Mass spectrometry detection system and ion source device
By designing an ion source device including a shell, a focus orifice plate, a spray capillary, a gas circuit assembly and a sample injection assembly, using electrospray technology and auxiliary gas flow, the problem of low sample ionization efficiency in traditional SESI mass spectrometry detection technology is solved, and more efficient sample ionization and detection effect are improved.
Patent Information
- Application Number
- CN202011269264.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2020-11-13
- Publication Date
- 2025-04-01
- Estimated Expiration
- 2040-11-13
AI Technical Summary
Traditional SESI mass spectrometry detection technology has low ionization efficiency on samples, resulting in poor detection results.
An ion source device is designed, including a housing, a focus orifice plate, a spray capillary, a gas circuit assembly and a sample injection assembly. The device forms an electrospray in the ionization chamber through electrospraying technology and uses auxiliary air flow to improve the ionization efficiency and detection effect of the sample.
The ionization efficiency of the sample is improved, the detection effect is improved, and the collision and contamination of the sample in the inner wall of the shell is avoided, background interference is reduced, and the sensitivity of the method is improved.
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Figure CN112309823B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of mass spectrometry detection, and in particular to a mass spectrometry detection system and an ion source device. Background Art
[0002] With the development of mass spectrometry detection technology, electrospray ionization (ESI) and secondary electrospray ionization (SESI) have emerged. Among them, ESI usually dissolves the sample to be detected in a solvent and sprays it in the form of electrospray, so that the sample is ionized to form charged ions. SESI is a new mass spectrometry (MS) ionization technology derived from ESI. Its ionization process can be summarized as follows: a high-purity solution without a sample is formed into charged micro-droplets through ESI. These charged micro-droplets are sprayed and contacted with samples (including gas phase molecules or aerosol particles (solid or liquid)) to ionize the sample to form charged ions. However, the traditional SESI has a low ionization efficiency for samples, resulting in poor sample detection effect. Summary of the invention
[0003] Based on this, it is necessary to overcome the defects of the prior art and provide a mass spectrometry detection system and an ion source device, which can improve the ionization efficiency and ensure the detection effect.
[0004] The technical scheme is as follows: an ion source device, comprising: a shell and a focusing orifice plate, wherein the shell is provided with an ionization chamber, the shell is also provided with an inlet, an outlet and an air inlet communicated with the ionization chamber, the outlet and the air inlet are respectively located at opposite ends of the shell, the focusing orifice plate is connected to the shell, the focusing orifice plate is provided with a through hole, the through hole is communicated with the outlet, and the through hole is also used to communicate with a mass spectrometer inlet of a mass spectrometer; a spray capillary, the spray capillary penetrates the shell and extends into the interior of the ionization chamber, the spray end of the spray capillary faces the through hole and the spray area formed covers the through hole; an air path component, the air path component is provided with a first blowing end, the first blowing end is communicated with the air inlet, and the auxiliary gas of the first blowing end enters the ionization chamber through the air inlet; and an injection component, the output end of the injection component is communicated with the injection port, and the input end of the injection component is used to pass a sample to be tested.
[0005] When the above-mentioned ion source device is working, the sample to be tested (including gas phase molecules or aerosol particles (solid or liquid)) enters the sample injection assembly through the input end of the sample injection assembly, and enters the ionization chamber through the injection port from the output end of the sample injection assembly. The electrospray forms an electrospray through the spray capillary and is sprayed into the ionization chamber. When the electrospray contacts the sample to be tested, the sample to be tested is ionized to form charged ions. At the same time, the auxiliary gas at the first blowing end of the gas path assembly enters the ionization chamber through the air inlet and flows toward the through hole. On the one hand, it can enter the mass spectrometer inlet of the mass spectrometer through the through hole of the focusing orifice plate together with the charged ions, and the mass spectrometer performs mass spectrometry detection and analysis on the charged ions to obtain the components of the sample to be tested; on the other hand, since the auxiliary gas flows from the end of the shell away from the focusing orifice plate to the focusing orifice plate, the auxiliary gas can concentrate the sample to be tested on the side where the focusing orifice plate is located, which can not only avoid the sample to be tested from colliding with the inner wall of the shell and causing pollution, but also play a protective role and improve the ionization efficiency of the sample to be tested. In addition, the spray end of the spray capillary is facing the through hole and the spray area formed covers the through hole, so that as long as the sample to be tested enters the through hole, it will contact the electrospray and send ionization, thereby improving the ionization efficiency of the sample to be tested. In addition, under the action of the focusing orifice plate, charged ions can be focused and enter the mass spectrometer. In this way, the ionization efficiency can be improved and the detection effect can be guaranteed. Secondly, the contact ionization of the electrospray and the sample to be tested is carried out in an ionization chamber with good sealing performance, and the air outside the housing can enter the ion chamber and the mass spectrometer, thereby avoiding the generation of background interference and reducing the sensitivity of the method.
