CN115253381B - Gas positive pressure type solid phase extraction device - Google Patents

Gas positive pressure type solid phase extraction device Download PDF

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Publication number
CN115253381B
CN115253381B CN202211071268.5A CN202211071268A CN115253381B CN 115253381 B CN115253381 B CN 115253381B CN 202211071268 A CN202211071268 A CN 202211071268A CN 115253381 B CN115253381 B CN 115253381B
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plate
extraction
liquid adding
pipeline
liquid
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CN115253381A (en
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罗瑞峰
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Xinjiang Academy of Agricultural and Reclamation Sciences
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Xinjiang Academy of Agricultural and Reclamation Sciences
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/14Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the introduction of the feed to the apparatus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/16Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the fluid carrier
    • B01D15/163Pressure or speed conditioning
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/24Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the treatment of the fractions to be distributed
    • B01D15/242Intermediate storage of effluents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/24Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the treatment of the fractions to be distributed
    • B01D15/247Fraction collectors

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The application discloses a positive pressure gas solid phase extraction device, which comprises: the device comprises a pressurizing device, an extraction column and a collecting device; the pressurizing device presses the liquid into the extraction column by pressurization, and the collecting device collects the liquid flowing out of the extraction column; the liquid flows into the collecting device after passing through the extraction column, the specific substances in the liquid are remained in the extraction column, and then the specific substances are eluted into the collecting device through the eluent. Solves the problems of the existing solid phase extraction device that: uneven pressurization in the extraction process leads to low extraction efficiency; and the liquid adding device cannot uniformly add liquid to a plurality of extraction columns at the same time. The solid phase extraction device achieves a gas positive pressure type solid phase extraction device which can control the pressurizing size and the liquid adding device to simultaneously and uniformly add liquid to a plurality of extraction columns; the extraction efficiency of the solid phase extraction device is improved.

Description

Gas positive pressure type solid phase extraction device
Technical Field
The application relates to the technical field of solid phase extraction devices, in particular to a gas positive pressure type solid phase extraction device.
Background
Solid Phase Extraction (SPE) is a sample pretreatment technology developed in recent years, and is developed by combining liquid-Solid Extraction and column liquid chromatography, and is mainly used for separating, purifying and concentrating samples. Existing solid phase extraction devices are classified into negative pressure type and positive pressure type.
The positive pressure type has a gas positive pressure type and a plunger rod positive pressure type. The gas positive pressure type solid phase extraction device is mainly characterized in that the upper end of a solid phase extraction column is pressurized through a gas pressurizing system to form an up-down pressure difference for sample liquid extraction, and in order to ensure the consistency of extraction, the gas positive pressure type solid phase extraction device is required to independently set a control valve for each column, the pressure control system is complex, and the liquid adding is complex and the extraction efficiency is low. The plunger rod positive pressure type solid phase extraction device mainly comprises a plunger rod and a small column cavity, wherein a piston cavity is formed by the plunger rod and the small column cavity to push sample liquid to extract, so that the plunger rod is required to be washed for multiple times in each step in the extraction process to prevent pollution among samples, and the extraction time of each sample is prolonged intangibly. In addition, the plunger rod and the small column can be matched for sealing, and the plunger rod positive pressure device is not strong in universality.
The existing solid phase extraction device comprises: uneven pressurization in the extraction process leads to low extraction efficiency; and the liquid adding device cannot uniformly add liquid to a plurality of extraction columns at the same time.
Disclosure of Invention
In view of the above, the main object of the present application is to provide a gas positive pressure type solid phase extraction device capable of controlling the pressurizing size and the liquid adding device to uniformly add liquid to a plurality of extraction columns at the same time.
In order to achieve the above purpose, the technical scheme of the application is realized as follows:
a positive gas pressure type solid phase extraction device comprising: the device comprises a pressurizing device, an extraction column and a collecting device; the pressurizing device is communicated with the feed inlet of the extraction column, and the feed inlet of the collecting device is connected with the discharge outlet of the extraction column;
further comprises: sealing the liquid adding plate; the sealed liquid feeding plate is arranged above the extraction column and is communicated with the pressurizing device through a pressurizing connecting pipe.
In a preferred embodiment, the pressurizing means comprises: the device comprises a supercharger, a pressurizing bottle and a three-way sealing cover; the three-way sealing cover seals the pressurizing bottle, and the pressurizer is communicated with a pressurizing port of the pressurizing bottle;
a long pipe and a short pipe are arranged in the pressurized bottle, the long pipe stretches into the bottom of the liquid level in the pressurized bottle, and the short pipe stretches into the upper side of the liquid level in the pressurized bottle; the three-way sealing cover is communicated with a long pipe or a short pipe of the pressurized bottle.
