Expansion low-temperature column oven device of gas chromatograph-mass spectrometer

Abstract

The invention discloses a gas chromatograph-mass spectrometer extended low-temperature column oven device which comprises a gas chromatographic column oven, a low-temperature column oven body and a low-temperature column oven cover, an inner container is arranged in the gas chromatographic column oven, the gas chromatograph-mass spectrometer extended low-temperature column oven device further comprises sliding rails, a chromatographic column hanging frame and a lifting structure, a pair of sliding rails is arranged on the opposite side faces of the inner container, and the lifting structure is arranged on the sliding rails. Box body sliding blocks are arranged on the two sides of the low-temperature column oven body respectively, box cover sliding blocks are arranged on the two sides of the low-temperature column oven cover respectively, and the box body sliding blocks and the box cover sliding blocks located on the same side are aligned and then jointly inserted into the sliding rails on the same side and can slide along the sliding rails; the chromatographic column hanger is rotatably mounted on the lifting structure; a heating disc and a fan are mounted in the gas chromatographic column oven; and the heating disc is positioned between the low-temperature column oven and the fan and faces the low-temperature column oven. According to the device, the chromatographic separation of permanent gas and low-boiling-point compounds by a single capillary column is realized, the rapid switching of common test and an extended low-temperature column oven is realized, and the variable adjustment of the distance between the chromatographic column and a protective sieve plate is realized.

Description

Technical Field

[0001] The present invention relates to the technical field of analytical instruments, and in particular to an extended low-temperature column oven device for a gas chromatography-mass spectrometry instrument. Background Art

[0002] Gas chromatography-mass spectrometry instruments usually use capillary chromatographic columns for analytical testing. However, it is often difficult to chromatographically separate permanent gases and low-boiling compounds using a single capillary chromatographic column. The chromatographic separation of permanent gases and low-boiling compounds is mainly achieved by reducing the initial temperature and heating rate of the column oven, using special gas phases, and multiple different types of chromatographic columns. Ordinary gas chromatography-mass spectrometry instruments have a high market share, but the minimum operating temperature of the column oven is often higher than the ambient temperature, and it is impossible to effectively chromatographically separate permanent gases and low-boiling compounds by reducing the initial temperature and heating rate of the column oven. Modifying an ordinary gas phase into a special gas phase for a single or a few samples and using multiple professional chromatographic columns is not only cumbersome but also not friendly to most instruments. Summary of the Invention

[0003] The purpose of the present invention is to overcome the deficiencies of the above-mentioned prior art and provide an extended low-temperature column oven device for a gas chromatography-mass spectrometry instrument.

[0004] The present invention is achieved through the following technical solutions: An extended low-temperature column oven device for a gas chromatography-mass spectrometry instrument includes a gas chromatography column oven, a low-temperature column oven body, and a low-temperature column oven cover. An inner container is provided in the gas chromatography column oven, and it further includes a slide rail and a chromatographic column hanger. A pair of slide rails are symmetrically opened on a pair of opposite side faces of the inner container. Box body sliders are respectively provided on both sides of the low-temperature column oven body, and box cover sliders are respectively provided on both sides of the low-temperature column oven cover. After the box body sliders and the box cover sliders on the same side are aligned, they are jointly inserted into the slide rail on the same side and can slide along the slide rail. The low-temperature column oven body and the low-temperature column oven cover are buckled up and down to form a low-temperature column oven. A lifting structure is installed in the low-temperature column oven, and the chromatographic column hanger is rotatably installed on the lifting structure and its height is adjusted by the lifting structure. A heating plate and a fan are installed in the gas chromatography column oven. The heating plate is located between the low-temperature column oven and the fan and faces the low-temperature column oven.

[0005] The cooperation between the slider and the slide rail can push or pull out the low-temperature column oven body or the low-temperature column oven cover. The setting of the lifting structure can adjust the height of the chromatographic column hanger. The setting of the heating plate and the fan can release heat and evenly distribute the heat throughout the chamber, thereby heating the entire low-temperature column oven as a whole, and then radiating the heat to the chromatographic column in the box. Chromatographic separation of permanent gases and low-boiling compounds is achieved through temperature control.

[0006] The slide rail is a long groove, and the cross-section of the long groove is a T-shaped structure; the box body slider and the box cover slider are long sliders with the same structure, and the long slider is an L-shaped cross-section structure. The box body slider and the box cover slider are aligned to form a T-shaped cross-section structure and are inserted into the T-shaped long groove of the slide rail together and can slide along the long groove. The cooperation between the L-shaped slider and the T-shaped long groove can better constrain the stable sliding of the slider.

[0007] A protective sieve plate is provided at the bottom of the low-temperature column temperature box body, and the protective sieve plate is located below the chromatographic column hanger.

