CN109060770B - Surface enhanced Raman detection chip box for on-site rapid detection - Google Patents
Surface enhanced Raman detection chip box for on-site rapid detection Download PDFInfo
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- CN109060770B CN109060770B CN201811308985.9A CN201811308985A CN109060770B CN 109060770 B CN109060770 B CN 109060770B CN 201811308985 A CN201811308985 A CN 201811308985A CN 109060770 B CN109060770 B CN 109060770B
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- 238000001514 detection method Methods 0.000 title claims abstract description 87
- 238000001069 Raman spectroscopy Methods 0.000 title claims abstract description 27
- 239000002904 solvent Substances 0.000 claims abstract description 147
- 238000012360 testing method Methods 0.000 claims abstract description 54
- 210000004907 gland Anatomy 0.000 claims abstract description 34
- 238000011084 recovery Methods 0.000 claims abstract description 33
- 238000007789 sealing Methods 0.000 claims abstract description 33
- 238000005192 partition Methods 0.000 claims abstract description 17
- 239000011229 interlayer Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims description 27
- 238000000605 extraction Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 3
- 238000003780 insertion Methods 0.000 claims description 3
- 230000037431 insertion Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 15
- 239000007787 solid Substances 0.000 abstract description 12
- 238000004458 analytical method Methods 0.000 abstract description 11
- 238000001237 Raman spectrum Methods 0.000 abstract description 3
- 238000000638 solvent extraction Methods 0.000 abstract description 3
- 238000002791 soaking Methods 0.000 abstract 2
- 239000000523 sample Substances 0.000 description 81
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 18
- 150000001875 compounds Chemical class 0.000 description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 10
- 239000002689 soil Substances 0.000 description 9
- 238000001228 spectrum Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- 238000004611 spectroscopical analysis Methods 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 239000000835 fiber Substances 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000479 surface-enhanced Raman spectrum Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- Health & Medical Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention belongs to the technical field of Raman spectrum detection, and particularly relates to a surface-enhanced Raman detection chip box for on-site rapid detection. The device comprises a chip box, a gland, a pull rod, a spring, a piston, two solvent tanks, a spring lower bracket, a guide pipe, a siphon pipe assembly, a plurality of one-way valves, a sealing interlayer, a sealing cover, a sample bin, a sample tank, a drainage tube, a partition board, a detection window cover and a solvent recovery tank; the method comprises the steps of sequentially soaking solid samples in solvents in two solvent tanks by utilizing a positive pressure principle and a negative pressure principle, sequentially dripping different solvents after soaking the samples on the surface of a detection chip, and then testing the surface of the chip; the method has the advantages of simple operation and strong practicability, is suitable for on-site solid sample rapid solvent extraction and analysis, and can provide rapid and effective technical support for various on-site solid sample detection works.
Description
Technical Field
The invention belongs to the technical field of Raman spectrum detection, and particularly relates to a surface-enhanced Raman spectrum detection chip box for rapidly extracting and analyzing a solvent of a solid sample on site.
Background
In recent years, rapid detection and analysis on site has been increasingly demanded in the fields of forensic science, environmental detection, food safety, and the like. These field operations often involve complex microscale organic detection. The trace amount of organic matters is small in quantity and low in concentration, and qualitative and quantitative analysis is needed by utilizing an advanced detection technology so as to obtain important information such as molecular structure, chemical composition, physicochemical properties and the like.