[0006] In one embodiment, the ion source device also includes an ultraviolet lamp and / or a corona discharge needle; when the ion source device includes the ultraviolet lamp, a light-transmitting portion opposite to the spray area is provided on the shell, and the ultraviolet lamp transmits ultraviolet light to the spray area through the light-transmitting portion; when the ion source device includes the corona discharge needle, the corona discharge needle penetrates the shell and extends into the ionization chamber, and the discharge end of the corona discharge needle is located in the spray area.
[0007] In one embodiment, the ion source device further includes a first heating element, and the first heating element is used to heat the shell.
[0008] In one embodiment, there are a plurality of first heating elements, and the plurality of first heating elements are evenly spaced and arranged on the housing.
[0009] In one embodiment, the spray capillary is a fused silica capillary.
[0010] In one embodiment, the shell is also provided with a flow balancing chamber and a flow balancing plate for separating the ionization chamber from the flow balancing chamber, the flow balancing plate is provided with a plurality of flow balancing holes, the flow balancing chamber is connected with the ionization chamber through the flow balancing holes, and the air inlet is provided on the shell wall of the flow balancing chamber and is connected with the flow balancing chamber.
[0011] In one embodiment, the shell further includes a filling block, one side of the filling block is connected to the middle portion of the flow equalizing plate, and the other opposite side of the filling block is connected to the shell, the flow equalizing chamber is an annular chamber circumferentially arranged around the filling block, and the flow equalizing holes are arranged at intervals around the flow equalizing plate.
[0012] In one embodiment, the spray capillary penetrates the shell, the filling block, and the flow equalizing plate and then extends into the ionization chamber, so that the spray capillary is located in the middle of the ionization chamber and the spray end of the spray capillary faces the through hole.
[0013] In one embodiment, the gas path assembly is further provided with a second blowing end, and a gas flow spacer is provided on the side of the focusing orifice plate facing away from the ionization chamber and on the end face of the injection end of the mass spectrometer, the gas flow spacer is connected to the through hole, and the second gas blowing end is connected to the gas flow spacer.
[0014] In one embodiment, the through hole includes a conical section whose aperture gradually increases from the side of the focusing orifice plate facing the ionization chamber to the side away from the ionization chamber, and a straight section connected to the conical section; the through hole can be loaded into the injection end of the mass spectrometer, the hole wall of the conical section is used to form an airflow gap with the end face of the injection end of the mass spectrometer, and the inner wall of the straight section is used to seal with the side wall of the injection end of the mass spectrometer; the gas path assembly is also provided with a second blowing end, and the second blowing end is connected to the airflow gap.
[0015] In one embodiment, the air circuit assembly includes a first air inlet pipe, a second air inlet pipe and a third air inlet pipe, one end of the first air inlet pipe is used to introduce the auxiliary gas, the other end of the first air inlet pipe is respectively connected to one end of the second air inlet pipe and one end of the third air inlet pipe, the other end of the second air inlet pipe is the first blowing end, and the other end of the third air inlet pipe is the second blowing end.
[0016] In one embodiment, a first flow regulating valve and a first filter are provided on the first air intake pipe.
[0017] In one of the embodiments, the gas circuit assembly further includes an exhaust pipe, the other end of the first air inlet pipe is also connected to the exhaust pipe, and a second flow regulating valve is provided on the exhaust pipe.
[0018] In one embodiment, the injection assembly includes a first injection tube and a second injection tube; one end of the first injection tube is used to be connected to the injection port, and the other end of the first injection tube is used to pass the sample to be tested; one end of the second injection tube is used to be connected to the injection port, and the other end of the second injection tube is used to pass the sample to be tested.
[0019] In one embodiment, the injection assembly further includes a second filter and a second heating element, wherein the second filter is used to filter out particles in the sample to be tested that enters the first injection tube, and the second heating element is used to heat the sample to be tested.
[0020] In one embodiment, the injection assembly further includes a third filter, and the third filter is used to filter out volatile organic compounds in the sample to be tested that enters the second injection tube.
[0021] A mass spectrometry detection system comprises the ion source device and a mass spectrometer, wherein a mass spectrometer inlet of the mass spectrometer is connected to the through hole.
[0022] In the above-mentioned mass spectrometry detection system, the sample to be tested (including gas phase molecules or aerosol particles (solid or liquid)) enters the sample injection assembly through the input end of the sample injection assembly, and enters the ionization chamber through the injection port from the output end of the sample injection assembly. The electrospray forms an electrospray through the spray capillary and is sprayed into the ionization chamber. When the electrospray contacts the sample to be tested, the sample to be tested is ionized to form charged ions. At the same time, the auxiliary gas at the first blowing end of the gas path assembly enters the ionization chamber through the air inlet and flows toward the through hole. On the one hand, it can enter the mass spectrometer inlet of the mass spectrometer through the through hole of the focusing orifice plate together with the charged ions, and the mass spectrometer performs mass spectrometry detection and analysis on the charged ions to obtain the components of the sample to be tested; on the other hand, since the auxiliary gas flows from the end of the shell away from the focusing orifice plate to the focusing orifice plate, the auxiliary gas can concentrate the sample to be tested on the side where the focusing orifice plate is located, which can not only avoid the sample to be tested from colliding with the inner wall of the shell and causing pollution, but also play a protective role and improve the ionization efficiency of the sample to be tested. In addition, the spray end of the spray capillary is facing the through hole and the spray area formed covers the through hole, so that as long as the sample to be tested enters the through hole, it will contact the electrospray and send ionization, thereby improving the ionization efficiency of the sample to be tested. In addition, under the action of the focusing orifice plate, charged ions can be focused and enter the mass spectrometer. In this way, the ionization efficiency can be improved and the detection effect can be guaranteed. Secondly, the contact ionization of the electrospray and the sample to be tested is carried out in an ionization chamber with good sealing performance, and the air outside the housing can enter the ion chamber and the mass spectrometer, thereby avoiding the generation of background interference and reducing the sensitivity of the method. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] The drawings constituting a part of this application are used to provide a further understanding of the present invention. The illustrative embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute improper limitations on the present invention.
