CN109060770A - A kind of field quick detection surface-enhanced Raman detection chip box - Google Patents
A kind of field quick detection surface-enhanced Raman detection chip box Download PDFInfo
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- CN109060770A CN109060770A CN201811308985.9A CN201811308985A CN109060770A CN 109060770 A CN109060770 A CN 109060770A CN 201811308985 A CN201811308985 A CN 201811308985A CN 109060770 A CN109060770 A CN 109060770A
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- 238000001514 detection method Methods 0.000 title claims abstract description 71
- 238000001069 Raman spectroscopy Methods 0.000 title claims abstract description 29
- 239000002904 solvent Substances 0.000 claims abstract description 146
- 238000012360 testing method Methods 0.000 claims abstract description 57
- 238000005192 partition Methods 0.000 claims abstract description 38
- 238000011084 recovery Methods 0.000 claims abstract description 33
- 210000004907 gland Anatomy 0.000 claims abstract description 30
- 238000007789 sealing Methods 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims description 29
- 238000000605 extraction Methods 0.000 claims description 7
- 238000003780 insertion Methods 0.000 claims description 5
- 230000037431 insertion Effects 0.000 claims description 5
- 208000002925 dental caries Diseases 0.000 claims description 3
- 238000003032 molecular docking Methods 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 abstract description 12
- 239000007787 solid Substances 0.000 abstract description 12
- 238000000899 pressurised-fluid extraction Methods 0.000 abstract description 3
- 238000001237 Raman spectrum Methods 0.000 abstract description 2
- 238000007654 immersion Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 80
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 14
- 230000009471 action Effects 0.000 description 10
- 239000000126 substance Substances 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 150000001875 compounds Chemical class 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
- 239000000203 mixture Substances 0.000 description 6
- 239000002689 soil Substances 0.000 description 6
- 238000004611 spectroscopical analysis Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 229960004756 ethanol Drugs 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 230000003595 spectral effect Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 230000007480 spreading Effects 0.000 description 3
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 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
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000011017 operating method Methods 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
- -1 sealing cover Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- 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 Raman spectrum detection technique field, specially a kind of field quick detection surface-enhanced Raman detection chip box.Including chip cartridges, gland, pull rod, spring, piston, two solvent tanks, spring lower bracket, conduit, siphon component, several check valves, sealed compartment, sealing cover, sample bin, sample jar, drainage tube, partition, detection window lid and solvent recovery tank;It utilizes positive pressure and principle of negative pressure, and after solvent successively impregnates solid sample in two solvent tanks, the different solvents after making immersion sample are successively added drop-wise to detection chip surface again, then test chip surface;The present invention have the advantages that easily to operate it is practical, be suitable for on-site solids sample Accelerated solvent extraction and analysis, can for all kinds of on-site solids sample detections work quickly and effectively technical support be provided.
Description
Technical field
The invention belongs to Raman spectrum detection technique fields, and in particular to a kind of on-site solids sample Accelerated solvent extraction and
The Surface enhanced Raman spectroscopy detection chip box of analysis.
Background technique
In recent years, field quick detection and analysis the fields such as forensic science, environment measuring, food safety demand increasingly
Increase.These works on the spot often relate to complicated micro- trace organic substance detection.Micro- trace organic substance quantity is few and concentration is low,
It needs to carry out qualitative and quantitative analysis using advanced detection technique, to obtain its molecular structure, chemical composition, physicochemical property etc.
Important information.
Quick detection for field sample can provide the test knot of quick direct-reading equipped with the portable spectrometer of optical fiber
Fruit, for laboratory outside on-site test work be undoubtedly a kind of even more ideal and suitable technological means.Infrared spectroscopy and general
Logical Raman spectroscopy has many advantages, such as that analysis time is short, instrument is portable, but these technologies to the Detection capability of compound very
It is limited, it is unable to satisfy the detection needs of micro- trace concentration levels.And the low concentration level detection of trace even ultra trace is for existing
Instrument analysis technology be the bottleneck for being not easy to break through always.Therefore, it is badly in need of research and establishes effective micro- trace organic substance
Quick separating and detection technique are to meet the actual needs that all kinds of on-site tests work.Surface enhanced Raman spectroscopy (SERS) skill
Art, using the interaction in SERS substrate between nanostructure and molecule, can not only the sample extremely low to concentration have
Effect detection, and it is applied basically for all sample environment.SERS technology is as a kind of strong analysis means, using model
Continuous expansion is enclosed, works and is more and more widely used in Different field sample detection.Solid sample is in all kinds of scenes
A kind of very common sample type, the chemical composition in solid sample just can be suitably used for SERS base after usually requiring solvent extraction
The detection at bottom.However, less suitable for solid sample Accelerated solvent extraction and the SERS device detected or device at present.