For the rapid detection of field samples, the portable spectrometer equipped with the optical fiber can provide a rapid direct-reading test result, and is certainly a more ideal and proper technical means for the field detection work outside a laboratory. The infrared spectrum and the common Raman spectrum technology have the advantages of short analysis time, portability of the instrument and the like, but the detection capability of the technology on the compounds is very limited, and the detection requirement of the trace quantity concentration level cannot be met. And trace and even ultra trace low concentration level detection is always a bottleneck which is not easy to break through for the existing instrument analysis technology. Therefore, research and establishment of effective micro trace organic matter rapid separation and detection technology are urgently needed to meet the actual needs of various field detection works. Surface Enhanced Raman Spectroscopy (SERS) techniques, which utilize interactions between nanostructures and molecules on SERS substrates, not only enable the efficient detection of extremely low concentration samples, but are also suitable for substantially all sample environments. The SERS technology is taken as a powerful analysis means, the application range is continuously expanded, and the SERS technology is increasingly widely applied to different field sample detection works. Solid samples are a very common sample type in various fields, and the compound components in the solid samples usually need to be extracted by a solvent before the detection of a SERS substrate can be achieved. However, there are fewer devices or apparatus currently available for rapid solvent extraction and SERS detection of solid samples.
Therefore, the invention aims to design and develop the surface enhanced Raman detection chip box which is simple and convenient to operate, strong in practicability and suitable for on-site solid sample rapid solvent extraction and analysis, and provides rapid and effective technical support for various on-site solid sample detection works.
Disclosure of Invention
The invention aims to provide a small, portable and rapid detection surface-enhanced Raman detection chip box aiming at the requirement of rapid detection of a solid sample on site.
The invention provides a surface-enhanced Raman detection chip box for field rapid detection, which comprises a chip box, a gland, a pull rod, a spring, a piston, a first solvent tank, a spring lower bracket, a conduit, a second solvent tank, a siphon component, a first one-way valve, a second one-way valve, a third one-way valve, a fourth one-way valve, a fifth one-way valve, a sealing interlayer, a sealing cover, a sample bin, a sample tank, a drainage tube, a baffle, a detection window cover and a solvent recovery tank;
the chip box 1 is a sealed box body, and a sealing interlayer 17 is arranged in the chip box 1 to divide the chip box 1 into a first cavity and a second cavity; the gland 2, the pull rod 3, the spring 4, the piston 5, the first solvent tank 6 and the spring lower bracket 7 are arranged in a first cavity, the conduit 8 passes through the sealing interlayer 17 and enters a second cavity, and the second solvent tank 10, the siphon pipe 11, the sample bin 19, the sample tank 20, the drainage tube 22, the partition board 24 and the solvent recovery tank 27 are arranged in the second cavity;
The top surface of the first cavity of the chip box 1 is provided with a first opening, the gland 2 is arranged at the first opening, and the bottom of the gland 2 is connected with the piston 5 through the pull rod 3;
the first solvent tank 6 is a cavity with an open top; the piston 5 is hermetically arranged at the opening of the first solvent tank 6 and can move up and down along the inner wall of the first solvent tank 6;
the spring lower support frame 7 is arranged at the bottom of the first solvent tank 6 in a nested manner; the spring 4 is vertically nested outside the first solvent tank 6; the upper end of the spring 4 is connected with the bottom of the gland 2, and the lower end of the spring 4 is connected with the spring lower support frame 7;
One end of the conduit 8 is arranged near the bottom of the lower end of the first solvent tank 6, the conduit 8 passes through the sealing interlayer 17, and the other end of the conduit is connected with the bottom of the sample tank 20 through the second one-way valve 13, so that liquid can only enter the sample tank 20 in one way;
A branch air pipe is arranged on the conduit 8, an air outlet of the branch air pipe is arranged in the second cavity, and the first one-way valve 12 is arranged on the branch air pipe, so that air can only enter the conduit 8 in one direction and liquid cannot flow out from the first one-way valve 12 through the conduit 8;
