阅读说明：本技术 质谱和色谱的接口装置及安装方法 (Interface device for mass spectrum and chromatogram and installation method ) 是由 林建强 吴键波 马乔 段炼 刘立鹏 胡建坤 韩双来 于 2020-12-31 设计创作，主要内容包括：本发明提供了质谱和色谱的接口装置及安装方法,所述质谱和色谱的接口装置包括色谱柱；端盖具有依次设置的第一轴向延伸部、径向部分、第二轴向延伸部和第三轴向延伸部；第一轴向延伸部内具有中空的内径扩大段,所述径向部分具有通孔；所述第二轴向延伸部连接所述径向部分周向,所述第二轴向延伸部的外径小于第三轴向延伸部的外径；所述受压件设置在所述内径扩大段内,并被所述挤压件挤压；保护管设置在所述径向部分的一侧,色谱柱依次穿过所述保护管、径向部分的通孔、受压件和挤压件的通孔；套筒设置在所述保护管的外侧,一端与所述第三轴向延伸部连接,另一端具有安装位；密封件套在所述第二轴向延伸部的外侧。本发明具有密封好、误差小等优点。(The invention provides an interface device of a mass spectrum and a chromatogram and an installation method, wherein the interface device of the mass spectrum and the chromatogram comprises a chromatographic column; the end cover is provided with a first axial extension part, a radial part, a second axial extension part and a third axial extension part which are arranged in sequence; the first axial extension has a hollow inner diameter expansion section therein, and the radial part has a through hole; the second axial extension is connected with the periphery of the radial part, and the outer diameter of the second axial extension is smaller than that of the third axial extension; the compression piece is arranged in the inner diameter expansion section and is extruded by the extrusion piece; the protective tube is arranged on one side of the radial part, and the chromatographic column sequentially penetrates through the protective tube, the through hole of the radial part, the through hole of the compression piece and the through hole of the extrusion piece; the sleeve is arranged on the outer side of the protection tube, one end of the sleeve is connected with the third axial extension part, and the other end of the sleeve is provided with an installation position; a seal is sleeved outside the second axial extension. The invention has the advantages of good sealing, small error and the like.)

1. An interface for mass spectrometry and chromatography comprising a chromatography column; it is characterized in that the interface device for mass spectrum and chromatogram further comprises:

an end cap having a first axial extension, a radial portion, a second axial extension, and a third axial extension disposed in that order; in a direction from the third axial extension to the first axial extension, the first axial extension having a hollow inner diameter expansion section therein, the radial portion having a through bore; the second axial extension is connected with the periphery of the radial part, and the outer diameter of the second axial extension is smaller than that of the third axial extension;

the extrusion part and the compression part are respectively provided with a through hole, the compression part is arranged in the inner diameter expansion section, and the extrusion part extrudes the compression part in the inner diameter expansion section;

the protective tube is arranged on one side, back to the first axial extension part, of the radial part, and the chromatographic column sequentially penetrates through the protective tube, the through hole of the radial part, the through hole of the pressure piece and the through hole of the extrusion piece; the heater is used for heating the chromatographic column in the protective tube;

the sleeve is arranged on the outer side of the protection tube, one end of the sleeve is connected with the third axial extension part, and the other end of the sleeve is provided with an installation position; the sealing element is sleeved on the outer side of the second axial extension part and is positioned on one side of the end part of the third axial extension part.

2. The interface of mass spectrometry and chromatography according to claim 1, wherein the pressure piece has an enlarged outer diameter in a direction from the second axial portion to the axial extension.

3. Interface for mass spectrometry and chromatography according to claim 1, characterized in that the side of the radial portion facing the protective tube has a groove adapted for the insertion of a protective tube end.

4. The mass spectrometry and chromatography interface device of claim 3, wherein the recess and the protective tube have a thermal barrier therebetween.

5. The interface of mass spectrometry and chromatography as claimed in claim 1, wherein the heater and the sleeve have an insulating layer therebetween, and the heater and the radial portion have an insulating layer therebetween.

6. The mass spectrometry and chromatography interface of claim 1, wherein the extrusion has external threads and the inner wall of the first axial extension has internal threads that mate with the external threads.

7. The interface of mass spectrometry and chromatography of claim 1, wherein the end of the pressure receiving member adjacent to the extrusion member has an axially extending male portion having a through hole adapted for a chromatography column to pass through, the extrusion member having a recess adapted to receive the male portion.

