CN114136950A - Jet device for ultraviolet excitation time-resolved Raman - Google Patents

Jet device for ultraviolet excitation time-resolved Raman Download PDF

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Publication number
CN114136950A
CN114136950A CN202111453967.1A CN202111453967A CN114136950A CN 114136950 A CN114136950 A CN 114136950A CN 202111453967 A CN202111453967 A CN 202111453967A CN 114136950 A CN114136950 A CN 114136950A
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China
Prior art keywords
injector
reagent bottle
sample
nozzle
push
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CN202111453967.1A
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Chinese (zh)
Inventor
朱刚贝
吴红琳
母健
曾阳阳
李逊
王赞浩
宋云飞
于国洋
郑朝阳
杨延强
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Institute of Fluid Physics of CAEP
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Institute of Fluid Physics of CAEP
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Priority to CN202111453967.1A priority Critical patent/CN114136950A/en
Publication of CN114136950A publication Critical patent/CN114136950A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65Raman scattering
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N2021/0106General arrangement of respective parts
    • G01N2021/0112Apparatus in one mechanical, optical or electronic block

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  • Health & Medical Sciences (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)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The invention discloses a jet device for ultraviolet excited time-resolved Raman, which comprises a reagent bottle, a double-push injection pump and a jet nozzle; the double-push injection pump comprises a displacement table, a left side injector and a right side injector, and an injection cylinder port of the left side injector and an injection cylinder port of the right side injector are connected with the reagent bottle and the jet nozzle through hoses; when the pushing displacement table moves leftwards or rightwards, the push rod of the left injector is pressed into or pulled out of the injection tube to push the sample in the injection tube into the jet flow nozzle or suck the sample in the reagent bottle, and the push rod of the right injector is pulled out of or pressed into the injection tube to suck the sample in the reagent bottle or push the sample in the reagent bottle into the jet flow nozzle. The device can continuously and stably provide sample output, increase the duration time of a single experiment, and increase the acquisition time when acquiring the spectrum, thereby effectively improving the signal-to-noise ratio.