An air guide port 9 is arranged at one side of the top of the second solvent tank 10, a third one-way valve 14 is arranged on the air guide port 9, the third one-way valve 14 enables air to enter the second solvent tank 10 in a one-way manner, and the solution in the second solvent tank 10 cannot flow out from the third one-way valve 14;
the top of the second cavity of the chip box 1 is also provided with a second opening corresponding to the opening of the sample tank 20, and the top opening of the sample tank 20 is matched and butted with the second opening; the sealing cover 18 is arranged at the second opening of the chip box 1 in a sealing manner and is used for sealing and covering the sample tank 20; the bottom of the sample tank 20 is connected with the second solvent tank 10 through a siphon pipe 11, and a fourth one-way valve 15 is arranged on the siphon pipe 11, so that liquid can only enter the sample tank 20 in one way;
The bin body of the sample bin 19 is provided with meshes, and the sample bin 19 is detachably arranged in the sample tank 20, so that the replacement is convenient;
The drainage tube 22 is arranged at the upper part of the sample tank 20, and the baffle 24 is arranged below the drainage tube 22; the area of the baffle plate 24, which is opposite to the liquid outlet of the drainage tube 22, is a placing area of the test chip 23; a third opening is arranged on the top surface of the second cavity of the chip box 1 above the liquid outlet of the drainage tube 22; the detection window cover 25 is a transparent cover and is hermetically arranged on the third opening;
The side wall of the chip box 1 is provided with a socket for the extraction/insertion of a partition board 24 as a chip replacing port 26, and the socket is sealed after the partition board 24 is inserted;
The solvent recovery tank 27 is arranged below the partition board 24, a drainage opening 28 is arranged on one side, close to the placement area of the test chip 23, of the solvent recovery tank 27, and a fifth one-way valve 16 is arranged at the lower end of the drainage opening 28, so that liquid can flow into the solvent recovery tank 27 in one way; the baffle 24 does not block the drain opening 28;
the branching tracheal orifice of the conduit 8, the outlet of the draft tube 22 and the baffle 24 are located in the same closed space 21 in the second cavity, the volume of which is smaller than the volume of the first solvent tank 6.
In the invention, the materials of the chip box, the solvent tank, the sealing cover, the detection window cover, the solution recovery tank, the sample tank and the sample bin are plastics or metals.
In the present invention, the first solvent tank 6 and the second solvent tank 10 are cylindrical or rectangular parallelepiped in shape.
According to the invention, after the gland is extruded, the solution in the first solvent tank can be guaranteed to flow into the solvent recovery tank, and the negative pressure generated by the rebound of the gland can be guaranteed to flow into the solvent recovery tank.
In the present invention, the test chip 23 is a solid material such as a chip type or a sheet type with surface enhanced raman activity to be tested.
In the present invention, the volume of the solution recovery tank 27 is larger than the sum of the volumes of the first solvent tank 6 and the second solvent tank 10.
In the present invention, the solvent filled in the first solvent tank 6 and the second solvent tank 10 is one or a mixture of ethanol, methanol, acetonitrile, n-hexane, ethyl acetate, acetone, deionized water, toluene, and other liquids.
In the present invention, the liquid level in the second solvent tank 10 is lower than the height of the upper corner of the siphon tube 11.
When the invention is used, the operation steps are as follows:
(1) Placing a sample to be tested into a sample bin in the sample tank, and closing the sealing cover; inserting a baffle plate from a chip replacing port, and mounting a test chip on the baffle plate; the first solvent tank and the second solvent tank respectively store the solvent A and the solvent B, wherein the liquid level in the second solvent tank is lower than the height of the upper end corner of the siphon pipe.
(2) Pressing down the gland to drive the pull rod and the piston to move downwards; under the downward action of the piston, the solvent A in the first solvent tank flows into the sample tank through the guide pipe, gradually submerges the sample bin and the sample to be tested in the sample bin, extracts organic matters in the sample to be tested, and drips to the surface of the test chip through the drainage tube;
The excessive solvent A flows to the baffle plate and flows into the solvent recovery tank through the fifth one-way valve along the drainage opening, in the process, the second one-way valve is opened upwards, and the first one-way valve and the fourth one-way valve are closed.
