Large-volume solid-phase extraction device

Abstract

The utility model belongs to the technical field of chemical analysis appliances, and particularly relates to a large-volume solid-phase extraction device which comprises a large-volume sample bottle, a flow guide pipe, a solid-phase extraction column, a vacuum drainage bottle and a tail liquid collecting box which are sequentially connected in a sealed mode, a flow guide control valve is arranged on the flow guide pipe, and the vacuum drainage bottle comprises a drainage bottle body. The top of the drainage bottle body is provided with an exhaust tube opening and a solid-phase extraction column connector, the exhaust tube opening is communicated with a negative-pressure exhaust device, a control valve is arranged on the exhaust tube, a shell of the drainage bottle body is sleeved with a jacket in a sealed mode, and the drainage bottle body is communicated with the jacket through an opening in the lower end. The lower end of the clamping sleeve is communicated with the tail liquid collecting box through a drainage pipe, a control valve is arranged on the drainage pipe, the top of the clamping sleeve is communicated with the top of the tail liquid collecting box through a ventilation pipe, and an air valve is arranged on the ventilation pipe. According to the utility model, the negative pressure can quickly reach the pressure required by an experiment, the cost is low, the occupied space is small, and the pressure adjustment is simple and quick.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical analysis instruments, and particularly relates to a large-volume solid-phase extraction device. Background Art

[0002] Solid phase extraction is a sample pretreatment technology developed in recent years. It is mainly used for sample separation, purification and enrichment. Its main purpose is to reduce sample matrix interference and improve detection sensitivity. Large-volume solid phase extraction is one of the necessary pretreatment methods for trace substance detection. When persistent pollutants in the environment and food, such as agricultural and animal residues, mycotoxins, heavy metals and other harmful substances are detected, due to their very low content, solid phase extraction is often required for enrichment and purification of target substances in a large number of samples during trace level analysis. During analysis, the convenience, universality and economy of solid phase extraction devices used in daily experiments are very important. In the existing technology, fully automated large-volume solid phase extraction instruments are expensive, and solid phase extraction The columns and receiving bottles are specially matched, with poor universality and high analysis cost. In addition, it is difficult to achieve the perfect combination of large-volume elution and negative pressure suction in the existing commercial solid-phase extraction devices. Although they are easy to use, they generally have the following problems: 1. The large-volume waste liquid receiving box connected to the solid-phase extraction column is integrated with the negative pressure vacuum chamber, and its sealing is difficult to ensure and control, which greatly increases the vacuuming time. Waste liquid is also easy to enter the vacuuming device and damage the vacuuming equipment; 2. When the filler particles are small and the liquid outflow is subject to large resistance or even blockage, it is impossible to keep the liquid flow smooth by timely adjusting the negative pressure; 3. The structure is complex, the cost is high, and the equipment occupies a large volume, which is inconvenient to move or carry. Utility Model Content

[0003] In view of the above problems, the purpose of the utility model is to provide a large-volume solid-phase extraction device which can quickly make the negative pressure reach the pressure required for the experiment, has a simple structure, low cost, occupies a small space, and can timely adjust the negative pressure to keep the liquid outflow smooth when the liquid flow is subject to large resistance or even blockage.

[0004] The purpose of the utility model is achieved through the following technical solutions: a large-volume solid-phase extraction device, comprising a support mechanism, a large-volume sample bottle, a guide tube, a solid-phase extraction column, a vacuum drainage bottle and a tail liquid collection box, wherein the large-volume sample bottle is placed on the support mechanism, the lower end of the large-volume sample bottle is sealed with the guide tube, the guide tube is provided with a guide control valve, the lower end of the guide tube is detachably sealed with the solid-phase extraction column, the solid-phase extraction column, the vacuum drainage bottle and the tail liquid collection box are sequentially connected from top to bottom through a detachable sealed connection structure, The vacuum drainage bottle comprises a drainage bottle body, a suction pipe port and a solid phase extraction column interface are arranged on the top of the drainage bottle body, the suction pipe port is connected with a negative pressure suction device through a suction pipe, and a control valve is arranged on the suction pipe, a jacket is sealed on the outer shell of the drainage bottle body, the drainage bottle body is connected with the jacket through an opening at the lower end, the lower end of the jacket is connected with the tail liquid collection box through a drainage pipe, a control valve is arranged on the drainage pipe, the top of the jacket is connected with the top of the tail liquid collection box through a ventilation pipe, and an air valve is arranged on the ventilation pipe.

