CN217006603U - Flat-plate membrane type electric membrane extraction device - Google Patents
Flat-plate membrane type electric membrane extraction device Download PDFInfo
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- CN217006603U CN217006603U CN202220576531.5U CN202220576531U CN217006603U CN 217006603 U CN217006603 U CN 217006603U CN 202220576531 U CN202220576531 U CN 202220576531U CN 217006603 U CN217006603 U CN 217006603U
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Abstract
A flat membrane type electric membrane extraction device is characterized in that: the device comprises a sample bottle, a receiving bottle, a working electrode, a counter electrode, a flat microporous fiber membrane, a power-on device and a magnetic stirring device, wherein the sample bottle and the receiving bottle can be arranged in an up-down structure or a left-right structure, and the flat microporous fiber membrane is clamped between the sample bottle and the receiving bottle; the device can realize the rapid separation of the target object under the assistance of electricity, the selectivity of the flat microporous fiber membrane and the extraction solvent loaded on the membrane enables the device to have stronger purification capacity, the receiving bottle with a special structure endows the device with an oversized enrichment multiple, and the device has very high application value in the fields of sample pretreatment and analysis and detection.
Description
Technical Field
The utility model relates to the field of sample pretreatment, in particular to a flat-plate membrane type electric membrane extraction device.
Background
Relative to rapidly developing analytical instruments, the pretreatment of matrix purification has become a bottleneck problem restricting the development of analytical chemistry. Since the compounds to be assayed are often trace or even ultra-trace components in the sample, the complex matrix in the sample poses a great challenge to its accurate quantitative detection. Therefore, the development of a simple, rapid, green and efficient sample pretreatment technology for extracting compounds in a complex matrix has important significance for removing matrix interference and improving the sensitivity and accuracy of an analysis method.
The electromembrane extraction technology is a novel sample pretreatment technology proposed by Pedersen-Bjergaard et al in 2006, and the separation principle is that under the action of an electric field, charged analytes move to an electrode with opposite electrical property to the charged analytes and pass through a supporting liquid membrane to enter receiving liquid. In the process of the electric membrane extraction, the mass transfer process of an analyte mainly takes electromigration as a main part, so that the extraction time is greatly shortened; meanwhile, due to the selectivity of the supported liquid membrane, the electro-membrane extraction technology has stronger purification capacity, so that the electro-membrane extraction technology is rapidly developed in the field of sample pretreatment. In practical application, the hollow fiber membrane type electric membrane extraction is gradually developed into more convenient and flexible flat membrane type electric membrane extraction. However, the enrichment capability of the technology for the compounds to be tested is still limited by the lag of the development of the flat-plate membrane type electric membrane extraction device. Huang et al used 10-1000. mu.L pipette tips and 2.0 ml centrifuge tubes to make a flat-plate membrane-type electromembrane extraction device, and the volume of the sample phase and the receiving phase in the experiment were both 600. mu.L, and could not achieve enrichment of the compounds to be measured (Journal of Chromatography A, 2014, 1326: 7-12). The utility model discloses an application number is 201921883701.9's utility model discloses a separation or enrichment metal ion's electromembrane extraction device, because feed liquid solution accumulator is 2~10 times of analytic solution accumulator, and feed liquid pond volume is 1~2 times of analytic pond, and the device's enrichment multiple is the biggest only 10, though can further improve the enrichment multiple through continuous more material changing liquid phase solution, this can improve the operation complexity of device, consuming time power.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a flat-plate membrane type electric membrane extraction device aiming at the existing problems, which can realize the quick separation of a target object under the assistance of electricity, further realize the simultaneous separation, purification and enrichment of trace or even ultra-trace compounds in a complex matrix, and has high application value in the fields of sample pretreatment and analysis and detection.
