CN220474569U - Mass spectrum real-time sampling device based on double capillaries - Google Patents
Mass spectrum real-time sampling device based on double capillaries Download PDFInfo
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- CN220474569U CN220474569U CN202322016836.8U CN202322016836U CN220474569U CN 220474569 U CN220474569 U CN 220474569U CN 202322016836 U CN202322016836 U CN 202322016836U CN 220474569 U CN220474569 U CN 220474569U
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- 238000005070 sampling Methods 0.000 title claims description 23
- 238000001819 mass spectrum Methods 0.000 title claims description 13
- 238000002347 injection Methods 0.000 claims abstract description 48
- 239000007924 injection Substances 0.000 claims abstract description 48
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 20
- 230000001105 regulatory effect Effects 0.000 claims abstract description 16
- 238000007789 sealing Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims description 6
- 230000009977 dual effect Effects 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 14
- 230000008859 change Effects 0.000 abstract description 9
- 230000007613 environmental effect Effects 0.000 abstract description 8
- 238000004458 analytical method Methods 0.000 abstract description 7
- 238000012423 maintenance Methods 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000000605 extraction Methods 0.000 abstract description 5
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- 230000008569 process Effects 0.000 description 9
- 238000001514 detection method Methods 0.000 description 7
- 238000009776 industrial production Methods 0.000 description 6
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- 239000012535 impurity Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
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- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The utility model discloses a dual-capillary-based mass spectrometry real-time sample injection device, which comprises a pressure buffer cavity, wherein the pressure buffer cavity adopts a four-way interface, the lower interface of the pressure buffer cavity is connected with a vacuum pump, the left interface of the pressure buffer cavity is connected with a sample injection tee joint through a sample capillary, the sample injection tee joint is respectively connected with a sample injection port and a sample pump, and the right interface of the pressure buffer cavity is connected with a mass spectrometer through a mass spectrometry capillary. According to the utility model, two-stage capillaries are adopted to carry out rapid sample injection on gas, and the aperture of the air extraction pipeline is changed through the regulating valve, so that the pressure between the two capillaries is maintained, and the influence of environmental pressure change on a quantitative result is reduced. The device is combined with a high-performance mass spectrometer, so that real-time sample injection and analysis of gases with different concentrations can be realized in a complex industrial environment, and the sealing valve can be used for realizing rapid maintenance of the sample injection device and conversion between the sample injection device and a chromatographic module.
Description
Technical Field
The utility model belongs to the technical field of sample injection devices for industrial production on-line detection, and particularly relates to a mass spectrum real-time sample injection device based on double capillaries.
Background
With the development of social industrialization, the quality of products, the running condition of devices and environmental effects brought by industrial processes are receiving more and more attention. The reaction process is monitored according to the gas released in the industrial production process, so as to optimize the production link, improve the quality and quantity of the product, save the resources and reduce the energy consumption. Therefore, the online instrument and meter has become an indispensable measurement and control tool in the production operation of the modern industry.
The process mass spectrometer is an instrument which is arranged on site and is used for carrying out qualitative and quantitative analysis on gas by utilizing a mass spectrometry, and separation analysis is realized by utilizing the motion rule of charged particles in a magnetic field or an electric field. The process mass spectrometer can realize real-time, multi-point and multi-component detection, and has the characteristics of high automation degree, wide measurement range, high analysis speed, high instrument stability, good reliability and the like compared with the traditional detection means, and is frequently used for industrial process gas detection.
The sample injection modes generally adopted by mass spectrometers in the process of online monitoring of industrial production at present are as follows: capillary direct sample injection, membrane sample injection and chromatographic sample injection.
