CN112885702B - Sampling device of mass spectrometer - Google Patents
Sampling device of mass spectrometer Download PDFInfo
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- CN112885702B CN112885702B CN202110390390.8A CN202110390390A CN112885702B CN 112885702 B CN112885702 B CN 112885702B CN 202110390390 A CN202110390390 A CN 202110390390A CN 112885702 B CN112885702 B CN 112885702B
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- cylinder
- sample
- electric atomizing
- sample introduction
- mass spectrometer
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0431—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples
- H01J49/0445—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples with means for introducing as a spray, a jet or an aerosol
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0404—Capillaries used for transferring samples or ions
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a sampling device of a mass spectrometer, which comprises a capillary tube and a plurality of electric atomizing needles, wherein a plurality of automatic regulating and controlling devices capable of controlling the using quantity of the electric atomizing needles according to the total sampling quantity are arranged between the electric atomizing needles and the capillary tube, the using quantity of the electric atomizing needles can be reasonably and automatically regulated according to the total sampling quantity of a sample through the arranged electric atomizing needles and the capillary tube, the atomizing degree of the sample can be effectively controlled, the accuracy of a detection result is ensured, meanwhile, a sliding part arranged in a sample feeding cylinder can control the moving distance of a connecting plate according to the pressure inside a sampling groove, so that the using time of the electric atomizing needles can be effectively regulated, the accuracy of sample detection is further improved.
Description
Technical Field
The invention relates to the technical field of news transmission, in particular to a mass spectrometer sample injection device.
Background
The mass spectrometer takes an ion source, a mass analyzer and an ion detector as cores, wherein the ion source is a device for ionizing sample molecules under a high vacuum condition, the ionized molecules can be further fragmented into a plurality of fragment ions and neutral particles with smaller mass due to receiving excessive energy, the fragment ions and the neutral particles can obtain average kinetic energy with the same energy under the action of an accelerating electric field and enter the mass analyzer, and the mass analyzer is a device for separating ions with different masses entering the mass analyzer at the same time according to the mass-to-charge ratio m/e. The separated ions enter an ion detector in sequence, amplified ion signals are collected and processed by a computer to be drawn into mass spectrograms, the ion source, the mass analyzer and the ion detector are all of various types, when a mass spectrometer is used for sample injection, a sample firstly enters a spray needle through a capillary vessel by an injector, and then the subsequent detection operation is carried out after the separation of the ion source,
however, the conventional electrospray interface is only suitable for a system with a mobile phase flow rate of 1-5 μ l/min, manual injection is required during sample injection, and the force cannot be kept one system during each injection, so that the sample entering the electrospray needle cannot be ensured to be sprayed in time during sample injection, and when the atomization degree of the sample is not enough or the content of the filled inert gas is not enough, the entered sample cannot be completely separated after entering an ion source, so that the detection result cannot be obtained or the deviation occurs, and the detection work of the sample is influenced.
Disclosure of Invention
The present invention aims to provide a sample introduction device for a mass spectrometer, so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: the utility model provides a mass spectrometer sampling device, includes capillary and electric atomizing needle, and the electric atomizing needle is equipped with a plurality of, a plurality of be equipped with the automatic regulation and control device that can control the use quantity of electric atomizing needle according to the total amount of advancing kind between electric atomizing needle and the capillary.
Preferably, the automatic regulation and control device includes the sampling cylinder that communicates with the electric atomization needle screw thread, the first screw thread section of thick bamboo of one side fixedly connected with in the electric atomization needle outside is kept away from to the sampling cylinder, the one end that first screw thread section of thick bamboo was kept away from to the sampling cylinder is equipped with the setting element that can go on fixing to the sampling cylinder, the inside sample introduction groove that is equipped with of sampling cylinder, the one end that the electric atomization needle was kept away from to the sample introduction groove is equipped with can carry out the locating part sealed to the sampling cylinder, the inside regulating part that can close the use quantity of control electric atomization needle according to its inside pressure that is equipped with of sample introduction groove, through the automatic regulation and control device that is equipped with to the effect of the electric atomization needle is used to the total amount reasonable use that the realization got into according to the sample.