[0024] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.
[0025] Figure 1 A schematic structural diagram of an ion source device according to an embodiment of the present invention;
[0026] Figure 2 A schematic diagram of the structure of a gas path component of an ion source device according to an embodiment of the present invention;
[0027] Figure 3 is a structural schematic diagram of an ion source device according to another embodiment of the present invention;
[0028] Figure 4 It is a schematic structural diagram of a gas path component of an ion source device according to another embodiment of the present invention.
[0029] 10. Shell; 11. Ionization chamber; 12. Sample inlet; 13. Sample outlet; 14. Air inlet; 15. Flow equalization chamber; 16. Flow equalization plate; 161. Flow equalization hole; 17. Filling block; 20. Focusing orifice plate; 21. Through hole; 211. Conical section; 212. Straight section; 22. Air flow interval; 23. Annular sleeve; 24. Sealing ring; 30. Spray capillary; 31. Spray area; 40. Air path assembly; 41. First blowing end; 42. Second blowing end; 43. First air inlet pipe ; 44. second air inlet pipe; 45. third air inlet pipe; 46. first flow regulating valve; 47. first filter; 48. exhaust pipe; 49. second flow regulating valve; 50. injection assembly; 51. first injection tube; 52. second injection tube; 53. second filter; 54. second heating element; 55. third filter; 60. mass spectrometer; 61. mass spectrometer inlet; 62. injection end; 70. ultraviolet lamp; 80. corona discharge needle; 90. first heating element; 100. charged ions. DETAILED DESCRIPTION
[0030] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific embodiments of the present invention are described in detail below in conjunction with the accompanying drawings. In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without violating the connotation of the present invention, so the present invention is not limited by the specific embodiments disclosed below.
[0031] See also Figure 1 and Figure 2 , Figure 1 The structure diagram of the ion source device according to one embodiment of the present invention is shown. Figure 2 The structure diagram of the gas circuit component 40 of the ion source device according to an embodiment of the present invention is shown. An ion source device provided by an embodiment of the present invention includes a housing 10, a focusing orifice plate 20, a spray capillary 30, a gas circuit component 40 and a sample injection component 50.
[0032] The housing 10 is provided with an ionization chamber 11, and the housing 10 is also provided with an inlet 12, an outlet 13 and an air inlet 14 which are communicated with the ionization chamber 11. The outlet 13 and the air inlet 14 are respectively located at opposite ends of the housing 10. The focusing orifice plate 20 is connected to the housing 10, and the focusing orifice plate 20 is provided with a through hole 21. The through hole 21 is communicated with the outlet 13, and the through hole 21 is also used to communicate with the mass spectrometer inlet 61 of the mass spectrometer 60. The spray capillary 30 penetrates the housing 10 and extends into the interior of the ionization chamber 11, and the spray end of the spray capillary 30 faces the through hole 21 and the spray area 31 formed covers the through hole 21. The gas circuit component 40 is provided with a first blowing end 41, and the first blowing end 41 is communicated with the air inlet 14, and the auxiliary gas of the first blowing end 41 enters the ionization chamber 11 through the air inlet 14. The output end of the sample injection component 50 is connected to the sample injection port 12, and the input end of the sample injection component 50 is used to introduce the sample to be tested.