Description

Jet device for ultraviolet excitation time-resolved Raman
Technical Field
The invention relates to the technical field of spectrum detection, in particular to a jet device for ultraviolet excitation time-resolved Raman.
Background
Excited state structure dynamics (such as light-induced electron transfer, proton transfer, energy transfer, and other effects) play an important role in the research fields of chemistry, biology, and material science. The ultraviolet excitation time-resolved raman technology is an important means for studying excited state structure dynamics because it can directly give excited state vibration mode layout dynamics and thus give structural information.
The traditional ultraviolet excitation time-resolved raman faces the following problems when measuring liquid samples: 1) when the surface of the sample is excited by strong ultraviolet light, the sample is locally decomposed, gasified by heating and sputtered, so that the spectral stability is poor; 2) the skin depth of the exciting light is far less than that of the detecting light, and the effective ratio of the exciting space to the detecting space is small. Therefore, a jet flow method for converting a sample into a flowing vertical liquid column with a sub-millimeter magnitude is proposed at home and abroad to reduce thermal gasification and sputtering and improve the effective ratio of an excitation space to a detection space.
Current fluidics mainly use syringe pumps and capillaries, such devices require large amounts of sample and the duration of a single experiment is limited; secondly, the pressure of the jet flow is not controllable, so that the generated liquid column is unstable, and the obtained spectrum has poor stability. Therefore, it is necessary to develop a fluidic device suitable for liquid ultraviolet excitation time-resolved raman, and to improve spectral stability and detection duration.
In view of this, the present application is specifically made.
Disclosure of Invention
The invention aims to solve the technical problems that a large number of samples are needed by the existing equipment, the duration time of a single experiment is limited, and the invention aims to provide a novel jet device for ultraviolet excitation time-resolved Raman.
The invention is realized by the following technical scheme:
a fluidic device for ultraviolet excitation time-resolved Raman comprises a reagent bottle, a double-push injection pump and a fluidic nozzle; the double-push injection pump comprises a displacement table, and a left side injector and a right side injector which are respectively arranged at two sides of the displacement table, wherein the left side injector and the right side injector are arranged in opposite directions, a push rod is connected to the displacement table, and an injection cylinder port of the left side injector and an injection cylinder port of the right side injector are connected with a reagent bottle and a jet nozzle through hoses; when the displacement table is pushed to move leftwards, the push rod of the left injector is pressed into the injection tube to push the sample in the injection tube into the jet flow nozzle, and the push rod of the right injector is pulled out of the injection tube to suck the sample in the reagent bottle; when the displacement table is pushed to move rightwards, the push rod of the left injector is pulled out of the injection tube to suck the sample in the reagent bottle, and the push rod of the right injector is pressed into the injection tube to push the sample in the injection tube into the jet nozzle; the reagent bottle is provided with a backflow hole, a liquid outlet of the jet nozzle is arranged right above the backflow hole, and a sample sprayed from the jet nozzle can penetrate through the backflow hole to enter the reagent bottle.
The double-push injection pump further comprises a shell, the injection tube of the left injector and the injection tube of the right injector are fixed inside the shell, and the displacement table can reciprocate left and right under the control of the controller.
A first check valve is arranged between the left injector and the jet nozzle, a third check valve is arranged between the left injector and the jet nozzle, a second check valve is arranged between the right injector and the jet nozzle, and a fourth check valve is arranged between the right injector and the jet nozzle.
The front end of the jet flow nozzle is provided with a pressure feedback system, the pressure feedback system comprises a pressure gauge and a computer, the pressure gauge is used for monitoring the hydraulic pressure at the front end of the jet flow nozzle and feeding data back to the computer, and the computer calculates the appropriate flow rate according to the hydraulic pressure and feeds the appropriate flow rate back to the controller of the double-push injection pump to control the movement speed of the displacement table.
The working principle of the jet device is as follows: firstly, a sample is filled into a reagent bottle, the left side injector and the right side injector do not have the sample, a controller is started to control a displacement platform to move leftwards, a push rod of the left side injector is pressed into an injection tube to extrude air, a push rod of the right side injector is pulled out of the injection tube to draw the sample in the reagent bottle, then the displacement platform is controlled to move rightwards, the right side injector injects the sample into a jet nozzle through a check valve II, the sample is sprayed out from the jet nozzle and is subjected to spectrum detection by using an instrument, the left side injector pumps the sample into the reagent bottle through a check valve III, and in the process, the check valve I and the check valve IV have the effect of preventing the sample from flowing back; then the displacement table repeats the leftward and rightward movement, and can continuously inject the sample into the nozzle, so that the continuous output of the sample is realized, and the acquisition time of a single experiment can be increased according to the actual needs of the experiment.
