Capillary column cleaning device

Abstract

The utility model provides a capillary column cleaning device, which relates to the technical field of gas chromatography devices and comprises a bottom plate, a fixing frame, a first capillary frame, a second capillary frame, a capillary hollow column, a solvent bottle, a waste liquid bottle and a gas circuit control device. The first capillary frame and the second capillary frame are adjacently installed in buckles on the fixing frame, the solvent bottle is installed on a bottom plate between the first capillary frame and the second capillary frame, the waste liquid bottle is installed on a bottom plate on one side of the second capillary frame, the capillary hollow column is installed on the first capillary frame, and the air inlet end of the capillary hollow column is connected with the air path control device. According to the gas chromatography capillary column cleaning device disclosed by the invention, the problems that the existing gas chromatography capillary column cleaning device is complicated in design structure, the capillary column is tedious to clean, and the existing gas chromatography capillary column cleaning device is inconvenient to use in a common laboratory can be solved.

Description

Technical Field

[0001] The utility model relates to the technical field of gas chromatography devices, in particular to a capillary column cleaning device. Background Art

[0002] High-performance quartz capillary columns are important components of gas chromatographs. Generally, capillary columns are tens of meters long or even longer. During use, the quartz capillary column is easily contaminated and the column efficiency is reduced due to factors such as samples, analysis time, column temperature, etc., resulting in baseline drift, poor peak shape, disappearance of the target, etc. The usual solution is to age the capillary column, that is, to set a programmed temperature condition under the condition of carrier gas, control the maximum baking temperature to be lower than the maximum temperature of the capillary column by 20°C, and at the same time, with the help of the carrier gas flowing through the capillary column, the contaminants remaining in the column are baked out at high temperature to restore the performance of the capillary column. Since some non-volatile compounds (high molecular weight or high boiling point) are difficult to restore to normal through high-temperature aging after entering the capillary column, the use of a suitable organic solvent to clean the contaminated capillary column cavity can effectively eliminate internal residues and restore the performance of the capillary column.

[0003] However, there is no special equipment for capillary column cleaning on the market, and the existing patented cleaning devices are complex in design and structure, and the capillary column cleaning is cumbersome, which is not convenient for promotion and use in ordinary laboratories. Therefore, this application proposes a capillary column cleaning device. Utility Model Content

[0004] In order to overcome the problems in the background technology, the utility model provides a capillary column cleaning device to solve the problem that the current gas chromatography capillary column cleaning device has a complex design structure, cumbersome capillary column cleaning, and is not convenient for use in ordinary laboratories.

[0005] A capillary column cleaning device comprises a bottom plate, a fixing frame, a capillary rack 1, a capillary rack 2, an empty capillary column, a solvent bottle, a waste liquid bottle and an air path control device, wherein the fixing frame is vertically mounted on the bottom plate, the capillary rack 1 and the capillary rack 2 are adjacently mounted in buckles on the fixing frame, the solvent bottle is mounted on the bottom plate between the capillary rack 1 and the capillary rack 2, the waste liquid bottle is mounted on the bottom plate on one side of the capillary rack 2, the empty capillary column is mounted on the capillary rack 1, the air inlet end of the empty capillary column is connected to the air path control device, the air outlet end of the empty capillary column is inserted into the solvent bottle through the sealing septum of the solvent bottle, and the sealing septum of the waste liquid bottle is inserted with an emptying column.

[0006] Furthermore, the gas path control device comprises a gas chromatograph inlet and a carrier gas generator connected to the gas chromatograph inlet, and the gas inlet end of the capillary empty column is connected to the gas chromatograph inlet.

[0007] Furthermore, a transition plate is installed on the fixed frame between the capillary rack 1 and the capillary rack 2, and the transition plate is in an upwardly arched arc shape, and the solvent bottle is installed on the bottom plate between the transition plate and the capillary rack 2.

[0008] Furthermore, a magnetic plate is provided on the bottom plate, and magnetic blocks and the magnetic plate are provided at the bottom of the solvent bottle and the waste liquid bottle for magnetic mounting.

[0009] Compared with the prior art, the beneficial effects of the utility model are:

[0010] The present application is provided with a fixing frame, a capillary frame 1, a capillary frame 2, an empty capillary column, a solvent bottle, and a waste liquid bottle. The capillary column to be cleaned is convenient to install and not easy to be damaged during cleaning. The injection port and the carrier gas generator of the gas chromatograph are used as the gas path control device, and the empty capillary column is used as the carrier gas pipeline. The cleaning solvent in the solvent bottle is pressed into the cavity of the capillary column to be cleaned through the pressure difference for continuous cleaning. After passing through the capillary column, the solvent flows into the waste liquid collection bottle. The washing operation is simple and convenient, which solves the problem that the current gas chromatography capillary column cleaning device is complicated in design structure, the capillary column cleaning is cumbersome, and it is not convenient for ordinary laboratories to use. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] In order to clearly illustrate the technical solutions in the embodiments of the present utility model, the drawings required for use in describing the embodiments are described.