[0008] The lifting structure includes a lifting screw, a screw hole and a cylindrical rotating body; the screw hole is opened at the center of the top of the low-temperature column temperature box cover, and the top of the chromatographic column hanger is provided with a mounting hole and a mounting groove, and the mounting hole is communicated with the mounting groove; the lifting screw is screwed into the screw hole, and the lower end of the lifting screw passes through the mounting hole and is connected to the cylindrical rotating body. The cylindrical rotating body is located in the mounting groove, and the diameter of the cylindrical rotating body is larger than the aperture of the mounting hole. The arrangement of the mounting hole and the mounting groove can constrain the cylindrical rotating body and prevent the lifting structure from falling off the chromatographic column hanger.

[0009] A box body handle is installed on the low-temperature column temperature box body, and a box cover handle is installed on the low-temperature column temperature box cover, and the box body handle and the box cover handle are opposite in position.

[0010] The gas chromatograph column temperature box and the low-temperature column temperature box body are both box bodies made of stainless steel, and the low-temperature column temperature box cover is a box cover made of stainless steel.

[0011] Compared with the prior art, the advantages of the present invention are as follows: By externally connecting a low-temperature column temperature box to a gas chromatograph-mass spectrometer, the use temperature range of the gas chromatograph column temperature box is expanded, and chromatographic separation of permanent gases and low-boiling compounds by a single capillary column is realized; through the slide rail and slider structure, rapid switching between ordinary tests and an extended low-temperature column temperature box is achieved, as well as rapid addition of liquid nitrogen before low-temperature tests; through the chromatographic column hanger in the box, variable adjustment of the distance between the chromatographic column and the protective sieve plate is realized. Description of the Drawings

[0012] Figure 1 It is a schematic structural diagram of an embodiment of the present invention;

[0013] Figure 2 It is a front view of the internal structure of an embodiment of the present invention;

[0014] Figure 3 It is a left view of the internal structure of an embodiment of the present invention;

[0015] Figure 4This is the test effect diagram of the embodiment of the present invention.

[0016] Meanings of the reference numerals in the figure: 1, mass spectrometer; 2, mass spectrometry transmission line; 3, gas chromatography injection port; 4, lifting screw; 5, low-temperature column oven cover; 6, cover slider; 7, slide rail; 8, box body slider; 9, gas chromatography column oven; 10, capillary chromatography column; 11, chromatography column hanger; 12, low-temperature column oven body; 13, inner liner; 14, heating plate; 15, fan; 16, gas chromatography column oven door; 17, cover handle; 18, box body handle; 19, protective sieve plate; 20, screw hole; 21, cylindrical rotating body. Detailed implementation manners

[0017] The content of the present invention will be further described in detail below in conjunction with the accompanying drawings and specific implementation manners.

[0018] Embodiment

[0019] Refer to Figures 1 to 3 , which is an extended low-temperature column oven device for a gas chromatography-mass spectrometry 1 combined instrument, including a gas chromatography column oven 9, a low-temperature column oven body 12 and a low-temperature column oven cover 5. An inner liner 13 is provided in the gas chromatography column oven 9. It also includes a slide rail 7 and a chromatography column hanger 11. A pair of slide rails 7 are symmetrically arranged on a set of opposite side faces of the inner liner 13. Box body sliders 8 are respectively provided on both sides of the low-temperature column oven body 12, and cover sliders 6 are respectively provided on both sides of the low-temperature column oven cover 5. After the box body slider 8 and the cover slider 6 on the same side are aligned, they are jointly inserted into the slide rail 7 on the same side and can slide along the slide rail 7; the low-temperature column oven body 12 and the low-temperature column oven cover 5 are buckled up and down to form a low-temperature column oven. A lifting structure is installed in the low-temperature column oven, and the chromatography column hanger 11 is rotatably installed on the lifting structure and its height is adjusted by the lifting structure; a heating plate 14 and a fan 15 are installed in the gas chromatography column oven 9. The heating plate 14 is located between the low-temperature column oven and the fan 15 and faces the low-temperature column oven.

[0020] The cooperation between the slider and the slide rail 7 can push or pull out the low-temperature column oven body 12 or the low-temperature column oven cover 5; the setting of the lifting structure can adjust the height of the chromatography column hanger 11; the setting of the heating plate 14 and the fan 15 can release heat and evenly distribute the heat to the entire chamber, and then heat the low-temperature column oven as a whole, so as to radiate the heat to the chromatography column in the box, and realize the chromatographic separation of permanent gases and low-boiling compounds by the chromatography column through temperature regulation.

[0021] The slide rail 7 is a long groove, and the cross-section of the long groove is a T-shaped structure; the box body slider 8 and the box cover slider 6 are long sliders with the same structure. The long slider has an L-shaped cross-section. The box body slider 8 and the box cover slider 6 are aligned to form a T-shaped cross-section and are inserted into the T-shaped long groove of the slide rail 7 together and can slide along the long groove. The cooperation between the L-shaped slider and the T-shaped long groove can better restrain the stable sliding of the slider.