Be equipped with the backward flow hole on the reagent bottle, the sample of blowout can get back to the reagent bottle in from the jet nozzle, realizes the recovery cycle of sample and uses, can reduce the use amount of sample, saves the cost.
The pressure feedback system is arranged in front of the jet nozzle and is used for monitoring the hydraulic pressure at the front end of the jet nozzle by the pressure gauge, feeding data back to the computer, calculating the appropriate flow rate through a control program and feeding the appropriate flow rate back to the double-push injection pump, so that the hydraulic pressure is adjusted by controlling the movement speed of the displacement table, and the pressure is stable and controllable finally.
The jet flow nozzle further comprises a hose connector, a capillary tube connector and a capillary tube which are sequentially connected, the hose connector is connected with the hose, the inner diameter of the hose is smaller than 5mm, the inner diameter of the capillary tube is smaller than 0.5mm, and the sample liquid column penetrates through the backflow hole and is injected into the reagent bottle.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. according to the jet device for ultraviolet-excited time-resolved Raman provided by the embodiment of the invention, the continuous output of the sample can be realized through the continuous leftward and rightward movement of the displacement table, the spectrum acquisition time of a single experiment can be increased according to the actual needs of the experiment, and the signal-to-noise ratio of data is improved;
2. according to the jet device for ultraviolet-excited time-resolved Raman provided by the embodiment of the invention, the sample sprayed from the jet nozzle can return to the reagent bottle, so that the sample can be recycled, the use amount of the sample can be reduced, and the cost is saved.
Drawings
In order to more clearly illustrate the technical solutions of the exemplary embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and that for those skilled in the art, other related drawings can be obtained from these drawings without inventive effort.
FIG. 1 is a block diagram of a fluidic device provided in accordance with an embodiment of the present invention;
FIG. 2 is a block diagram of a dual push syringe pump according to an embodiment of the present invention;
FIG. 3 is a block diagram of a fluidic nozzle provided in accordance with an embodiment of the present invention;
FIG. 4 is a structural diagram of a detecting device according to an embodiment of the present invention;
fig. 5 is a time-resolved raman spectrum of nitromethane provided in an embodiment of the present invention.
Reference numbers and corresponding part names:
1-reagent bottle, 2-hose, 3-double-push injection pump, 31-left injector, 32-right injector, 33-displacement table, 41-first check valve, 42-second check valve, 43-third check valve, 44-fourth check valve, 51-pressure gauge, 52-computer, 6-jet nozzle, 61-hose connector, 62-capillary connector, 63-capillary tube, 71-first lens, 72-second lens, 73-parabolic mirror, 74-band stop filter, 75-third lens, 76-spectrometer acquisition system and 8-sample liquid column.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. However, it will be apparent to one of ordinary skill in the art that: it is not necessary to employ these specific details to practice the present invention. In other instances, well-known structures, circuits, materials, or methods have not been described in detail so as not to obscure the present invention.
Throughout the specification, reference to "one embodiment," "an embodiment," "one example," or "an example" means: the particular features, structures, or characteristics described in connection with the embodiment or example are included in at least one embodiment of the invention. Thus, the appearances of the phrases "one embodiment," "an embodiment," "one example" or "an example" in various places throughout this specification are not necessarily all referring to the same embodiment or example. Furthermore, the particular features, structures, or characteristics may be combined in any suitable combination and/or sub-combination in one or more embodiments or examples. Further, those of ordinary skill in the art will appreciate that the illustrations provided herein are for illustrative purposes and are not necessarily drawn to scale. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In the description of the present invention, the terms "front", "rear", "left", "right", "upper", "lower", "vertical", "horizontal", "upper", "lower", "inner", "outer", etc. indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and therefore, should not be construed as limiting the scope of the present invention.
Example 1
As shown in fig. 1, a fluidic device for uv-excited time-resolved raman according to an embodiment of the present invention includes a reagent bottle 1, a double-push syringe pump 3, and a fluidic nozzle 6; the double-push injection pump 3 comprises a displacement table 33 and a left side injector 31 and a right side injector 32 which are respectively arranged at two sides of the displacement table 33, the left side injector 31 and the right side injector 32 are arranged in opposite directions, push rods are connected to the displacement table 33, an injection cylinder opening of the left side injector 31 and an injection cylinder opening of the right side injector 32 are connected with the reagent bottle 1 and the jet nozzle 6 through hoses 2, wherein the hoses 2 of the left side injector 31 and the right side injector 32 form a loop which is connected with the double-push injection pump 3 in parallel; when the pushing displacement table 33 moves to the left, the push rod of the left injector 31 is pressed into the syringe to push the sample therein into the jet nozzle 6, and the push rod of the right injector 32 is pulled out of the syringe to suck the sample in the reagent bottle 1; when the displacement table 33 is pushed to move rightwards, the push rod of the left injector 31 is pulled out of the injection tube to suck the sample in the reagent bottle 1, the push rod of the right injector 32 is pressed into the injection tube to push the sample in the injection tube into the jet nozzle 6, a backflow hole is formed in the reagent bottle 1, the liquid outlet of the jet nozzle 6 is arranged right above the backflow hole, and the sample liquid column 8 sprayed out of the jet nozzle 6 can penetrate through the backflow hole to enter the reagent bottle 1.