[0012] Figure 1 It is a schematic diagram of the overall structure of the utility model;

[0013] Figure 2 This is a schematic diagram of the fixing frame structure of the utility model;

[0014] Figure 3 It is a schematic diagram of the connection structure of the utility model.

[0015] 1-bottom plate, 11-magnetic plate, 2-fixed frame, 21-clip, 3-capillary rack 1, 4-capillary rack 2, 5-empty capillary column, 6-solvent bottle, 7-waste liquid bottle, 8-gas path control device, 81-gas chromatograph injection port, 82-carrier gas generator, 9-capillary column to be cleaned, 10-transition plate, 20-magnetic block. DETAILED DESCRIPTION

[0016] In order to make the purpose, technical solution and beneficial effects of the present invention clearer, the preferred embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings to facilitate understanding by technicians.

[0017] The utility model discloses a capillary column cleaning device, see Figure 1-3A capillary column cleaning device comprises a base plate 1, a fixing frame 2, a capillary rack 1 3, a capillary rack 2 4, a capillary empty column 5, a solvent bottle 6, a waste liquid bottle 7 and an air path control device 8, wherein the fixing frame 2 is vertically mounted on the base plate 1, the capillary rack 1 3 and the capillary rack 2 4 are adjacently mounted in the buckle 21 on the fixing frame 2, the solvent bottle 6 is mounted on the base plate 1 between the capillary rack 1 3 and the capillary rack 2 4, the waste liquid bottle 7 is mounted on the base plate 1 on one side of the capillary rack 2 4, the capillary empty column 4 is mounted on the capillary rack 1 3, the air inlet end of the capillary empty column 4 is connected to the air path control device 8, the air outlet end of the capillary empty column 4 is inserted into the solvent bottle 6 through the sealing septum of the solvent bottle 6, and the sealing septum of the waste liquid bottle 7 is inserted with an emptying column 71.

[0018] The bottom plate 1 can move the fixed frame 2 close to the gas circuit control device 8 for convenient pipeline connection. The capillary rack 1 3 and the capillary rack 2 4 can be installed with a capillary empty column 5 and a capillary column to be cleaned 9. The capillary empty column 5 is a common commercially available chromatographic fused silica capillary column empty column with a length of not less than 1m. The fixed frame 2 is convenient for stably installing the capillary rack 1 3 and the capillary rack 2 4 through the buckle 21, so that the capillary empty column 5 and the capillary column to be cleaned 9 can be smoothly led out and stably connected with the solvent bottle 6, the waste liquid bottle 7 and the gas circuit control device 8 to avoid capillary breakage, and ensure that the capillary is smoothly cleaned by pressure difference and detergent. The solvent bottle can use a 40mL purge and capture injection bottle, and the sealing gasket is made of polytetrafluoroethylene (PTFE) to be compatible with the solvent Bottle 6 is adapted to waste liquid bottle 7, which is made of glass and is used to collect cleaning waste liquid. When connected, one end of the empty capillary column 5 is connected to the gas path control device 8, and the other end is led out through the sealing septum and inserted into the solvent bottle 6, with the nozzle being more than 1 cm away from the liquid surface of the cleaning solvent. The outlet end of the capillary column 9 to be cleaned is inserted into the solvent bottle 6 through the sealing septum, and the nozzle extends to a sufficient depth below the liquid surface. The injection port end is inserted into the waste liquid bottle 7 and fixed so that the lower end of the emptying column 71 is located above the liquid surface. The gas path control device 8 presses the cleaning solvent in the solvent bottle 6 into the cavity of the capillary column 9 to be cleaned through the pressure difference generated by the empty capillary column 5 for continuous cleaning. The solvent flows into the waste liquid bottle 7 after passing through the capillary column 9 to be cleaned, and the washing operation is simple and convenient.

[0019] See also Figure 1-3 The gas path control device 8 includes a gas chromatograph inlet 81 and a carrier gas generator 82 connected to the gas chromatograph inlet 81. The gas inlet end of the capillary empty column 4 is connected to the gas chromatograph inlet 81. The gas path part directly utilizes the gas path system and electronic pressure control module of the laboratory gas chromatograph, which can accurately control the carrier gas flow rate and cleaning time.

[0020] See also Figure 1-3A transition plate 10 is installed on the fixed frame 2 between the capillary rack 1 3 and the capillary rack 2 4. The transition plate 10 is in an upward arc shape. The solvent bottle 6 is installed on the bottom plate 1 between the transition plate 10 and the capillary rack 2 4, which facilitates the smooth insertion of the port of the capillary empty column 5 into the solvent bottle 6 to avoid damage to the column during installation and cleaning.