In a preferred embodiment, the sealing charging plate comprises: the device comprises a pipeline lower plate, a pipeline middle plate, a pipeline upper plate and a liquid adding plate fixing frame; the pipeline lower plate, the pipeline middle plate and the pipeline upper plate are sequentially stacked from bottom to top, and the liquid adding plate fixing frame is used for fixing and supporting the three layers of liquid adding plates; sealing bayonets are arranged on two sides of the liquid adding plate fixing frame;
a liquid adding hole is formed in the middle of the upper plate penetrating through the pipeline;
the pipeline middle plate is provided with an I-shaped middle plate pipeline, the middle plate pipeline comprises two transverse middle plate pipelines and a longitudinal middle plate pipeline, and the bottom of the transverse middle plate pipeline is provided with a middle plate round hole;
the pipeline lower plate is provided with two horizontal pipelines, the horizontal pipelines are arranged right below the horizontal middle plate pipeline, a plurality of longitudinal pipelines are arranged perpendicular to the horizontal pipelines, the end points of two sides of each longitudinal pipeline are provided with liquid dropping round holes, the liquid dropping round holes are provided with flow limiting valves, outlets of the flow limiting valves are communicated with the solid phase extraction column adapter, outlets of the solid phase extraction column adapter are connected with the solid phase extraction column, and two ends of each longitudinal pipeline are respectively provided with a lower plate one-way valve channel;
the pipeline middle plate is provided with a middle plate sealing hole which is positioned right above the lower plate one-way valve channel; an upper plate sealing hole is formed in the pipeline upper plate, and the upper plate sealing hole is positioned right above the middle plate sealing hole;
and a liquid adding plate one-way valve is arranged through the upper plate sealing hole and the middle plate sealing hole.
In a preferred embodiment, a liquid adding device is further arranged above the sealing liquid adding plate, and the liquid adding device is arranged in the middle of the upper surface of the sealing liquid adding plate; one end of the liquid adding device is communicated with the pressurizing connecting pipe, and the other end of the liquid adding device is communicated with the liquid adding hole.
In a preferred embodiment, the liquid adding device comprises: the device comprises a display, a pressure gauge, a protective shell, a damper and a Hall flow pump;
the three-way adapter, the damper and the Hall flow pump are arranged below the protective shell, one end of the damper is communicated with a liquid adding one-way valve, and the other end of the damper is connected with the Hall flow pump; the other end of the liquid adding one-way valve is communicated with the pressurizing connecting pipe; the other end of the Hall flow pump is connected with the three-way adapter; the other end of the three-way adapter is communicated with the liquid filling opening, a pressure gauge above the protective shell is connected with the three-way adapter, and a display is embedded above the protective shell; the display is in communication connection with the hall flow pump.
In a preferred embodiment, the extraction column is provided with a plurality of extraction columns; the extraction column is placed on the extraction fixing frame;
the extraction fixing frame is of an upper layer structure and a lower layer structure; the extraction fixing frames on the upper layer and the lower layer are provided with extraction column fixing holes.
In a preferred embodiment, the collecting device comprises: a waste liquid tank and a receiving test tube rack;
the waste liquid tank is of a cuboid structure, a collecting opening is formed in the center of the upper surface of the waste liquid tank, and the upper surface of the waste liquid tank is recessed inwards around the collecting opening; the side surface of the waste liquid tank is communicated with a waste liquid discharge valve pipe, and the other side surface is integrally designed with a handle structure; the side surface of the waste liquid tank is integrally provided with a waste liquid tank positioning rod;
the receiving test tube rack is divided into an upper layer structure, a middle layer structure and a lower layer structure, and test tube placing holes are formed in the upper layer and the middle layer of the receiving test tube rack; the receiving test tube rack side is provided with the test tube rack locating lever integrally.
In a preferred embodiment, further comprising: a system bracket; the system support is of a cuboid frame structure, four horizontal ribs below the system support are not arranged, and a horizontal extraction support rod is arranged on the upper surface of the system support.
In a preferred embodiment, a test tube rack placing table is arranged in the system bracket, and the test tube rack placing table is provided with a drawing mechanism and a lifting mechanism in a matching way;
the drawing mechanism is characterized in that two cross bars are oppositely and horizontally arranged in the middle of the vertical direction of the cuboid frame structure, and the cross bars are horizontally and slidably connected with the test tube rack placing table through sliding rails; two test tube lifting slide rails are respectively arranged above the two cross bars;
the lifting mechanism is arranged below the test tube rack placing table;
and a positioning groove is formed in the side, close to the test tube rack placing table, of the horizontal sliding rail.