(3) Releasing the gland, enabling the gland to move upwards under the action of the spring, and simultaneously driving the pull rod and the piston to move upwards, wherein the gland is lifted to the top end (the gland is not contacted with the third one-way valve before being lifted to the top end); the piston rises to form negative pressure in the first solvent tank, and under the action of the negative pressure, the first one-way valve is opened to enable air in the closed space of the second cavity of the chip box to be sucked into the guide pipe, so that the closed space is in a negative pressure state, and the negative pressure state acts on the sample tank through the drainage tube; under the action of pressure difference, solvent B in the second solvent tank flows into the sample tank through the fourth one-way valve by the siphon, gradually submerges the sample bin and the sample in the sample bin, reaches the surface of the test chip after passing through the drainage tube, flows into the solvent recovery tank through the fifth one-way valve along the drainage opening after excessive solvent flows to the baffle, and in the process, the second one-way valve is closed, and both the first one-way valve and the fourth one-way valve are opened.
(4) After the process is finished, the following modes can be adopted for analysis and test: ① Opening a detection window, and vertically aligning the Raman fiber probe downwards to a test chip below the detection window, so that the Raman scattered beam passes through the detection window to detect the test chip for spectrum test, and a detection result is obtained; ② And (3) extracting the baffle and the test chip from the chip replacement port, and testing under a Raman spectrometer to obtain a detection result.
If the detection is needed again, the proper solvent can be added into the first solvent tank and the second solvent tank again, a new test chip is inserted from the chip replacing port, and the solvent in the solvent recovery tank is poured out and emptied, so that the operation is performed according to the method. If the test chip is required to be stored, the test chip is only required to be stored in the chip box.
The surface enhanced Raman detection chip box is simple and convenient to operate, high in practicability and suitable for rapid extraction and detection of on-site solid samples, and provides rapid and effective technical support for extraction and detection of compounds in various on-site solid samples.
Drawings
Fig. 1 is a schematic diagram of a surface enhanced raman detection chip box for in-situ rapid detection.
The reference numerals shown in fig. 1 are respectively 1a chip box, 2a gland, 3a pull rod, 4a spring, 5a piston, 6a first solvent tank, 7a sub-spring support, 8a guide pipe, 9 a gas guide port, 10a second solvent tank, 11 a siphon pipe, 12 a first one-way valve, 13a second one-way valve, 14a third one-way valve, 15a fourth one-way valve, 16 a fifth one-way valve, 17 a sealing interlayer, 18 a sealing cover, 19 a sample bin, 20 a sample tank, 21 a closed space, 22 a drainage pipe, 23 a test chip, 24 a partition board, 25 a detection window cover, 26 a chip replacement port, 27 a solvent recovery tank, 28 a drainage opening.
Detailed Description
The device comprises a chip box, a gland, a pull rod, a spring, a piston, a first solvent tank, a spring lower bracket, a guide pipe, a second solvent tank, a siphon pipe component, a first one-way valve, a second one-way valve, a third one-way valve, a fourth one-way valve, a fifth one-way valve, a sealing interlayer, a sealing cover, a sample bin, a sample tank, a drainage pipe, a partition plate, a detection window cover and a solvent recovery tank;
The chip box 1 is a sealed cuboid box body, and is made of plastic, and a sealing interlayer 17 is arranged in the chip box 1 to divide the chip box 1 into a first cavity and a second cavity; the gland 2, the pull rod 3, the spring 4, the piston 5, the first solvent tank 6 and the spring lower support 7 are arranged in a first cavity, the conduit 8 traverses the sealing interlayer 17, and the rest is arranged in a second cavity.