[0005] Furthermore, the support mechanism comprises a support rod vertically arranged on the base, a support plate is connected to the support rod via a cantilever, and the large-volume sample bottle is placed in an opening on the support plate.

[0006] Furthermore, the drainage bottle body and the jacket are both inverted cones, and the capacity of the vacuum drainage bottle is no more than one third of the capacity of the tail liquid collection box.

[0007] Furthermore, a plurality of solid phase extraction column interfaces are provided on the top of the drainage bottle body, and the lower end of the solid phase extraction column can be sealed and connected to the drainage bottle body through the solid phase extraction column interface, and other interfaces among the plurality of solid phase extraction column interfaces that are not connected to the solid phase extraction column are provided with a detachable sealing structure.

[0008] Furthermore, the detachable sealing structure is a sealing rod, which has a simple structure and is easy to seal and withdraw.

[0009] Furthermore, the top of the drainage bottle body is flush with the top of the jacket and is integrally connected, and the vacuum drainage bottle is placed on a supporting platform on the top of the tail liquid collection box.

[0010] Furthermore, a discharge control valve is provided on the discharge pipe outlet of the tail liquid collection box.

[0011] Furthermore, the large-volume sample bottle is a large-capacity syringe. When the liquid outflow encounters great resistance or even obstruction, positive pressure is applied to the liquid through the syringe, and used in conjunction with the negative-pressure vacuum drainage bottle to increase the pressure difference at both ends of the solid phase extraction column, so that the liquid outflow remains smooth.

[0012] Furthermore, the guide tube includes a guide hose and a straight tube connected to the lower end of the guide hose. The straight tube is made of a material with good thermal conductivity, and a heater is provided on the outer wall of the straight tube. The heater can be used to heat the liquid flowing through the straight tube to meet the extraction temperature as needed.

[0013] Furthermore, the heater comprises a tubular jacket coaxially sleeved with the straight tube, sealing rings are integrally connected to both ends of the tubular jacket, a sealing gasket is arranged between the sealing ring and the straight tube, and the tubular jacket is provided with an inlet pipe and an outlet pipe for heating gas to enter and exit.

[0014] In the utility model, during the experiment, the large volume sample bottle is first placed on the supporting mechanism, and the lower end of the large volume sample bottle is connected with the guide tube, the solid phase extraction column, the vacuum drainage bottle and the tail liquid collection box in sequence from top to bottom, the sealing and firmness of the connection of each component are checked, the upper sample liquid is placed in the large volume sample bottle through the upper liquid port of the large volume sample bottle, and the upper liquid port is sealed, the guide control valve on the guide tube is opened, the control valve on the exhaust pipe is opened, and the negative pressure exhaust setting is started to exhaust the air in the vacuum drainage bottle. At this time, the control valve on the drainage pipe and the air valve on the ventilation pipe are opened. The valve is closed. At this time, only negative pressure pumping is required for the vacuum drainage bottle, which greatly reduces the capacity of negative pressure pumping. The negative pressure in the vacuum drainage bottle can quickly reach the negative pressure required for the experiment. The sample liquid flows from the drainage tube through the solid phase extraction column into the drainage bottle body and into the jacket through the opening at the lower end of the drainage bottle body. When the liquid level in the jacket rises and overflows the opening at the lower end of the drainage bottle body to reach a certain height, the liquid isolates the air pressure in the drainage bottle body from the jacket and the air pressure between the tail liquid collection box connected to the jacket through the drainage tube. When the liquid level in the vacuum drainage bottle continues to rise, the drainage tube can be opened to The control valve arranged on the pipe discharges the liquid into the tail liquid collection box. When the control valve is opened, the opening of the control valve should be controlled so that the flow rate of the liquid discharged into the tail liquid collection box is adapted to the flow rate of the liquid flowing into the drainage bottle body, so as to avoid the liquid flow rate of the liquid discharged into the tail liquid collection box being too fast so that the liquid at the lower end of the drainage bottle body cannot be emptied and air isolation cannot be achieved. The jacket can be used as a buffer gap to store the liquid flowing out of the drainage bottle body, so as to facilitate the observation and control of the liquid discharge, so that the air pressure between the drainage body and the tail liquid collection box is always in a liquid isolation state, and at the same time, avoid the liquid level in the drainage bottle body being too high during extraction. Enter the negative pressure exhaust device to damage the device. In addition, due to the negative pressure state in the vacuum drainage bottle, when the pressure difference between the vacuum drainage bottle and the tail liquid collection box is too large and the liquid cannot be discharged into the tail liquid collection box smoothly, open the air valve on the ventilation pipe, and the jacket and the tail liquid collection box are connected through the ventilation pipe, so that the air pressure in the two is balanced, so that the liquid in the liquid jacket is discharged smoothly, and then the ventilation valve is closed. At this time, due to the drop of liquid level, the opening at the lower end of the drainage bottle body is exposed, and the drainage bottle body is connected with the jacket to make the air pressure in the two reach a new balance, thereby realizing negative pressure regulation and ensuring the smooth discharge of waste liquid.