In a preferred embodiment, the system holder is snap-connected to the sealing filler plate by means of a spring.
The gas positive pressure type solid phase extraction device has the following beneficial effects:
a positive gas pressure type solid phase extraction device comprising: a pressurizing device, an extraction column and a collecting device; the pressurizing device presses the liquid into the extraction column by pressurization, and the collecting device collects the liquid flowing out of the extraction column; the extraction column is pressurized or filled with liquid through the pressurizing device, the liquid flows into the collecting device after passing through the extraction column, the specific substances in the liquid are remained in the extraction column, and then the specific substances are eluted into the collecting device through the eluent. The pressurizing device includes: sealing the liquid adding plate; the sealed liquid feeding plate is arranged above the extraction column, and the sealed liquid feeding plate is communicated with the three-way sealing cover through a pressurizing connecting pipe.
Solves the problems of the existing solid phase extraction device that: uneven pressurization in the extraction process leads to low extraction efficiency; and the liquid adding device cannot uniformly add liquid to a plurality of extraction columns at the same time. The solid phase extraction device achieves a gas positive pressure type solid phase extraction device which can control the pressurizing size and the liquid adding device to uniformly add liquid to a plurality of extraction columns at the same time; the extraction efficiency of the solid phase extraction device is improved.
Drawings
In order to more clearly illustrate the embodiments of the application or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic perspective view of a gas positive pressure type solid phase extraction device according to the present embodiment;
FIG. 2 is a schematic diagram of the sealing liquid adding plate of the positive pressure type solid phase extraction device according to the embodiment;
fig. 3 is a schematic diagram of an extraction holder and an extraction column of a positive pressure type solid phase extraction device according to the embodiment;
FIG. 4 is a schematic diagram of an exploded view of a liquid feeding device of a positive pressure type solid phase extraction device according to the present embodiment;
fig. 5 is a schematic diagram of the structure of a receiving rack of a gas positive pressure type solid phase extraction device according to the present embodiment;
FIG. 6 is a schematic diagram showing the structure of a waste liquid tank of a positive pressure type solid phase extraction device according to the present embodiment;
fig. 7 is a schematic diagram of the structure of the non-placed receiving rack and the extraction holder of the liquid adding device of the gas positive pressure type solid phase extraction device according to the embodiment.
[ Main reference numerals Specification ]
1. A pressurizing device; 11. a supercharger; 12. a pressurized bottle; 13. a three-way sealing cover; 14. a pressurizing connecting pipe;
2. sealing the liquid adding plate;
21. a pipeline lower plate; 211. a lower plate one-way valve passage; 212. a horizontal pipeline; 213. a wale pipe;
214. a liquid dropping round hole; 215. a solid phase extraction column adapter;
22. a pipeline middle plate; 221. a middle plate round hole; 222. a middle plate sealing hole; 223. a middle plate pipeline;
23. a pipeline upper plate; 231. a liquid adding hole; 232. the upper plate seals the hole;
24. a liquid adding plate fixing frame; 25. a liquid adding plate one-way valve;
3. a liquid adding device; 31. a display; 32. a pressure gauge; 33. a protective housing; 34. a damper; 35. a hall flow pump; 36. a liquid adding one-way valve; 37. three-way adapter
4. An extraction column; 5. extracting a fixing frame; 6. an extraction column fixing hole;
78. a collecting device;
7. a waste liquid tank; 71. a collection port; 72. a waste liquid discharge valve tube; 73. a waste liquid tank positioning rod;
8. receiving a test tube rack; 81. a test tube placement hole; 82. a test tube rack positioning rod;
9. a system bracket; 91. a horizontal extraction support rod; 92. a cross bar; 93. test tube rack placing table;
94. a drawing mechanism; 941. a horizontal slide rail; 942. a positioning groove;
95. a lifting mechanism; 951. lifting the slide rail;
10. and a spring buckle.
Detailed Description
The method of the present application will be described in further detail with reference to the accompanying drawings.
It should be noted that, without conflict, the embodiments of the present application and features of the embodiments may be combined with each other. The application will be described in detail below with reference to the drawings in connection with embodiments.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present application. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
It should be noted that the terms "first," "second," and the like in the description and the claims of the present application and the above figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate such that embodiments of the application described herein may be capable of being practiced otherwise than as specifically illustrated and described. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
Spatially relative terms, such as "above … …," "above … …," "upper surface at … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial location relative to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "above" or "over" other devices or structures would then be oriented "below" or "beneath" the other devices or structures. Thus, the exemplary term "above … …" may include both orientations of "above … …" and "below … …". The device may also be positioned in other different ways (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
A positive gas pressure type solid phase extraction device comprising: the device comprises a pressurizing device, an extraction column and a collecting device; the pressurizing device is communicated with the feed inlet of the extraction column, and the feed inlet of the collecting device is connected with the discharge outlet of the extraction column;
further comprises: sealing the liquid adding plate; the sealed liquid feeding plate is arranged above the extraction column and is communicated with the pressurizing device through a pressurizing connecting pipe.