In order to achieve the purpose, one of the technical schemes of the flat-plate membrane type electric membrane extraction device provided by the utility model is as follows:
a flat membrane type electric membrane extraction device comprises a sample bottle, a receiving bottle, a working electrode, a counter electrode, a flat microporous fiber membrane, a power-up device and a magnetic stirring device, wherein an upward extension pipe is arranged on the side surface of the sample bottle, and the outlet of the extension pipe is higher than the top of the sample bottle; the receiving bottle is of an inverted T structure and consists of an upper vertical cavity and a bottom flat cavity which are communicated with each other, the diameter of the bottom flat cavity is completely consistent with that of the top of the sample bottle, the height of the bottom flat cavity is far smaller than that of the sample bottle, and the diameter of the upper vertical cavity is far smaller than that of the bottom flat cavity; the flat microporous fiber membrane is clamped between the sample bottle and the bottom of the receiving bottle; one end of the working electrode penetrates through the extension tube and extends into the sample bottle, the other end of the working electrode is connected with the power-on device through a lead, one end of the counter electrode extends into the receiving bottle through the top opening of the upper vertical cavity, and the other end of the counter electrode is connected with the power-on device.
In order to ensure the device has super large enrichment times and stronger purification capacity, the height of the bottom flat cavity is 1/20-1/500 of the height of the sample bottle; the upper vertical chamber diameter is 1/5-1/30 of the bottom flattened chamber diameter.
In order to achieve the purpose, the second technical scheme of the flat-plate membrane type electric membrane extraction device provided by the utility model is as follows:
a flat membrane type electric membrane extraction device comprises a sample cell, a receiving cell, a working electrode, a counter electrode, a flat microporous fibrous membrane, a power-up device and a magnetic stirring device, wherein the sample cell and the receiving cell are arranged in a left-right structure, and a convex extension cell is arranged on the top surface of the sample cell; the receiving pool consists of a left receiving pool and a receiving pool branch pipe positioned on the right which are mutually communicated, the receiving pool branch pipe extends upwards, and the top of the receiving pool branch pipe is higher than the top of the left receiving pool; dull and stereotyped microporous fiber membrane centre gripping is between sample cell and left side receiving cell, and the sample cell is unanimous completely with the fitting surface bore of left side receiving cell, and sample cell length is greater than left side receiving cell length far away, and the protruding formula of passing of working electrode extends the pond and stretches into the sample cell, and the other end passes through the wire and adds the electric installation and be connected, and the open-top that the receiving cell branch pipe was passed through to the one end of counter electrode stretches into in the receiving cell, and the other end adds the electric installation with being connected and is connected.
In order to ensure the device has super large enrichment times and stronger purification capacity, the length of the left receiving pool is 1/20-1/500 of the length of the sample pool; the cross-sectional caliber of the receiving branch pipe is 1/5-1/30 of the cross-sectional caliber of the left receiving pool.
In the present invention, the sample vial/cell is placed on a magnetic stirrer, the rotor of which is placed in the sample vial/cell.
The flat microporous fibrous membrane is a flat polypropylene microporous fibrous membrane, the aperture is 0.2 mu m, and the thickness is 100 mu m-200 mu m.
The working electrode and the counter electrode are both platinum wires with the diameter of 0.3 mm.
The power-on device is a power supply of the electrophoresis apparatus, and the voltage applied by the power-on device is 1V-100V.
The magnetic stirring device comprises a magnetic stirrer and a rotor, wherein the magnetic stirrer is arranged below the sample bottle/pool, and the rotor is placed in the sample bottle/pool.
The utility model is used as follows
1. Adjusting the pH value of the sample solution by acid or alkali, transferring the sample solution into a sample bottle/pool, adding a rotor into the sample bottle/pool, and placing the sample bottle/pool on a magnetic stirrer;
2. the flat microporous fiber membrane is clamped between a sample bottle/pool and a receiving bottle/pool, and an extraction solvent is coated on the surface of the flat microporous fiber membrane;
3. injecting a receiving phase into the receiving bottle/pool, inserting the working electrode into the sample solution, inserting the counter electrode into the receiving phase, and respectively connecting the working electrode and the counter electrode to a power-up device through leads;
4. starting the magnetic stirrer and the power-on device, starting the extraction process, extracting for a certain time (1-30 min), and then closing the power-on device and the magnetic stirrer;
5. and drawing the counter electrode out of the receiving phase, and taking a certain amount of extract out of the receiving bottle by using a micro-sampling needle for analysis and detection.