[0015] Beneficial effects: The utility model can make the negative pressure quickly reach the pressure required for the experiment, has a simple structure, low cost, small space occupation, simple and quick pressure regulation, and can timely adjust the negative pressure to keep the liquid outflow smooth when the liquid flow is subject to large resistance or even blockage. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] The present invention is described in more detail below by way of example with reference to the accompanying drawings, in which:

[0017] Figure 1 : The structural diagram of embodiment 1 of the utility model.

[0018] Figure 2 : A schematic structural diagram of a vacuum drainage bottle in Example 1 of the present invention.

[0019] Figure 3 : Schematic diagram of the installation structure of the heater in Example 2 of the utility model.

[0020] In the figure: 01. Support mechanism, 02. Large volume sample bottle, 03. Diversion tube, 04. Diversion control valve, 05. Adapter, 011. Support rod, 012. Support plate, 021. Upper liquid port, 031. Diversion hose, 032. Straight pipe, 033. Heater, 0331. Tubular jacket, 0332. Sealing ring, 0333. Sealing gasket, 0334. Inlet pipe, 0335. Outlet pipe, 1. Solid phase extraction column, 2. Vacuum drainage bottle, 3. Tail liquid collection box, 4. Support platform, 21. Drainage bottle body, 22. Vacuum pipe port, 23. Solid phase extraction column interface, 24. Control valve, 25. Jacket, 26. Removable sealing structure, 31. Drainage control valve, 211. Opening, 251. Drainage tube, 252. Control valve, 253. Ventilation pipe, 254. Air valve. DETAILED DESCRIPTION

[0021] In the present utility model, for the convenience of description, the relative position relationship of each component is described according to the layout of the drawings in the specification, such as: the position relationship of up, down, left, right, etc. is determined according to the layout direction in the drawings in the specification.

[0022] Example 1, reference Figure 1 , Figure 2A large volume solid phase extraction device comprises a support mechanism 01, a large volume sample bottle 02, a guide tube 03, a solid phase extraction column 1, a vacuum drainage bottle 2 and a tail liquid collection box 3, wherein the large volume sample bottle 02 is placed on the support mechanism 01, the lower end of the large volume sample bottle 02 is sealedly connected with the guide tube 03, the guide tube 03 is provided with a guide control valve 04, the lower end of the guide tube 03 is detachably sealed and connected to the solid phase extraction column 1 through an adapter 05, the solid phase extraction column 1, the vacuum drainage bottle 2 and the tail liquid collection box 3 are sequentially connected from top to bottom through a detachable sealing connection structure, and the vacuum drainage bottle 2 comprises a drainage bottle body 2 1. A suction pipe port 22 and a solid phase extraction column interface 23 are provided on the top of the drainage bottle body 21. The suction pipe port 22 is connected to the negative pressure suction device through a suction pipe, and a control valve 24 is provided on the suction pipe. A jacket 25 is sealed on the outer shell of the drainage bottle body 21. The drainage bottle body 21 is connected to the jacket 25 through an opening 211 at the lower end. The lower end of the jacket 25 is connected to the tail liquid collection box 3 through a drainage pipe 251. A control valve 252 is provided on the drainage pipe 251. The top of the jacket 25 is connected to the top of the tail liquid collection box 3 through a vent pipe 253, and an air valve 254 is provided on the vent pipe 253.