In a preferred embodiment, the pressurizing means comprises: the device comprises a supercharger, a pressurizing bottle and a three-way sealing cover;
a gas positive pressure type solid phase extraction apparatus according to fig. 1 to 7, comprising: a pressurizing device 1 and an extraction column 4 and a collecting device 78; the pressurizing device 1 is communicated with a feed inlet of the extraction column 4, and a feed inlet of the collecting device 78 is connected with a discharge outlet of the extraction column 4; the pressurizing device 1 presses the liquid into the extraction column 4 by pressurization, and the collecting device 78 collects the liquid flowing out of the extraction column 4; the extraction column is pressurized or charged by the pressurizing means 1, the liquid flows into the collecting means 78 after passing through the extraction column 4, the specific substances in the liquid are left in the extraction column, and the specific substances are eluted into the collecting means 78 by the eluting solution.
The pressurizing device 1 further includes: sealing the liquid adding plate 2; the sealed liquid feeding plate is arranged above the extraction column 4, and the sealed liquid feeding plate 2 is communicated with the three-way sealing cover 13 through a pressurizing connecting pipe 14. The sealing liquid adding plate 2 not only plays a role in pressurization, but also a special pipeline is designed in the sealing liquid adding plate 2 so that liquid can be uniformly added into the extraction column 4. The liquid can be added for a plurality of extraction columns 3 at a time, so that the liquid adding speed is improved, and the extraction efficiency of the positive pressure solid phase extraction device is further improved.
Solves the problems of the existing solid phase extraction device that: uneven pressurization in the extraction process leads to low extraction efficiency; and the liquid adding device 3 cannot uniformly add liquid to the plurality of extraction columns 4 at the same time. The solid phase extraction device achieves a gas positive pressure type solid phase extraction device which can control the pressurizing size and the liquid adding device 3 can simultaneously and evenly add liquid to a plurality of extraction columns 4; the extraction efficiency of the solid phase extraction device is improved.
In order to ensure that the filling device 3 is able to accurately and uniformly fill the individual extraction columns 4 with liquid from the bottle. The pressurizing device 1 further includes: a supercharger 11, a pressurizing bottle 12 and a three-way sealing cover 13; the three-way sealing cover 13 seals the pressurizing bottle 12, and the pressurizer 11 is communicated with a pressurizing port of the pressurizing bottle 12; a long pipe and a short pipe are arranged in the pressurized bottle 12, the long pipe stretches into the bottom of the liquid level in the pressurized bottle, and the short pipe stretches into the upper side of the liquid level in the pressurized bottle 12; the three-way sealing cover 13 is communicated with a long pipe or a short pipe of the pressurized bottle 12. When the tee joint is connected with a long pipe in the pressurized bottle 12, liquid below the bottle is pressed into the extraction column 4 through the tee joint sealing cover 13, and when the tee joint is connected with a short pipe in the pressurized bottle 12, air above the bottle is pressed into the extraction column 4 through the tee joint sealing cover 13.
In order to increase the efficiency of the sealing liquid adding plate 2 in adding liquid. The sealing liquid adding plate 2 comprises: a pipeline lower plate 21, a pipeline middle plate 22, a pipeline upper plate 23 and a liquid adding plate fixing frame 24; the pipeline lower plate 21, the pipeline middle plate 22 and the pipeline upper plate 23 are sequentially stacked from bottom to top, and the liquid adding plate fixing frame 24 is used for fixing the peripheral edges of the three liquid adding plates; a liquid adding hole 231 is formed through the middle part of the pipeline upper plate 23; the pipeline middle plate 22 is provided with an I-shaped middle plate pipeline 223, the middle plate pipeline 223 comprises two transverse middle plate pipelines and a longitudinal middle plate pipeline, and the bottom of the transverse middle plate pipeline is provided with a middle plate round hole 221; the pipeline lower plate 21 is provided with two horizontal pipelines 212, the horizontal pipelines 212 are arranged right below the horizontal middle plate pipeline, a plurality of longitudinal pipelines 213 are arranged perpendicular to the horizontal pipelines 212, the middle point of each longitudinal pipeline 213 corresponds to right below the middle plate round hole 221, and two ends of each longitudinal pipeline 213 are respectively provided with a lower plate one-way valve channel 211; the middle plate of the pipeline is provided with a middle plate sealing hole 222, and the middle plate sealing hole 222 is positioned right above the lower plate one-way valve channel 211; an upper plate sealing hole 232 is formed in the pipeline upper plate, and the upper plate sealing hole 232 is positioned right above the middle plate sealing hole 222; a liquid feeding plate check valve 25 is provided through the upper plate seal hole 232 and the middle plate seal hole 222.