Compared with the prior art, the utility model has the following advantages and beneficial effects:
the flat-plate membrane type electric membrane extraction device provided by the utility model is simple to operate, low in reagent dosage, low in cost, green and efficient; the rapid separation of the target object is realized under the assistance of electricity, the selectivity of the flat microporous fiber membrane and the extraction solvent loaded on the membrane enables the device to have stronger purification capacity, and a receiving bottle with a special structure (comprising an inverted T structure in the first scheme and a receiving tank branch pipe structure in the second scheme) endows the device with an ultra-large enrichment factor; the device will separate, purify and the integration step is integrated, need not the middle transfer and weather the redissolution, has shortened the pretreatment time to effectively prevent the sample loss that causes among the phase transition process, improved the degree of accuracy and precision, have very high practicality in sample pretreatment and analysis and detection field. The flat-plate membrane type electric membrane extraction device can be applied to detection of smoke components and biomarkers thereof.
Drawings
Figure 1 is a schematic structural diagram of a first technical scheme of the utility model (embodiment 1),
fig. 2 is a cross-sectional view of the receiver bottle of fig. 1.
Fig. 3 is a cross-sectional view of the sample vial of fig. 1.
In FIGS. 1-3: 1. the device comprises a power-on device, 2, a lead wire a, 3, a lead wire b, 4, a counter electrode, 5, a working electrode, 6, an upper vertical cavity, 7, a bottom flat cavity, 8, a flat microporous fiber membrane, 9, a sample bottle, 10, an extension tube, 11, a magnetic stirrer and 12, a rotor.
Figure 4 is a schematic structural view of a second technical scheme of the utility model (example 2),
FIG. 5 is a cross-sectional view of the receiving tank of FIG. 4.
Fig. 6 is a cross-sectional view of the sample cell of fig. 4.
In FIGS. 4-6: 1. the device comprises an energizing device, 2, a lead a, 3, a lead b, 4, a counter electrode, 5, a working electrode, 6', a receiving pool branch pipe, 7', a left receiving pool, 8, a flat microporous fiber membrane, 9', a sample pool, 10', a convex extending pool, 11, a magnetic stirrer and 12, a rotor.
Detailed Description
The utility model is further described below with reference to the accompanying drawings (examples):
example 1
As shown in figure 1, the flat membrane type electric membrane extraction device comprises a sample bottle 9, a receiving bottle, a working electrode 5, a counter electrode 4, a flat microporous fibrous membrane 8, a power-on device 1 and a stirring device, wherein the sample bottle 9 is provided with an extension tube 10, the outlet of the extension tube is higher than the top of the sample bottle, the receiving bottle is of an inverted T structure and consists of an upper vertical cavity 6 and a bottom flat cavity 7 which are communicated with each other, the diameter of the bottom flat cavity 7 is completely consistent with that of the top of the sample bottle 9, the height of the bottom flat cavity 7 is far smaller than that of the sample bottle 9, the diameter of the upper vertical cavity 6 is far smaller than that of the bottom flat cavity 7, the flat microporous fibrous membrane 8 is clamped between the sample bottle 9 and the bottom flat cavity 7 through a clamping plate, one end of the working electrode penetrates through the extension tube and extends into the sample bottle 9, the other end of the working electrode is connected with the power-on device 1 through a lead b3, one end of the counter electrode 4 extends into the receiving bottle through the opening at the top of the upper vertical cavity 6, the other end is connected with the electrifying device 1 through a lead a2, the sample bottle 9 is arranged on a magnetic stirrer 11, and a rotor 12 of the magnetic stirrer is arranged in the sample bottle 9.
When the lead b3 is connected with the positive pole of the power-on device 1, the lead a2 is connected with the negative pole of the power-on device 1; conversely, the lead b3 and the lead a2 are connected to the negative electrode and the positive electrode of the charging device 1, respectively. The forward and reverse connections are determined by smoke components and biomarkers thereof.
More specifically, the upper vertical chamber 6 and the lower flat chamber 7 of the receiving flask are in communication, between which the liquid can flow freely (see fig. 2).