[0033] When the above-mentioned ion source device is in operation, the sample to be tested (including gas phase molecules or aerosol particles (solid or liquid)) enters the sample injection assembly 50 through the input end of the sample injection assembly 50, and enters the ionization chamber 11 through the injection port 12 from the output end of the sample injection assembly 50. The electrospray forms an electrospray through the spray capillary 30 and is sprayed into the ionization chamber 11. When the electrospray contacts the sample to be tested, the sample to be tested is ionized to form charged ions 100. At the same time, the auxiliary gas of the first blowing end 41 of the gas path assembly 40 enters the ionization chamber 11 through the gas inlet 14 and flows toward the through hole 14. 21 flows, on the one hand, it can enter the mass spectrometer entrance 61 of the mass spectrometer 60 through the through hole 21 of the focusing orifice plate 20 together with the charged ions 100, and the mass spectrometer 60 performs mass spectrometry detection and analysis on the charged ions 100 to obtain the components of the sample to be tested; on the other hand, since the auxiliary gas flows from the end of the housing 10 away from the focusing orifice plate 20 to the focusing orifice plate 20, the auxiliary gas can concentrate the sample to be tested on the side where the focusing orifice plate 20 is located, which can not only prevent the sample to be tested from colliding with the inner wall of the housing 10 and causing pollution, but also play a protective role and improve the ionization efficiency of the sample to be tested. In addition, the spray end of the spray capillary 30 faces the through hole 21 and the spray area 31 formed covers the through hole 21, so that as long as the sample to be tested enters the through hole 21, it will contact the electrospray and send ionization, thereby improving the ionization efficiency of the sample to be tested. In addition, under the action of the focusing orifice plate 20, the charged ions 100 can be focused and enter the mass spectrometer 60. In this way, the ionization efficiency can be improved and the detection effect can be guaranteed. Secondly, the contact ionization of the electrospray and the sample to be tested is carried out in the ionization chamber 11 with good sealing performance, so that the air outside the housing 10 can enter the ion chamber and the mass spectrometer 60, thereby avoiding the generation of background interference and reducing the sensitivity of the method.
[0034] It should be noted that the auxiliary gas is specifically, for example, nitrogen, helium, hydrogen or other inert gases that do not participate in chemical reactions, which are not limited here and are set according to actual needs.
[0035] See also Figure 1 and Figure 2Further, the ion source device also includes an ultraviolet lamp 70 and / or a corona discharge needle 80. When the ion source device includes the ultraviolet lamp 70, a light-transmitting portion opposite to the spray area 31 is provided on the shell 10, and the ultraviolet lamp 70 injects ultraviolet light into the spray area 31 through the light-transmitting portion; when the ion source device includes the corona discharge needle 80, the corona discharge needle 80 penetrates the shell 10 and extends into the ionization chamber 11, and the discharge end of the corona discharge needle 80 is located in the spray area 31. In this way, the ultraviolet light emitted by the ultraviolet lamp 70 is incident on the spray area 31, and / or the discharge end of the corona discharge needle 80 discharges in the spray area 31, both of which can enhance the ionization ability so that weak polar substances or non-polar substances (low-level substances such as alkane substances) can be ionized, so that it can not only be used to ionize polar substances, but also weak polar or non-polar substances, the types of substances that can be ionized are increased, and product performance is improved.
[0036] It should be noted that the ultraviolet lamp 70 and the corona discharge needle 80 can be replaced and combined with other ionization devices according to actual needs. Other ionization devices include, but are not limited to, normal pressure ionization ionization devices such as flow afterglow discharger (FA-APGD), low temperature plasma (LTP), and microwave plasma torch (MPT), all of which can enhance the analytical ionization capability of the ion source device for the chemical components in the sample to be tested.
[0037] It should also be noted that the spray capillary 30 , the ultraviolet lamp 70 , the corona discharge needle 80 and the injection port 12 can be changed and adjusted according to actual needs, and no limitation is made here.
[0038] See also Figure 1 and Figure 2 In one embodiment, the ion source device further includes a first heating element 90. The first heating element 90 is used to heat the shell 10. In this way, the first heating element 90 heats the shell 10 when working, so that the temperature of the sample to be tested in the shell 10 is maintained in a preset temperature range (for example, 85°C-95°C), so that the water vapor carried by the sample to be tested entering the ionization chamber 11 will not condense on the wall of the ionization chamber 11, and the sample to be tested is prevented from adhering to the wall of the ionization chamber 11, thereby ensuring the cleanliness of the wall of the ionization chamber 11, and avoiding cross contamination caused by residues on the wall of the ionization chamber 11 during different tests.
[0039] See also Figure 1 and Figure 2In one embodiment, there are multiple first heating elements 90, and the multiple first heating elements 90 are evenly spaced and arranged on the shell 10. In this way, when the multiple first heating elements 90 perform heating work, it can be achieved that each part of the shell 10 is heated more evenly, and the temperature of each part of the ionization chamber 11 can be uniform, so as to avoid condensation of water vapor on the wall of the ionization chamber 11 and avoid adhesion of the sample to be tested on the wall of the ionization chamber 11, thereby ensuring the cleanliness of the wall of the ionization chamber 11. Specifically, the first heating element 90 can be a heating wire, a heating rod, or a heating plate attached to the outer wall of the shell 10, etc., which is not limited here.
[0040] See also Figure 1 and Figure 2 In one embodiment, the spray capillary 30 is a fused silica capillary. In this way, the electrospray solvent passes through the fused silica capillary to form a nanoliter electrospray, and the flow rate of the nanoliter electrospray is small, and the effect on the gas velocity flow field can be ignored, so that the interaction between the primary electrospray and the sample gas flow is not disturbed, and the ionization efficiency can be guaranteed. At the same time, the undesirable phenomenon that the sample gas flow is disturbed and causes the sample gas flow to collide and remain on the wall of the ionization chamber 11 can be avoided.
