CN218769408U

CN218769408U - Real-time gas sampling device suitable for mass spectrometer

Info

Publication number: CN218769408U
Application number: CN202222830796.6U
Authority: CN
Inventors: 黄泽建; 高佳奇
Original assignee: Shanghai Limu Scientific Instrument Co ltd
Current assignee: Shanghai Limu Scientific Instrument Co ltd
Priority date: 2022-10-26
Filing date: 2022-10-26
Publication date: 2023-03-28
Anticipated expiration: 2032-10-26

Abstract

The utility model discloses a real-time gas sample introduction device suitable for a mass spectrometer, which comprises a sample introduction port, wherein the sample introduction port is respectively connected with a shunt port and a sample micropore joint through a sample introduction tee joint, and the shunt port is connected with a sampling pump; the sample micropore joint is connected with a vacuum mass spectrometer through a mass spectrum micropore joint; the sample micropore joint is internally provided with a detachable sheet structural member, and sample micropores are arranged on the sheet structural member. The utility model discloses a two-stage micropore has promoted kind speed as the appearance mode of advancing of mass spectrum to through vacuum pump and microporous regulation, maintain the pressure between two micropores, reduced because of the influence that the ambient pressure changes and lead to the fact the ration process. The filter device is arranged to avoid the influence of substances such as liquid drops, dust and the like in the environment on the device and instruments. The sealing valve is arranged, so that the components are maintained under the condition of not damaging the vacuum of the mass spectrum, the rapid maintenance of the sample injection device and the conversion between the sample injection device and the chromatographic module are realized, and the application range and the flexibility of the instrument are improved.

Description

Real-time gas sampling device suitable for mass spectrometer

Technical Field

The utility model relates to a sampling device of mass spectrograph belongs to the technical field of mass spectrograph, especially relates to a real-time gaseous sampling device suitable for mass spectrograph.

Background

With the development of industry, people pay more attention to process optimization, production safety, quality assurance, energy conservation, efficiency improvement and the like of industrial production, and for industrial production processes such as fuel cells, catalysts, synthesis gas and the like mainly based on gas-solid multiphase reaction, the production state can be monitored according to gas components released in the reaction process, so that qualitative and quantitative analysis on the gas is often needed.

Mass spectrometry is an analysis method, which can provide abundant structural information in one analysis, has high specificity and high sensitivity, and is widely applied to compound identification work in various subject fields. The working principle of the mass spectrum is as follows: the method comprises the steps of ionizing sample molecules in a specific mode, separating different ions by using an electromagnetic field, receiving and detecting, processing signals, and displaying in mass spectrograms and other modes to finish qualitative and quantitative analysis of substances.

The mass spectrometer has the characteristics of high automation degree, high stability, good reliability and the like, can reflect the production process in real time, can be used for monitoring the quality of products and the running condition of devices, and has become a common analysis, measurement and control tool in modern industrial production management and production running.

At present, mass spectrometers applied to industrial production online monitoring mainly comprise an RGA (residual gas analyzer) and a GC-MS (gas chromatography-mass spectrometer), and both have technical defects for real-time detection of trace substances in a reaction process.

The RGA instrument has the advantages of portability and high detection speed, but the sensitivity of the instrument is insufficient, the detection range is limited, in addition, the RGA generally adopts a capillary sampling mode, the sampling amount can be influenced by the environmental pressure and the sample type, and when the working environment or the components to be detected change, the quantitative effect of the instrument cannot be ensured. Therefore, the instrument is not suitable for the detection of low concentration components and often can only be operated in an atmospheric environment.

The GC-MS has excellent sensitivity and detection range, but the size is large, and because the GC-MS relies on a chromatographic column for separation, the analysis flow usually needs dozens of minutes, and the real-time state of the gas to be detected cannot be reflected. Therefore, the instrument is not suitable for portable and real-time detection in industrial production.