8. The method of installing a mass spectrometry and chromatography interface device of any one of claims 1 to 7, the method comprising:

the chromatographic column passes through the protective tube, the through hole of the radial part, the through hole of the pressure piece and the through hole of the extrusion piece;

extruding the compression piece by using the extrusion piece, sealing the compression piece and the radial part, and sealing the compression piece and the chromatographic column;

securing the sleeve to the chromatography module;

the second axial extension part is inserted into a mounting through hole of the mass spectrum vacuum cavity, and the diameter of the mounting through hole is smaller than the outer diameter of the third axial extension part;

connecting the vacuum chamber and chromatography module, the seal between the vacuum chamber and the third axial extension is compressed.

Technical Field

The invention relates to a mass spectrum and a chromatogram, in particular to an interface device and a method for the mass spectrum and the chromatogram.

Background

The GC/MSD interface is used to introduce the separated sample gas from the chromatographic column into a mass analyzer for analysis. When the quality detector detects a sample, a better vacuum environment is often needed, and a leakage point is easily introduced by the GC/MSD interface in the process of introducing the sample gas into the vacuum cavity. In addition, the column is prone to cooling during transport, resulting in adsorption of a small amount of sample gas, leading to broadening of the peak width of the sample gas, and is therefore critical for heat tracing of the GC/MSD interface.

The solution of the existing instrument is to bolt the GC/MSD interface to one side of the analyzer box and seal it with an O-ring gasket. The GC/MSD interface enters the GC column box at one end, which is threaded and can be attached to the column using a nut and gasket. The other end of the interface is inserted through a vacuum chamber into the ion source. The GC/MSD interface is heated by a cartridge electric heater and the temperature is monitored by a sensor (thermocouple) in the interface. The defects in the prior art are as follows:

1. it can be seen from the model of the GC/MSD interface that at least 4 sealing points are introduced.

2. The location of the liner to column seal is furthest to the right from the vacuum chamber, which means that the column channel in the middle of the liner is evacuated and therefore when tracing the column, heat transfer is effected primarily by virtue of the elongate curve formed by the column in contact with the liner channel, which tends to be unevenly heat-conductive.

3. When sliding the chromatography column into the GC/MSD interface, it needs to be pulled out of the vacuum chamber and the ends of the chromatography column cut and adjusted. During this process, fragments of the chromatography column easily fall into the vacuum chamber and may damage the turbomolecular pump.

Disclosure of Invention

In order to solve the defects in the prior art, the invention provides an interface device for mass spectrometry and chromatography.

The purpose of the invention is realized by the following technical scheme:

an interface for mass spectrometry and chromatography comprising a chromatography column; the interface device for mass spectrometry and chromatography further comprises:

an end cap having a first axial extension, a radial portion, a second axial extension, and a third axial extension disposed in that order; in a direction from the third axial extension to the first axial extension, the first axial extension having a hollow inner diameter expansion section therein, the radial portion having a through bore; the second axial extension is connected with the periphery of the radial part, and the outer diameter of the second axial extension is smaller than that of the third axial extension;

the extrusion part and the compression part are respectively provided with a through hole, the compression part is arranged in the inner diameter expansion section, and the extrusion part extrudes the compression part in the inner diameter expansion section;

the protective tube is arranged on one side, back to the first axial extension part, of the radial part, and the chromatographic column sequentially penetrates through the protective tube, the through hole of the radial part, the through hole of the pressure piece and the through hole of the extrusion piece; the heater is used for heating the chromatographic column in the protective tube;

the sleeve is arranged on the outer side of the protection tube, one end of the sleeve is connected with the third axial extension part, and the other end of the sleeve is provided with an installation position; the sealing element is sleeved on the outer side of the second axial extension part and is positioned on one side of the end part of the third axial extension part.

The invention also aims to provide a method for adjusting the interface device of the mass spectrum and the chromatogram, which is realized by the following technical scheme:

according to the installation method of the interface device of the mass spectrum and the chromatogram, the installation method comprises the following steps:

the chromatographic column passes through the protective tube, the through hole of the radial part, the through hole of the pressure piece and the through hole of the extrusion piece;

extruding the compression piece by using the extrusion piece, sealing the compression piece and the radial part, and sealing the compression piece and the chromatographic column;

securing the sleeve to the chromatography module;

the second axial extension part is inserted into a mounting through hole of the mass spectrum vacuum cavity, and the diameter of the mounting through hole is smaller than the outer diameter of the third axial extension part;

connecting the vacuum chamber and chromatography module, the seal between the vacuum chamber and the third axial extension is compressed.