Therefore, a kind of easy to operate, practical, instant fastly suitable for on-site solids sample the present invention is directed to design and develop
Agent is extracted and the surface-enhanced Raman detection chip box of analysis, provides quickly and effectively for the work of all kinds of on-site solids sample detections
Technical support.
Summary of the invention
The needs that it is an object of the invention to quickly detect for on-site solids sample provide a kind of small-sized, portable, quick
Detection surface-enhanced Raman detection chip box.
Field quick detection provided by the present invention surface-enhanced Raman detection chip box, including chip cartridges, gland, drawing
Bar, spring, piston, the first solvent tank, spring lower bracket, conduit, the second solvent tank, siphon component, the first check valve, second
Check valve, third check valve, the 4th check valve, the 5th check valve, sealed compartment, sealing cover, sample bin, sample jar, drainage tube,
Partition, detection window lid and solvent recovery tank;
The chip cartridges 1 are the box body of a sealing, and sealed compartment 17 is set in chip cartridges 1, and chip cartridges 1 are separated into first
Two cavitys of cavity and the second cavity;The gland 2, pull rod 3, spring 4, piston 5, the first solvent tank 6 and spring lower bracket 7 are set
It is placed in the first cavity, conduit 8 crosses sealed compartment 17 and enters the second cavity, the second solvent tank 10, siphon pipe 11, sample bin
19, sample jar 20, drainage tube 22, partition 24 and solvent recovery tank 27 are set in the second cavity;
The top surface of first cavity of the chip cartridges 1 is equipped with the first opening, and gland 2 is set to the first opening, and 2 bottom of gland is logical
It crosses pull rod 3 and piston 5 connects;
First solvent tank 6 is open-topped cavity;Piston 5 it is closed be set to 6 opening of the first solvent tank, and can edge
The inner wall of first solvent tank 6 moves up and down;
7 nested type of spring lower bracing frame is set to 6 bottom of the first solvent tank;Spring 4 is nested in outside the first solvent tank 6 vertically
Side;And 4 upper end of spring is connected with 2 bottom of gland, 4 lower end of spring is connect with spring lower bracing frame 7;
Described 8 one end of conduit is set at the nearly bottom in 6 lower end of the first solvent tank, and conduit 8 passes through sealed compartment 17, and the other end passes through
Second one-way valve 13 is connected with 20 bottom of sample jar, makes liquid that can only unidirectionally enter sample jar 20;
The conduit 8 is equipped with branch's tracheae, which is set in the second cavity, and the first check valve 12 is set
It is placed on branch's tracheae, makes air that can only unidirectionally enter conduit 8, and liquid cannot be made to flow out through conduit 8 from the first check valve 12;
Second solvent tank, 10 top side is equipped with air guide port 9, and third check valve 14 is set on air guide port 9, third check valve
14 enable air to unidirectionally enter in the second solvent tank 10, and solution in the second solvent tank 10 cannot be made outside from third check valve 14
Outflow;
20 top opening of sample jar, 20 aperture position of top surface counter sample tank of the second cavity of chip cartridges 1 also are provided with
Two openings, 20 top opening of sample jar and the second opening matching docking;The sealing cover 18 is sealed at chip cartridges 1 second and opens
At mouthful, sealing covers sample jar 20;The bottom of sample jar 20 is connect by siphon pipe 11 with the second solvent tank 10, the 4th check valve
15 are set on siphon pipe 11, enable liquid that can only unidirectionally enter sample jar 20;
The warehouse of the sample bin 19 is equipped with mesh, and sample bin 19 is detachably arranged in sample jar 20, convenient for replacement;
The drainage tube 22 is set to 20 top of sample jar, and partition 24 is set to 22 lower section of drainage tube;Partition 24 faces drainage tube
The region of 22 liquid outlets is test 23 rest area of chip;The top surface of second cavity of the chip cartridges 1 above 22 liquid outlet of drainage tube
Position is open equipped with third;Testing window lid 25 is transparency cover, is sealed in third opening;
1 side wall of chip cartridges is equipped with one for 24 extractions of partition/insertion socket, replaces mouth 26 as chip, partition 24 is inserted
After entering, by spigot seal;
The solvent recovery tank 27 is set to 24 lower section of partition, and 27 top of solvent recovery tank is close to the one of test 23 rest area of chip
Side is equipped with drainage opening 28, and 28 lower ends of drainage opening are equipped with the 5th check valve 16, liquid can be made unidirectionally to flow into solvent recovery tank 27;
Partition 24 does not block drainage opening 28;
Branch's tracheae nozzle of the conduit 8, the liquid outlet of drainage tube 22 and partition 24 are located at same close in the second cavity
It closes in space 21, the spatial volume is less than 6 volume of the first solvent tank.
