CN112289674A - Mass spectrum direct sample feeding device - Google Patents
Mass spectrum direct sample feeding device Download PDFInfo
- Publication number
- CN112289674A CN112289674A CN202011269871.5A CN202011269871A CN112289674A CN 112289674 A CN112289674 A CN 112289674A CN 202011269871 A CN202011269871 A CN 202011269871A CN 112289674 A CN112289674 A CN 112289674A
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- Prior art keywords
- capillary
- capillary tube
- heat insulation
- heating
- mass spectrum
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- 238000001819 mass spectrum Methods 0.000 title claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 44
- 238000007789 sealing Methods 0.000 claims abstract description 34
- 238000005070 sampling Methods 0.000 claims abstract description 19
- 238000001514 detection method Methods 0.000 claims abstract description 7
- 238000009413 insulation Methods 0.000 claims description 28
- 238000009529 body temperature measurement Methods 0.000 claims description 17
- 238000002347 injection Methods 0.000 claims description 10
- 239000007924 injection Substances 0.000 claims description 10
- 238000004949 mass spectrometry Methods 0.000 claims description 10
- 239000013013 elastic material Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 description 7
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 230000003044 adaptive effect Effects 0.000 description 1
- 238000012863 analytical testing Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005040 ion trap Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- H01J49/0468—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample
-
- 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
- H01J49/0468—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample
- H01J49/0486—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample with means for monitoring the sample temperature
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a mass spectrum direct sampling device which comprises a sampling flange, a capillary sealing joint, a capillary and a heating and heat-insulating assembly, wherein the sampling flange is hermetically arranged on a cavity of a mass spectrometer, one end of the capillary penetrates through the sampling flange and extends into the cavity of the mass spectrometer, the capillary sealing joint is arranged along the circumferential direction of the capillary, one end of the capillary is arranged between the sampling flange and the capillary, the other end of the capillary sealing joint is provided with the heating and heat-insulating assembly along the circumferential direction, and the capillary can be replaced with different sizes according to detection requirements.
Description
Technical Field
The invention relates to the field of mass spectrometry instruments, in particular to a direct mass spectrometry sample injection device.
Background
Mass spectrometry (also called mass spectrometry) is a spectroscopic method parallel to spectroscopy, and generally means a special technique widely applied to various subject fields for identifying compounds by preparing, separating and detecting gas phase ions. Mass spectrometry provides abundant structural information in one analysis, and the combination of separation technology and mass spectrometry is a breakthrough in separation science methods. Among the numerous analytical testing methods, mass spectrometry is considered to be a universal method with both high specificity and high sensitivity, and is widely used.
Small-sized and portable mass spectrometers are increasingly widely used in the field of on-site on-line rapid detection and analysis, such mass spectrometers generally adopt a capillary direct sample introduction or membrane sample introduction manner, a metal capillary is generally welded on a flange by adopting the capillary direct sample introduction manner, and once the capillary is welded on the flange, the size of the capillary is fixed. When different application scenes are faced, the vacuum degree requirements are different, and in order to meet different vacuum degrees, capillaries with different sizes (length, inner diameter and outer diameter) need to be replaced. If a capillary tube with one size needs to be replaced, the welding flange needs to be replaced at the same time, the method is high in cost and low in replacement speed, and the requirement for portable in-situ mass spectrum on-site rapid detection and analysis cannot be met. Therefore, a method and a device which can be applied to different scenes, meet the requirements of different vacuum degrees and quickly replace capillaries with different sizes are urgently needed.
Patent document CN206657797U discloses a sample injection capillary heating device for a high vacuum mass spectrometer, which is provided with a cavity, a heater sleeve, a heating rod, a stainless steel tube, a seal sleeve, a sample injection capillary, a temperature controller and a temperature sensor; however, the design mainly aims at the problems of replacement and heating of the capillary tube in a high vacuum scene, and the capillary tube is heated in a mode that a stainless steel tube and a heating sleeve are welded together; the sizes of the capillary tubes are fixed because the sizes of the stainless steel tube and the heating sleeve are fixed; if different capillaries need to be replaced, the adaptive stainless steel tube and the heating sleeve need to be replaced correspondingly, so that the cost is high; moreover, the method is only suitable for a high-vacuum time-of-flight mass spectrometer, has no effect on a low-vacuum mass spectrometer, and has a narrow application range.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a mass spectrum direct sample feeding device.