The sample bottle 9 has an extension tube 10, the outlet of the extension tube 10 is higher than the top of the sample bottle 9 (see FIG. 3)
In this embodiment, since the bottom flat chamber 7 of the receiving flask is much lower in height than the sample flask 9 and the upper vertical chamber 6 is much smaller in diameter than the bottom flat chamber 7, the volume of the receiving flask is much smaller than the volume of the sample flask, thereby giving the device an extra large enrichment factor. The smaller diameter of the upper vertical chamber 6 ensures a sufficiently high liquid level despite the smaller volume of the receiving phase in the receiving flask, which in turn facilitates the sampling operation.
The diameter of the bottom flat cavity 7 is completely consistent with that of the top of the sample bottle 9, so that the sealing performance of the flat microporous fiber membrane can be ensured, and liquid leakage is prevented.
Example 2
As shown in fig. 4, a flat membrane type electric membrane extraction device comprises a sample cell 9', a receiving cell, a working electrode 5, a counter electrode 4, a flat microporous fibrous membrane 8, a power-up device 1, and a magnetic stirring device, wherein the sample cell 9' and the receiving cell 6 'are arranged in a left-right structure, and a convex extension cell 10' is arranged on the top surface of the sample cell; the receiving tank consists of a left receiving tank 7 'and a receiving tank branch pipe 6' which are communicated with each other, the receiving tank branch pipe 6 'extends upwards, and the top of the receiving tank branch pipe is higher than that of the left receiving tank 7'; dull and stereotyped micropore fibrous membrane 8 centre gripping is between sample cell 9 'and left side receiving cell 7', and the matching surface bore of sample cell and left side receiving cell is identical completely, and sample cell 9 'length is far greater than left side receiving cell 7' length, and the protruding formula of passing of working electrode 5 extends in the sample cell 10', and the other end passes through the wire and is connected with power device 1, and the open-top that receiving cell branch pipe 6' was passed through to the one end of counter electrode 4 stretches into in the receiving cell, and the other end with connect power device 1 and be connected.
In order to ensure the device has super large enrichment factor and stronger purification capacity, the length of the left receiving pool 7 'is 1/20-1/500 of the length of the sample pool 9'; the cross-sectional caliber of the receiving tank branch pipe 6 'is 1/5-1/30 of the cross-sectional caliber of the left receiving tank 7'.
More specifically, the receiving tank branch pipe 6 'in the receiving tank communicates with the left receiving tank 7' and liquid can flow freely therebetween (see fig. 5).
The top surface of the sample cell 9 'is provided with a convex extending cell 10' (see figure 6)
In this embodiment, the length of the left receiving pool 7 'is much smaller than that of the sample pool 9', and the section caliber of the receiving pool branch pipe 6 'is much smaller than that of the left receiving pool 7', so that the device is endowed with an extra large enrichment factor. The small diameter of the receiving tank branch pipe 6' ensures a sufficiently high liquid level despite the small volume of the receiving phase in the receiving flask, which in turn facilitates the sampling operation.
The section of the left receiving pool 7 'is completely consistent with the diameter of the top of the sample pool 9', which can ensure the sealing performance of the flat microporous fiber membrane and prevent liquid leakage.
When the utility model is used for separating, purifying and enriching specific compounds, two electrodes are respectively connected with the anode and the cathode of the power-on device according to the existing form of a target object in a sample bottle. When the existing form of the target object in the sample bottle is positively charged, the lead 3 and the lead 2 are respectively connected with the anode and the cathode of the power-on device 1, and when the existing form of the target object in the sample bottle is negatively charged, the lead 3 and the lead 2 are respectively connected with the cathode and the anode of the power-on device 1, so that the target object can be rapidly separated under the assistance of electricity.