In the present invention, the chip cartridges, solvent tank, sealing cover, detection window lid, solution recovery tank, sample jar and sample
The material in storehouse is plastics or metal.
In the present invention, the shape of first solvent tank 6 and the second solvent tank 10 is cylindrical body or cuboid.
In the present invention, the gland can guarantee that all solvent recovery tank is arrived in trickling to solution in the filling of the first solvent after squeezing,
And gland rebound generation negative pressure can guarantee the second solvent fill in solution all trickling into solvent recovery tank.
In the present invention, the test chip 23 is the chip type to be measured with surface reinforced Raman active, sheet type etc.
Solid material.
In the present invention, the volume of the solution recovery tank 27 is greater than the first solvent tank 6 and the volume of the second solvent tank 10 is total
With.
In the present invention, filling solvent is ethyl alcohol, methanol, acetonitrile, just in first solvent tank 6 and the second solvent tank 10
One of liquid such as hexane, ethyl acetate, acetone, deionized water, toluene or its mixed solvent.
In the present invention, liquid level is lower than height at 11 upper side corners of siphon pipe in second solvent tank 10.
The present invention is in use, operating procedure is as follows:
(1) sample to be tested is put into sample jar inner sample storehouse, closes sealing cover;It is inserted into partition from chip replacement mouth, is surveyed
Examination chip is mounted on partition;Storage of solvent A and solvent B is distinguished in first solvent tank and the second solvent tank, wherein the second solvent
Liquid level is lower than height at siphon pipe pipeline upper side corners in tank.
(2) pull rod is driven by lower cover and piston moves downward;It is molten in the first solvent tank under the action of piston is downward
Agent A flows into sample jar via conduit, and gradually submerges the sample to be tested of sample bin and its inside, and solvent A extracts in sample to be tested
Organic matter, then by drainage tube, drop to test chip surface;
Excessive solvent A is open along drainage after trickling to partition and flows into solvent recovery tank through the 5th check valve, in this course,
Second one-way valve upwardly opens, and the first check valve and the 4th check valve are turned off.
(3) gland is decontroled, gland moves upwards under the action of the spring, while driving pull rod and piston upwards, pressure
It covers and rises to top (gland does not contact before rising to top with third check valve);Piston rises so that in the first solvent tank
Negative pressure is formed, under the action of negative pressure, the first check valve is opened, so that the air in the confined space of the second cavity of chip cartridges
It is inhaled into conduit, confined space is made to be in negative pressure state, which acts on sample jar further through drainage tube;In pressure
Under the action of difference, the solvent B in the second solvent tank flows into sample jar via the 4th check valve by siphon pipe, gradually submerges sample
The sample in storehouse and its inside, then reach test chip surface after drainage tube, excessive solvent is opened after trickling to partition along drainage
Solvent recovery tank is flowed into mouthful through the 5th check valve, during this, second one-way valve is closed, the first check valve and the 4th check valve
Open.
(4) it is finished to the above process, following methods can be used and carry out analysis test: 1. open detection window, Raman
Fibre-optical probe is directed at the test chip below detection window vertically downward, and Raman spreading beam is made to detect test by detection window
Chip carries out spectrum test, obtains testing result;2. partition is extracted out from chip replacement mouth together with test chip, in Raman
It is tested under spectrometer, obtains testing result.
If you need to detect again, solvent appropriate can be added in the first solvent tank and the second solvent tank again, be replaced from chip
It changes at mouth and is inserted into new test chip, and the solvent in solvent recovery tank is poured out and is emptied, operated according to the above method.If you need to
Test chip is saved, test chip need to only be resided in chip cartridges.
