CN212646486U - Sealed electrolytic cell device for in-situ detection by combining Raman spectroscopy and mass spectrometry - Google Patents
Sealed electrolytic cell device for in-situ detection by combining Raman spectroscopy and mass spectrometry Download PDFInfo
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- CN212646486U CN212646486U CN202021529340.0U CN202021529340U CN212646486U CN 212646486 U CN212646486 U CN 212646486U CN 202021529340 U CN202021529340 U CN 202021529340U CN 212646486 U CN212646486 U CN 212646486U
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- 238000001514 detection method Methods 0.000 title claims abstract description 20
- 238000001819 mass spectrum Methods 0.000 claims abstract description 33
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- 239000007788 liquid Substances 0.000 claims abstract description 21
- 238000000926 separation method Methods 0.000 claims abstract description 21
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 239000003792 electrolyte Substances 0.000 claims description 8
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 8
- 230000007797 corrosion Effects 0.000 claims description 7
- 238000005260 corrosion Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
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- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 3
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- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
The utility model discloses an in-situ detection sealed electrolytic cell device combining Raman spectroscopy and mass spectrometry. The electrolytic cell device comprises a working electrode, a reference electrode, a counter electrode, a Raman electrolytic cell and a mass spectrum sampling tube; the Raman electrolytic cell comprises a flange base body, an optical window, a flange cover, a gas-liquid separation membrane, a porous metal supporting sheet and a flange bottom; the center of the flange base body is provided with a through hole, the top of the flange base body is sequentially fixed with an optical window and a flange cover from bottom to top, and the bottom of the flange base body is sequentially fixed with a gas-liquid separation membrane, a porous metal support sheet and a flange bottom from top to bottom; the reference electrode and the counter electrode are respectively fixed on two sides of the flange matrix, and the working electrode is fixed between the gas-liquid separation membrane and the flange matrix; an L-shaped through hole penetrating through the side wall or a vertical through hole penetrating through the bottom surface is formed in the center of the bottom of the flange, and the mass spectrum sampling pipe is installed in the L-shaped through hole or the vertical through hole. The utility model discloses can realize raman and mass spectrum antithetical couplet and ally use, can catch electrochemical signal, raman signal and mass spectrum signal simultaneously.
Description
Technical Field
The utility model relates to an electrochemistry detects technical field, in particular to sealed electrolytic cell device of normal position detection of raman and mass spectrum antithetical couplet usefulness.
Background
With the continuous development of electrochemical reactions, people have increasingly studied the mechanism of electrochemical reactions, wherein the research using the in-situ method draws much attention because the whole reaction can be monitored in real time. The in-situ electrochemical Raman spectrum reflects information of molecular vibration, rotation and the like of a detected sample and is used for researching and analyzing a molecular structure, and the in-situ electrochemical mass spectrum can analyze the change condition of dynamic products, intermediate products or adsorbates with less than single layer number along with the electrode potential and time. Therefore, the combination of in-situ Raman and in-situ mass spectrometry is a predictable ideal method for measuring the electrochemical reaction mechanism.
However, the detection equipment capable of realizing the combination of Raman and mass spectrometry at home and abroad at the present stage is generally applicable to the single in-situ Raman or in-situ mass spectrometry test of an electrolytic cell, and has the disadvantages of complex structure of a testing device, difficult assembly and difficult subsequent characterization after reaction, thereby seriously hindering the exploration of people on the intermediate process mechanism of the electrochemical reaction.
At present, no report of the combination of in-situ Raman and in-situ mass spectrum exists, so that the development of the sealed electrolytic cell device for in-situ detection of the combination of Raman and mass spectrum has important significance for researching the mechanism of electrochemical reaction.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to overcome prior art's defect and not enough, provide a sealed electrolytic cell device of normal position detection that raman and mass spectrum ally oneself with, the device has realized raman spectroscopy appearance and mass spectrum appearance and has used jointly, can catch electrochemical signal, raman signal and mass spectrum signal simultaneously under the electrochemical reaction condition.