Compared with the prior art, the invention has the beneficial effects that:

1. the sealing points are few, and the reliability is high;

the entire interface device introduces only two sealing points: the adopted sealing mode is reliable between the pressure piece and the radial part and between the pressure piece and the chromatographic column;

2. the structure is simple and the processing is easy;

the two key parts of the extrusion part and the compression part adopt the design of a revolving body, the structure is simple, and the processing of a slender hole on a machined part is avoided by utilizing a stainless steel guide pipe;

3. heat tracing is uniform;

the positions of the sealing points of the chromatographic column and the interface device are moved from the rightmost side far away from the vacuum cavity to the position close to the vacuum cavity, so that the whole section of the protection tube is in a normal-pressure environment, and therefore, air bath heating can be provided in the process of carrying out heat tracing on the chromatographic column, the heat tracing is more uniform, and the components to be detected are prevented from being adsorbed and condensed in the chromatographic column;

4. the installation is convenient, and the adjustment in a vacuum cavity is avoided;

when installing chromatographic column to interface arrangement, can accomplish outside the vacuum cavity, compare and adjust the chromatographic column in that the vacuum cavity is inside, convenient and fast more has avoided the chromatogram fragment to fall into the vacuum cavity moreover, damages the risk of turbo molecular pump.

Drawings

The disclosure of the present invention will become more readily understood with reference to the accompanying drawings. As is readily understood by those skilled in the art: these drawings are only for illustrating the technical solutions of the present invention and are not intended to limit the scope of the present invention. In the figure:

FIG. 1 is a schematic diagram of a mass spectrometry and chromatography interface apparatus according to an embodiment of the present invention;

fig. 2 is a schematic structural diagram of a portion of an interface device for mass spectrometry and chromatography according to an embodiment of the present invention.

Detailed Description

Fig. 1-2 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. Some conventional aspects have been simplified or omitted for the purpose of teaching the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.

Example 1:

fig. 1-2 show a schematic structural diagram of an interface device for mass spectrometry and chromatography according to an embodiment of the present invention, as shown in fig. 1-2, the interface device for mass spectrometry and chromatography includes:

a chromatographic column 10 for separating various components to be measured in a substance and sending the separated components to an ion source in a vacuum chamber 81 for ionization;

an end cap having a first axial extension 11, a radial portion 12, a second axial extension 13 and a third axial extension 14 arranged in that order; in the direction from the third axial extension 14 to the first axial extension 11, the first axial extension 11 has a hollow inner diameter expansion section therein, and the radial portion 12 has a through hole; the second axial extension 13 connects the radial partial circumferences, the outer diameter of the second axial extension 13 is smaller than that of the third axial extension 14;

an extrusion member 21 and a pressure receiving member 22, the extrusion member 21 and the pressure receiving member 22 having through holes, respectively, the pressure receiving member 22 being disposed in the inner diameter expansion section, the extrusion member 21 extruding the pressure receiving member 22 in the inner diameter expansion section;

a protection pipe 31 and a heater 41, wherein the protection pipe 31 is arranged on one side of the radial part 12 opposite to the first axial extension part 11, and the chromatographic column 10 sequentially passes through the protection pipe 31, the through hole of the radial part 12, the through hole of the pressure piece 22 and the through hole of the extrusion piece 21; the heater 41 is used for heating the chromatographic column 10 in the protection tube 31;

a sleeve 61 and a seal 18, said sleeve 61 being arranged outside said protective tube 31, one end being connected to said third axial extension 14 and the other end having a mounting location; the seal 18 is fitted around the outside of the second axial extension 13, on the side of the end of the third axial extension 14.

In order to seal the vacuum chamber from the outside, further, the outer diameter of the pressure receiving member 22 is increased in the direction from the third axial extension 14 to the first axial extension 11.

For fixing the protective tube, the side of the radial portion 12 facing the protective tube 31 is further provided with a groove 15 adapted for insertion of the end of the protective tube 31.

In order to prevent the end cap from being heated and heated, a heat insulation layer is further arranged between the groove 15 and the protection pipe 31.

In order to prevent heat loss, further, an insulating layer 51 is provided between the heater 41 and the sleeve 61, and an insulating layer 71 is provided between the heater 41 and the radial portion 12.

In order to press the pressure member to achieve sealing, further, the pressure member 21 has an external thread, and the inner wall of the first axial extension 11 has an internal thread matching the external thread.

In order to compress the pressure piece to achieve sealing, further, the end of the pressure piece 22 adjacent to the pressure piece 21 is provided with an outer convex part 23 extending along the axial direction, the outer convex part 23 is provided with a through hole suitable for the chromatography column 10 to pass through, and the pressure piece 21 is provided with a groove suitable for accommodating the outer convex part 23.