[0022] A protective sieve plate 19 is provided at the bottom of the low-temperature column temperature box body 12, and the protective sieve plate 19 is located below the chromatographic column hanging rack 11.

[0023] The lifting structure includes a lifting screw 4, a screw hole 20 and a cylindrical rotating body 21; the screw hole 20 is opened at the center of the top of the low-temperature column temperature box cover 5. The top of the chromatographic column hanging rack 11 is provided with a mounting hole and a mounting groove, and the mounting hole communicates with the mounting groove; the lifting screw 4 is screwed into the screw hole 20, and the lower end of the lifting screw 4 passes through the mounting hole and is connected to the cylindrical rotating body 21. The cylindrical rotating body 21 is located in the mounting groove, and the diameter of the cylindrical rotating body 21 is larger than the diameter of the mounting hole. The arrangement of the mounting hole and the mounting groove can restrain the cylindrical rotating body 21 and prevent the lifting structure from falling off the chromatographic column hanging rack 11. In this embodiment, the distance between the chromatographic column and the protective sieve plate 19 can be adjusted by rotating the lifting screw 4.

[0024] A box body handle 18 is installed on the low-temperature column temperature box body 12, and a box cover handle 17 is installed on the low-temperature column temperature box cover 5. The box body handle 18 and the box cover handle 17 are opposite in position.

[0025] The gas chromatograph column temperature box 9 and the low-temperature column temperature box body 12 are both box bodies made of stainless steel, and the low-temperature column temperature box cover 5 is a box cover made of stainless steel.

[0026] In this embodiment, a gas chromatograph column temperature box door 16 is installed on the front side of the gas chromatograph column temperature box 9. A gas chromatograph injection port 3 is provided on the top of the gas chromatograph column temperature box 9. The capillary chromatographic column 10 is suspended on the chromatographic column hanging rack 11. For this device, only the extended low-temperature column temperature box slide rail 7 needs to be installed in advance. During use, place the extended low-temperature column temperature box containing the chromatographic column on the slide rail 7, connect the chromatographic column with the injection port of the gas chromatograph-mass spectrometer 1 and the mass spectrometry transmission line 2, and add liquid nitrogen to realize the gas chromatograph-mass spectrometer 1 for chromatographic separation of permanent gases and low-boiling compounds.

[0027] The application process of this embodiment is as follows:

[0028] Place the capillary chromatographic column 10 on the chromatographic column hanger 11 and put them together into the low-temperature column oven 12. After aligning the lid slider 6 of the low-temperature column oven lid 5 with the oven body slider 8 of the low-temperature column oven body 12, insert it into the pre-installed slide rail 7. Pull the oven body handle 18 to leave enough space for observing the inside of the oven between the low-temperature column oven lid 5 and the low-temperature column oven body 12. Rotate the lifting screw 4 and the cylindrical rotating body 21 on the lid screw hole 20 to observe and adjust the distance between the capillary chromatographic column 10 and the protective sieve plate 19. Connect the capillary chromatographic column 10 to the gas chromatograph injection port 3 and the mass spectrometry transmission line 2 of the mass spectrometer 1.

[0029] Set the temperature rising program before analysis and testing. Pull the oven body handle 18 to leave enough space between the low-temperature column oven lid 5 and the low-temperature column oven body 12. After adding an appropriate amount of liquid nitrogen, push the low-temperature column oven body 12 back. Close the door 16 of the gas chromatograph column oven. After the instrument is ready, click to run. At this time, heat is released by the heating plate 14 in the gas chromatograph column oven 9, and the heat is evenly distributed throughout the oven chamber by the fan 15 in the oven, thereby heating the whole low-temperature column oven, and then radiating the heat to the capillary chromatographic column 10 in the low-temperature column oven, and realizing the chromatographic separation of permanent gases and low-boiling compounds by a single capillary chromatographic column 10 at an extremely low initial column temperature and a slow temperature rising rate.

[0030] After use, disconnect the connection between the capillary chromatographic column 10 and the gas chromatograph injection port 3 and the mass spectrometry transmission line 2 of the mass spectrometer 1. Pull the lid handle and the oven body handle 18 together to remove the extended low-temperature column oven, and then install the chromatographic column and switch back to the conventional gas chromatograph-mass spectrometer 1 combined instrument.