The capillary tube direct sampling mode has a simple structure, but because the capillary tube direct sampling mode directly communicates the external environment with the mass spectrometer, the sampling amount can be influenced by the environmental pressure and the sample types, so when the working environment or the components to be detected change, the stability of the internal environment of the mass spectrometer is difficult to ensure, and dust and liquid drop impurities in the sample easily enter the inside of the mass spectrometer, thereby causing damage. The membrane sample injection mode has stronger anti-interference capability, is suitable for high-pressure and liquid sample injection, but due to the selective permeability of the membrane, the applicable sample types are fewer, and the membrane is not suitable for complex industrial environment monitoring. The chromatographic sample injection mode has excellent separation capability, but has larger volume and long sample injection period, cannot reflect the real-time state of the gas to be detected, and is not suitable for portable and real-time detection in industrial production.
In order to realize real-time monitoring and control of industrial production processes, it is required that an online process mass spectrometer can respond rapidly to a variety of samples. Therefore, the current common capillary direct sample injection, membrane sample injection and chromatographic sample injection can not meet the sample injection requirement of an online mass spectrometer on industrial production monitoring.
Disclosure of Invention
The utility model aims to provide the real-time sample injection device which can be used for rapidly injecting various samples and ensuring the stability of the internal environment of a mass spectrometer instrument, thereby ensuring the analysis performance of the instrument and improving the applicability of the instrument.
In order to achieve the above purpose, the present utility model adopts the following technical scheme:
the utility model provides a mass spectrum real-time sampling device based on double capillary, includes pressure buffer chamber, pressure buffer chamber adopts the cross interface, the lower interface connection vacuum pump in pressure buffer chamber, the left interface in pressure buffer chamber passes through sample capillary and connects the tee bend that advances, advance the tee bend and connect sample inlet and sampling pump respectively, the right interface in pressure buffer chamber passes through mass spectrum capillary and connects the mass spectrometer.
Preferably, the sampling tee is connected with a sampling pump through a shunt port.
Preferably, the mass spectrometry capillary is connected to the mass spectrometer by a sealing valve.
Preferably, the left interface and the right interface of the pressure buffer cavity are respectively connected with the sample capillary and the mass spectrum capillary through rubber pads.
Preferably, the sample capillary is connected with the sample feeding tee joint through a filtering device.
Preferably, the upper interface of the pressure buffer cavity is connected with a vacuum gauge; the lower interface of the pressure buffer cavity is connected with a vacuum pump through a regulating valve, and the vacuum gauge is connected with the regulating valve through a signal.
Preferably, the pore diameters of the sample capillary and the mass spectrum capillary are 0.1-0.3mm.
Compared with the prior art, the utility model has the following beneficial effects:
the utility model can rapidly respond to various samples by taking the two-stage capillary as a sample injection mode of the process mass spectrum. The pressure change of the environment is monitored through the vacuum gauge, and the aperture of the air extraction pipeline is changed by utilizing the regulating valve, so that the environmental pressure of the instrument sample inlet is maintained. The interference caused by impurities in the environment is reduced through the filtering device, so that the influence of environmental change on the detection result of the instrument is reduced. The device combines with a high-performance mass spectrometer, can realize real-time sample injection and analysis of gases with different concentrations in a complex industrial environment, and can also realize rapid maintenance of a sample injection device and conversion between the sample injection device and a chromatographic module by utilizing a sealing valve. The device can rapidly maintain the components, can be rapidly converted into the chromatographic sample injection device, has low cost, short maintenance time and strong stability, and greatly improves the flexibility and the application range of the process mass spectrometer.
Drawings
FIG. 1 is a schematic diagram of a dual capillary-based mass spectrometry real-time sample injection device according to the present utility model;
fig. 2 is a schematic cross-sectional structure diagram of a dual-capillary-based mass spectrometry real-time sample injection device according to the present utility model.
The numbers in the figure are as follows:
1. a sample inlet; 2. sampling tee joint; 3. a shunt port; 4. a filtering device; 5. a sample capillary; 6. a pressure buffer chamber; 7. a vacuum gauge; 8. a regulating valve; 9. a vacuum pump; 10. a mass spectrometry capillary; 11. a sealing valve; 12. a mass spectrometer.