In order to ensure that the gas or liquid added into the extraction column 4 can be unobstructed and that no liquid overflows during the liquid adding process, the sealing is good. A liquid adding device 3 is further arranged above the sealing liquid adding plate 2, and the liquid adding device 3 is arranged in the middle of the upper surface of the sealing liquid adding plate 2; one end of the liquid adding device 3 is communicated with the pressurizing connecting pipe 14, and the other end is communicated with the liquid adding hole 231. Not only can reduce the waste of the overflow liquid to the liquid, but also can avoid the problem that the solid-phase pressurized extraction device is polluted. Further improving the extraction efficiency of the solid phase extraction device.
The gas and liquid fed to the extraction column for stabilizing the pressurizing means 3 are stable and controllable. The liquid adding device 3 comprises: a display 31, a pressure gauge 32, a protective housing 33, a damper 34, a hall flow pump 35; the three-way adapter 37, the damper 34 and the Hall flow pump 35 are protected below the protective shell, one end of the damper 34 is communicated with the liquid adding one-way valve 36, and the other end of the damper is connected with the Hall flow pump 35; the other end of the liquid adding one-way valve 36 is communicated with the pressurizing connecting pipe 14; the other end of the Hall flow pump 35 is connected with the three-way adapter 37; the other end of the three-way adapter is communicated with the liquid filling port, a 0.6MPa pressure gauge 32 above the protective shell is connected with the three-way adapter 37, and a display 31 is embedded above the protective shell; the display 31 is communicatively connected to the hall flow pump 35. The liquid adding plate one-way valve 25 is communicated with the pressurizing device 1, and gas and liquid enter the damper 34 after the pressure is increased. The damper 34 can reduce the pressure fluctuation of the gas and the liquid so that the pressure is constant when the gas and the liquid enter the extraction column 4. The hall flow pump 35 is used to calculate the volume of liquid added. The three-way adapter 37 is connected with the Hall flow path pump 34, the 0.6MPa pressure gauge 32 and the liquid adding hole 231 on the pipeline board 23 to form a flow path.
In order to ensure that the extraction holder 5 can accurately receive the liquid added by the liquid adding device 3. The extraction column 4 is provided with a plurality of extraction columns; the extraction column 4 is placed on the extraction fixing frame 5; the extraction fixing frame 5 is of an upper layer structure and a lower layer structure; the extraction fixing frames 5 on the upper layer and the lower layer are provided with extraction column fixing holes 6. The arrangement of the two-layer structure can ensure that the extraction column 4 is stably fixed to the extraction fixing frame 5. It is ensured that the extraction column can be aligned to the solid phase extraction column adapter 215 below the lower plate of the upper seal addition plate 2. The extraction fixing frame 5 is made of cold-rolled aluminum plate material, has the length and width of 31cm multiplied by 18.5cm multiplied by 5.0cm, is provided with 40 round holes with the diameter of 2cm, and can be used for placing 12mL solid-phase extraction columns. The round holes of the solid phase extraction columns with the specifications of 3mL, 6mL and the like can be formed by using the cold-rolled aluminum plates with the same length and width according to the requirements.
In order to distinguish between the different liquids flowing out of the collecting extraction column 4. The collection device 78 includes: a waste liquid tank 7 and a receiving rack 8; the waste liquid tank 7 is of a cuboid structure, a collection port 71 is formed in the center of the upper surface of the cuboid structure, and the upper surface of the cuboid structure is recessed inwards around the collection port 71; the side surface of the cuboid structure is communicated with a waste liquid discharge valve pipe 72; the other side surface is integrally designed with a handle structure; the waste liquid tank 7 is provided with a waste liquid tank positioning rod 73 integrally on the side surface thereof. The waste liquid tank locating rod 73 can be accurately fixed on the test tube rack placing table 93, and waste liquid in all extraction columns is collected. The receiving test tube rack 8 is divided into an upper layer structure, a middle layer structure and a lower layer structure, and test tube placing holes 81 are formed in the upper layer and the middle layer of the receiving test tube rack 8; the side face of the receiving test tube rack 8 is integrally provided with a test tube rack positioning rod 82. The test tube rack positioning rod 82 can be accurately fixed on the test tube rack placing table 93, and liquid to be collected in all extraction columns is guaranteed to be collected. The waste liquid flows out of the extraction column 4 and falls on the upper inclined surface of the waste liquid tank 7, flows into the waste liquid tank 7 from the collection port 71, and is collected in the waste liquid bottle by the waste liquid discharge valve pipe 72. Wherein the length, width and height of the waste liquid tank 7 are 31cm multiplied by 18.5cm multiplied by 10.0cm; the middle round hole is 5.0cm away from the cylinder bottom.