Preferably, the setting element includes and rotates with a kind section of thick bamboo and be connected with the locating frame, a plurality of locating lever of locating frame outside fixedly connected with, a plurality of the fixed cover in the one end outside that the locating frame was kept away from to the locating lever has connect the rotation handle, one side fixedly connected with second screw thread section of thick bamboo that a kind section of thick bamboo was kept away from to the locating frame is through the setting element that is equipped with to the realization carries out the effect fixed to a kind section of thick bamboo.
Preferably, the locating part is including fixed the closing plate of cup jointing in the capillary outside, it has the intake pipe to lie in the fixed intercommunication in capillary one side on the closing plate, it is connected with two threaded rods, two to rotate on the closing plate the threaded rod is kept away from the equal screw thread in the one end outside of capillary and is cup jointed the stop collar, and stop collar and advance a kind section of thick bamboo fixed connection, two the threaded rod is kept away from the equal fixed cup joint in the one end outside of stop collar and is had the handle, through the locating part that is equipped with to the realization carries out sealed effect to advancing a kind section of thick bamboo.
Preferably, the regulating part is including seting up at a plurality of adjustment tank, a plurality of advancing kind inslot portion all be equipped with a plurality of magnet, a plurality of all adsorb on the magnet has iron prop, a plurality of the one end that magnet was kept away from to the iron prop is equipped with the connecting piece, through the regulating part that is equipped with to the realization is convenient to carry out the effect of dismantling to the connecting block.
Preferably, the connecting piece is including fixed cup joint the connecting block in the iron prop outside, the inside spread groove that is equipped with of connecting block, the inside sliding connection of spread groove has the connecting plate, one side fixedly connected with spliced pole of connecting block is kept away from to the connecting plate, the one end fixedly connected with rubber buffer of connecting plate is kept away from to the spliced pole, the connecting cylinder has been cup jointed in the slip of the rubber buffer outside, and the fixed intercommunication of connecting cylinder and electric atomizing needle, be equipped with the slider between connecting plate and the connecting block, and the slider is located inside the spread groove, through the connecting piece that is equipped with to the realization is through the effect of the use quantity of pressure control electric atomizing needle.
Preferably, the slider includes two reset springs of fixed connection between connecting plate and connecting block, two be equipped with a location section of thick bamboo between the reset spring, and a location section of thick bamboo and connecting block fixed connection, the inside sliding connection of a location section of thick bamboo has the slide bar, and slide bar and connecting plate fixed connection, through the slider that is equipped with to the realization carries out the effect controlled to the displacement of connecting plate.
Preferably, the sealing plate is made of hard rubber materials, and the sealing plate is arranged, so that the sampling cylinder is reasonably sealed.
Compared with the prior art, the invention has the beneficial effects that:
when the sample feeding device is used, the electric atomizing needles and the capillaries are arranged, the electric atomizing needles are provided with a plurality of electric atomizing needles, so that in the process of atomizing a sample, the using number of the electric atomizing needles can be reasonably and automatically adjusted according to the total sample feeding amount of the sample through the automatic adjusting and controlling device arranged between the electric atomizing needles and the capillaries, the atomizing degree of the sample can be effectively controlled, the accuracy of a detection result is ensured, meanwhile, the sliding part arranged in the sample feeding cylinder can control the moving distance of the connecting plate according to the pressure in the sample feeding groove, the using time of the electric atomizing needles can be effectively adjusted, meanwhile, the sample feeding cylinder is convenient to use, the positioning part and the limiting part are arranged on the sample feeding cylinder, the using convenience of the sample feeding device is further improved, and the accuracy of sample detection is further improved.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a side-expanded view of the overall structure of the present invention;
FIG. 3 is an expanded view of the overall structure of the present invention;
FIG. 4 is a side sectional view of a sample introduction cylinder structure according to the present invention;
FIG. 5 is a side cross-sectional view of a connector structure of the present invention;
FIG. 6 is an enlarged view of the structure of area A in FIG. 2 according to the present invention.