[0021] See also Figure 1-3 A magnetic plate 11 is provided on the bottom plate 1, and a magnetic block 20 is provided at the bottom of the solvent bottle 6 and the waste liquid bottle 7 for magnetic installation with the magnetic plate 11, which is convenient for adjusting the position and fixing, so that the end of the capillary can be smoothly inserted into the sealing gasket, avoiding the problem of pipeline damage and cleaning failure caused by the movement and tipping of the solvent bottle 6 and the waste liquid bottle 7 after the pipeline is connected.

[0022] Working process:

[0023] Taking the cleaning of a contaminated HP-5 quartz capillary column as an example, its stationary phase is (5%-phenyl)-methylpolysiloxane, which is widely used in the detection and analysis of semi-volatile organic compounds such as chlorinated hydrocarbons, phthalates, anilines, organochlorine pesticides, polycyclic aromatic hydrocarbons, etc. It is the most common non-polar capillary column in the laboratory. According to the column characteristics:

[0024] First, add 20 mL of chromatographically pure dichloromethane into the solvent bottle 6, cover the sealing septum, and ensure the pipeline is sealed; then, fix one end of the capillary empty column 5 to the gas chromatograph injection port 81, and insert the other end into the solvent bottle 6 containing 20 mL of dichloromethane at a distance of 1 meter from the cleaning solvent liquid surface. cm or more; then, insert the outlet end of the capillary column 9 to be cleaned into the solvent bottle 6 and immerse it under the liquid surface, and insert the inlet end of the capillary column 9 to be cleaned into the waste liquid bottle 7; after the device is connected, start the gas chromatograph device, control the carrier gas generator 82 to set the pressure control module of the gas chromatograph inlet 81 to the constant flow mode, set the carrier gas flow rate to 2mL / min, and continuously pass high-purity carrier gas (helium) into the empty capillary column 5 for 5min. The cleaning solvent in the solvent bottle 6 can be pressed into the cavity of the capillary column 9 to be cleaned by using the pressure difference for continuous cleaning. After the solvent passes through the chromatographic column, it flows into the waste liquid bottle 7. After the liquid is cleaned, the outlet end of the capillary column 9 to be cleaned is removed from the liquid surface, and the air flow continuously empties the residual solvent in the column. The carrier gas is passed for 5min to clean the residual solvent in the empty column and the quartz capillary column. After the cleaning is completed, the quartz capillary column can be restored to normal use by cutting off 3~5 cm at both ends, and the waste liquid is properly disposed of after collection. The device is simple and convenient for cleaning the capillary column and can be used for cleaning various contaminated quartz capillary columns.

[0025] What is described above is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes within the technical scope disclosed by the present invention according to the technical scheme and the utility model concept of the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A capillary column cleaning device, characterized in that: The invention comprises a base plate (1), a fixing frame (2), a capillary rack 1 (3), a capillary rack 2 (4), an empty capillary column (5), a solvent bottle (6), a waste liquid bottle (7) and an air path control device (8), wherein the fixing frame (2) is vertically mounted on the base plate (1), the capillary rack 1 (3) and the capillary rack 2 (4) are adjacently mounted in a buckle (21) on the fixing frame (2), and the solvent bottle (6) is mounted between the capillary rack 1 (3) and the capillary rack 2 (4). The waste liquid bottle (7) is mounted on the bottom plate (1) between the capillary racks (4) and the second capillary rack (4). The capillary empty column (5) is mounted on the capillary rack (3). The air inlet end of the capillary empty column (5) is connected to the air path control device (8). The air outlet end of the capillary empty column (5) is inserted into the solvent bottle (6) through the sealing gasket of the solvent bottle (6). The sealing gasket of the waste liquid bottle (7) is inserted with an emptying column (71).

2. The capillary column cleaning device according to claim 1, characterized in that: The gas path control device (8) comprises a gas chromatograph inlet (81) and a carrier gas generator (82) connected to the gas chromatograph inlet (81), and the gas inlet end of the capillary empty column (5) is connected to the gas chromatograph inlet (81).

3. The capillary column cleaning device according to claim 1, characterized in that: A transition plate (10) is installed on the fixed frame (2) between the capillary frame 1 (3) and the capillary frame 2 (4), and the transition plate (10) is in an upwardly arched arc shape. The solvent bottle (6) is installed on the bottom plate (1) between the transition plate (10) and the capillary frame 2 (4).

4. The capillary column cleaning device according to claim 1, characterized in that: A magnetic attraction plate (11) is provided on the bottom plate (1), and magnetic attraction blocks (20) are provided at the bottom of the solvent bottle (6) and the waste liquid bottle (7) and are magnetically mounted on the magnetic attraction plate (11).

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