A system rack 9 for integrating the individual components of the solid phase extraction device; the system bracket 9 is a cuboid frame structure, the cuboid frame structure does not have four horizontal edges below, and a horizontal extraction bracket supporting rod 91 is arranged on the upper surface of the cuboid frame structure;
to address the replacement and positioning of the different collection devices 78. A test tube rack placing table 93 is arranged in the system bracket 9, and the test tube rack placing table 93 is provided with a drawing mechanism 94 and a lifting mechanism 95 in a matched manner; the drawing mechanism 94 is formed by horizontally arranging two cross bars 92 in opposite directions in the middle of the vertical direction of the cuboid frame structure, and the cross bars 92 are horizontally and slidably connected with the test tube rack placing table 93 through horizontal slide rails 941; two test tube lifting slide rails 951 are respectively arranged above the two cross bars 92.
The lifting mechanism 95 is arranged below the test tube rack placing table 93; the side of the horizontal slide rail 941, which is close to the test tube rack placing table 93, is provided with a positioning groove 942.
The horizontal slide 941 can pull out the test-tube rack and place the platform 93, and this test-tube rack is placed the platform 93 and is used for placing waste liquid groove 7 and receiving test-tube rack 8, horizontal slide 941 is close to the test-tube rack is placed the platform 93 side and has been seted up constant head tank 942, enables waste liquid groove 7 and receiving test-tube rack 8 accurate positioning. After the waste liquid tank 7 or the receiving rack 8 is placed, the rack placing table 93 is pushed in. When the position reaches the predetermined position, the waste liquid tank 7 or the receiving rack 8 is lifted to the predetermined position by the lifting mechanism 95.
In order to ensure that the sealing liquid adding plate 2 can be in close communication with the extraction column. The system bracket 9 is connected with the sealing liquid adding plate 2 through a spring buckle 10. The spring buckles 10 are symmetrically arranged on two sides of the liquid adding plate fixing frame 24, and more spring buckles 10 can be arranged according to different requirements.
Working principle: firstly, placing an extraction column 4 into an extraction column fixing hole 6; the extraction holder 5 with the extraction column 4 placed is fixed to the system frame 9.
And secondly, overlapping the alignment position of the sealing liquid adding plate 2 with the extraction fixing frame 5.
Thirdly, the test tube rack placing table 93 is pulled out, and the waste liquid tank 7 is placed in the test tube rack placing table 93 in an aligned mode; the test tube rack placing table 93 is pushed to a position, and the waste liquid tank 7 is lifted by the lifting mechanism, so that the distance between the upper end of the waste liquid tank 7 and the lower end of the extraction column is less than 0.5cm.
Fourthly, connecting the pressurizing device 1 with the liquid adding device 3; the activated solution added to the solid phase extraction column 4 was sealed with a three-way seal cap 13 in a pressurized bottle 12.
And fifthly, the three-way sealing cover 13 is communicated with the long pipe, the pressurizing device is used for pressurizing, the air pressure at the upper part of the pressurizing bottle 12 is increased, and the activated solution is pressed into the liquid adding device 3 and the pipeline of the sealing liquid adding plate 2. Since the extraction column 4 is not completely sealed, the pressure of the flowing activating liquid in the extraction column 4 is identical to the outside, and the activating liquid flows through the extraction column 4 by gravity into the waste liquid tank 7. Because the front end of the sealing liquid adding plate 2 is provided with the liquid adding plate one-way valve 25 and the damper 34, certain pressure is needed to flow through; the flow path liquid in the sealing liquid adding plate 2 has a certain pressure and fluctuates less, and the volume of the solution flowing into each column is substantially the same at the same time. According to the volume of the solution required by each small column and the number of the small columns, the total volume of the required solution can be calculated and accurately controlled by a flowmeter.
And sixthly, after the activating solution is added, the sealing liquid adding plate 2 is taken down, when the activating solution of the extraction column flows out, the sample extracting solution is added, the sealing liquid adding plate 2 is aligned and installed again, and the sealing liquid adding plate 2 and the extraction fixing frame 5 are locked by the spring buckle 10.