[0041] It should be noted that the electrospray generated by the conventional ESI method usually has a flow rate of 5 ml / min, and the flow rate in the electrospray region 31 is relatively high, which will have a relatively large interference effect on the airflow. However, the inner diameter of the fused silica capillary in this embodiment is usually 20 μm-50 μm, and the flow rate generated is usually 100 nL / min, and the flow rate is negligible, which will not interfere with the airflow.
[0042] It should be noted that fused quartz is an amorphous state of silicon oxide, a type of glass, not a molten state. Fused quartz is a substance that is made by melting natural high-purity silicon dioxide in an electric furnace at a temperature above 1760°C and then rapidly cooling it to form a glassy substance.
[0043] See also Figure 1 and Figure 2 In one embodiment, the housing 10 is further provided with a flow equalizing chamber 15 and a flow equalizing plate 16 for separating the ionization chamber 11 from the flow equalizing chamber 15. The flow equalizing plate 16 is provided with a plurality of flow equalizing holes 161, and the flow equalizing chamber 15 is connected to the ionization chamber 11 through the flow equalizing holes 161. The air inlet 14 is provided on the shell wall of the flow equalizing chamber 15 and is connected to the flow equalizing chamber 15. In this way, the auxiliary gas of the first blowing end 41 first enters the flow equalizing chamber 15 through the air inlet 14, and then enters the ionization chamber 11 through the flow equalizing holes 161 after being equalized in the flow equalizing chamber 15, so that the gas entering the ionization chamber 11 is more uniform, which is conducive to pushing the sample to be tested to the spray area 31.
[0044] See also Figure 1 and Figure 2In one embodiment, the shell 10 further includes a filling block 17. One side of the filling block 17 is connected to the middle portion of the flow equalizing plate 16, and the other opposite side of the filling block 17 is connected to the shell 10. The flow equalizing chamber 15 is an annular chamber circumferentially arranged around the filling block 17. The flow equalizing holes 161 are arranged at intervals around the flow equalizing plate 16. In this way, the auxiliary gas entering the ionization chamber 11 from the flow equalizing chamber 15 can better prevent the sample to be tested from flowing toward the wall of the ionization chamber 11, so as to prevent the sample to be tested from colliding with the inner wall of the ionization chamber 11 and causing contamination, thereby playing a protective role and improving the ionization efficiency of the sample to be tested.
[0045] In one embodiment, the spray capillary 30 passes through the shell 10 , the filling block 17 , and the flow equalizing plate 16 and then extends into the ionization chamber 11 , so that the spray capillary 30 is located in the middle of the ionization chamber 11 and the spray end of the spray capillary 30 faces the through hole 21 .
[0046] See also Figure 3 and Figure 4 , Figure 3 FIG. 1 is a schematic diagram showing the structure of an ion source device according to another embodiment of the present invention. Figure 4 The schematic diagram of the structure of the gas circuit component 40 of the ion source device of another embodiment of the present invention is illustrated. In one embodiment, the gas circuit component 40 is also provided with a second blowing end 42, and the side of the focusing orifice plate 20 facing away from the ionization chamber 11 and the end face of the injection end 62 of the mass spectrometer 60 are provided with a gas flow interval 22, the gas flow interval 22 is communicated with the through hole 21, and the second blowing end 42 is communicated with the gas flow interval 22. Among them, the mass spectrometer inlet 61 of the mass spectrometer 60 is arranged on the injection end 62 of the mass spectrometer 60. The second blowing end 42 delivers the auxiliary gas into the gas flow interval 22, and the auxiliary gas is drawn into the inside of the mass spectrometer 60 along the gas flow interval 22 by the mass spectrometer 60. Among them, when the auxiliary gas enters the inside of the mass spectrometer 60 through the mass spectrometer inlet 61 together with the charged ions 100 at the through hole 21, the auxiliary gas can avoid the collision of the sample ions and remain on the mouth wall of the mass spectrometer inlet 61.
[0047] See also Figure 3 and Figure 4In order to ensure the sealing performance, the gas path component 40 also includes an annular sleeve 23, which is sleeved on the outside of the injection end 62. The inner wall of one end of the annular sleeve 23 and the outer wall of the injection end 62 are sealed by a sealing ring 24. The other end face of the annular sleeve 23 is sealed and fitted to the side of the focusing hole plate 20 away from the ionization chamber 11, and the annular sleeve 23 is wrapped around the periphery of the through hole 21, so as to avoid the external environment of the auxiliary air flow channel, and also to avoid the external air from entering the mass spectrometer 60 through the air flow interval 22. In this way, the sealing is better and the detection effect is guaranteed. The contact ionization of the electrospray and the sample to be tested is carried out in the ionization chamber 11 with better sealing, and the air outside the shell 10 can enter the ion chamber and the mass spectrometer 60, so as to avoid the background interference and reduce the sensitivity of the method.