The top surface of the first cavity of the chip box 1 is provided with a first opening, the gland 2 is arranged at the first opening, and the bottom of the gland 2 is connected with the piston 5 through the pull rod 3; the first solvent tank 6 is a cylindrical bottle with an open top; the piston 5 is a cylinder, the diameter of which is matched with the inner diameter of the first solvent tank 6, is hermetically arranged at the opening of the first solvent tank 6 and can move up and down along the inner wall of the first solvent tank 6; the spring lower support frame 7 is arranged at the bottom of the first solvent tank 6 in a nested manner; the inner diameter of the spring 4 is larger than the outer diameter of the first solvent tank 6, and the spring is vertically nested outside the first solvent tank 6; and the upper end of the spring 4 is connected with the bottom of the gland 2, and the lower end of the spring 4 is connected with the spring lower supporting frame 7.
The conduit 8 is arranged near the bottom of the lower end of the first solvent tank 6, the conduit 8 passes through the sealing interlayer 17 and enters the second cavity, and is connected with the bottom of the sample tank 20 through the second one-way valve 13, so that liquid can enter the sample tank 20 in one way;
the conduit 8 is provided with a branch air pipe, an air outlet of the branch air pipe is arranged in the second cavity, and the first one-way valve 12 is arranged on the branch air pipe, so that air can enter the conduit 8 in one direction, and liquid cannot flow out from the first one-way valve 12 through the conduit 8.
An air guide port (9) is arranged on one side of the top of the second solvent tank 10, a third one-way valve 14 is arranged on the air guide port (9), the third one-way valve 14 enables air to enter the second solvent tank 10 in a one-way mode, and solution in the second solvent tank 10 cannot flow out of the third one-way valve 14.
The sample tank 20 is a cuboid bottle with an opening at the top, a second opening is also arranged on the top surface of the second cavity of the chip box 1 corresponding to the opening position of the sample tank 20, and the opening at the top of the sample tank 20 is matched and butted with the second opening; the sealing cover 18 is arranged at the second opening of the chip box 1 in a sealing manner and is used for sealing and covering the sample tank 20; the bottom of the sample tank 20 is connected with the second solvent tank 10 through a siphon pipe 11, and a fourth one-way valve 15 is arranged on the siphon pipe 11, so that liquid can only enter the sample tank 20 in one way; the liquid level in the second solvent tank 10 is lower than the height of the upper corner of the siphon tube 11.
The bin body of the sample bin 19 is provided with meshes, and the sample bin 19 is detachably arranged in the sample tank 20, so that the replacement is convenient;
The drainage tube 22 is arranged at the upper part of the sample tank 20, and the baffle 24 is arranged below the drainage tube 22; the area of the baffle plate 24, which is opposite to the liquid outlet of the drainage tube 22, is a placing area of the test chip 23; a third opening is arranged on the top surface of the second cavity of the chip box 1 above the liquid outlet of the drainage tube 22; the detection window cover 25 is a transparent cover, and is hermetically disposed on the third opening.
The side wall of the chip box 1 is provided with a socket for the extraction/insertion of the partition board 24, and the socket is sealed after the partition board 24 is inserted as a chip replacing port 26.
The solvent recovery tank 27 is arranged below the partition board 24, a drainage opening 28 is arranged on one side, close to the placement area of the test chip 23, of the solvent recovery tank 27, and a fifth one-way valve 16 is arranged at the lower end of the drainage opening 28, so that liquid can flow into the solvent recovery tank 27 in one way; the baffle 24 does not block the drain opening 28.
The branching tracheal orifice of the conduit 8, the outlet of the draft tube 22 and the baffle 24 are located in the same closed space 21 in the second cavity, the volume of which is smaller than the volume of the first solvent tank 6.
The volume of the solution recovery tank 27 is larger than the sum of the volumes of the first solvent tank 6 and the second solvent tank 10.
The test chip 23 is a chip having surface enhanced raman activity to be tested.
The solvent filled in the first solvent tank 6 and the second solvent tank 10 is one or a mixture of ethanol, methanol, acetonitrile, n-hexane, ethyl acetate, acetone, deionized water, toluene and other liquids.
After the gland is extruded, the solution in the first solvent tank can be guaranteed to flow into the solvent recovery tank, and the negative pressure generated by the rebound of the gland can be guaranteed to flow into the solvent recovery tank.