The invention provides a mass spectrum direct sampling device which comprises a sampling flange, a capillary tube sealing joint, a capillary tube and a heating heat insulation assembly, wherein the capillary tube is arranged on the sampling flange;
the sampling flange is hermetically arranged on the cavity of the mass spectrometer, one end of the capillary tube penetrates through the sampling flange and extends into the cavity of the mass spectrometer, the capillary tube sealing joint is arranged along the circumferential direction of the capillary tube, one end of the capillary tube sealing joint is arranged between the sampling flange and the capillary tube, and the other end of the capillary tube sealing joint is provided with a heating and heat-insulating assembly along the circumferential direction;
the capillary tube can be changed into different sizes according to the detection requirement.
Preferably, the different sizes include capillaries of the same outer diameter and different inner diameters, and capillaries of different outer diameters.
Preferably, when the capillary tubes with the same outer diameter and different inner diameters are replaced, the capillary tubes can be replaced after the heating and heat insulation assembly is disassembled.
Preferably, when the capillary tubes with different outer diameters are replaced, the capillary tubes with different outer diameters and the capillary tube sealing joints with corresponding sizes can be replaced by sequentially disassembling the heating and heat insulation assembly, the capillary tubes and the capillary tube sealing joints.
Preferably, the heating and heat-insulating assembly comprises a heating temperature measuring assembly and a heat-insulating assembly;
the heating temperature measurement assembly is arranged outside the capillary tube, and the heat insulation assembly is arranged along the circumferential direction of the heating temperature measurement assembly and connected with the sample feeding flange.
Preferably, the heating temperature measuring assembly and the heat insulation assembly can be detachably mounted.
Preferably, the capillary sealing joint is made of elastic materials.
Preferably, the sample introduction flange is in sealed connection with the mass spectrometer chamber.
Preferably, the heat insulation assembly is provided with a capillary hole, and the capillary tube extends from the inner part of the capillary sealing joint to the outer part of the heat insulation assembly through the capillary hole.
Preferably, a cable port is formed in the heat insulation assembly and used for installing a cable, and the cable is connected with the heating temperature measurement assembly.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention can quickly replace capillaries with different sizes according to different application scenes, has high speed and is particularly suitable for portable in-situ mass spectrometers.
2. The invention meets the requirements of different vacuum degrees, can be applied to high-vacuum flight time mass spectrum, magnetic mass spectrum and orbit trap mass spectrum, can also be applied to medium-low vacuum ion trap mass spectrum and quadrupole mass spectrum, and has wide application range.
3. The invention has low cost and low manufacturing cost and meets the requirement of batch production.
4. According to the invention, the combination of the heating temperature measurement assembly, the heat insulation assembly and the structure effectively realizes the temperature control of the capillary tube and the isolation of a heat source from the outside, the heat transfer efficiency is improved, and the components are detachably connected, so that the device is safe and convenient and has strong practicability.
5. The capillary tube sealing joint disclosed by the invention is made of an elastic material, so that the sealing and the dismounting are convenient, and a certain protection effect on the capillary tube can be realized.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic structural view of the present invention;
fig. 2 is a schematic diagram of the interface of the present invention with a mass spectrometer.
The figures show that:
1-sample introduction flange 2-capillary tube sealing joint
3-capillary 4-heating temperature measuring component
5-insulation assembly 6-cable
7-Mass spectrometer chamber.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
The invention provides a mass spectrum direct sampling device, which can be used for quickly replacing capillaries with different sizes, can be applied to mass spectrometer sampling devices with different scenes and meeting different vacuum degree requirements, and has low cost and wide application range.
As shown in fig. 1-fig. 2, including advancing kind flange 1, capillary sealing joint 2, capillary 3 and the thermal-insulated subassembly of heating, advance kind flange 1 seal installation on mass spectrograph cavity 7, the one end of capillary 3 is passed advance kind flange 1 and extend to the inside of mass spectrograph cavity 7, capillary sealing joint 2 follows capillary 3's circumference is arranged and one end is arranged between advancing kind flange 1 and capillary 3, wherein, capillary sealing joint 2 preferably adopts elastic material, can realize sealing, can play certain guard action to capillary 3 again. The other end of the capillary tube sealing joint 2 is provided with a heating and heat-insulating assembly along the circumferential direction, and the capillary tube 3 can be replaced by different sizes according to the detection requirement.