[0023] The support mechanism 01 includes a support rod 011 vertically arranged on a base, and a support plate 012 is connected to the support rod 011 via a cantilever. The large-volume sample bottle 02 is placed in an opening on the support plate 012 .

[0024] The drainage bottle body 21 and the jacket 25 are both inverted cones. The capacity of the vacuum drainage bottle 2 is not greater than one-third of the capacity of the tail liquid collection box 3. A plurality of solid phase extraction column interfaces 23 are provided on the top of the drainage bottle body 21. The lower end of the solid phase extraction column 1 can be sealed and connected to the drainage bottle body 21 through the solid phase extraction column interface 23. The other interfaces of the plurality of solid phase extraction column interfaces 23 that are not connected to the solid phase extraction column 1 are provided with a detachable sealing structure 26. The detachable sealing structure 26 is a sealing rod with a simple structure and is easy to seal and extract. A discharge control valve 31 is provided on the discharge pipe outlet of the tail liquid collection box 3.

[0025] The large-volume sample bottle 02 is a large-capacity syringe. When the liquid outflow encounters great resistance or even obstruction, the syringe applies positive pressure to the liquid and is used in conjunction with the negative-pressure vacuum drainage bottle 2 to increase the pressure difference at both ends of the solid phase extraction column 1, so that the liquid outflow remains smooth.

[0026] In the present invention, during the experiment, the large volume sample bottle 02 is first placed on the support mechanism 01, and the guide tube 03, the solid phase extraction column 1, the vacuum drainage bottle 2 and the tail liquid collection box 3 are sequentially connected from top to bottom at the lower end of the large volume sample bottle 02, and the sealing and firmness of the connection of each component are checked. The sample liquid is placed in the large volume sample bottle 02 through the upper liquid port 021 of the large volume sample bottle 02, and the upper liquid port 021 is sealed, the guide control valve 04 on the guide tube 03 is opened, the control valve 24 on the exhaust pipe is opened, and the negative pressure exhaust setting is started to exhaust the air in the vacuum drainage bottle 2. At this time, the control valve 252 on the drainage tube 251 and the ventilation pipe 2 The air valve 254 on 53 is closed. At this time, only the vacuum drainage bottle 2 needs to be evacuated under negative pressure, which greatly reduces the capacity of negative pressure evacuation. The negative pressure in the vacuum drainage bottle 2 can quickly reach the negative pressure required for the experiment. The sample liquid flows from the guide tube 03 through the solid phase extraction column 1 into the drainage bottle body 21 and flows into the jacket 25 through the opening 211 at the lower end of the drainage bottle body 21. When the liquid level in the jacket 25 rises and overflows the opening 211 at the lower end of the drainage bottle body 21 to reach a certain height, the liquid isolates the air pressure in the drainage bottle body 21 from the air pressure between the jacket 25 and the tail liquid collection box 3 connected to the jacket 25 through the drainage tube 251. When the liquid level in the vacuum drainage bottle 2 continues to rise, , the liquid can be discharged into the tail liquid collection box 3 by opening the control valve 252 arranged on the drainage tube 251. When the control valve 252 is opened, the opening of the control valve 252 should be controlled so that the flow rate of the liquid discharged into the tail liquid collection box 3 is adapted to the flow rate of the liquid flowing into the drainage bottle body 21, so as to avoid the liquid flow rate of the tail liquid collection box 3 being too fast so that the liquid at the lower end of the drainage bottle body 21 cannot be emptied and air isolation can be achieved. The jacket 25 can be used as a buffer gap to store the liquid flowing out of the drainage bottle body 21, so as to facilitate the observation and control of the liquid discharge, so that the air pressure between the drainage body 21 and the tail liquid collection box 3 is always in an isolated state, and at the same time, it is avoided that the liquid level in the drainage bottle body 21 is too high during extraction. Liquid enters the negative pressure exhaust device and damages the device. In addition, since the vacuum drainage bottle 2 is in a negative pressure state, when the pressure difference between the vacuum drainage bottle 2 and the tail liquid collection box 3 is too large, resulting in the liquid being unable to be smoothly discharged into the tail liquid collection box 3, the air valve 254 on the vent pipe 253 is opened, and the jacket 25 is connected to the tail liquid collection box 3 through the vent pipe 253, so that the air pressure in the two reaches a balance, so that the liquid in the liquid jacket 25 is smoothly discharged, and then the vent valve 254 is closed. At this time, due to the drop in the liquid level, the opening 211 at the lower end of the drainage bottle body 21 is exposed, and the drainage bottle body 21 is connected to the jacket 25 so that the air pressure in the two reaches a new balance, thereby realizing negative pressure regulation and ensuring smooth discharge of waste liquid.