In the figure: 1-a capillary tube; 2-an electric atomizing needle; 3-automatic regulating and controlling device; 4-sample feeding cylinder; 5-a first threaded cylinder; 6-a positioning member; 7-a sample introduction groove; 8-a limiting member; 9-an adjustment member; 10-a positioning frame; 11-a positioning rod; 12-a turning handle; 13-a second threaded cylinder; 14-sealing plate; 15-air inlet pipe; 16-a threaded rod; 17-a stop collar; 18-a handle; 19-an adjustment tank; 20-a magnet; 21-iron column; 22-a connector; 23-connecting blocks; 24-a connecting trough; 25-a connecting plate; 26-connecting column; 27-rubber plug; 28-a connector barrel; 29-a slide; 30-a return spring; 31-a positioning cylinder; 32-sliding bar.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-6, the present invention provides a technical solution: the utility model provides a mass spectrometer sampling device, includes capillary 1 and electric atomizing needle 2, and electric atomizing needle 2 is equipped with a plurality of, a plurality of be equipped with the automatic regulation and control device 3 that can be according to the total amount control electric atomizing needle 2's of advancing the appearance use quantity between electric atomizing needle 2 and the capillary 1.
The automatic regulation and control device 3 comprises a sample cylinder 4 in threaded communication with the electric atomizing needle 2, one side of the sample cylinder 4, which is far away from the outer side of the electric atomizing needle 2, is fixedly connected with a first threaded cylinder 5, one end of the sample cylinder 4, which is far away from the first threaded cylinder 5, is provided with a positioning part 6 capable of fixing the sample cylinder 4, a sample introduction groove 7 is arranged inside the sample cylinder 4, one end of the sample introduction groove 7, which is far away from the electric atomizing needle 2, is provided with a limiting part 8 capable of sealing the sample cylinder 4, and an adjusting part 9 capable of reasonably controlling the using number of the electric atomizing needle 2 according to the internal pressure intensity is arranged inside the sample introduction groove 7;
the positioning piece 6 comprises a positioning frame 10 which is rotationally connected with the sample injection cylinder 4, a plurality of positioning rods 11 are fixedly connected to the outer side of the positioning frame 10, a rotating handle 12 is fixedly sleeved on the outer side of one end, far away from the positioning frame 10, of each positioning rod 11, and a second threaded cylinder 13 is fixedly connected to one side, far away from the sample injection cylinder 4, of the positioning frame 10;
the limiting part 8 comprises a sealing plate 14 fixedly sleeved on the outer side of the capillary tube 1, an air inlet pipe 15 is fixedly communicated with one side of the capillary tube 1 on the sealing plate 14, the sealing plate 14 is rotatably connected with two threaded rods 16, the outer sides of the ends, far away from the capillary tube 1, of the two threaded rods 16 are both in threaded sleeve connection with a limiting sleeve 17, the limiting sleeve 17 is fixedly connected with the sample injection cylinder 4, and the outer sides of the ends, far away from the limiting sleeve 17, of the two threaded rods 16 are both fixedly sleeved with a handle 18;
the adjusting part 9 comprises a plurality of adjusting grooves 19 arranged in the sample feeding groove 7, a plurality of magnets 20 are arranged in the plurality of adjusting grooves 19, iron columns 21 are adsorbed on the plurality of magnets 20, and connecting parts 22 are arranged at one ends, far away from the magnets 20, of the plurality of iron columns 21;
the connecting piece 22 comprises a connecting block 23 fixedly sleeved outside the iron column 21, a connecting groove 24 is formed in the connecting block 23, a connecting plate 25 is connected in the connecting groove 24 in a sliding manner, a connecting column 26 is fixedly connected to one side, far away from the connecting block 23, of the connecting plate 25, a rubber plug 27 is fixedly connected to one end, far away from the connecting plate 25, of the connecting column 26, a connecting cylinder 28 is sleeved outside the rubber plug 27 in a sliding manner, the connecting cylinder 28 is fixedly communicated with the electric atomizing needle 2, a sliding piece 29 is arranged between the connecting plate 25 and the connecting block 23, and the sliding piece 29 is located inside the connecting groove 24;
the sliding part 29 comprises two return springs 30 fixedly connected between the connecting plate 25 and the connecting block 23, a positioning cylinder 31 is arranged between the two return springs 30, the positioning cylinder 31 is fixedly connected with the connecting block 23, a sliding rod 32 is slidably connected inside the positioning cylinder 31, and the sliding rod 32 is fixedly connected with the connecting plate 25;