For industrial production, in order to realize real-time monitoring and control of the production process, instruments are required to detect substances with various concentrations, and excellent response speed and environmental adaptability are also required. Therefore, the conventional RGA and GC-MS can not meet the monitoring requirement of industrial production.

SUMMERY OF THE UTILITY MODEL

The utility model aims at providing a gaseous sampling device suitable for mass spectrograph can work under multiple industrial environment, realizes advancing kind and detecting in real time of gaseous sample, when guaranteeing instrument analysis performance, improves its suitability.

In order to achieve the above purpose, the utility model adopts the following technical scheme:

a real-time gas sample introduction device suitable for a mass spectrometer comprises a sample introduction port, wherein the sample introduction port is respectively connected with a flow dividing port and a sample micropore joint through a sample introduction tee joint, and the flow dividing port is connected with a sampling pump; the sample microporous joint is connected with a vacuum mass spectrometer through a mass spectrum microporous joint; the sample micropore joint is internally provided with a detachable sheet structure member, and the sheet structure member is provided with sample micropores.

Preferably, a detachable sheet structural member is arranged in the mass spectrum micropore joint, and mass spectrum micropores are formed in the sheet structural member.

Preferably, the pore size of the sample micropores is generally 10 to 100 μm.

Preferably, the pore size of the mass spectrometry microwells is generally in the range of 10 to 50 μm.

Preferably, be equipped with the preceding stage vacuum chamber between sample micropore joint and the mass spectrum micropore joint, the preceding stage vacuum chamber adopts criss-cross four way connection, sample micropore joint and mass spectrum micropore joint are connected respectively to the both ends mouth about the preceding stage vacuum chamber, pressure sensor and vacuum pump are connected respectively to the upper and lower both ends mouth of preceding stage vacuum chamber, pressure sensor passes through signal connection control system, control system control drive vacuum pump.

Preferably, a filtering joint is arranged between the sample introduction tee joint and the sample micropore joint, and a filtering device is arranged in the filtering joint.

Preferably, a sealing valve is arranged between the mass spectrum micropore joint and the mass spectrometer.

Compared with the prior art, the utility model discloses possess following beneficial effect:

1. the utility model realizes gas sample introduction through two-stage micropores to ensure real-time analysis of the components to be measured;

2. the utility model controls the pressure between the two micropores through the vacuum pump and the pressure sensor to ensure the sampling flow rate;

3. the utility model separates liquid drops and dust in the sample gas through the filtering device, and prevents the liquid drops and dust from damaging the sample feeding device and the mass spectrometer;

4. the utility model discloses a seal valve control is gaseous advances kind to protect the mass spectrum instrument. The utility model discloses can work under multiple industrial environment, realize advancing kind and detecting in real time of gaseous sample, when guaranteeing instrument analysis performance, improve its suitability.

To sum up, the utility model discloses a two-stage micropore has greatly promoted kind speed as the kind mode of advancing of mass spectrum to through to vacuum pump and microporous regulation, maintain the pressure between two micropores, reduced because of the ambient pressure changes the influence that causes the ration process, increased the reliability of instrument. A filtering device is arranged in front of the micropores, so that the influence of substances such as liquid drops, dust and the like in the environment on the device and instruments is avoided. The sealing valve is arranged in front of the mass spectrometer, so that the components can be adjusted under the condition of not damaging the vacuum of the mass spectrometer, the rapid maintenance of the sample injection device and the conversion between the sample injection device and the chromatographic module are facilitated, the mass spectrometer can perform real-time rapid detection on samples in different ranges, and the application range and the flexibility of the instrument are greatly improved.

Drawings

Fig. 1 is a schematic structural diagram of a real-time gas sampling device suitable for a mass spectrometer provided by the present invention;

fig. 2 is the utility model provides a gas flow path schematic diagram of real-time gas sampling device during operation suitable for mass spectrograph.