Operation of the present invention is easy, it is practical, drawn suitable for on-site solids sample rapidly extracting and the surface enhanced of detection
Graceful detection chip box is the extraction and detection of the compound in all kinds of on-site solids samples, provides quickly and effectively technical support.
Detailed description of the invention
Fig. 1 is a kind of schematic diagram of field quick detection surface-enhanced Raman detection chip box.
Label shown in Fig. 1 is respectively that 1 is chip cartridges, and 2 be gland, and 3 be pull rod, and 4 be spring, and 5 be piston, and 6 be
One solvent tank, 7 be spring lower bracing frame, and 8 be conduit, and 9 be air guide port, and 10 be the second solvent tank, and 11 be siphon pipe, and 12 be first
Check valve, 13 be second one-way valve, and 14 be third check valve, and 15 be the 4th check valve, and 16 be the 5th check valve, 17 for sealing every
Layer, 18 be sealing cover, and 19 be sample bin, and 20 be sample jar, and 21 be confined space, and 22 be drainage tube, and 23 be test chip, and 24 are
Partition, 25 be testing window lid, and 26 replace mouth for chip, and 27 be solvent recovery tank, and 28 be drainage opening.
Specific embodiment
The present invention includes chip cartridges, gland, pull rod, spring, piston, the first solvent tank, spring lower bracket, conduit, second
Solvent tank, siphon component, the first check valve, second one-way valve, third check valve, the 4th check valve, the 5th check valve, sealing
Interlayer, sealing cover, sample bin, sample jar, drainage tube, partition, detection window lid and solvent recovery tank;
The chip cartridges 1 are the cuboid box body of a sealing, and using plastic material, sealed compartment 17 is set in chip cartridges 1,
Chip cartridges 1 are separated into two cavitys of the first cavity and the second cavity or so;The gland 2, pull rod 3, spring 4, piston 5,
One solvent tank 6 and spring lower bracket 7 are set in the first cavity, and conduit 8 crosses sealed compartment 17, remaining is set to the second chamber
In body.
The top surface of first cavity of the chip cartridges 1 is equipped with the first opening, and gland 2 is set to the first opening, 2 bottom of gland
Portion is connected by pull rod 3 and piston 5;First solvent tank 6 is open-topped cylindrical body bottle;Piston 5 is cylindrical body, diameter
Match with 6 internal diameter of the first solvent tank, closed is set to 6 opening of the first solvent tank, and can be along the inner wall of the first solvent tank 6
It moves up and down;7 nested type of spring lower bracing frame is set to 6 bottom of the first solvent tank;4 internal diameter of spring is greater than the first solvent tank
6 outer diameters are nested in 6 outside of the first solvent tank vertically;And 4 upper end of spring is connected with 2 bottom of gland, under 4 lower end of spring and spring
Support frame 7 connects.
The conduit 8 is set at the nearly bottom in 6 lower end of the first solvent tank, and conduit 8 passes through sealed compartment 17 and enters the second chamber
Body is connected by second one-way valve 13 with 20 bottom of sample jar, and liquid is enable unidirectionally to enter sample jar 20;
The conduit 8 is equipped with branch's tracheae, and branch's air pipe outlet is set in the second cavity, the setting of the first check valve 12
In on branch's tracheae, enabling air to unidirectionally enter conduit 8, and liquid cannot be made to flow out through conduit 8 from the first check valve 12.
Second solvent tank, 10 top side is equipped with air guide port (9), and third check valve 14 is set on air guide port (9), the
Three check valves 14 enable air to unidirectionally enter in the second solvent tank 10, and solution in the second solvent tank 10 cannot be made unidirectional from third
Valve 14 flows outwardly.
The sample jar 20 is cuboid bottle, and the top surface counter sample tank 20 of top opening, the second cavity of chip cartridges 1 is opened
Mouth position also is provided with the second opening, 20 top opening of sample jar and the second opening matching docking;18 sealed set of sealing cover
In 1 second opening of chip cartridges, sealing covers sample jar 20;The bottom of sample jar 20 passes through siphon pipe 11 and the second solvent tank 10
Connection, the 4th check valve 15 are set on siphon pipe 11, make liquid that can only unidirectionally enter sample jar 20;Second solvent tank 10
Middle liquid level is lower than height at 11 upper side corners of siphon pipe.
