come in many different forms in fact It is existing, however it is not limited to embodiment described herein.On the contrary, purpose of providing these embodiments is makes public affairs to the utility model The understanding for opening content is more thorough and comprehensive.
It should be noted that it can directly on the other element when element is referred to as " being fixed on " another element Or there may also be elements placed in the middle.When an element is considered as " connection " another element, it, which can be, is directly connected to To another element or it may be simultaneously present centering elements.When an element is considered as " being located at " another element, it can To be directly to another element or may be simultaneously present centering elements.
Unless otherwise defined, all technical and scientific terms used herein are led with the technology for belonging to the utility model The normally understood meaning of the technical staff in domain is identical.Terminology used in the description of the utility model herein only be The purpose of description specific embodiment, it is not intended that in limitation the utility model.Term as used herein "and/or" includes Any and all combinations of one or more related listed items.
Shown in Figure 1, an embodiment of the present invention provides a kind of matter with mass spectrum sample rapid draing function Spectrometer 10 comprising vacuum for vacuum instrument is into varying device 100, ion source 200, mass analyzer 300, ion detection Device and controller 400.Wherein, shown in Figure 2, the vacuum for vacuum instrument specifically includes vacuum into device 100 is varied Sample introduction mechanism 110, vacuum pump component 120 and power detector.
It is shown in Figure 3, vacuum sample introduction mechanism 110 include vacuum tank 111, the sealing cover 112 outside vacuum tank 111 with And it is located at backing plate assemblies 113 and driving assembly 114 in vacuum tank 111.
Vacuum tank 111 has vacuum chamber 1111 and is connected to the sample holes 1112 of vacuum chamber 1111, and sealing cover 112 is for beating On or off closes the outer openings of sample holes 1112, and backing plate assemblies 113 are mounted on driving assembly 114, and driving assembly 114 is electrically Connection controller 400 when backing plate assemblies 113 are moved to seal in sample holes 1112 for driving backing plate assemblies 113 mobile When side opening, adapter cavity 116 is formed between backing plate assemblies 113 and sealing cover 112.
Vacuum pump component 120 includes molecular pump 121 and fore pump 122.Molecular pump 121 is connected to vacuum chamber 1111, molecule Pump 121 is also connected to fore pump 122, and fore pump 122 is connected to sample holes 1112.Controller 400 is electrically connected molecular pump 121 and preceding Grade pump 122.
Shown in Figure 3, vacuum pump component 120 includes pre- pumping valve 123, return-air valve 124, muffler 125 and pre- pumping pipe 126, fore pump 122 is connected to sample holes 1112 by taking out pipe 126 in advance;Pre- valve 123 of taking out is located on pre- pumping pipe 126, and muffler 125 connects Logical sample holes 1112, return-air valve 124 are located on muffler 125.Muffler 125 is not shown in Fig. 3.
Power detector connection molecule pump 121 is for obtaining the power of molecular pump to obtain molecule pump power.Power detection Device is not shown in Fig. 1-Figure 12.
Ion source 200 is mounted in vacuum tank 111 at ion and accelerating the sample ionization on sample target 20.
Mass analyzer 300 is connected to vacuum chamber 111 to distinguish for the ion to different quality number with the flight time.
Ion detector is used to detect the intensity of the ion of every kind of mass number.
Above-mentioned vacuum takes out pipe 126 into the installation between pre- pumping valve 123 and adapter cavity 116 of device 100 is varied in advance, in advance when pumping, Fore pump 122 is only able to satisfy the pre- work requirements taken out and require and be able to satisfy molecular pump 121, and molecular pump 121 is unlikely to shut down, It can so guarantee the vacuum state in vacuum chamber 1111.When being taken out in advance to adapter cavity 116, since fore pump 122 is not only wanted Meet 121 fore vacuum degree of molecular pump also and to take out in advance the gas in adapter cavity 116, therefore molecule pump power will be affected, When opening pre- pumping valve 123, molecule pump power becomes larger;Pre- take out stablizes a period of time, molecular pump power stability;It is pre- to take out a period of time Afterwards, the gas in adapter cavity 116 is taken out to the greatest extent, and molecule pump power just restores normal.By detection molecules pump power, can judge whole It is a it is pre- be pumped through journey and take out state in advance, do not need additionally to increase forevacuum ga(u)ge and judge the pre- pumping state of adapter cavity 116, and pass through Power also can determine whether the sealing cover 112 on vacuum tank 111 has covered, and molecule pump power will be maintained at if not covering High power operation.