The numbers in the figure are as follows:

101. a sample inlet; 102. a sample introduction tee joint; 103. a shunt port; 104. a filter adapter; 105. a sample microporous joint; 106. a backing stage vacuum chamber; 107. a pressure sensor; 108. a vacuum pump; 109. mass spectrometry microporous joints; 110. a sealing valve; 111. a mass spectrometer. 201. A filtration device; 202. sample micropores; 203. and (5) carrying out mass spectrometry on the micropores.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments.

As shown in fig. 1 and fig. 2, for the utility model provides a real-time gas sampling device suitable for a mass spectrometer, the device comprises a sample inlet 101 from left to right, the sample inlet 101 is respectively connected with a shunt port 103 and a sample micropore joint 105 through a sample inlet tee 102, the shunt port 103 is connected with a sampling pump; the sample micropore joint 105 is connected with a mass spectrum micropore joint 109 through a preceding stage vacuum cavity 106, and the mass spectrum micropore joint 109 is connected with a vacuum mass spectrometer 111; a detachable sheet-shaped structure member is arranged in the sample micropore joint 105, a sample micropore 202 is arranged on the sheet-shaped structure member, the aperture of the sample micropore 202 is generally 10-100 μm, and the pressure in the foreline vacuum chamber 106 is further maintained by replacing the sample micropores 202 with different apertures. The mass spectrum micropore joint 109 is internally provided with a detachable sheet structure, the sheet structure is provided with mass spectrum micropores 203, and the aperture of the mass spectrum micropores 203 is generally 10-50 μm.

The foreline vacuum chamber 106 adopts a cross-shaped four-way joint, the left and right ports of the foreline vacuum chamber 106 are respectively connected with the sample microporous joint 105 and the mass spectrum microporous joint 109, the upper and lower ports of the foreline vacuum chamber 106 are respectively connected with the pressure sensor 107 and the vacuum pump 108, the pressure sensor 107 is connected with the control system through signals, and the control system controls and drives the vacuum pump 108. The pressure sensor 107 monitors the pressure inside the foreline vacuum chamber 106 in real time, and the vacuum pump 108 is used to ensure that the pressure inside the foreline vacuum chamber 106 is stable.

Further, a filtering joint 104 is arranged between the sample introduction tee 102 and the sample micropore joint 105, and a filtering device 201 with a filtering hole is arranged in the filtering joint 104.

Further, a sealing valve 110 is arranged between the mass spectrum micropore joint 109 and a mass spectrometer 111. When the sealing valve 110 is closed, the micro-pores and other parts can be replaced without breaking the vacuum inside the mass spectrometer 111, thereby improving the efficiency of maintenance of the device. In addition, by adjusting the sealing valve 110, the rapid switching from micropore sampling to chromatographic sampling can be realized, and the flexibility of the device is improved.

The working principle of the utility model is as follows:

a sample to be measured is connected to the sample inlet 101, a sampling pump is connected to the shunt port 103, and the pressure sensor 107, the vacuum pump 108 and the sealing valve 110 are opened, so that a pressure gradient is formed between the sample inlet 101 and the mass spectrometer 111 because the inside of the mass spectrometer 111 is a high vacuum environment.

When the device works, as shown in the arrow direction of fig. 2, sample gas enters the sample inlet tee 102 from the sample inlet 101, most of the sample gas flows out from the flow splitting port 103 under the action of the sampling pump, a small part of the sample gas enters the filtering device 201 inside the filtering connector 104 under the action of pressure gradient, and the filtering device 201 can prevent substances such as liquid drops, dust and the like doped in the sample gas from entering a pipeline, so that rear micropores are prevented from being blocked, and the instrument is prevented from being damaged. After passing through the filter 201, the sample gas flow enters the foreline vacuum chamber 106 through the sample microporous joint 202 under the action of the pressure gradient. The pressure sensor 107 monitors the pressure inside the foreline vacuum chamber 106 in real time, and the vacuum pump 108 is used to ensure that the pressure inside the foreline vacuum chamber 106 is stable. Most of the sample gas is exhausted by the vacuum pump 108, and a small part of the sample molecular flow passes through the mass spectrum micropores 203 in the mass spectrum micropore joint 109 under the action of the pressure gradient, passes through the sealing valve 110, and finally enters the mass spectrometer 111 for analysis.