Operating example 1
The first solvent tank and the second solvent tank of the chip box of the used surface-enhanced Raman detection device are respectively filled with absolute ethyl alcohol and normal hexane in advance, wherein the normal hexane liquid level in the second solvent tank is lower than the height of the corner of the upper end of the pipeline of the siphon assembly 11, and the test chip assembled on the shelf is a commercial KLARITE SERS chip.
Step 1: and opening a detection window, performing spectrum test on a test chip below the detection window by using a Raman fiber probe to obtain a background signal of a detection substrate, comparing results in the subsequent sample analysis and detection, and determining whether the detection substrate contains impurities interfering with the detection result.
Step 2: closing the detection window, opening the sealing cover, placing the soil sample containing the compound to be detected into a part of sample bin in the sample tank, and closing the sealing cover.
Step 3: the gland is pressed down by hand to drive the pull rod and the piston to move downwards, so that absolute ethyl alcohol in the first solvent tank can only enter the sample tank through the guide pipe flow and the second one-way valve, and the sample bin and soil samples in the sample bin are gradually immersed; the absolute ethyl alcohol solution with the extracted compound components reaches the surface of the test chip after passing through the drainage tube, excessive solvent flows to the baffle plate and flows into the solvent recovery tank along the drainage opening through the one-way valve, in the process, the second one-way valve is opened, and the first one-way valve and the fourth one-way valve are both in a closed state.
Step 4: the gland is released, so that the gland moves upwards under the action of the spring, and simultaneously, the pull rod and the piston are driven to move upwards (the gland is not contacted with the one-way valve before rising to the top end). The first solvent tank is raised to form negative pressure, the first one-way valve is opened under the action of the negative pressure, and under the action of pressure difference, the n-hexane solvent in the second solvent tank flows into the sample tank through the siphon pipe assembly via the fourth one-way valve in the closed space, so that the sample bin and the sample to be detected in the sample bin are gradually immersed. The n-hexane solution with the extracted compound components reaches the surface of the test chip after passing through the drainage tube, excessive solvent flows to the baffle plate and flows into the solvent recovery tank along the drainage opening through the one-way valve, in the process, the second one-way valve is closed, and the first one-way valve and the fourth one-way valve are both opened.
Step 5: after the process is finished, the surface of the test chip contains the compound components in the soil, and the analysis and the test can be carried out in two ways: ① Opening a detection window, and vertically aligning the Raman fiber probe downwards to a test chip below the detection window, so that the Raman scattered beam passes through the detection window to detect the test chip for spectrum test, and a detection result, namely a spectrum signal of a compound in soil, is obtained; ② And (3) extracting the partition plate and the test chip from the chip replacement port, and testing under a Raman spectrometer to obtain a detection result, namely a spectrum signal of the compound in the soil.
If the detection is needed again, the corresponding solvents can be added into the first solvent tank and the second solvent tank again, a new test chip is inserted from the chip replacing port, and the solvents in the solvent recovery tank are poured out, so that the operation is performed according to the method. If the test chip is required to be stored, the test chip is only required to be stored in the chip box by closing the detection window.
Working example 2
And armor alcohol and ethyl acetate are respectively filled in a first solvent tank and a second solvent tank of the chip box of the used surface-enhanced Raman detection device in advance, wherein the liquid level of the ethyl acetate in the second solvent tank is lower than the height of the corner at the upper end of a pipeline of the siphon component 11, and a test chip assembled on the shelf is a commercial Q-SERS chip.
Step 1: and opening a detection window, performing spectrum test on a test chip below the detection window by using a Raman fiber probe to obtain a background signal of a detection substrate, comparing results in the subsequent sample analysis and detection, and determining whether the detection substrate contains impurities interfering with the detection result.
Step 2: closing the detection window, opening the sealing cover, placing the concrete sample containing the compound to be detected into a part of sample bin in the sample tank, and closing the sealing cover.