Further, in a preferred embodiment, the heating and heat insulation assembly comprises a heating temperature measurement assembly 4 and a heat insulation assembly 5, the heating temperature measurement assembly 4 is installed outside the capillary tube 3, and the heat insulation assembly 5 is arranged along the circumferential direction of the heating temperature measurement assembly 4 and is connected with the sampling flange 1. In practical application, the heating temperature measurement component 4 and the heat insulation component 5 can be detachably mounted, for example, the heat insulation component 5 is connected with the sample injection flange 1 through bolts.
Specifically, different sizes of capillary 3 include the capillary 3 of the different internal diameters of the same external diameter and different external diameters and capillary 3, when changing the different internal diameters of capillary 3 of the same external diameter, can change through having dismantled after the thermal-insulated subassembly of heating capillary 3, dismantle thermal-insulated subassembly 5 earlier promptly, dismantle heating temperature measurement subassembly 4 again, the change time is no longer than 3 min. When the capillary tubes 3 with different outer diameters are replaced, the capillary tubes 3 with different outer diameters can be replaced after the heat insulation assembly 5, the heating temperature measurement assembly 4, the capillary tubes 3 and the capillary tube sealing joints 2 are detached in sequence, the capillary tube sealing joints 2 with the sizes corresponding to the capillary tubes 3 are replaced after the capillary tubes 3 are replaced, and the whole replacement time is not more than 5 min.
In practical application, the sample introduction flange 1 and the mass spectrometer chamber 7 can be sealed and connected by adopting a sealing O-ring mode.
In practical application, be provided with cable mouth and capillary hole on the thermal-insulated subassembly 5, the cable mouth is used for installing cable 6, cable 6 with heating temperature measurement subassembly 4 is connected for the power supply of equipment, capillary 3 extends to the outside of thermal-insulated subassembly 5 through the capillary hole from the inside of capillary sealing joint 2, and capillary 3 protrudes to the outside of thermal-insulated subassembly 5 and is convenient for the sample that awaits measuring to get into from the one end of capillary 3, and the heating temperature measurement subassembly 4 companion of flowing through is heated, is ionized, is detected in getting into the mass spectrograph.
The working principle of the invention is as follows:
according to the detection requirement, the size of a capillary tube 3 is selected, a sample injection flange 1 is hermetically connected with a mass spectrometer cavity 7, a capillary tube sealing joint 2 matched with the capillary tube 3 is selected, the capillary tube sealing joint 2 is installed in an installation hole in the middle of the sample injection flange 1, one end of the capillary tube 3 penetrates through the capillary tube sealing joint 2 and extends into the mass spectrometer cavity 7, the length of the capillary tube 3 extending into the mass spectrometer cavity 7 is determined according to the position of an ionization source, the capillary tube 3 is hermetically fixed by the capillary tube sealing joint 2, a heating temperature measurement component 4 is fixed on the capillary tube 3 in a coating mode and can be detached, a heat insulation component 5 wraps the heating temperature measurement component and is connected with the sample injection flange 1, a sample to be detected enters from one end of the capillary tube 3, and flows through the capillary tube.
In the description of the present application, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the present application and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present application.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (10)
1. A mass spectrum direct sample introduction device is characterized by comprising a sample introduction flange (1), a capillary tube sealing joint (2), a capillary tube (3) and a heating heat insulation assembly;
the sample injection flange (1) is hermetically mounted on a mass spectrometer chamber (7), one end of the capillary tube (3) penetrates through the sample injection flange (1) and extends into the mass spectrometer chamber (7), the capillary tube sealing joint (2) is arranged along the circumferential direction of the capillary tube (3), one end of the capillary tube sealing joint is arranged between the sample injection flange (1) and the capillary tube (3), and the other end of the capillary tube sealing joint (2) is provided with a heating and heat insulation component along the circumferential direction;
the capillary tube (3) can be changed into different sizes according to the detection requirement.
2. A direct mass spectrometry sample introduction device according to claim 1, wherein the different dimensions comprise capillaries (3) of the same outer diameter and different inner diameters and capillaries (3) of different outer diameters.
3. A mass spectrum direct sampling device according to claim 2, characterized in that when the capillary tubes (3) with the same outer diameter and different inner diameters are replaced, the capillary tubes (3) can be replaced after the heating and heat insulation assembly is disassembled.