[0048] See also Figure 1 and Figure 2 In one embodiment, the through hole 21 includes a tapered section 211 whose aperture gradually increases from the side of the focusing orifice plate 20 facing the ionization chamber 11 to the side away from the ionization chamber 11, and a straight section 212 connected to the tapered section 211. The through hole 21 can be loaded into the injection end 62 of the mass spectrometer 60, the hole wall of the tapered section 211 is used to form an airflow interval 22 with the end face of the injection end 62 of the mass spectrometer 60, and the inner wall of the straight section 212 is used to seal with the side wall of the injection end 62 of the mass spectrometer 60. The gas path assembly 40 is also provided with a second blowing end 42, and the second blowing end 42 is connected to the airflow interval 22. Specifically, the second blowing end 42 passes through the focusing orifice plate 20 and is connected to the airflow interval 22. In this way, the end of the conical section 211 with a smaller diameter is formed on the side of the focusing orifice plate 20 facing the ionization chamber 11, so that the diameter of the opening on the side of the focusing orifice plate 20 facing the ionization chamber 11 is smaller, which can play a focusing role; in addition, the hole wall of the conical section 211 gradually increases, and can cooperate with the end face of the injection end 62 of the mass spectrometer 60 to form an airflow gap 22, and the end of the conical section 211 with a larger aperture is connected to the straight section 212, and the straight section 212 is sealed with the side wall of the injection end 62, and the overall airtightness is good.
[0049] In one embodiment, the shape of the through hole 21 can be designed according to the shape of the end face of the injection end 62 of the mass spectrometer 60. When the end face of the injection end 62 of the mass spectrometer 60 is not a conical surface, the through hole 21 does not need to be designed with a conical section 211, but can be set as two straight sections 212 that are interconnected, for example, wherein the aperture of one straight section 212 is relatively small, and the aperture of the other straight section 212 is relatively large and is used to seal with the side wall of the injection end 62.
[0050] In one embodiment, the number of focusing orifice plates 20 is at least one, and additional focusing orifice plates 20 may be provided according to actual needs, and the specific number is not limited here. Optionally, electrodes may be provided on the focusing orifice plate 20, or electrodes may not be provided, that is, according to actual needs, the focusing orifice plate 20 may be replaced with an electrode. When the focusing orifice plate 20 is provided with electrodes, the provided electrodes make the focusing effect of the focusing orifice plate 20 better, and can focus the charged sample ions so that the charged ions 100 enter the mass spectrometer inlet 61, thereby preventing the sample ions from colliding or adsorbing on the wall and causing losses.
[0051] See also Figure 1 and Figure 2 In one embodiment, the gas circuit assembly 40 includes a first air inlet pipe 43, a second air inlet pipe 44 and a third air inlet pipe 45. One end of the first air inlet pipe 43 is used to introduce auxiliary gas, and the other end of the first air inlet pipe 43 is respectively connected to one end of the second air inlet pipe 44 and one end of the third air inlet pipe 45, the other end of the second air inlet pipe 44 is a first blowing end 41, and the other end of the third air inlet pipe 45 is a second blowing end 42.
[0052] See also Figure 1 and Figure 2 Furthermore, the first air inlet pipe 43 is provided with a first flow regulating valve 46 and a first filter 47. Specifically, the first filter 47 may be, for example, an activated carbon filter for filtering out volatile organic matter, or other filters, which are not limited here. The auxiliary gas flow rate entering the first air inlet pipe 43 may be controlled by the first flow regulating valve 46, so that the auxiliary gas flow rate entering the first air inlet pipe 43 is within a preset range.
[0053] See also Figure 1 and Figure 2 Furthermore, the gas circuit assembly 40 further includes an exhaust pipe 48. The other end of the first air inlet pipe 43 is also connected to the exhaust pipe 48, and the exhaust pipe 48 is provided with a second flow regulating valve 49.
[0054] See also Figure 1 and Figure 2Further, the injection assembly 50 includes a first injection tube 51 and a second injection tube 52. One end of the first injection tube 51 is used to communicate with the injection port 12, and the other end of the first injection tube 51 is used to pass the sample to be tested. One end of the second injection tube 52 is used to communicate with the injection port 12, and the other end of the second injection tube 52 is used to pass the sample to be tested. In this way, when the first injection tube 51 is turned on, the sample to be tested, which is a gas, is passed into the injection port 12 and sent to the ionization chamber 11 through the first injection tube 51, and the second injection tube 52 is in a closed state, that is, the gas detection and analysis work is performed; when the second injection tube 52 is in an open state, the sample to be tested, which is an aerosol particle, is passed into the injection port 12 and sent to the ionization chamber 11 through the second injection tube 52, and the first injection tube 51 is in a closed state, that is, the aerosol particle detection and analysis work is performed.
[0055] It should be noted that the first injection tube 51 and the second injection tube 52 are both connected to the injection port 12 via a three-way tube, or the first injection tube 51 is connected to the second injection tube 52, and then the second injection tube 52 is connected to the injection port 12, which is not limited here.
[0056] See also Figure 1 and Figure 2 Furthermore, the sample injection assembly 50 further includes a second filter 53 and a second heating element 54. The second filter 53 is used to filter out particles in the sample to be tested that enters the first sample injection tube 51, and the second heating element 54 is used to heat the sample to be tested.