Step 3: the gland is pressed down by hand to drive the pull rod and the piston to move downwards, so that the methanol in the first solvent tank can only enter the sample tank through the guide pipe flow and the second one-way valve, and the sample bin and the soil sample in the sample bin are gradually immersed; the methanol solution with the extracted compound component reaches the surface of the test chip after passing through the drainage tube, excessive solvent flows to the baffle plate and flows into the solvent recovery tank along the drainage opening through the one-way valve, in the process, the second one-way valve is opened, and the first one-way valve and the fourth one-way valve are both in a closed state.
Step 4: the gland is released, so that the gland moves upwards under the action of the spring, and simultaneously, the pull rod and the piston are driven to move upwards (the gland is not contacted with the one-way valve before rising to the top end). The first check valve is opened under the action of negative pressure, and the ethyl acetate solvent in the second solvent tank flows into the sample tank through the siphon pipe assembly via the fourth check valve under the action of pressure difference, so that the sample bin and the sample in the sample bin are gradually immersed. The ethyl acetate solution with the extracted compound components reaches the surface of the test chip after passing through the drainage tube, excessive solvent flows to the baffle plate and flows into the solvent recovery tank along the drainage opening through the one-way valve, in the process, the second one-way valve is closed, and the first one-way valve and the fourth one-way valve are both opened.
Step 5: after the process is finished, the surface of the test chip contains the compound components in the soil, and the analysis and the test can be carried out in two ways: ① Opening a detection window, and vertically aligning the Raman fiber probe downwards to a test chip below the detection window, so that the Raman scattered beam passes through the detection window to detect the test chip for spectrum test, and a detection result, namely a spectrum signal of a compound in soil, is obtained; ② And (3) extracting the partition plate and the test chip from the chip replacement port, and testing under a Raman spectrometer to obtain a detection result, namely a spectrum signal of the compound in the soil.
If the detection is needed again, the corresponding solvents can be added into the first solvent tank and the second solvent tank again, a new test chip is inserted from the chip replacing port, and the solvents in the solvent recovery tank are poured out, so that the operation is performed according to the method. If the test chip is required to be stored, the test chip is only required to be stored in the chip box by closing the detection window.
Claims (3)
1. The surface-enhanced Raman detection chip box for the on-site rapid detection is characterized by comprising a chip box (1), a gland (2), a pull rod (3), a spring (4), a piston (5), a first solvent tank (6), an under-spring support frame (7), a guide pipe (8), a second solvent tank (10), a siphon (11), a first one-way valve (12), a second one-way valve (13), a third one-way valve (14), a fourth one-way valve (15), a fifth one-way valve (16), a sealing interlayer (17), a sealing cover (18), a sample bin (19), a sample tank (20), a drainage tube (22), a baffle plate (24), a detection window cover (25) and a solvent recovery tank (27);
The chip box (1) is a sealed box body, and a sealing interlayer (17) is arranged in the chip box (1) to divide the chip box (1) into a first cavity and a second cavity; the gland (2), the pull rod (3), the spring (4), the piston (5), the first solvent tank (6) and the underfloor support frame (7) are arranged in a first cavity, the conduit (8) traverses the sealing interlayer (17), and the second solvent tank (10), the siphon (11), the sample bin (19), the sample tank (20), the drainage tube (22), the partition board (24) and the solvent recovery tank (27) are arranged in the second cavity;
The top surface of the first cavity of the chip box (1) is provided with a first opening, the gland (2) is arranged at the first opening, and the bottom of the gland (2) is connected with the piston (5) through the pull rod (3);
the first solvent tank (6) is a cavity with an open top; the piston (5) is hermetically arranged at the opening of the first solvent tank (6) and can move up and down along the inner wall of the first solvent tank (6);