In a specific example, the outer openings of sample holes 1112 are opened in the upper surface of sample introduction case, sample holes 1112 Inside opening is opened in the inner wall that sample cavity is located at top.
Further, sealing cover 112 is rotationally connected with vacuum tank 111.
In a specific example, the outer peripheral surface of sealing cover 112 is protruding with sealing edge, and sealing edge is around sealing cover 112 Periphery, the size of sealing cover 112 and the size fit of sample holes 1112, when the outer openings of sealing cover 112 and sample holes 1112 When being embedded cooperation, sealing edge is abutted with the outer wall of sample introduction case.
In a specific example, vacuum sample introduction mechanism 110 further includes sealing ring, and sealing ring is around sealing cover 112 and seals Circle connection sealing edge.
In a specific example, the volume of adapter cavity 116 is 1-600cm3
Further, vacuum tank 111 is equipped with control channel.One end of control channel is connected to sample holes 1112, the other end It is opened on the outer surface of vacuum tank 111, the pre- outer openings taken out pipe 126 and be connected to control channel with muffler 125.
Shown in Figure 3 in a specific example, vacuum sample introduction mechanism 110 further includes sealing element 115, and sealing element 115 exists It is not shown in Fig. 1 and Fig. 2.Sealing element 115 is located at the outside of vacuum tank 111 and is connected on vacuum tank 111 to seal control The outer openings in channel, sealing element 115 are equipped with aspirating hole and return-air hole, and aspirating hole and return-air hole pass through control channel It is connected to sample holes 1112.Pre- valve 123 of taking out is connected on sealing element 115 to be used to open or close aspirating hole.Return-air valve 124 It is connected to be used to open or close return-air hole on sealing element 115, pre- pipe 126 of taking out is connected to aspirating hole, and muffler 125 is connected to back Stomata.
Vacuum pump component 120 include further include return-air mouth 129 and air exhaust nozzle 128, muffler 125 passes through return-air mouth 129 It is connected to return-air hole, exhaust tube is connected to by air exhaust nozzle 128 with aspirating hole.
In a specific example, the power of molecular pump 121 is 0W-300W, preferably 0W-150W, and pre- pumping pipe 126 is close The internal diameter of one end of the sample holes is 0.01mm-2mm, preferably 0.18mm.Be arranged molecular pump 121 power be 0W-150W, The pre- internal diameter for taking out pipe 126 close to one end of sample holes is 0.01mm-2mm, realizes the good purpose of at low cost, pre- pumping effect, in advance Take out internal diameter of the pipe 126 close to one end of sample holes be not easy to it is excessive be also not susceptible to it is too small.If pre- pipe 126 of taking out is close to the one of sample holes The internal diameter at end is excessive, then needs the fore pump 122 of high pumping rate, can so bring problem at high cost and that volume noise is big, such as The pre- internal diameter for taking out pipe 126 close to one end of sample holes is too small, then the overlong time that fore pump 122 aspirates influences the crystallization of sample Degree, and then the sensitivity of instrument detection, reproducibility are influenced, and cause sample injection time long, sample injection time length can then bring inspection The low problem of the rate that tests the speed.
Further, vacuum pump component 120 further includes vacuum tube 127, and molecular pump 121 is connected to prime by vacuum tube 127 Pump 122, the internal diameter of vacuum tube 127 are greater than the pre- internal diameter for taking out pipe 126.
Preferably, taking out valve 123 in advance is solenoid valve, and return-air valve 124 is solenoid valve, and controller 400 is electrically connected pre- pumping valve 123, return-air valve 124.The above-mentioned vacuum for vacuum instrument passes through the pre- pumping valve 123, return-air valve 124 of setting into device 100 is varied It is that solenoid valve improves the degree of automation, saves into varying the time.