The above examples are only for illustrating the technical solutions of the present invention, but not for limiting the same, and those skilled in the art should understand that: the technical solutions described in the above embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A flat membrane type electric membrane extraction device is characterized by comprising a sample bottle, a receiving bottle, a working electrode, a counter electrode, a flat microporous fiber membrane, a power-up device and a magnetic stirring device, wherein the sample bottle and the receiving bottle are arranged in an up-down structure, an upward extension pipe is arranged on the side surface of the sample bottle, and the outlet of the extension pipe is higher than the top of the sample bottle; the receiving bottle is of an inverted T structure and consists of an upper vertical cavity and a bottom flat cavity which are mutually communicated, the diameter of the bottom flat cavity is completely consistent with that of the top of the sample bottle, the height of the bottom flat cavity is far smaller than that of the sample bottle, and the diameter of the upper vertical cavity is far smaller than that of the bottom flat cavity; the flat microporous fiber membrane is clamped between the sample bottle and the bottom of the receiving bottle; one end of the working electrode penetrates through the extension tube and extends into the sample bottle, the other end of the working electrode is connected with the power-on device through a lead, one end of the counter electrode extends into the receiving bottle through the top opening of the upper vertical cavity, and the other end of the counter electrode is connected with the power-on device.
2. The flat-plate membrane type electro-membrane extraction device according to claim 1, wherein the bottom flat chamber has a height of 1/20-1/500 of the height of the sample bottle.
3. The flat-plate membrane electro-membrane extraction device of claim 1, wherein the diameter of the upper vertical chamber is 1/5-1/30 of the diameter of the bottom flat chamber.
4. A flat membrane type electric membrane extraction device is characterized by comprising a sample cell, a receiving cell, a working electrode, a counter electrode, a flat microporous fiber membrane, a power-up device and a magnetic stirring device, wherein the sample cell and the receiving cell are arranged in a left-right structure, and a convex extension cell is arranged on the top surface of the sample cell; the receiving pool consists of a left receiving pool and a receiving pool branch pipe positioned on the right which are mutually communicated, the receiving pool branch pipe extends upwards, and the top of the receiving pool branch pipe is higher than the top of the left receiving pool; dull and stereotyped microporous fiber membrane centre gripping is between sample cell and left side receiving cell, and the sample cell is unanimous completely with the fitting surface bore of left side receiving cell, and sample cell length is greater than left side receiving cell length far away, and the protruding formula of passing of working electrode extends the pond and stretches into the sample cell, and the other end passes through the wire and adds the electric installation and be connected, and the open-top that the receiving cell branch pipe was passed through to the one end of counter electrode stretches into in the receiving cell, and the other end adds the electric installation with being connected and is connected.
5. The flat-plate membrane-type electro-membrane extraction device according to claim 4, wherein the length of the left receiving cell is 1/20-1/500 of the length of the sample cell.
6. The flat-plate membrane type electro-membrane extraction device as claimed in claim 4, wherein the cross-sectional caliber of the receiving branch pipe is 1/5-1/30 of the cross-sectional caliber of the left receiving tank.
7. The flat-plate membrane type electric membrane extraction device as claimed in claim 1 or 4, wherein the flat-plate microporous fibrous membrane is a flat-plate polypropylene microporous fibrous membrane, the pore diameter is 0.2 μm, and the thickness is 100 μm-200 μm.
8. The flat-plate membrane-type electro-membrane extraction device according to claim 1 or 4, wherein the working electrode and the counter electrode are both platinum wires with a diameter of 0.3 mm.
9. The flat-plate membrane type electric membrane extraction device as claimed in claim 1 or 4, wherein the power supply device is an electrophoresis apparatus power supply, and the voltage applied by the power supply device is 1V-100V.
10. The flat-plate membrane electro-membrane extraction device according to claim 1 or 4, characterized in that the magnetic stirring device comprises a magnetic stirrer and a rotor, the magnetic stirrer is arranged below the sample bottle/cell, and the rotor is arranged in the sample bottle/cell.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202220576531.5U CN217006603U (en) | 2022-03-17 | 2022-03-17 | Flat-plate membrane type electric membrane extraction device |
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| CN202220576531.5U CN217006603U (en) | 2022-03-17 | 2022-03-17 | Flat-plate membrane type electric membrane extraction device |
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| CN217006603U true CN217006603U (en) | 2022-07-19 |
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| CN202220576531.5U Active CN217006603U (en) | 2022-03-17 | 2022-03-17 | Flat-plate membrane type electric membrane extraction device |
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