The warehouse of the sample bin 19 is equipped with mesh, and sample bin 19 is detachably arranged in sample jar 20, convenient for replacement;
The drainage tube 22 is set to 20 top of sample jar, and partition 24 is set to 22 lower section of drainage tube;Partition 24 faces drainage tube
The region of 22 liquid outlets is test 23 rest area of chip;The top surface of second cavity of the chip cartridges 1 above 22 liquid outlet of drainage tube
Position is open equipped with third;Testing window lid 25 is transparency cover, is sealed in third opening.
1 side wall of chip cartridges is equipped with one for 24 extractions of partition/insertion socket, replaces mouth 26, partition as chip
After 24 insertions, by spigot seal.
The solvent recovery tank 27 is set to 24 lower section of partition, and 27 top of solvent recovery tank is close to test 23 rest area of chip
Side be equipped with drainage opening 28, drainage opening 28 lower ends be equipped with the 5th check valve 16, liquid can be made unidirectionally to flow into solvent recovery
Tank 27;Partition 24 does not block drainage opening 28.
Branch's tracheae nozzle of the conduit 8, the liquid outlet of drainage tube 22 and partition 24 are located at same in the second cavity
In a confined space 21, the spatial volume is less than 6 volume of the first solvent tank.
The volume of the solution recovery tank 27 is greater than the volume summation of the first solvent tank 6 and the second solvent tank 10.
Test chip 23 is the chip to be measured with surface reinforced Raman active.
Filling solvent is ethyl alcohol, methanol, acetonitrile, n-hexane, acetic acid in first solvent tank 6 and the second solvent tank 10
One of liquid such as ethyl ester, acetone, deionized water, toluene or its mixed solvent.
The gland can guarantee that all solvent recovery tank is arrived in trickling to solution in the filling of the first solvent after squeezing, and gland rebounds
The negative pressure of generation can guarantee that the solution in the filling of the second solvent all trickles into solvent recovery tank.
Operation example 1
It is filling anhydrous in advance respectively in surface-enhanced Raman detection the first solvent tank of device chip cartridges used and the second solvent tank
Ethyl alcohol and n-hexane, wherein n-hexane liquid level is lower than height at 11 pipeline upper side corners of siphon component, shelf in the second solvent tank
The test chip of upper assembly is the Klarite SERS chip of commercialization.
Step 1: opening detection window, spectrum survey is carried out to the test chip below detection window using Raman fiber optic probe
Examination obtains the background signal of detection substrate, and result compares when for subsequent sample analysis detection, whether can also confirm detection substrate
Impurity containing interference detection results.
Step 2: closing detection window, open sealing cover, the pedotheque containing untested compound is put into sample jar
Portion's sample bin in, close sealing cover.
Step 3: driving pull rod by lower cover with hand and piston moves downward, make the dehydrated alcohol in the first solvent tank can only
Enough the pedotheque of sample bin and its inside is gradually submerged into sample jar via conduit stream and second one-way valve;Extraction has chemical combination
The ethanol solution of object ingredient reaches test chip surface after drainage tube, and excessive solvent is opened after trickling to partition along drainage
Mouth flows into solvent recovery tank through check valve, and second one-way valve is opened during this, and the first check valve and the 4th check valve are located
In closed state.
Step 4: decontroling gland, move upwards gland under the action of the spring, while pull rod and piston being driven to transport upwards
Dynamic (gland does not contact before rising to top with check valve).Piston rises so that negative pressure is formed in the first solvent tank, in negative pressure
Under the action of, the first check valve is opened, and in confined space, under the action of pressure difference, the n-hexane in the second solvent tank is molten
Agent flows into sample jar via the 4th check valve by siphon component, gradually submerges the sample to be tested of sample bin and its inside.It mentions
The hexane solution of chemical composition is taken to reach test chip surface, edge after excessive solvent trickles to partition after drainage tube
Drainage opening flows into solvent recovery tank through check valve, and second one-way valve is closed during this, and the first check valve and the 4th is unidirectionally
Valve is opened.