Seventhly, completely sealing the extraction column, mobilizing the tee joint sealing cover 13 to communicate with the short pipe and increasing the pressure, and guiding air into the liquid adding device 3, the sealing liquid adding plate 2 and the upper end of the extraction column; because the damper 34 is arranged in the system, pressure pulsation during pressurization is eliminated, and the pressure fluctuation at the upper end of the extraction column is smaller.
And eighth step, when the extracting solution in the extraction column 4 is completely flowed, the three-way sealing cover 13 on the pressurizing bottle 12 is adjusted to be communicated with the long pipe, the washing solution is added into the pressurizing bottle 12 in advance, the pressure is increased, and the washing solution is pressed into the liquid adding device 3, the sealing liquid adding plate 2 and the extraction column 4. According to the volume of the solution required by each extraction column 4 and the number of extraction columns 4, the total volume of the solution required can be calculated and accurately controlled by a flow meter.
And ninth, when the washing solution in the extraction column 4 is completely discharged, the liquid adding plate check valve 25 on the sealed liquid adding plate 2 is closed.
Tenth, the waste liquid tank 7 is lowered by the lifting mechanism 95 and taken out.
Eleventh, the receiving rack 8 with test tubes is mounted on the rack placing table 93. The receiving test tube rack 8 is lifted by the lifting mechanism 95 to be about 0.5cm away from the lower end of the extraction column 4 and extends into the test tube port.
Twelfth, adding the eluting solution into the pressurized bottle 12, increasing the pressure, pressing the eluting solution into the liquid adding device 3, the sealed liquid adding plate 2 and the extraction column 4, and collecting the eluting solution into the test tube.
The foregoing description is only of the preferred embodiments of the present application, and is not intended to limit the scope of the present application.

Claims (7)

1. A positive gas pressure type solid phase extraction device, comprising: a pressurizing device (1), an extraction column (4) and a collecting device (78); the pressurizing device (1) is communicated with a feed inlet of the extraction column (4), and a feed inlet of the collecting device (78) is connected with a discharge outlet of the extraction column (4);
further comprises: a sealing liquid adding plate (2); the sealing liquid adding plate (2) is arranged above the extraction column (4), and the sealing liquid adding plate (2) is communicated with the pressurizing device (1) through a pressurizing connecting pipe (14);
the sealed liquid feeding board (2) includes: a pipeline lower plate (21), a pipeline middle plate (22), a pipeline upper plate (23) and a liquid adding plate fixing frame (24); the pipeline lower plate (21), the pipeline middle plate (22) and the pipeline upper plate (23) are sequentially stacked from bottom to top, and the liquid adding plate fixing frame (24) is used for fixing and supporting the peripheral edges of the liquid adding plate (2); sealing buckles are arranged on two sides of the liquid adding plate fixing frame (24);
a liquid adding hole (231) is formed through the middle part of the pipeline upper plate (23);
the pipeline middle plate (22) is provided with an I-shaped middle plate pipeline (223), the middle plate pipeline (223) comprises two transverse middle plate pipelines and a longitudinal middle plate pipeline, and the bottom of the transverse middle plate pipeline is provided with a middle plate round hole (221);
two horizontal pipelines (212) are arranged on the pipeline lower plate (21), the horizontal pipelines (212) are arranged right below the horizontal middle plate pipeline, a plurality of longitudinal pipelines (213) are arranged perpendicular to the horizontal pipelines (212), drip round holes (214) are formed in the end points of two sides of each longitudinal pipeline (213), a flow limiting valve is arranged at the drip round holes (214), an outlet of the flow limiting valve is communicated with a solid phase extraction column adapter (215), an outlet of the solid phase extraction column adapter (215) is connected with a solid phase extraction column (4), and two ends of each longitudinal pipeline (213) are respectively provided with a lower plate one-way valve channel (211);
the pipeline middle plate is provided with a middle plate sealing hole (222), and the middle plate sealing hole (222) is positioned right above the lower plate one-way valve channel (211); an upper plate sealing hole (232) is formed in the pipeline upper plate, and the upper plate sealing hole (232) is positioned right above the middle plate sealing hole (222);
a liquid adding plate one-way valve (25) is arranged through the upper plate sealing hole (232) and the middle plate sealing hole (222);
a liquid adding device (3) is further arranged above the sealing liquid adding plate (2), and the liquid adding device (3) is arranged in the middle of the upper surface of the sealing liquid adding plate (2); one end of the liquid adding device (3) is communicated with the pressurizing connecting pipe, and the other end of the liquid adding device is communicated with the liquid adding hole (231);
the liquid adding device (3) comprises: a display (31), a pressure gauge (32), a protective housing (33), a damper (34) and a Hall flow pump (35);
a three-way adapter (37), a damper (34) and a Hall flow pump (35) are arranged below the protective shell (33), one end of the damper (34) is communicated with a liquid adding one-way valve (36), and the other end of the damper is connected with the Hall flow pump (35); the other end of the liquid adding one-way valve (36) is communicated with the pressurizing connecting pipe; the other end of the Hall flow pump (35) is connected with the three-way adapter (37); the other end of the three-way adapter is communicated with the liquid adding hole (231), a pressure gauge (32) above the protective shell is connected with the three-way adapter (37), and a display (31) is embedded above the protective shell (33); the display (31) is in communication with the hall flow pump (35).