4. The direct mass spectrum sample introduction device according to claim 2, wherein when the capillary tubes (3) with different outer diameters are replaced, the capillary tubes (3) with different outer diameters and the capillary tube sealing joints (2) with corresponding sizes can be replaced by sequentially disassembling the heating and heat insulation assembly, the capillary tubes (3) and the capillary tube sealing joints (2).
5. The direct mass spectrum sampling device according to claim 1, wherein the heating and heat insulation assembly comprises a heating and temperature measuring assembly (4) and a heat insulation assembly (5);
the heating temperature measurement component (4) is installed outside the capillary tube (3), and the heat insulation component (5) is arranged along the circumferential direction of the heating temperature measurement component (4) and is connected with the sample feeding flange (1).
6. The direct mass spectrum sampling device according to claim 5, wherein the heating temperature measuring assembly (4) and the heat insulation assembly (5) can be detachably mounted.
7. The direct mass spectrum sampling device according to claim 1, wherein the capillary sealing joint (2) is made of an elastic material.
8. A direct mass spectrometry sample introduction device according to claim 1, wherein the sample introduction flange (1) is sealingly connected to the mass spectrometer chamber (7).
9. A direct mass spectrometry sample introduction device according to claim 5, wherein the heat insulation assembly (5) is provided with a capillary hole, and the capillary (3) extends from the inside of the capillary seal joint (2) to the outside of the heat insulation assembly (5) through the capillary hole.
10. The direct mass spectrum sampling device according to claim 5, wherein a cable port is arranged on the heat insulation assembly (5) for installing a cable (6), and the cable (6) is connected with the heating temperature measurement assembly (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011269871.5A CN112289674A (en) | 2020-11-13 | 2020-11-13 | Mass spectrum direct sample feeding device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011269871.5A CN112289674A (en) | 2020-11-13 | 2020-11-13 | Mass spectrum direct sample feeding device |
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| Publication Number | Publication Date |
|---|---|
| CN112289674A true CN112289674A (en) | 2021-01-29 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011269871.5A Pending CN112289674A (en) | 2020-11-13 | 2020-11-13 | Mass spectrum direct sample feeding device |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5416322A (en) * | 1994-04-21 | 1995-05-16 | International Business Machines Corporation | Interface for linking an atmospheric pressure thermogravimetric analyzer to a low pressure mass spectrometer |
| US5965883A (en) * | 1997-08-25 | 1999-10-12 | California Institute Of Technology | Capillary for electrospray ion source |
| US20020121596A1 (en) * | 2001-03-01 | 2002-09-05 | Science & Engineering Services, Inc. | Capillary ion delivery device and method for mass spectroscopy |
| US6667474B1 (en) * | 2000-10-27 | 2003-12-23 | Thermo Finnigan Llc | Capillary tube assembly with replaceable capillary tube |
| CN206657797U (en) * | 2017-04-17 | 2017-11-21 | 厦门原位科学仪器有限公司 | A kind of high vacuum mass spectrograph sample introduction capillary heating device |
| CN109585255A (en) * | 2018-12-17 | 2019-04-05 | 深圳至秦仪器有限公司 | Sealing device and sample injection apparatus for mass spectrographs |
-
2020
- 2020-11-13 CN CN202011269871.5A patent/CN112289674A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5416322A (en) * | 1994-04-21 | 1995-05-16 | International Business Machines Corporation | Interface for linking an atmospheric pressure thermogravimetric analyzer to a low pressure mass spectrometer |
| US5965883A (en) * | 1997-08-25 | 1999-10-12 | California Institute Of Technology | Capillary for electrospray ion source |
| US6667474B1 (en) * | 2000-10-27 | 2003-12-23 | Thermo Finnigan Llc | Capillary tube assembly with replaceable capillary tube |
| US20020121596A1 (en) * | 2001-03-01 | 2002-09-05 | Science & Engineering Services, Inc. | Capillary ion delivery device and method for mass spectroscopy |
| CN206657797U (en) * | 2017-04-17 | 2017-11-21 | 厦门原位科学仪器有限公司 | A kind of high vacuum mass spectrograph sample introduction capillary heating device |
| CN109585255A (en) * | 2018-12-17 | 2019-04-05 | 深圳至秦仪器有限公司 | Sealing device and sample injection apparatus for mass spectrographs |
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