The above-mentioned vacuum being made of vacuum sample introduction mechanism 110, vacuum pump component 120 and power detector is into varying device It is 100 at low cost, into vary vacuum state that is high-efficient and can accurately detecting in adapter cavity 116 can when it is used for mass spectrograph It is high to improve mass spectrometric mass spectrometry results accuracy.When varying in vacuum tank 111, pass through backing plate assemblies 113 and sealing cover The closing of sample holes 1112 is formed adapter cavity 116 by 112, and into adapter cavity 116, air inlet makes adapter cavity 116 be in normal pressure state, Sealing cover 112 is opened sample target 20 to be placed on backing plate assemblies 113, at this time sample target by sample point sample after sample target 20 Sample on 20 is in non-dry state, closes after sealing cover 112 by be pumped in adapter cavity 116 to adapter cavity 116 Pressure reach preset value, power detector connection molecule pump 121 passes through the inspection to molecule pump power to obtain molecule pump power Whether the vacuum state that surveying may determine that in adapter cavity 116 reaches requirement, and detection sensitivity is high, speed is fast and accuracy is good.
The problem of, poor sensitivity low come accuracy when detecting compared to traditional vacuum gauge, the utility model is used for The vacuum of vacuum instrument substantially reduces detection time into device 100 is varied, and is conducive to high-throughput quickly detection, can be applicable in It is used in the equipment such as mass spectrograph, for example mass spectrometric analysis speed of analysis instrument can be effectively improved, use scope is wide.In addition this reality Reduce the use of traditional forevacuum ga(u)ge, microswitch and vacuum gauge into device 100 is varied with novel vacuum, drops significantly Low cost.Further, when the pressure in adapter cavity 116 is gradually reduced, the sample on sample target 20 is gradual drying, and vacuum is dry The dry sample crystallization body made on sample target 20 is more evenly to improve the accuracy of sample analysis, sensitivity, resolution ratio and again Existing property.
The above-mentioned mass spectrograph 10 with mass spectrum sample rapid draing function is at low cost, analysis speed is fast, detection sensitivity is high, High resolution and favorable reproducibility.It is quick that the above-mentioned mass spectrograph 10 with mass spectrum sample rapid draing function can be realized mass spectrum sample Drying sample detection integration, vacuum sample introduction mechanism 110 are being realized into being realized while varying to the sample on sample target 20 Vacuum drying sample holes 1112 are closed by backing plate assemblies 113 and sealing cover 112 and are formed when being varied in vacuum tank 111 Adapter cavity 116 makes adapter cavity 116 be in normal pressure state 116 air inlet of adapter cavity, opens sealing cover 112, by sample point sample in After sample target 20, sample target 20 is placed on backing plate assemblies 113, the sample on sample target 20 is in non-dry state at this time, It closes after sealing cover 112 and preset value is reached by the pressure for be pumped in adapter cavity 116 to adapter cavity 116, in adapter cavity When pressure in 116 is gradually reduced, the sample on sample target 20 is gradual drying, and vacuum drying can make the sample knot on sample target 20 Crystal is more evenly to improve accuracy, sensitivity, resolution ratio and the reproducibility of sample analysis.
The crystallization effect comparative experiments obtained shown in Figure 11 and Figure 12 for the method for conventional method and the utility model, CHCA matrix and 3-HPA matrix respectively take 1 μ L point in sample target 20.The time of natural drying depends on ambient humidity, in environmental wet Under degree is 80%, the 1 μ L sample dry time takes about 20min, has mass spectrum sample rapid draing using the utility model The mass spectrograph 10 of function by vacuum drain in advance it is dry only need 2min, greatly save the time.It is dry that vacuum is also shown from Figure 11 and Figure 12 Dry method makes the crystallization of sample more evenly, and crystalline particle is smaller, the utility model with mass spectrum sample rapid draing function Mass spectrograph 10 is particularly suitable for the mass spectral analysis such as the blocking sample of the crystalline particle of 3-HPA.
Referring to shown in Figure 11 and Figure 12, the mass spectrograph 10 with mass spectrum sample rapid draing function of the utility model is used The crystallization effect of the crystallization effect and traditional natural seasoning drying sample that carry out sample drying sample compares, it is known that, 3-HPA Matrix is unevenly distributed in the crystallization of natural seasoning drying sample, and 3-HPA matrix has mass spectrum sample in the utility model The vacuum of the mass spectrograph 10 of product rapid draing function into vary carried out in device 100 it is vacuum drying crystallization be evenly distributed;CHCA Matrix is unevenly distributed in the crystallization of natural seasoning drying sample, and CHCA matrix has mass spectrum sample in the utility model The vacuum of the mass spectrograph 10 of rapid draing function into vary carried out in device 100 it is vacuum drying crystallization be evenly distributed.As it can be seen that phase Than in traditional first dry sample introduction again, the mass spectrograph of the utility model is completed dry work while sample introduction, is substantially reduced Test and analyze the time, be conducive to high-throughput quickly detection, due to sample drying time effects the speed of analysis, this The mass spectrograph of utility model can effectively improve analysis speed.