The purpose of the utility model can be realized by the following technical scheme: a sealed electrolytic cell device for in-situ detection of Raman and mass spectrometry comprises a working electrode, a reference electrode, a counter electrode, a Raman electrolytic cell and a mass spectrometry sample introduction tube;
the Raman electrolytic cell comprises a flange base body, an optical window, a flange cover, a gas-liquid separation membrane, a porous metal supporting sheet and a flange bottom; the center of the flange base body is provided with a through hole, the top of the flange base body is sequentially fixed with an optical window and a flange cover from bottom to top, and the bottom of the flange base body is sequentially fixed with a gas-liquid separation membrane, a porous metal support sheet and a flange bottom from top to bottom; the reference electrode and the counter electrode are respectively fixed on two sides of the flange matrix, and the working electrode is fixed between the gas-liquid separation membrane and the flange matrix;
the center of the flange bottom is provided with an L-shaped through hole penetrating through the side wall or a vertical through hole penetrating through the bottom surface, and the mass spectrum sampling pipe is arranged in the L-shaped through hole or the vertical through hole.
Further, the reference electrode is fixed on one side surface of the flange base body through a first fixing screw rod, and the counter electrode is fixed on the other side surface of the flange base body through a second fixing screw rod. The centers of the first fixing screw and the second fixing screw are provided with through holes, and the peripheries of the first fixing screw and the second fixing screw are provided with threads which can be matched with threaded holes arranged on the side surface of the flange base body. The reference electrode and the counter electrode extend into the flange base body through the first fixing screw rod and the second fixing screw rod respectively and are fixedly connected with the flange base body.
Further, a first sealing ring is arranged between the optical window and the flange base body; a second sealing ring is arranged between the first fixing screw and the flange base body; a third sealing ring is arranged between the second fixing screw and the flange base body; and a fourth sealing ring is arranged between the working electrode and the flange base body. The sealing performance of the electrolytic cell device can be improved by arranging a plurality of sealing rings.
Further, the first sealing ring, the second sealing ring, the third sealing ring and the fourth sealing ring are full-fluorine ether rubber sealing rings or silica gel sealing rings.
Furthermore, the optical window is made of sapphire glass sheets and calcium fluoride or potassium bromide.
Further, the working electrode may be a catalyst-coated carbon paper electrode, a gas diffusion electrode, or a catalyst-coated gold-plated teflon film, the reference electrode may use a silver chloride electrode, a mercury oxide electrode, or a reversible hydrogen electrode, and the counter electrode may use a platinum wire electrode, a nickel mesh electrode, a graphite rod electrode, or a carbon mesh electrode.
Further, the gas-liquid separation membrane is a porous polytetrafluoroethylene membrane, and the diameter range of membrane pores is between 0.2 microns and 10 microns.
Further, the material of the flange cover, the flange base body and the flange bottom can be corrosion-resistant plastic or corrosion-resistant metal.
Further, electrolyte can be injected into the flange base body, and the electrolyte is an acid solution, an alkali solution or an organic solution.
Further, the working electrode, the reference electrode and the counter electrode are connected with an electrochemical workstation, and the mass spectrum sampling tube is connected with a mass spectrum analyzer.
Compared with the prior art, the utility model, following advantage and beneficial effect have: the utility model discloses an electrolytic cell device can realize raman spectroscopy appearance and mass spectrum appearance's antithetical couplet usefulness, under the electrochemical reaction condition, can catch electrochemistry signal, raman signal and mass spectrum signal simultaneously. And simultaneously, the utility model discloses an electrolytic cell device simple structure, the equipment is convenient, and the part material is easy, and the leakproofness is good, has the significance to the research electrochemical reaction mechanism.
Drawings
FIG. 1 is an exploded view of an electrolytic cell assembly according to a first embodiment of the present invention;
FIG. 2 is a front view of FIG. 1;
FIG. 3 is a cross-sectional view of an electrolytic cell assembly according to an embodiment of the present invention;
FIG. 4 is an exploded view of an electrolytic cell apparatus according to a second embodiment of the present invention;
FIG. 5 is a front view of FIG. 4;
FIG. 6 is a sectional view of an electrolytic cell apparatus according to a second embodiment of the present invention.