When the environmental pressure changes, the pressure sensor 107 can detect the pressure change inside the foreline vacuum chamber 106 and feed back to the vacuum pump 108, and the pumping speed of the vacuum pump 108 is adjusted to ensure that the pressure inside the foreline vacuum chamber 106 is in a relatively stable state, typically about 50 Pa. When the environmental pressure changes too much, the vacuum pump 108 can be adjusted and the sample micro-holes 202 with different apertures can be replaced to further maintain the pressure inside the foreline vacuum chamber 106.

The utility model discloses a two-stage micropore has greatly promoted the speed of advancing as the appearance mode of mass spectrum to through to vacuum pump and microporous regulation, maintain the pressure between two micropores, reduced because of the influence that environmental pressure changes and lead to the fact quantitative process, increased the reliability of instrument. A filtering device is arranged in front of the micropores, so that the influence of substances such as liquid drops, dust and the like in the environment on the device and instruments is avoided. The sealing valve is arranged in front of the mass spectrometer, so that the components can be adjusted under the condition of not damaging the vacuum of the mass spectrometer, the rapid maintenance of the sample injection device and the conversion between the sample injection device and the chromatographic module are facilitated, the mass spectrometer can perform real-time rapid detection on samples in different ranges, and the application range and the flexibility of the instrument are greatly improved.

In the description of the present invention, it is to 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", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and for simplicity of description, but do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be construed as limiting the present invention.

Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically limited otherwise.

The above, only be the concrete implementation of the preferred embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art is in the technical scope of the present invention, according to the technical solution of the present invention and the utility model, the concept of which is equivalent to replace or change, should be covered within the protection scope of the present invention.

Claims

1. The real-time gas sample introduction device suitable for the mass spectrometer is characterized by comprising a sample introduction port (101), wherein the sample introduction port (101) is respectively connected with a flow splitting port (103) and a sample micropore joint (105) through a sample introduction tee joint (102), and the flow splitting port (103) is connected with a sampling pump; the sample microporous joint (105) is connected with a vacuum mass spectrometer (111) through a mass spectrum microporous joint (109); and a detachable sheet structure member is arranged in the sample micropore joint (105), and sample micropores (202) are arranged on the sheet structure member.

2. The real-time gas sampling device suitable for the mass spectrometer as claimed in claim 1, wherein a detachable sheet structure is arranged in the mass spectrometer micro-pore joint (109), and mass spectrometer micro-pores (203) are arranged on the sheet structure.

3. The device of claim 1, wherein the sample wells (202) have a pore size of generally 10-100 μm.

4. The device for real-time gas injection suitable for mass spectrometry according to claim 1, wherein the pore size of the mass spectrometry micropores (203) is generally 10-50 μm.

5. The real-time gas sampling device suitable for mass spectrometer of claim 1, characterized in that, be equipped with preceding stage vacuum chamber (106) between sample micropore joint (105) and mass spectrum micropore joint (109), preceding stage vacuum chamber (106) adopt criss-cross four way connection, sample micropore joint (105) and mass spectrum micropore joint (109) are connected respectively to both ends mouth about preceding stage vacuum chamber (106), pressure sensor (107) and vacuum pump (108) are connected respectively to the upper and lower both ends mouth of preceding stage vacuum chamber (106), pressure sensor (107) pass through signal connection control system, control system control drive vacuum pump (108).

6. The real-time gas sampling device suitable for the mass spectrometer as claimed in claim 1, wherein a filtering joint (104) is provided between the sampling tee (102) and the sample microporous joint (105), and a filtering device (201) is provided in the filtering joint (104).

7. The real-time gas sample introduction device suitable for the mass spectrometer as claimed in claim 1, wherein a sealing valve (110) is arranged between the mass spectrometer micropore joint (109) and the mass spectrometer (111).