Step 5: being finished to the above process, test chip surface contains the chemical composition in soil, and two kinds of sides can be used
Formula carries out analysis test: 1. open detection window, and Raman fiber optic probe is directed at the test core below detection window vertically downward
Piece makes Raman spreading beam detect test chip by detection window and carries out spectrum test, obtains testing result, i.e., change in soil
Close the spectral signal of object;2. partition is extracted out from chip replacement mouth together with test chip, surveyed under Raman spectrometer
Examination, obtains testing result, i.e., the spectral signal of compound in soil.
If you need to detect again, corresponding solvent can be added in the first solvent tank and the second solvent tank again, be replaced from chip
It changes at mouth and is inserted into new test chip, and the solvent in solvent recovery tank is poured out, operated according to the above method.If you need to save
Chip is tested, only need to close detection window, test chip is resided in chip cartridges.
Operation example 2
The surface-enhanced Raman used, which detects, distinguishes filling methanol in advance in the first solvent tank of device chip cartridges and the second solvent tank
And ethyl acetate, wherein ethyl acetate liquid level is lower than height at 11 pipeline upper side corners of siphon component, shelf in the second solvent tank
The test chip of upper assembly is the Q-SERS chip of commercialization.
Step 1: opening detection window, spectrum survey is carried out to the test chip below detection window using Raman fiber optic probe
Examination obtains the background signal of detection substrate, and result compares when for subsequent sample analysis detection, whether can also confirm detection substrate
Impurity containing interference detection results.
Step 2: closing detection window, open sealing cover, the concrete sample containing untested compound is put into sample jar
In interior portion's sample bin, sealing cover is closed.
Step 3: drive pull rod and piston moves downward by lower cover with hand, make the methanol in the first solvent tank be merely able to through
By conduit stream and second one-way valve into sample jar, the pedotheque of sample bin and its inside is gradually submerged;Extraction have compound at
The methanol solution divided reaches test chip surface after drainage tube, and excessive solvent is open along drainage through unidirectionally after trickling to partition
Valve flows into solvent recovery tank, and second one-way valve is opened during this, and the first check valve and the 4th check valve are in closing shape
State.
Step 4: decontroling gland, move upwards gland under the action of the spring, while pull rod and piston being driven to transport upwards
Dynamic (gland does not contact before rising to top with check valve).Piston rises so that negative pressure is formed in the first solvent tank, in negative pressure
Under the action of, the first check valve is opened, and under the action of pressure difference, the ethyl acetate solvent in the second solvent tank passes through siphon pipe
Component flows into sample jar via the 4th check valve, gradually submerges the sample of sample bin and its inside.Extraction has chemical composition
Ethyl acetate solution reaches test chip surface after drainage tube, and excessive solvent is unidirectional along drainage opening warp after trickling to partition
Valve flows into solvent recovery tank, and second one-way valve is closed during this, and the first check valve and the 4th check valve are opened.
Step 5: being finished to the above process, test chip surface contains the chemical composition in soil, and two kinds of sides can be used
Formula carries out analysis test: 1. open detection window, and Raman fiber optic probe is directed at the test core below detection window vertically downward
Piece makes Raman spreading beam detect test chip by detection window and carries out spectrum test, obtains testing result, i.e., change in soil
Close the spectral signal of object;2. partition is extracted out from chip replacement mouth together with test chip, surveyed under Raman spectrometer
Examination, obtains testing result, i.e., the spectral signal of compound in soil.
If you need to detect again, corresponding solvent can be added in the first solvent tank and the second solvent tank again, be replaced from chip
It changes at mouth and is inserted into new test chip, and the solvent in solvent recovery tank is poured out, operated according to the above method.If you need to save
Chip is tested, only need to close detection window, test chip is resided in chip cartridges.