Wherein: 1: flange cover, 2: optical window, 3: first seal ring, 4: flange base, 5: first connecting screw, 6: first coupling nut, 7: second seal ring, 8: first fixing screw, 9: reference electrode, 10: third seal ring, 11: second fixing screw, 12: counter electrode, 13: fourth seal ring, 14: working electrode, 15: gas-liquid separation membrane, 16: porous metal support sheet, 17: flange bottom, 18: third fixing screw, 19: mass spectrometer sample introduction tube, 20: second connecting screw, 21: l-shaped through-hole, 22: and a vertical through hole.
Detailed Description
The present invention will be described in further detail with reference to the following examples and drawings, but the present invention is not limited thereto.
Example one
As shown in fig. 1 and 2, an in-situ detection sealed electrolytic cell device combining raman and mass spectrometry comprises a working electrode, a reference electrode, a counter electrode, a raman electrolytic cell and a mass spectrometry sampling tube. The Raman electrolytic cell comprises a flange base body, an optical window, a flange cover, a gas-liquid separation membrane, a porous metal supporting sheet and a flange bottom.
The center of the flange base body is provided with a through hole, and the top of the flange base body is sequentially fixed with an optical window and a flange cover from bottom to top. The optical window is made of sapphire glass sheet, calcium fluoride (CaF2) or potassium bromide (KBr) and the like. Light rays of the raman spectrum analyzer mounted on the top of the electrolytic cell device in this embodiment can be projected into the flange base body from the optical window, and reflected light rays are obtained through the gas-liquid separation membrane. A first sealing ring is arranged between the optical window and the flange base body, and the optical window can be sealed. The flange cover covers the optical window, four through holes are formed in four corners of the flange cover, and the first connecting screw penetrates through the four through holes and is fixedly connected with the first connecting screw cap.
The bottom of the flange base body is sequentially fixed with a gas-liquid separation membrane, a porous metal support sheet and a flange bottom from top to bottom. The gas-liquid separation membrane is a porous polytetrafluoroethylene membrane, the diameter range of membrane pores is 0.2-10 microns, and gas generated by electrochemical reaction of electrolyte in the flange matrix can be permeated. The porous metal support sheet can support a gas-liquid separation membrane with a soft surface, and can also permeate gas due to the porous structure. The center of the top surface of the flange bottom is provided with an L-shaped through hole penetrating through the side wall, the top of the flange bottom is provided with an opening for fixing the porous metal support sheet, and the side surface of the flange bottom is provided with an L-shaped through hole for fixing the mass spectrum sampling tube. Four through holes are formed in four corners of the bottom of the flange, and four second connecting screws penetrate through the four through holes to connect the flange bottom and the flange base body.
And a working electrode, a reference electrode and a counter electrode are also fixed in the flange substrate. Wherein the working electrode is arranged between the gas-liquid separation membrane and the flange base body, and a fourth sealing ring is arranged between the working electrode and the flange base body for realizing sealing. The working electrode can be a carbon paper electrode coated with a catalyst, or various gas diffusion electrodes (such as a self-supporting graphene electrode plate, a self-supporting carbon nanotube electrode and the like), or a gold-plated polytetrafluoroethylene film coated with a catalyst, and the like. The reference electrode is installed in a side of the flange base body through a first fixing screw rod, a through hole is formed in the center of the first fixing screw rod, threads are arranged on the periphery of the through hole, and the reference electrode can be matched with threaded holes in the side wall of the flange base body. The reference electrode passes through inside first set screw stretches into the flange base member, in order to realize sealed, is equipped with the second sealing washer between first set screw and flange base member. As the reference electrode, various commercially available reference electrodes such as a silver chloride electrode (Ag/AgCl), a mercury oxide electrode (Hg/HgO) and a reversible hydrogen electrode can be used. And the counter electrode is arranged on the other side wall of the flange base body through a second fixing screw rod. The second fixing screw is the same as the first fixing screw, a through hole is formed in the center of the second fixing screw, and threads are arranged on the periphery of the second fixing screw. Likewise, a third sealing ring is provided between the second fastening screw and the flange base body for sealing purposes. As the counter electrode, a platinum wire electrode, a nickel mesh electrode, a graphite rod electrode, a carbon mesh electrode, or the like can be used.