Detailed Description
The following description of the embodiments of the present utility model will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present utility model, but not all embodiments.
As shown in fig. 1 and fig. 2, the utility model provides a dual-capillary-based mass spectrometry real-time sample injection device, which comprises a pressure buffer cavity 6, wherein the pressure buffer cavity 6 adopts a four-way interface, a lower interface of the pressure buffer cavity 6 is connected with a vacuum pump 9, a left interface of the pressure buffer cavity 6 is connected with a sample injection tee joint 2 through a sample capillary 5, the sample injection tee joint 2 is respectively connected with a sample injection port 1 and a shunt port 3, the shunt port 3 is connected with a sampling pump, and a right interface of the pressure buffer cavity 6 is connected with a mass spectrometer 12 through a mass spectrometry capillary 10.
Further, the mass spectrometry capillary 10 of the present utility model is connected to a mass spectrometer 12 through a sealing valve 11. When the ambient pressure changes too much, the sealing valve 11 may be closed and the sample capillary 5 of a different length may be replaced to further maintain the pressure inside the pressure buffer chamber 6.
Further, the left interface and the right interface of the pressure buffer chamber 6 are respectively connected with the sample capillary 5 and the mass spectrum capillary 10 through rubber pads.
Further, a sample capillary 5 of the present utility model is connected to the sample tee 2 via a filter device 4. The interference caused by impurities in the environment is reduced by the filtering device 4, so that the influence of environmental changes on the detection result of the instrument is reduced.
Further, the upper interface of the pressure buffer cavity 6 is connected with a vacuum gauge 7; the lower interface of the pressure buffer cavity 6 is connected with a vacuum pump 9 through a regulating valve 8, and the vacuum gauge 7 is connected with the regulating valve 8 through a signal. The vacuum gauge 7 can detect the pressure change in the pressure buffer cavity 6 and feed back to the regulating valve 8 in a signal mode and the like, and the pipe diameter of an air extraction flow path between the vacuum pump 9 and the pressure buffer cavity 6 is changed through the regulating valve 8, so that the pressure in the pressure buffer cavity 6 is ensured to be in a relatively stable state.
Further, the aperture of the sample capillary 5 and the mass spectrometry capillary 10 of the present utility model is 0.1 to 0.3mm.
The working principle of the utility model is as follows:
when the sample injection device works, a sample to be detected is connected to the sample injection port 1, a sampling pump is connected to the shunt port 3, and the vacuum gauge 7, the vacuum pump 9 and the sealing valve 11 are opened, so that a pressure gradient is formed between the sample injection port 1 and the mass spectrometer 12 due to the fact that the inside of the mass spectrometer 12 is in a high vacuum environment.
During sample injection, sample gas enters the sample injection tee joint 2 from the sample injection port 1, most of the sample gas flows out from the shunt port 3 under the action of the sampling pump, and the small part of the sample gas enters the filter device 4 under the action of the pressure gradient, so that the filter device 4 can prevent substances such as liquid drops and dust doped in the sample gas from entering the pipeline, and avoid blocking capillaries and damaging the instrument. After passing through the filter device 4, the sample gas flow enters the pressure buffer chamber 6 through the sample capillary 5 under the action of the pressure gradient. Most of the sample gas flows through the regulating valve 8 and the vacuum pump 9 to be discharged, and a small part of the sample molecular flow passes through the mass spectrum capillary 10, flows through the sealing valve 11 under the action of the pressure gradient, and finally enters the mass spectrometer 12 for analysis.
When the environment to be measured changes, the vacuum gauge 7 can detect the pressure change in the pressure buffer cavity 6 and feed back the pressure change to the regulating valve 8 in a signal mode and the like, and the pipe diameter of an air extraction flow path between the vacuum pump 9 and the pressure buffer cavity 6 is changed through the regulating valve 8, so that the pressure in the pressure buffer cavity 6 is ensured to be in a relatively stable state.