The utility model has further related to a kind of mass spectrum of mass spectrograph 10 with mass spectrum sample rapid draing function used Analysis method, it is shown in Figure 4, include the following steps:
112 sealing covers are closed, vacuum chamber is made to the suction of vacuum chamber 1111 with by molecular pump 121 by fore pump 122 1111 keep vacuum state, and the pressure in vacuum chamber 1111 is less than 1 × 10-3Pa。
Backing plate assemblies 113 are driven to be moved at the inside opening of sample holes 1112 to seal sample introduction by driving assembly 114 The inside opening in hole 1112 forms adapter cavity 116 between backing plate assemblies 113 and sealing cover 112, return-air valve 124 is opened, to transition 116 air inlet of chamber makes adapter cavity 116 be in normal pressure state, opens sealing cover 112.
By sample point sample after sample target 20, sample target 20 is placed on backing plate assemblies 113;Sealing cover 112 is closed, is closed Return-air valve 124 is closed, pre- pumping valve 123 is opened, carries out the pressure being pumped in adapter cavity 116 to adapter cavity 116 by fore pump 122 Reach preset value;It is by the preset value that the pressure that fore pump 122 be pumped in adapter cavity 116 to adapter cavity 116 reaches 10Pa-1000Pa。
Controller controls driving assembly 114 and drives backing plate assemblies 113 mobile to drive sample target 20 to be moved to ion source 200 Place, by ion source 200 by the sample ionization on sample target 20 at ion.
Power detector detection molecules pump power.The molecule pump power detected according to power detector judges adapter cavity Whether the pressure in 116 reaches pressure preset value.
Whether vacuum gauge detection vacuum chamber 1111 reaches vacuum state.
Ion source 200 at ion and accelerates the sample ionization on sample target 20.
Mass analyzer 300 distinguishes the ion of different quality number with the flight time.
Ion detector detects the intensity of the ion of every kind of mass number.
It is shown in Figure 5, judge whether the pressure in adapter cavity 116 reaches pressure preset value namely judge molecule pump power Whether meet curve requirement, specifically comprises the following steps:
Judge whether molecule pump power meets curve requirement: when the molecule pump power that power detector detects is pre- first If being risen in the period more than or equal to power preset value and being less than its rated power, and is big in the second preset time period In its initial operation power and be less than power preset value when, i.e., expression adapter cavity 116 in pressure reach pressure preset value, referring to Shown in Fig. 6.Wherein, rated power > power preset value > initial operation power.Wherein, the first preset time period is 10s-50s, Such as 30s.Second preset time period is 10s-50s, such as 30s.Power preset value can be 10W-250W.For example, in Fig. 6- Rated power shown in 10 is 150W, and power preset value is 80W, and initial operation power is 55W.
Judge whether the vacuum chamber reaches predetermined vacuum degree by vacuum gauge, the pressure in vacuum chamber is less than 1 × 10-3Pa When, indicate that the vacuum chamber reaches vacuum state.
Fore pump 122 is under normal pre- pumping state, and molecular pump power rating is as shown in Fig. 6 and Figure 10.It is not switched on pre- pumping Before valve 123, for molecular pump 121 with the operating of initial operation power, it is more than function that after opening pre- pumping valve 123, molecule pump power, which will increase, Rate preset value, but not be more than the rated power of molecular pump 121, and after the several seconds, the gas of adapter cavity 116, which is taken out, not to be had, molecular pump Power drops to stable state, closes pre- pumping valve 123, and molecule pump power is just restored to initial operation power, completes entirely pre- take out Process.Show the vacuum degree variation diagram in vacuum chamber 1111 in Figure 10, replacement sample target 20 (changing target), to adapter cavity 1111 into The pre- vacuum degree variation diagram taken out (pre- to take out) and enter vacuum chamber (into target) three phases with sample target 20 of row.