The first sealing ring, the second sealing ring, the third sealing ring and the fourth sealing ring are all-fluorine ether rubber sealing rings or silica gel sealing rings. The sealing performance of the electrolytic cell device can be improved by arranging a plurality of sealing rings.
The material of the flange cover, the flange base body and the flange bottom can be various corrosion-resistant plastics, such as Polytetrafluoroethylene (PTFE), nylon, polyether ether ketone (PEEK) and the like, or corrosion-resistant metal, such as titanium, stainless steel or other corrosion-resistant materials.
In order to realize the combination of the Raman spectrum analyzer and the mass spectrum analyzer, as shown in fig. 3, a mass spectrum sample introduction pipe is fixed in an L-shaped through hole at the bottom of a flange, the mass spectrum sample introduction pipe is fixed through a third fixing screw rod, a through hole is formed in the center of the third fixing screw rod, threads are arranged on the periphery of the end part of the mass spectrum sample introduction pipe, and the mass spectrum sample introduction pipe can be in threaded fit with the L-shaped through hole. The gas generated by electrochemical reaction of the electrolyte in the flange base body can enter a mass spectrometer connected with the mass spectrum sampling pipe through a gas-liquid separation membrane, a porous metal support, an L-shaped through hole and the mass spectrum sampling pipe.
In this embodiment, the usage principle of the sealed electrolytic cell device for in-situ detection by combining raman and mass spectrometry is as follows:
(1) assembling a three-electrode system: after the working electrode is prepared, the working electrode is placed on the upper portion of the gas-liquid separation membrane, the surface of the working electrode is guaranteed to be flat, and the flange bottom and the flange base body are guaranteed to be fixedly sealed through the fourth sealing ring and the second connecting screw rod. And then assembling a reference electrode and a counter electrode, wherein the reference electrode is hermetically fixed with the flange base body through a second sealing ring and a first fixing screw rod. And the counter electrode is hermetically fixed with the flange base body through a third sealing ring and a second fixing screw rod.
(2) Fixing the Raman electrolytic cell: electrolyte is added into the flange base body, the first sealing ring, the optical window and the flange cover are respectively added on the top of the flange base body from bottom to top, and the flange cover and the flange base body are ensured to be fixedly sealed through the first connecting screw rod and the first connecting screw cap.
(3) Connecting a mass spectrum sampling tube: the mass spectrum sample injection pipe is fixedly connected with the L-shaped through hole through a third fixing screw rod.
(4) And (3) system testing: and connecting the working electrode, the reference electrode and the counter electrode with an electrochemical workstation, connecting the mass spectrum sampling tube with an in-situ mass spectrum analyzer, and mounting the Raman spectrum analyzer on the top of the flange cover. Firstly, testing a background signal by using a Raman spectrum analyzer and a mass spectrum analyzer, then triggering an electrochemical workstation, and simultaneously obtaining an electrochemical reaction signal, a mass spectrum testing signal and a Raman spectrum signal by adopting a working mode of a potentiodynamic potential or a constant current.
(5) And after the test is finished, closing the instrument, closing the power supply and finishing the test.
Example two
In this embodiment, a vertical through hole perpendicular to the bottom is formed in the center of the top of the flange bottom, and in order to realize the combination of raman and mass spectrometry, as shown in fig. 4, 5 and 6, a mass spectrometry sample injection pipe is fixed in the vertical through hole at the flange bottom, the mass spectrometry sample injection pipe is fixed by a third fixing screw, a through hole is formed in the center of the third fixing screw, and threads are formed around the end part of the third fixing screw and can be in threaded fit with the vertical through hole. The gas generated by electrochemical reaction of the electrolyte in the flange base body can enter a mass spectrometer connected with the mass spectrum sampling pipe through a gas-liquid separation membrane, a porous metal support, a vertical through hole and the mass spectrum sampling pipe.
The other parts not mentioned in this embodiment are the same as those in the first embodiment.
The above-mentioned embodiments only represent some embodiments of the present invention, and the description thereof is specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, without departing from the spirit of the present invention, several variations and modifications can be made, which are within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.