[0031] Refer to Figure 4, is the test effect diagram of the embodiment of the present invention. The test conditions of the gas chromatography-mass spectrometry instrument are as follows: a methyl polysiloxane capillary column is used, the mass spectrometry scanning range is 2-150 amu, the temperature programming is to hold at 25°C for 5 min, rise to 40°C at 2°C / min, and then rise to 240°C at 10°C / min and hold for 10 min. Liquid nitrogen needs to be added to the low-temperature column oven before sample injection, and the test state should be entered as soon as possible after closing the column oven door. This method can effectively chromatographically separate permanent gases and low-boiling compounds on a common gas chromatography-mass spectrometry instrument. The description of the compounds corresponding to the retention time (RT) in the figure is as follows: 1. O2 (RT = 5.83 min); 2. N2 (RT = 5.98 min); 3. CO (RT = 6.72 min); 4. CH4 (RT = 6.97 min); 5. C2H6 (RT = 9.8 min); 6. N2O (RT = 10.07 min); 7. CO2 (RT = 10.26 min); 8. C2H4 (RT = 11.92 min); 9. C2H2 (RT = 16.14 min); 10. C3H8 (RT = 17.29 min); 11. H2S (RT = 18.05 min); 12. C2H5OH (RT = 20.85 min); 13. C3H6 (RT = 22.38 min); 14. C4H 10 (RT = 24.59 min); 15. C4H8 (RT = 27.71 min); 16. C5H 12 (RT = 28.83 min); 17. C5H 12 (RT = 29.23 min); 18. C5H 10 (RT = 31.15 min); 19. H2O (RT = 32.2 min); 20. C6H 14 (RT = 32.47 min); 21. C6H6 (RT = 36.03 min).

[0032] The above detailed description is a specific description of the feasible embodiments of the present invention. This embodiment is not intended to limit the patent scope of the present invention. Any equivalent implementation or modification without departing from the present invention shall be included in the patent scope of this case.

Claims

1. An extended low-temperature column oven device for a gas chromatography-mass spectrometry instrument, comprising a gas chromatography column oven, a low-temperature column oven body, and a low-temperature column oven cover. An inner container is provided in the gas chromatography column oven. It is characterized in that: It further includes a slide rail and a chromatographic column hanger. A pair of slide rails are symmetrically opened on a set of opposite side faces of the inner liner. Box body sliders are respectively arranged on two sides of the low-temperature column temperature box body, and box cover sliders are respectively arranged on two sides of the low-temperature column temperature box cover. The box body sliders and the box cover sliders on the same side are aligned and jointly inserted into the slide rail on the same side and can slide along the slide rail; the low-temperature column temperature box body and the low-temperature column temperature box cover are buckled up and down to form a low-temperature column temperature box. A lifting structure is installed in the low-temperature column temperature box. The chromatographic column hanger is rotatably installed on the lifting structure and its height is adjusted by the control of the lifting structure; a heating plate and a fan are installed in the gas chromatograph column temperature box. The heating plate is located between the low-temperature column temperature box and the fan and faces the low-temperature column temperature box.

2. The gas chromatography-mass spectrometry combined instrument extended low-temperature column oven device according to claim 1, characterized in that: The slide rail is a long strip groove, and the cross-section of the long strip groove is a T-shaped structure; the box body slider and the box cover slider are long strip sliders with the same structure. The long strip slider is an L-shaped cross-section structure. The box body slider and the box cover slider are aligned to form a T-shaped cross-section structure and jointly inserted into the long strip groove of the T-shaped structure of the slide rail and can slide along the long strip groove.

3. The gas chromatography-mass spectrometry combined instrument extended low-temperature column oven device according to claim 1, characterized in that: A protective sieve plate is arranged at the bottom of the low-temperature column temperature box body, and the protective sieve plate is located below the chromatographic column hanger.

4. The gas chromatography-mass spectrometry combined instrument extended low-temperature column oven device according to claim 1, characterized in that: The lifting structure includes a lifting screw, a screw hole and a cylindrical rotating body; the screw hole is opened at the center of the top of the low-temperature column temperature box cover. An installation hole and an installation groove are opened at the top of the chromatographic column hanger, and the installation hole is communicated with the installation groove; the lifting screw is screwed into the screw hole, and the lower end of the lifting screw passes through the installation hole and is connected with the cylindrical rotating body. The cylindrical rotating body is located in the installation groove, and the diameter of the cylindrical rotating body is larger than the aperture of the installation hole.

5. The gas chromatography-mass spectrometry combined instrument extended low-temperature column oven device according to claim 1, characterized in that: A box body handle is installed on the low-temperature column temperature box body, and a box cover handle is installed on the low-temperature column temperature box cover. The box body handle and the box cover handle are opposite in position.

6. The gas chromatography-mass spectrometry combined instrument extended low-temperature column oven device according to claim 1, wherein: The gas chromatograph column temperature box and the low-temperature column temperature box body are both box bodies made of stainless steel material, and the low-temperature column temperature box cover is a box cover made of stainless steel material.

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