[0057] Specifically, the second filter 53 is, for example, a particle filter. When the sample to be tested entering the first sample inlet tube 51 is gas, the particles contained in the gas can be completely filtered out, thereby improving the detection effect.
[0058] See also Figure 1 and Figure 2 Furthermore, the sampling assembly 50 further includes a third filter 55. The third filter 55 is used to filter out volatile organic matter in the sample to be tested that enters the second sampling tube 52. Specifically, the third filter 55 is, for example, an activated carbon filter, and when the sample to be tested that enters the second sampling tube 52 is an aerosol particle, the volatile organic matter in the sample to be tested can be filtered out.
[0059] Furthermore, in order to prevent the water vapor contained in the sample to be tested from condensing on the inner wall of the first injection tube 51 or the second injection tube 52, a third heating element is arranged around the tube wall of the first injection tube 51 or the second injection tube 52. The third heating element heats the first injection tube 51 or the second injection tube 52 to maintain the first injection tube 51 or the second injection tube 52 within a preset temperature range, thereby preventing the water vapor contained in the sample to be tested from condensing on the inner wall of the first injection tube 51 or the second injection tube 52.
[0060] See also Figure 1 and Figure 2 In one embodiment, a mass spectrometry detection system includes the ion source device of any of the above embodiments, and also includes a mass spectrometer 60. A mass spectrometer inlet 61 of the mass spectrometer 60 is connected to the through hole 21.
[0061] In the mass spectrometry detection system, the sample to be tested (including gas phase molecules or aerosol particles (solid or liquid)) enters the sample injection assembly 50 through the input end of the sample injection assembly 50, and enters the ionization chamber 11 through the injection port 12 from the output end of the sample injection assembly 50. The electrospray forms an electrospray through the spray capillary 30 and is sprayed into the ionization chamber 11. When the electrospray contacts the sample to be tested, the sample to be tested is ionized to form charged ions 100. At the same time, the auxiliary gas of the first blowing end 41 of the gas circuit assembly 40 enters the ionization chamber 11 through the gas inlet 14 and flows toward the through hole 2. 1 flows, on the one hand, it can enter the mass spectrometer entrance 61 of the mass spectrometer 60 through the through hole 21 of the focusing orifice plate 20 together with the charged ions 100, and the mass spectrometer 60 performs mass spectrometry detection and analysis on the charged ions 100 to obtain the components of the sample to be tested; on the other hand, since the auxiliary gas flows from the end of the housing 10 away from the focusing orifice plate 20 to the focusing orifice plate 20, the auxiliary gas can concentrate the sample to be tested on the side where the focusing orifice plate 20 is located, which can not only prevent the sample to be tested from colliding with the inner wall of the housing 10 and causing pollution, but also play a protective role and improve the ionization efficiency of the sample to be tested. In addition, the spray end of the spray capillary 30 faces the through hole 21 and the spray area 31 formed covers the through hole 21, so that as long as the sample to be tested enters the through hole 21, it will contact the electrospray and send ionization, thereby improving the ionization efficiency of the sample to be tested. In addition, under the action of the focusing orifice plate 20, the charged ions 100 can be focused and enter the mass spectrometer 60. In this way, the ionization efficiency can be improved and the detection effect can be guaranteed. Secondly, the contact ionization of the electrospray and the sample to be tested is carried out in the ionization chamber 11 with good sealing performance, so that the air outside the housing 10 can enter the ion chamber and the mass spectrometer 60, thereby avoiding the generation of background interference and reducing the sensitivity of the method.
[0062] The technical features of the above embodiments may be combined arbitrarily. To make the description concise, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.
[0063] The above embodiments only express several implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for those of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.
[0064] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.
[0065] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features. In the description of the present invention, the meaning of "plurality" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined.
[0066] In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements, unless otherwise clearly defined. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0067] In the present invention, unless otherwise clearly specified and limited, a first feature being "above" or "below" a second feature may mean that the first and second features are in direct contact, or the first and second features are in indirect contact through an intermediate medium. Moreover, a first feature being "above", "above" or "above" a second feature may mean that the first feature is directly above or obliquely above the second feature, or simply means that the first feature is higher in level than the second feature. A first feature being "below", "below" or "below" a second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature is lower in level than the second feature.
[0068] It should be noted that when an element is referred to as being "fixed to" or "disposed on" another element, it may be directly on the other element or there may be a central element. When an element is considered to be "connected to" another element, it may be directly connected to the other element or there may be a central element at the same time. The terms "vertical", "horizontal", "upper", "lower", "left", "right" and similar expressions used herein are for illustrative purposes only and are not intended to be the only implementation method.