the sealing plate 14 is made of hard rubber material;
the working principle is as follows: when a worker uses the device, firstly, the electric atomizing needle 2 is connected with the sample injection cylinder 4 through threads, then the sealing plate 14 is attached to the sample injection cylinder 4 and the handle 18 is rotated, the handle 18 drives the threaded rod 16 to rotate and is connected with the limiting sleeve 17 through threads at the same time, further, the sealing plate 14 is completely attached to the sample injection cylinder 4 and seals the sample injection groove 7, then, the position of the sample injection cylinder 4 is adjusted, firstly, the sample injection cylinder 4 is rotated, so that the sample injection cylinder 4 drives the first threaded cylinder 5 to rotate and is fixed with a sample injection structure, then, the rotating handle 12 is screwed, the rotating handle 12 drives the positioning frame 10 to rotate relative to the sample injection cylinder 4 through the positioning rod 11, further, the positioning frame 10 drives the second threaded cylinder 13 to enable the threaded cylinder to be communicated with the ion source lead-in pipe in a sealing manner, then, firstly, the worker injects inert gas into the sample injection groove 7 through the gas inlet pipe 15, then pushes the injector to be detected to push the sample into the sample injection groove 7 through the capillary 1, the sample entering the sample feeding groove 7 is combined with inert gas and is sprayed out through the electric atomizing needle 2;
when a worker introduces a sample into the sample injection groove 7, if the force of the worker is slightly larger, the total amount of the sample entering the sample injection groove 7 through the capillary 1 is larger than the pressure for atomizing the sample by one electric atomizing needle 2, because the atomization degree of the sample by one electric atomizing needle 2 is limited within a specified time, the pressure inside the sample injection groove 7 is increased, the connecting plate 25 extrudes the return spring 30 and moves inside the connecting groove 24 under the higher pressure, the connecting plate 25 drives the connecting column 26 to move while moving, so that the connecting column 26 drives the rubber plug 27 to separate from the connecting cylinder 28, the sample and the inert gas inside the sample injection groove 7 enter another electric atomizing needle 2 through the adjusting groove 19 to be atomized, and simultaneously, the moving distance of the connecting plate 25 is limited due to the limiting effect of the sliding rod 32 and the positioning cylinder 31, when getting through an electric atomizing needle 2 still not enough, will drive second and adjusting part 9 because of the reason of pressure and get through second electric atomizing needle 2 according to above-mentioned step, and then get through the reasonable pressure of 7 inside regulation sample introduction grooves of getting through of some atomizing needles for the degree of atomization of sample can in error range, and then realize the normal detection operation of sample, improved the detection efficiency of sample.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The utility model provides a mass spectrometer sampling device, includes capillary (1) and electric atomizing needle (2), and electric atomizing needle (2) are equipped with a plurality of, its characterized in that: an automatic regulating device (3) which can control the using number of the electric atomizing needles (2) according to the total amount of sample introduction is arranged between the electric atomizing needles (2) and the capillary tube (1), the automatic regulating and controlling device (3) comprises a sample feeding cylinder (4) which is in threaded communication with the electric atomizing needle (2), one side of the sample inlet cylinder (4) far away from the outer side of the electric atomizing needle (2) is fixedly connected with a first threaded cylinder (5), one end of the sampling cylinder (4) far away from the first threaded cylinder (5) is provided with a positioning piece (6) capable of fixing the sampling cylinder (4), a sample introduction groove (7) is arranged in the sample introduction cylinder (4), a limiting piece (8) capable of sealing the sample introduction cylinder (4) is arranged at one end of the sample introduction groove (7) far away from the electric atomizing needle (2), the sample injection groove (7) is internally provided with an adjusting piece (9) which can reasonably control the using quantity of the electric atomizing needles (2) according to the internal pressure.