Preferably, the double-push injection pump further comprises an injection tube of the left injector and an injection tube of the right injector of the shell are fixed in the shell, and the displacement table can reciprocate left and right under the control of the controller.
Preferably, a first check valve is arranged between the left injector and the jet nozzle, a third check valve is arranged between the left injector and the jet nozzle, a second check valve is arranged between the right injector and the jet nozzle, and a fourth check valve is arranged between the right injector and the jet nozzle.
Preferably, the front end of the jet nozzle is provided with a pressure feedback system, the pressure feedback system comprises a pressure gauge and a computer, the pressure gauge is used for monitoring the hydraulic pressure at the front end of the jet nozzle and feeding data back to the computer, and the computer calculates a proper flow rate according to the hydraulic pressure and feeds the proper flow rate back to the controller of the double-push injection pump to control the movement speed of the displacement table.
The working principle of the jet device is as follows: firstly, a sample is filled into a reagent bottle, the left side injector and the right side injector do not have the sample, a controller is started to control a displacement platform to move leftwards, a push rod of the left side injector is pressed into an injection tube to extrude air, a push rod of the right side injector is pulled out of the injection tube to draw the sample in the reagent bottle, then the displacement platform is controlled to move rightwards, the right side injector injects the sample into a jet nozzle through a check valve II, the sample is sprayed out from the jet nozzle and is subjected to spectrum detection by using an instrument, the left side injector pumps the sample into the reagent bottle through a check valve III, and in the process, the check valve I and the check valve IV have the effect of preventing the sample from flowing back; then the displacement table repeats the leftward and rightward movement, and can continuously inject the sample into the nozzle, so that the continuous output of the sample is realized, and the acquisition time of a single experiment can be increased according to the actual needs of the experiment.
Be equipped with the backward flow hole on the reagent bottle, the sample of blowout can get back to the reagent bottle in from the jet nozzle, realizes the recovery cycle of sample and uses, can reduce the use amount of sample, saves the cost.
The pressure feedback system is arranged in front of the jet nozzle and is used for monitoring the hydraulic pressure at the front end of the jet nozzle by the pressure gauge, feeding data back to the computer, calculating the appropriate flow rate through a control program and feeding the appropriate flow rate back to the double-push injection pump, so that the hydraulic pressure is adjusted by controlling the movement speed of the displacement table, and the pressure is stable and controllable finally.
Preferably, the fluidic nozzle further comprises a hose connector, a capillary connector and a capillary tube which are sequentially connected, the hose connector is connected with the hose, the inner diameter of the hose is less than 5mm, the inner diameter of the capillary tube is less than 0.5mm, and the sample liquid column penetrates through the backflow hole and is injected into the reagent bottle.
Example 2
As shown in fig. 4, an embodiment of the present invention provides a detection apparatus for uv-excited time-resolved raman, which includes a jet device, and a spectrometer acquisition system 76, a lens three 75, a band-stop filter 74, and a parabolic mirror 73, which are sequentially disposed, where a lens one 71 and a lens two 72 are disposed in a vertical direction of a sample liquid column 8 ejected by the jet device, the lens one is used to focus pump light on the sample liquid column 8, the lens two is used to focus probe light on the same focal point of the sample liquid column 8, and the parabolic mirror is disposed between the lens one and the lens two and the sample liquid column 8 and is used to collect backscattered light of collimated probe light and transmit the backscattered light to the band-stop filter; the band-stop filter is used for filtering Rayleigh scattered light, and the third lens is used for focusing the light passing through the band-stop filter into the spectrometer acquisition system for spectrum acquisition.
Example 3
The embodiment of the invention provides a measuring method for ultraviolet excitation time-resolved Raman, which comprises the following steps: 1) filling nitromethane into a reagent bottle of a jet device, starting a controller of a displacement table to push the displacement table to reciprocate leftwards and rightwards, and continuously ejecting a sample from a jet nozzle to form a sample liquid column; 2) femtosecond optical pulses with the repetition frequency of 1kHz are used as pumping light and are focused on a sample through a first lens, picosecond optical pulses with the repetition frequency of 1kHz are used as detection light and are focused on the sample through a second lens, and the focuses of the pumping light and the detection light are superposed; 3) collecting and collimating the back scattered light of the detection light through a parabolic mirror, filtering the Rayleigh scattered light through a band elimination filter, and focusing the light into a spectrometer collection system through a lens for spectrum collection; 4) and (4) collecting the Raman spectra for different time delays of the pumping light and the detection light, and measuring time-resolved Raman spectral dynamics.