When the ambient pressure is too great, besides adjusting the regulating valve 8, the sealing valve 11 can be closed, and the sample capillaries 5 with different lengths can be replaced to further maintain the pressure inside the pressure buffer cavity 6. This maintenance does not break the vacuum inside the mass spectrometer 12 and therefore does not take a long time to wait for the mass spectrometer vacuum to re-establish, and the device can also achieve rapid conversion of the process mass spectrometer from capillary sample injection to chromatographic sample injection, improving the flexibility of the device.
The utility model can rapidly respond to various samples by taking the two-stage capillary as a sample injection mode of the process mass spectrum. The pressure change of the environment is monitored through the vacuum gauge, and the aperture of the air extraction pipeline is changed by utilizing the regulating valve, so that the environmental pressure of the instrument sample inlet is maintained. The interference caused by impurities in the environment is reduced through the filtering device, so that the influence of environmental change on the detection result of the instrument is reduced. The device combines with a high-performance mass spectrometer, can realize real-time sample injection and analysis of gases with different concentrations in a complex industrial environment, and can also realize rapid maintenance of a sample injection device and conversion between the sample injection device and a chromatographic module by utilizing a sealing valve. The device can rapidly maintain the components, can be rapidly converted into the chromatographic sample injection device, has low cost, short maintenance time and strong stability, and greatly improves the flexibility and the application range of the process mass spectrometer.
In the description of the present utility model, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present utility model and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present utility model.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present utility model, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The foregoing is only a preferred embodiment of the present utility model, but the scope of the present utility model is not limited thereto, and any person skilled in the art, who is within the scope of the present utility model, should make equivalent substitutions or modifications according to the technical scheme of the present utility model and the inventive concept thereof, and should be covered by the scope of the present utility model.
Claims (7)
1. The utility model provides a mass spectrum real-time sampling device based on two capillaries, its characterized in that, includes pressure buffer chamber (6), pressure buffer chamber (6) adopts the cross interface, the lower interface connection vacuum pump (9) of pressure buffer chamber (6), sample tee bend (2) are connected through sample capillary (5) in the left interface of pressure buffer chamber (6), sample tee bend (2) are connected sample inlet (1) and sampling pump respectively, mass spectrometer (12) are connected through mass spectrum capillary (10) in the right interface of pressure buffer chamber (6).
2. The dual-capillary-based mass spectrometry real-time sampling device according to claim 1, wherein the sampling tee (2) is connected with a sampling pump through a shunt port (3).
3. The dual capillary-based mass spectrometry real-time sampling device according to claim 1, wherein the mass spectrometry capillary (10) is connected to a mass spectrometer (12) through a sealing valve (11).
4. The dual-capillary-based mass spectrometry real-time sample injection device according to claim 1, wherein the left interface and the right interface of the pressure buffer cavity (6) are respectively connected with the sample capillary (5) and the mass spectrometry capillary (10) through rubber pads.
5. The dual-capillary-based mass spectrometry real-time sampling device according to claim 1, wherein the sample capillary (5) is connected with a sampling tee (2) through a filtering device (4).
6. The dual-capillary-based mass spectrometry real-time sampling device according to claim 1, wherein the upper interface of the pressure buffer cavity (6) is connected with a vacuum gauge (7); the lower interface of the pressure buffer cavity (6) is connected with a vacuum pump (9) through a regulating valve (8), and the vacuum gauge (7) is connected with the regulating valve (8) through a signal.
7. The dual-capillary-based mass spectrometry real-time sampling device according to claim 1, wherein the pore diameters of the sample capillary (5) and the mass spectrometry capillary (10) are 0.1-0.3mm.
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CN202322016836.8U CN220474569U (en) | 2023-07-30 | 2023-07-30 | Mass spectrum real-time sampling device based on double capillaries |
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CN202322016836.8U CN220474569U (en) | 2023-07-30 | 2023-07-30 | Mass spectrum real-time sampling device based on double capillaries |
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2023
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