2. A mass spectrometer sample introduction device according to claim 1, characterised in that: the positioning piece (6) comprises a positioning frame (10) which is rotatably connected with the sample feeding barrel (4), a plurality of positioning rods (11) and a plurality of positioning rods are fixedly connected to the outer side of the positioning frame (10), the rotating handle (12) is fixedly sleeved on the outer side of one end, far away from the positioning frame (10), of the positioning frame (11), and a second threaded barrel (13) is fixedly connected to one side, far away from the sample feeding barrel (4), of the positioning frame (10).
3. The mass spectrometer sample introduction device according to claim 2, characterized in that: locating part (8) are including fixed closing cap (14) in capillary (1) outside, it has intake pipe (15) to lie in the fixed intercommunication in capillary (1) one side on closing cap (14), it has two threaded rods (16), two to rotate on closing cap (14) the equal screw thread in the one end outside that capillary (1) was kept away from in threaded rod (16) has cup jointed stop collar (17), and stop collar (17) and advance a kind section of thick bamboo (4) fixed connection, two the one end outside that stop collar (17) were kept away from in threaded rod (16) all fixedly cup jointed handle (18).
4. A mass spectrometer sample introduction device according to claim 3, characterised in that: regulating part (9) are including offering at a plurality of adjustment tank (19) of introduction groove (7) inside, a plurality of adjustment tank (19) inside all is equipped with a plurality of magnet (20), a plurality of all adsorb on magnet (20) has iron prop (21), a plurality of the one end that magnet (20) were kept away from in iron prop (21) is equipped with connecting piece (22).
5. A mass spectrometer sample introduction device according to claim 4, characterised in that: connecting piece (22) connect connecting block (23) in the iron prop (21) outside including fixed cover, connecting block (23) inside is equipped with connecting groove (24), connecting groove (24) inside sliding connection has connecting plate (25), one side fixedly connected with spliced pole (26) of connecting block (23) are kept away from in connecting plate (25), the one end fixedly connected with rubber buffer (27) of connecting plate (25) are kept away from in spliced pole (26), connecting cylinder (28) have been cup jointed in the sliding of rubber buffer (27) outside, and connecting cylinder (28) and electric atomization needle (2) fixed intercommunication, be equipped with slider (29) between connecting plate (25) and connecting block (23), and slider (29) are located inside connecting groove (24).
6. A mass spectrometer sample introduction device according to claim 5, characterised in that: slider (29) are including two reset spring (30) of fixed connection between connecting plate (25) and connecting block (23), two be equipped with a location section of thick bamboo (31) between reset spring (30), and a location section of thick bamboo (31) and connecting block (23) fixed connection, the inside sliding connection of a location section of thick bamboo (31) has slide bar (32), and slide bar (32) and connecting plate (25) fixed connection.
7. A mass spectrometer sample introduction device according to claim 6, characterised in that: the sealing plate (14) is made of hard rubber materials.
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CN112885702B true CN112885702B (en) | 2022-09-16 |
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JPH08138619A (en) * | 1994-11-08 | 1996-05-31 | Yokogawa Analytical Syst Kk | Sample introduction device for high frequency inductive coupling plasma mass spectrometer |
CA2243973A1 (en) * | 1996-01-19 | 1997-07-24 | Barry L. Karger | Subatmospheric, variable pressure sample delivery chamber for electrospray ionization/mass spectrometry and other applications |
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