[0027] Example 2, reference Figure 3As a further optimized design of Example 1, the top of the drainage bottle body 21 is flush with the top of the jacket 25 and is integrally connected. The vacuum drainage bottle 2 is placed on the support platform 4 on the top of the tail liquid collection box 3. The guide tube 03 includes a guide hose 031 and a straight tube 032 connected to the lower end of the guide hose 031. The straight tube 032 is made of a material with good thermal conductivity, and a heater 033 is provided on the outer wall of the straight tube 032. The heater 033 can be used to heat the liquid flowing through the straight tube 032 as needed to meet the extraction temperature. The heater 033 includes a tubular jacket 0331 coaxially sleeved with the straight tube 032. Sealing rings 0332 are integrally connected at both ends of the tubular jacket 0331. A sealing gasket 0333 is provided between the sealing ring 0332 and the straight tube 032. An inlet pipe 0334 and an outlet pipe 0335 for heating gas in and out are provided on the tubular jacket 0331.

[0028] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments. The above embodiments and descriptions are only preferred examples of the present invention and are not intended to limit the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention. The scope of protection of the present invention is defined by the attached claims and their equivalents.

Claims

1. A large volume solid phase extraction device, characterized in that: The invention comprises a supporting mechanism, a large-volume sample bottle, a flow guide tube, a solid phase extraction column, a vacuum drainage bottle and a tail liquid collection box, wherein the large-volume sample bottle is placed on the supporting mechanism, the lower end of the large-volume sample bottle is sealedly connected with the flow guide tube, the flow guide tube is provided with a flow guide control valve, the lower end of the flow guide tube is detachably sealedly connected with the solid phase extraction column, the solid phase extraction column, the vacuum drainage bottle and the tail liquid collection box are sequentially connected from top to bottom through a detachable sealed connection structure, the vacuum drainage bottle comprises a drainage bottle body, the A suction pipe port and a solid phase extraction column interface are provided on the top of the drainage bottle body. The suction pipe port is connected with the negative pressure suction device through a suction pipe, and a control valve is provided on the suction pipe. A jacket is sealed on the outer shell of the drainage bottle body. The drainage bottle body is connected with the jacket through an opening at the lower end. The lower end of the jacket is connected with the tail liquid collection box through a drainage pipe. A control valve is provided on the drainage pipe. The top of the jacket is connected with the top of the tail liquid collection box through a ventilation pipe, and an air valve is provided on the ventilation pipe.

2. A large volume solid phase extraction device as claimed in claim 1, characterized in that: The drainage bottle body and the jacket are both inverted cone-shaped, and the capacity of the vacuum drainage bottle is no more than one third of the capacity of the tail liquid collection box.

3. A large volume solid phase extraction device as claimed in claim 1, characterized in that: A plurality of solid phase extraction column interfaces are arranged on the top of the drainage bottle body, and other interfaces among the plurality of solid phase extraction column interfaces that are not connected to the solid phase extraction column are provided with a detachable sealing structure.

4. A large volume solid phase extraction device according to any one of claims 1 to 3, characterized in that: Large volume vials are larger capacity syringes.

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