Claims (10)
1. A sealed electrolytic cell device for in-situ detection of Raman and mass spectrometry is characterized by comprising a working electrode, a reference electrode, a counter electrode, a Raman electrolytic cell and a mass spectrometry sample inlet tube;
the Raman electrolytic cell comprises a flange base body, an optical window, a flange cover, a gas-liquid separation membrane, a porous metal supporting sheet and a flange bottom; the center of the flange base body is provided with a through hole, the top of the flange base body is sequentially fixed with an optical window and a flange cover from bottom to top, and the bottom of the flange base body is sequentially fixed with a gas-liquid separation membrane, a porous metal support sheet and a flange bottom from top to bottom; the reference electrode and the counter electrode are respectively fixed on two sides of the flange matrix, and the working electrode is fixed between the gas-liquid separation membrane and the flange matrix;
the center of the flange bottom is provided with an L-shaped through hole penetrating through the side wall or a vertical through hole penetrating through the bottom surface, and the mass spectrum sampling pipe is arranged in the L-shaped through hole or the vertical through hole.
2. The in-situ detection sealed electrolytic cell device for Raman and mass spectrometry of claim 1, wherein the reference electrode is fixed on one side surface of the flange substrate through a first fixing screw, and the counter electrode is fixed on the other side surface of the flange substrate through a second fixing screw.
3. The in-situ detection sealed electrolytic cell device for raman and mass spectrometry according to claim 2, wherein a first sealing ring is disposed between the optical window and the flange base; a second sealing ring is arranged between the first fixing screw and the flange base body; a third sealing ring is arranged between the second fixing screw and the flange base body; and a fourth sealing ring is arranged between the working electrode and the flange base body.
4. The in-situ detection sealed electrolytic cell device for Raman and mass spectrometry according to claim 3, wherein the first, second, third and fourth sealing rings are perfluoro-ether rubber sealing rings or silica gel sealing rings.
5. The in-situ detection sealed electrolytic cell device for Raman and mass spectrometry of claim 1, wherein the optical window is made of sapphire glass sheet, calcium fluoride or potassium bromide.
6. A raman and mass spectrometry in-situ detection sealed electrolytic cell device according to claim 1, wherein the working electrode is a catalyst coated carbon paper electrode, a gas diffusion electrode or a catalyst coated gold-plated teflon film, the reference electrode is a silver chloride electrode, a mercury oxide electrode or a reversible hydrogen electrode, and the counter electrode is a platinum wire electrode, a nickel mesh electrode, a graphite rod electrode or a carbon mesh electrode.
7. The in-situ detection sealed electrolytic cell device used in combination of Raman and mass spectrometry according to claim 1, wherein the gas-liquid separation membrane is a porous polytetrafluoroethylene membrane, and the diameter of the membrane pores ranges from 0.2 micrometers to 10 micrometers.
8. The in-situ detection sealed electrolytic cell device for raman and mass spectrometry according to claim 1, wherein the material of the flange cover, the flange base and the flange bottom can be corrosion-resistant plastic or corrosion-resistant metal.
9. The sealed electrolytic cell device for in-situ detection of raman and mass spectrometry according to claim 1, wherein an electrolyte is injected into the flange matrix, and the electrolyte is an acid solution, an alkali solution or an organic solution.
10. The sealed electrolytic cell device for in-situ detection of Raman and mass spectrometry of claim 1 or 6, wherein the working electrode, the reference electrode and the counter electrode are connected to an electrochemical workstation, and the mass spectrometry sampling tube is connected to a mass spectrometer.
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| CN202021529340.0U CN212646486U (en) | 2020-07-29 | 2020-07-29 | Sealed electrolytic cell device for in-situ detection by combining Raman spectroscopy and mass spectrometry |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114002284A (en) * | 2021-11-02 | 2022-02-01 | 上海交通大学 | Differential electrochemical mass spectrum flow electrolytic cell for carbon neutralization test and design method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114002284A (en) * | 2021-11-02 | 2022-02-01 | 上海交通大学 | Differential electrochemical mass spectrum flow electrolytic cell for carbon neutralization test and design method thereof |
| CN114002284B (en) * | 2021-11-02 | 2022-10-18 | 上海交通大学 | Differential electrochemical mass spectrum flow electrolytic cell for carbon neutralization test and design method thereof |
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