2. The positive pressure gas solid phase extraction apparatus as claimed in claim 1, wherein the pressurizing means (1) comprises: a supercharger (11), a pressurizing bottle (12) and a three-way sealing cover (13);
the three-way sealing cover (13) seals the pressurizing bottle (12), and the pressurizer (11) is communicated with a pressurizing port of the pressurizing bottle (12);
a long pipe and a short pipe are arranged in the pressurizing bottle (12), the long pipe stretches into the bottom of the liquid level in the pressurizing bottle (12), and the short pipe stretches into the upper side of the liquid level in the pressurizing bottle (12); the three-way sealing cover (13) is communicated with a long pipe or a short pipe of the pressurizing bottle (12).
3. A gas positive pressure type solid phase extraction apparatus according to claim 1, wherein the extraction column (4) is provided with a plurality of; the extraction column (4) is arranged on the extraction fixing frame (5);
the extraction fixing frame (5) is of an upper layer structure and a lower layer structure; the extraction fixing frames (5) on the upper layer and the lower layer are provided with extraction column fixing holes (6).
4. A gas positive pressure solid phase extraction device according to claim 1, wherein the collection device (78) comprises: a waste liquid tank (7) and a receiving test tube rack (8);
the waste liquid tank (7) is of a cuboid structure, a collecting opening (71) is formed in the center of the upper surface of the waste liquid tank (7), and the upper surface of the waste liquid tank (7) is recessed inwards around the collecting opening (71); the side surface of the waste liquid tank (7) is communicated with a waste liquid discharge valve pipe (72), and the other side surface is integrally designed with a handle structure; a waste liquid tank locating rod (73) is integrally arranged on the side surface of the waste liquid tank (7);
the receiving test tube rack (8) is of an upper, middle and lower three-layer structure, and test tube placing holes (81) are formed in the upper layer and the middle layer of the receiving test tube rack (8); and a test tube rack positioning rod (82) is integrally arranged on the side face of the receiving test tube rack (8).
5. The positive pressure gas phase extraction apparatus of claim 1, further comprising: a system support (9); the system support (9) is of a cuboid frame structure, the system support (9) is not provided with four horizontal edges below, and a horizontal extraction support rod (91) is arranged on the upper surface of the system support (9).
6. The positive pressure gas solid phase extraction device according to claim 5, wherein a test tube rack placing table (93) is arranged in the system bracket (9), and the test tube rack placing table (93) is provided with a drawing mechanism (94) and a lifting mechanism (95) in a matched manner;
two cross bars (92) are horizontally arranged in the middle of the cuboid frame structure in the vertical direction relatively, and the cross bars (92) are horizontally and slidably connected with a test tube rack placing table (93) through a drawing mechanism (94);
the drawing mechanism (94) is a horizontal sliding rail (941);
a positioning groove (942) is formed in the side, close to the test tube rack placing table (93), of the horizontal sliding rail (941);
two test tube lifting slide rails (951) are respectively arranged above the two cross bars (92);
the lifting mechanism (95) is arranged below the test tube rack placing table (93).
7. The positive pressure gas solid phase extraction device according to claim 6, wherein the system bracket (9) is connected with the sealing liquid adding plate (2) through a spring buckle (10).
CN202211071268.5A 2022-09-02 2022-09-02 Gas positive pressure type solid phase extraction device Active CN115253381B (en)

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Application Number Priority Date Filing Date Title
CN202211071268.5A CN115253381B (en) 2022-09-02 2022-09-02 Gas positive pressure type solid phase extraction device

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Application Number Priority Date Filing Date Title
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CN115253381B true CN115253381B (en) 2023-09-26

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104225958A (en) * 2014-08-29 2014-12-24 康国华 Pressurization solid phase extraction device
CN214763466U (en) * 2021-02-08 2021-11-19 曼哈格检测技术股份有限公司 Solid phase extraction-concentration integrated instrument

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104225958A (en) * 2014-08-29 2014-12-24 康国华 Pressurization solid phase extraction device
CN214763466U (en) * 2021-02-08 2021-11-19 曼哈格检测技术股份有限公司 Solid phase extraction-concentration integrated instrument

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