Claims (5)
1. a kind of field quick detection surface-enhanced Raman detection chip box, which is characterized in that including chip cartridges (1), gland
(2), pull rod (3), spring (4), piston (5), the first solvent tank (6), spring lower bracket (7), conduit (8), the second solvent tank
(10), siphon pipe (11), the first check valve (12), second one-way valve (13), third check valve (14), the 4th check valve (15),
5th check valve (16), sealed compartment (17), sealing cover (18), sample bin (19), sample jar (20), drainage tube (22), partition
(24), detection window lid (25) and solvent recovery tank (27);
The chip cartridges (1) are the box body of a sealing, and sealed compartment (17) is set in chip cartridges (1), by chip cartridges (1) point
It is divided into two cavitys of the first cavity and the second cavity;The gland (2), pull rod (3), spring (4), piston (5), the first solvent tank
(6) it is set in the first cavity with spring lower bracket (7), conduit (8) crosses sealed compartment (17), the second solvent tank (10), rainbow
Suction pipe (11), sample bin (19), sample jar (20), drainage tube (22), partition (24) and solvent recovery tank (27) are set to second
In cavity;
The top surface of first cavity of the chip cartridges (1) is equipped with the first opening, and gland (2) is set to the first opening, gland (2)
Bottom is connected by pull rod (3) and piston (5);
First solvent tank (6) is open-topped cavity;Piston (5) it is closed be set to the first solvent tank (6) opening,
And it can move up and down along the inner wall of the first solvent tank (6);
7 nested type of spring lower bracing frame is set to the first solvent tank (6) bottom;Spring (4) is nested in the first solvent vertically
On the outside of tank (6);And spring (4) upper end same gland (2) bottom connects, spring (4) lower end is connect with spring lower bracing frame (7);
Described conduit (8) one end is set at the nearly bottom in the first solvent tank (6) lower end, conduit (8) pass through sealed compartment (17) into
Enter the second cavity, the other end is connected by second one-way valve (13) with sample jar (20) bottom, makes liquid that can only unidirectionally enter sample
Product tank (20);
The conduit (8) is equipped with branch's tracheae, which is set in the second cavity, the first check valve
(12) it is set on branch's tracheae, makes air that can only unidirectionally enter conduit (8), and liquid cannot be made single from first through conduit (8)
It is flowed out to valve (12);
Second solvent tank (10) top side is equipped with air guide port (9), and third check valve (14) is set on air guide port (9), the
Three check valves (14) enable air to unidirectionally to enter in the second solvent tank (10), and solution cannot be made in the second solvent tank (10) from the
Three check valves (14) flow outwardly;
Top surface counter sample tank (20) aperture position of sample jar (20) top opening, the second cavity of chip cartridges (1) is set
There are the second opening, sample jar (20) top opening and the second opening matching docking;The sealing cover (18) is sealed at chip
(1) second opening of box, sealing cover sample jar (20);The bottom of sample jar (20) passes through siphon pipe (11) and the second solvent tank
(10) it connects, the 4th check valve (15) is set on siphon pipe (11), makes liquid that can only unidirectionally enter sample jar (20);
The warehouse of the sample bin (19) is equipped with mesh, and sample bin (19) is detachably arranged in sample jar (20), convenient for replacing
It changes;
The drainage tube (22) is set to sample jar (20) top, and partition (24) is set to below drainage tube (22);Partition (24) is just
It is test chip (23) rest area against the region of drainage tube (22) liquid outlet;Chip cartridges above drainage tube (22) liquid outlet
(1) top side location of the second cavity is open equipped with third;Detection window lid (25) is transparency cover, is sealed at third opening
On;
Chip cartridges (1) side wall is equipped with one for the socket of partition (24) extraction/insertion, replaces mouth (26) as chip, every
After plate (24) insertion, by spigot seal;
The solvent recovery tank (27) is set to below partition (24), puts above solvent recovery tank (27) close to test chip (23)
The side for setting area is equipped with drainage opening (28), and drainage opening (28) lower end is equipped with the 5th check valve (16), can make liquid one-way flow
Enter solvent recovery tank (27);Partition (24) does not block drainage opening (28);
Branch's tracheae nozzle of the conduit (8), the liquid outlet of drainage tube (22) and partition (24) are located at same in the second cavity
In one confined space (21), the spatial volume is less than the first solvent tank (6) volume.
2. surface-enhanced Raman detection chip box as described in claim 1, which is characterized in that test chip (23) is to be measured
Chip with surface reinforced Raman active.
3. surface-enhanced Raman detection chip box as described in claim 1, which is characterized in that first solvent tank (6) and
The shape of second solvent tank (10) is cylindrical body or cuboid.
4. surface-enhanced Raman detection chip box as described in claim 1, which is characterized in that the appearance of the solution recovery tank 27
Product is greater than the volume summation of the first solvent tank (6) and the second solvent tank (10).
5. surface-enhanced Raman detection chip box as described in claim 1, which is characterized in that in second solvent tank (10)
Liquid level is lower than height at siphon pipe (11) upper side corners.
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