The installation method of the interface device for mass spectrometry and chromatography in the embodiment of the invention comprises the following steps:

the chromatographic column 10 passes through the through holes of the protective tube 31, the radial portion 12, the pressure receiving member 22 and the pressure member 21;

the compression piece 22 is compressed by the compression piece 21, the compression piece 22 is sealed with the radial part 12, and the compression piece 22 is sealed with the chromatographic column 10;

securing the sleeve 61 to the chromatography module 91;

the second axial extension 13 is inserted into a mounting through hole of a mass spectrometer vacuum chamber 81, and the diameter of the mounting through hole is smaller than the outer diameter of the third axial extension 14;

the vacuum chamber 81 and the chromatography module 91 are connected, and the seal 18 between the vacuum chamber 81 and the third axial extension 14 is compressed.

Example 2:

an application example of the interface device for mass spectrometry and chromatography and the installation method according to embodiment 1 of the present invention.

In this application example, as shown in fig. 1, the end cap has a first axial extension 11, a radial portion 12, a second axial extension 13, and a third axial extension 14, which are arranged in this order; in the direction from the third axial extension 14 to the first axial extension 11, the first axial extension 11 has a hollow inner diameter expansion section therein, and the radial portion 12 has a through hole; the second axial extension 13 is connected with the radial part 12 in the circumferential direction, and the outer diameter of the second axial extension 13 is smaller than that of the third axial extension 14;

the pressure member 21 and the pressure member 22 respectively have through holes, the pressure member 22 is disposed in the inner diameter expansion section, and the outer diameter of the pressure member 22 is expanded in the direction from the third axial extension 14 to the first axial extension 11 to match the shape of the inner diameter expansion section; the end part of the pressure piece 22 adjacent to the extrusion piece 21 is provided with an outer convex part 23 extending along the axial direction, the outer convex part 23 is provided with a through hole suitable for the chromatography column 10 to pass through, and the extrusion piece 21 is provided with a groove suitable for accommodating the outer convex part 23; the extrusion part 21 is provided with an external thread which is matched with the internal thread of the inner diameter expansion section, so that the extrusion part 21 is fixed in the inner diameter expansion section and the compression part 22 in the inner diameter expansion section is extruded by rotation;

the protection tube 31 is made of stainless steel and is disposed on a side of the radial portion 12 facing away from the first axial extension 11, specifically: the side of the radial part 12 facing the protective pipe 31 is provided with a groove 15 suitable for inserting the end of the protective pipe, one end of the protective pipe 31 is inserted into the groove 15, and a heat insulation layer is arranged between the groove 15 and the protective pipe 31; the chromatographic column 10 passes through the protective tube 31, the through hole of the radial part 12, the through hole of the pressure piece 22 and the through hole of the extrusion piece 21 in sequence; the heater 41 is a heating wire, is arranged on the outer side of the protection tube 31, and is used for heating the chromatographic column 10 in the protection tube 31 to prevent adsorption and water condensation; an insulating layer 71 is arranged between the heater 41 and the radial part 12;

the sleeve 61 is arranged outside the protection tube 31, one end of the sleeve is fixed on the third axial extension part 14 through a screw, and the other end of the sleeve is provided with a mounting position; the sealing element 18 is sleeved outside the second axial extension 13 and is arranged on one side of the end part of the third axial extension 14; the insulating layer 51 is disposed between the heater 41 and the sleeve 61.

The installation method of the interface device for mass spectrometry and chromatography in the embodiment of the invention comprises the following steps:

the chromatography column 10 passes through the through holes of the protective tube 31, the through hole of the radial portion 12, the pressure receiving member 22, and the pressing member 21 (including the through hole in the convex portion);

rotating the extrusion member 21 to axially extrude the compression member 22, wherein the extrusion member 22 comprises the extrusion of the groove of the extrusion member 21 to the convex part 23 of the compression member 22, and the compression member 22 is extruded and deformed in the axial direction and the radial direction, so that the compression member 22 is sealed with the radial part 12, and the compression member 22 is sealed with the chromatographic column 10;

securing the sleeve 61 to the chromatography module 91: fixing the sleeve 61 on the chromatographic mold 91 by using a screw;

the second axial extension 13 is inserted into a mounting through hole of the mass spectrometer vacuum chamber 81, and the diameter of the mounting through hole is smaller than the outer diameter of the third axial extension 14 but not smaller than the outer diameter of the second axial extension 13;

the vacuum chamber 81 and the chromatography module 91 are connected, and the sealing member 18 between the vacuum chamber 81 and the third axial extension 14 is pressed, thereby sealing the vacuum chamber 81 from the outside.