Claims
1. An ion source device, characterized in that: The ion source device comprises: A shell and a focusing orifice plate, wherein the shell is provided with an ionization chamber, and the shell is also provided with an inlet, an outlet and an air inlet communicated with the ionization chamber, the outlet and the air inlet are respectively located at opposite ends of the shell, the focusing orifice plate is connected to the shell, the focusing orifice plate is provided with a through hole, the through hole is communicated with the outlet, and the through hole is also used to communicate with a mass spectrometer inlet of a mass spectrometer; A spray capillary, the spray capillary passes through the shell and extends into the interior of the ionization chamber, the spray end of the spray capillary faces the through hole and the formed spray area covers the through hole; An air circuit component, wherein the air circuit component is provided with a first air blowing end, the first air blowing end is connected to the air inlet, and the auxiliary gas of the first air blowing end enters the ionization chamber through the air inlet; and An injection assembly, the output end of which is connected to the injection port, and the input end of which is used to introduce a sample to be tested; The shell is also provided with a flow equalizing chamber and a flow equalizing plate for separating the ionization chamber from the flow equalizing chamber, the flow equalizing plate is provided with a plurality of flow equalizing holes, the flow equalizing chamber is connected with the ionization chamber through the flow equalizing holes, the air inlet is arranged on the shell wall of the flow equalizing chamber and is connected with the flow equalizing chamber; the shell also includes a filling block, one side of the filling block is connected with the middle part of the flow equalizing plate, and the other opposite side of the filling block is connected with the shell, the flow equalizing chamber is an annular chamber arranged circumferentially around the filling block; the spray capillary penetrates the shell, the filling block and the flow equalizing plate and then extends into the ionization chamber, and the spray capillary is located in the middle part of the ionization chamber.
2. The ion source device according to claim 1, characterized in that: The ion source device also includes an ultraviolet lamp and / or a corona discharge needle; when the ion source device includes the ultraviolet lamp, a light-transmitting portion opposite to the spray area is provided on the shell, and the ultraviolet lamp injects ultraviolet light into the spray area through the light-transmitting portion; when the ion source device includes the corona discharge needle, the corona discharge needle penetrates the shell and extends into the ionization chamber, and the discharge end of the corona discharge needle is located in the spray area.
3. The ion source device according to claim 1, characterized in that: The ion source device further includes a first heating element, and the first heating element is used to heat the shell.
4. The ion source device according to claim 3, characterized in that: There are a plurality of first heating elements, and the plurality of first heating elements are evenly spaced and arranged on the shell.
5. The ion source device according to claim 1, characterized in that: The spray capillary is a fused silica capillary.
6. The ion source device according to claim 1, characterized in that: The flow balancing holes are arranged at intervals around the flow balancing plate.
7. The ion source device according to claim 1, characterized in that: The gas path component is also provided with a second blowing end, and the side of the focusing hole plate facing away from the ionization chamber and the end face of the injection end of the mass spectrometer are provided with an airflow gap, the airflow gap is connected to the through hole, and the second blowing end is connected to the airflow gap.
8. The ion source device according to claim 1, characterized in that: The through hole comprises a conical section whose aperture gradually increases from the side of the focusing orifice plate facing the ionization chamber to the side away from the ionization chamber, and a straight section connected to the conical section; the through hole can be loaded into the injection end of the mass spectrometer, the hole wall of the conical section is used to form an airflow gap with the end face of the injection end of the mass spectrometer, and the inner wall of the straight section is used to seal with the side wall of the injection end of the mass spectrometer; the gas path assembly is also provided with a second blowing end, and the second blowing end is connected to the airflow gap.
9. The ion source device according to claim 7 or 8, characterized in that: The air circuit assembly includes a first air inlet pipe, a second air inlet pipe and a third air inlet pipe. One end of the first air inlet pipe is used to introduce the auxiliary gas, and the other end of the first air inlet pipe is respectively connected to one end of the second air inlet pipe and one end of the third air inlet pipe. The other end of the second air inlet pipe is the first blowing end, and the other end of the third air inlet pipe is the second blowing end.
10. The ion source device according to claim 9, characterized in that: The first air inlet pipe is provided with a first flow regulating valve and a first filter.
11. The ion source device according to claim 9, characterized in that: The gas circuit assembly also includes an exhaust pipe, the other end of the first air inlet pipe is also connected to the exhaust pipe, and a second flow regulating valve is provided on the exhaust pipe.
12. The ion source device according to claim 1, characterized in that: The injection assembly includes a first injection tube and a second injection tube; one end of the first injection tube is used to be connected to the injection port, and the other end of the first injection tube is used to pass the sample to be tested; one end of the second injection tube is used to be connected to the injection port, and the other end of the second injection tube is used to pass the sample to be tested.
13. The ion source device according to claim 12, characterized in that: The injection assembly further includes a second filter and a second heating element. The second filter is used to filter out particles in the sample to be tested that enters the first injection tube, and the second heating element is used to heat the sample to be tested.
14. The ion source device according to claim 12, characterized in that: The sampling assembly further comprises a third filter, and the third filter is used to filter out volatile organic matter in the sample to be tested that enters into the second sampling tube.
15. A mass spectrometry detection system, characterized in that: The mass spectrometry detection system comprises the ion source device according to any one of claims 1 to 14, and further comprises a mass spectrometer, wherein a mass spectrometer inlet of the mass spectrometer is connected to the through hole.
Citation Information
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