Fig. 5 is a time-resolved raman spectrogram of nitromethane obtained by using the apparatus and method of the present invention, in this embodiment, the acquisition time of each spectrum is 40 minutes, the obtained noise level reaches 0.1counts, and the signal-to-noise ratio of the data is greatly improved.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. The jet device for ultraviolet excited time-resolved Raman is characterized by comprising a reagent bottle (1), a double-push injection pump (3) and a jet nozzle (6);
the double-push injection pump (3) comprises a displacement table (33), and a left side injector (31) and a right side injector (32) which are respectively arranged at two sides of the displacement table (33), wherein the left side injector (31) and the right side injector (32) are arranged in opposite directions, a push rod is connected to the displacement table (33), and an injection cylinder port of the left side injector (31) and an injection cylinder port of the right side injector (32) are connected with the reagent bottle (1) and the jet nozzle (6) through hoses (2);
when the pushing displacement table (33) moves leftwards or rightwards, the push rod of the left injector (31) is pressed into or pulled out of the injection tube to push the sample in the injection tube into the jet flow nozzle (6) or suck the sample in the reagent bottle (1), and the push rod of the right injector (32) is pulled out of or pressed into the injection tube to suck the sample in the reagent bottle (1) or push the sample in the reagent bottle into the jet flow nozzle (6).
2. Fluidic device for uv-excited time-resolved raman according to claim 1, characterized in that said double-push syringe pump (3) further comprises a housing inside which the cartridges of the left injector (31) and the right injector (32) are fixed, the displacement table (33) being able to reciprocate left and right under the control of the controller.
3. The fluidic device for uv-excited time-resolved raman according to claim 1, wherein a first check valve (41) is disposed between the left injector (31) and the fluidic nozzle (6), a third check valve (43) is disposed between the left injector and the reagent bottle (1), a second check valve (42) is disposed between the right injector (32) and the fluidic nozzle (6), and a fourth check valve (44) is disposed between the right injector and the reagent bottle (1).
4. The fluidic device for uv-excited time-resolved raman according to claim 2, wherein a pressure feedback system (5) is provided at the front end of the fluidic nozzle (6), the pressure feedback system (5) comprises a pressure gauge (51) and a computer (52), the pressure gauge (51) is used for monitoring the hydraulic pressure at the front end of the fluidic nozzle (6) and feeding back data to the computer (52), and the computer (52) calculates a proper flow rate according to the hydraulic pressure and feeds back the proper flow rate to the controller of the double-push injection pump (3) to control the movement speed of the displacement table (33).
5. The fluidic device for ultraviolet-excited time-resolved raman according to claim 1, wherein the reagent bottle (1) is provided with a backflow hole, the liquid outlet of the fluidic nozzle (6) is disposed right above the backflow hole, and the sample liquid column (8) ejected from the fluidic nozzle (6) can pass through the backflow hole to enter the reagent bottle (1).
6. Fluidic device for uv-excited time-resolved raman according to claim 1, characterized in that the fluidic nozzle (6) employs a capillary (63).
7. Fluidic device for uv-excited time-resolved raman according to claim 6, characterized in that the fluidic nozzle (6) further comprises a hose connector (61), a capillary connector (62) and a capillary (63) connected in sequence, the capillary (63) being placed inside the capillary connector (62), the hose connector (61) being connected to the hose (2).
8. Fluidic device for uv-excited time-resolved raman according to claim 6, characterized in that the inner diameter of the capillary is <0.5 mm.
9. Fluidic device for uv-excited time-resolved raman according to claim 6, characterized in that the end of the capillary (63) is flush with the capillary joint.
10. Fluidic device for uv-excited time-resolved raman according to claim 1, characterized in that the inner diameter of the hose is <5 mm.
CN202111453967.1A 2021-12-01 2021-12-01 Jet device for ultraviolet excitation time-resolved Raman Pending CN114136950A (en)

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Application Number Priority Date Filing Date Title
CN202111453967.1A CN114136950A (en) 2021-12-01 2021-12-01 Jet device for ultraviolet excitation time-resolved Raman

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Application Number Priority Date Filing Date Title
CN202111453967.1A CN114136950A (en) 2021-12-01 2021-12-01 Jet device for ultraviolet excitation time-resolved Raman

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104339056A (en) * 2014-10-28 2015-02-11 苏州市宝玛数控设备有限公司 Working fluid circulation filter device of wire cut electrical discharge machine
CN206045103U (en) * 2016-07-22 2017-03-29 东华理工大学 Two-way continuous syringe pump
CN108693165A (en) * 2018-07-10 2018-10-23 西北大学 A kind of time-resolved Raman spectro scopy equipment

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104339056A (en) * 2014-10-28 2015-02-11 苏州市宝玛数控设备有限公司 Working fluid circulation filter device of wire cut electrical discharge machine
CN206045103U (en) * 2016-07-22 2017-03-29 东华理工大学 Two-way continuous syringe pump
CN108693165A (en) * 2018-07-10 2018-10-23 西北大学 A kind of time-resolved Raman spectro scopy equipment

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Application publication date: 20220304