the spring lower support frame (7) is arranged at the bottom of the first solvent tank (6) in a nested manner; the spring (4) is vertically nested outside the first solvent tank (6); the upper end of the spring (4) is connected with the bottom of the gland (2), and the lower end of the spring (4) is connected with the lower spring support frame (7);
One end of the conduit (8) is arranged at the lower end of the first solvent tank (6) near the bottom, the conduit (8) passes through the sealing interlayer (17) to enter the second cavity, and the other end of the conduit is connected with the bottom of the sample tank (20) through the second one-way valve (13), so that liquid can only enter the sample tank (20) in one direction;
a branch air pipe is arranged on the guide pipe (8), an air outlet of the branch air pipe is arranged in the second cavity, and the first one-way valve (12) is arranged on the branch air pipe, so that air can only enter the guide pipe (8) in one direction and liquid cannot flow out of the first one-way valve (12) through the guide pipe (8);
An air guide port (9) is arranged at one side of the top of the second solvent tank (10), a third one-way valve (14) is arranged on the air guide port (9), the third one-way valve (14) enables air to enter the second solvent tank (10) in a one-way manner, and solution in the second solvent tank (10) cannot flow out from the third one-way valve (14);
The top of the second cavity of the chip box (1) is provided with a second opening corresponding to the opening of the sample tank (20), and the top opening of the sample tank (20) is matched and butted with the second opening; the sealing cover (18) is arranged at the second opening of the chip box (1) in a sealing manner and seals and covers the sample tank (20); the bottom of the sample tank (20) is connected with the second solvent tank (10) through a siphon (11), and a fourth one-way valve (15) is arranged on the siphon (11) so that liquid can only enter the sample tank (20) in one way;
The bin body of the sample bin (19) is provided with meshes, and the sample bin (19) is detachably arranged in the sample tank (20) so as to be convenient to replace;
The drainage tube (22) is arranged at the upper part of the sample tank (20), and the baffle plate (24) is arranged below the drainage tube (22); the area of the baffle plate (24) which is opposite to the liquid outlet of the drainage tube (22) is a placing area of the test chip (23); a third opening is arranged at the top surface of the second cavity of the chip box (1) above the liquid outlet of the drainage tube (22); the detection window cover (25) is a transparent cover and is hermetically arranged on the third opening;
the side wall of the chip box (1) is provided with a socket for the extraction/insertion of a partition board (24) as a chip replacing port (26), and the socket is sealed after the partition board (24) is inserted;
The solvent recovery tank (27) is arranged below the partition board (24), a drainage opening (28) is formed in one side, close to the placement area of the test chip (23), of the solvent recovery tank (27), and a fifth one-way valve (16) is arranged at the lower end of the drainage opening (28) so that liquid can flow into the solvent recovery tank (27) in one direction; the baffle plate (24) does not shade the drainage opening (28);
the branch air pipe orifice of the guide pipe (8), the liquid outlet of the drainage pipe (22) and the partition plate (24) are positioned in the same closed space (21) in the second cavity, and the volume of the space is smaller than that of the first solvent tank (6);
The test chip (23) is a chip with surface enhanced Raman activity to be tested;
the volume of the solvent recovery tank (27) is greater than the sum of the volumes of the first solvent tank (6) and the second solvent tank (10).
2. The surface enhanced raman detection chip cartridge according to claim 1, wherein the first solvent tank (6) and the second solvent tank (10) are in the shape of a cylinder or a cuboid.
3. A surface enhanced raman detection chip cartridge as claimed in claim 1, characterized in that the liquid level in the second solvent tank (10) is lower than the height at the upper corner of the siphon (11).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811308985.9A CN109060770B (en) | 2018-11-05 | 2018-11-05 | Surface enhanced Raman detection chip box for on-site rapid detection |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811308985.9A CN109060770B (en) | 2018-11-05 | 2018-11-05 | Surface enhanced Raman detection chip box for on-site rapid detection |
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| CN109060770B true CN109060770B (en) | 2024-04-26 |
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