Fore pump 122 is under improper pre- pumping state, there is following three kinds of situations.
(1) it is preset when the molecule pump power that power detector detects does not rise to power in the first preset time period Value, shown in Figure 7 or molecule pump power constantization.This may be that pumping is managed since the internal diameter for taking out pipe 126 in advance is too small, or in advance 126 are plugged, and need to change pre- pumping pipe 126 at this time.
(2) it is more than power preset value that molecule pump power goes up in the first preset time period, but in the second preset time period Do not decline inside, it is shown in Figure 8.This is because the sealing cover 112 on vacuum tank 111 does not cover or has foreign matter baffle seal lid 112, it needs to overhaul or replace sealing cover 112 at this time.
(3) molecule pump power continuous rise in the first preset time period to its rated power and keeps rated power to In two preset time periods, molecule pump power is gradually reduced to zero in third preset time period, indicates that molecular pump 121 shuts down, It is shown in Figure 9.This is because the internal diameter for taking out pipe 126 in advance is excessive, or the failures such as gas leakage occur for pre- pipe 126 of taking out, and pre- pumping is caused to be lost It loses, needs to overhaul or replace pre- pumping pipe 126 at this time.
The mass spectrometric analysis method of the above-mentioned mass spectrograph 10 with mass spectrum sample rapid draing function used is realized in sample introduction While complete dry work, substantially reduce and test and analyze the time, be conducive to high-throughput quickly detection.Above-mentioned mass spectral analysis side Method is easy to operate, saves time power, tests and analyzes that high-efficient, accuracy is high, high sensitivity, high resolution and favorable reproducibility.
The above-mentioned vacuum for vacuum instrument into the method for varying into vary it is high-efficient and can accurately detect vacuum chamber 1111 with And the vacuum state in adapter cavity 116 whether reach into vary require.It is right by molecular pump 121 when being varied in vacuum tank 111 The suction of vacuum chamber 1111 makes vacuum chamber 1111 keep vacuum state, by backing plate assemblies 113 and sealing cover 112 by sample holes 1112 Closing forms adapter cavity 116, and into adapter cavity 116, air inlet makes adapter cavity 116 be in normal pressure state, opens sealing cover 112, will Sample target 20 is placed on backing plate assemblies 113 by sample point sample after sample target 20, and the sample on sample target 20 is in non-at this time Drying regime closes after sealing cover 112 and reaches preset value by the pressure for be pumped in adapter cavity 116 to adapter cavity 116, Power detector connection molecule pump 121 may determine that adapter cavity by the detection to molecule pump power to obtain molecule pump power Whether the vacuum state in 116 reaches requirement, and detection sensitivity is high, speed is fast and accuracy is good.Compared to traditional low vacuum The problem of advising, poor sensitivity low come accuracy when detecting adapter cavity vacuum state, the vacuum of the utility model into the method for varying, The sensitivity and accuracy for improving the retrieval of adapter cavity vacuum state shorten sample injection time indirectly, when shortening sample drying Between, when the pressure in adapter cavity 116 is gradually reduced, the sample on sample target 20 is gradual drying, and vacuum drying can make sample target Sample crystallization body on 20 is more evenly conducive to high-throughput quickly detection, can be adapted for using in the equipment such as mass spectrograph, use Range is wide, can effectively improve for example mass spectrometric analysis speed of analysis instrument, improve accuracy, the sensitivity, resolution of sample analysis Rate and reproducibility.In addition the method for the utility model reduces traditional target lid microswitch, forevacuum ga(u)ge and vacuum gauge It uses, substantially reduces cost.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, all should be considered as described in this specification.
Above-described embodiments merely represent several embodiments of the utility model, the description thereof is more specific and detailed, But it should not be understood as limiting the scope of the patent of the utility model.It should be pointed out that for the common of this field For technical staff, without departing from the concept of the premise utility, various modifications and improvements can be made, these all belong to In the protection scope of the utility model.Therefore, the scope of protection shall be subject to the appended claims for the utility model patent.

Claims (8)

1. a kind of vacuum for vacuum instrument is into varying device, which is characterized in that including vacuum sample introduction mechanism, vacuum pump component And power detector;
The vacuum sample introduction mechanism includes vacuum tank, the sealing cover outside the vacuum tank and is located in the vacuum tank Backing plate assemblies and driving assembly;The vacuum tank has the sample holes of vacuum chamber and the connection vacuum chamber, the sealing cover The outer openings of the sample holes are used to open or close, the backing plate assemblies are mounted in the driving component, the drive Dynamic component seals the inside openings of the sample holes for driving the backing plate assemblies mobile, when the backing plate assemblies are moved to When, the sample holes are sealed to form adapter cavity by the backing plate assemblies and the sealing cover;
The vacuum pump component includes molecular pump, fore pump, takes out valve, return-air valve, muffler and pre- pumping pipe in advance;The molecular pump Be connected to the vacuum chamber, the molecular pump is also connected to the fore pump, the fore pump by described in pre- the pumpings pipe connection into Sample hole;The pre- pumping valve is located on the pre- pumping pipe, and the muffler is connected to the sample holes, and the return-air valve is located at described return On tracheae;
The power detector connects the molecular pump for obtaining the power of molecular pump to obtain molecule pump power.
2. the vacuum according to claim 1 for vacuum instrument is into varying device, which is characterized in that on the vacuum tank Equipped with control channel, one end of the control channel is connected to the sample holes, and the other end is opened on the outer surface of the vacuum tank, The pre- outer openings taken out pipe and be connected to the control channel with the muffler.
3. the vacuum according to claim 2 for vacuum instrument is into varying device, which is characterized in that the vacuum sample introduction Mechanism further includes sealing element;The sealing element is located at the outside of the vacuum tank and is connected on the vacuum tank described in sealing The outer openings of control channel, the sealing element are equipped with aspirating hole and return-air hole, the aspirating hole and the return-air hole Be connected to by the control channel with the sample holes, the pre- pumping valve be connected on the sealing element to be used to open or The aspirating hole is closed, the return-air valve is connected on the sealing element to be used to open or close the return-air hole, described Pre- pipe of taking out is connected to the aspirating hole, and the muffler is connected to the return-air hole.
4. the vacuum for vacuum instrument according to claim 1 to 3 is into varying device, which is characterized in that institute The power for stating molecular pump is 0W-300W, and the pre- internal diameter managed close to one end of the sample holes of taking out is 0.01mm-2mm.
5. the vacuum according to claim 4 for vacuum instrument is into varying device, which is characterized in that the pre- pumping pipe leans on The internal diameter of one end of the nearly sample holes is 0.18mm, and the power of the molecular pump is 0W-150W.
6. the vacuum for vacuum instrument according to claim 1 to 3 is into varying device, which is characterized in that institute Stating vacuum pump component further includes vacuum tube;The molecular pump is connected to the fore pump by the vacuum tube, the vacuum tube Internal diameter is greater than the internal diameter of described pre- one end for taking out the close sample holes of pipe.
7. the vacuum for vacuum instrument according to claim 1 to 3 is into varying device, which is characterized in that institute Stating pre- pumping valve is solenoid valve.
8. the vacuum for vacuum instrument according to claim 1 to 3 is into varying device, which is characterized in that institute Stating return-air valve is solenoid valve.
CN201821939535.5U 2018-11-23 2018-11-23 Vacuum for vacuum instrument is into varying device Active CN209446521U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109444249A (en) * 2018-11-23 2019-03-08 广州禾信康源医疗科技有限公司 Vacuum for vacuum instrument is into varying device
CN113421817A (en) * 2021-05-25 2021-09-21 珠海美华医疗科技有限公司 Sample inlet and outlet device of mass spectrometer and mass spectrometer
CN113745091A (en) * 2021-09-15 2021-12-03 深圳泰莱生物科技有限公司 Control system and method of mass spectrum device

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109444249A (en) * 2018-11-23 2019-03-08 广州禾信康源医疗科技有限公司 Vacuum for vacuum instrument is into varying device
CN113421817A (en) * 2021-05-25 2021-09-21 珠海美华医疗科技有限公司 Sample inlet and outlet device of mass spectrometer and mass spectrometer
CN113421817B (en) * 2021-05-25 2022-06-28 珠海美华医疗科技有限公司 Sample inlet and outlet device of mass spectrometer and mass spectrometer
CN113745091A (en) * 2021-09-15 2021-12-03 深圳泰莱生物科技有限公司 Control system and method of mass spectrum device

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