CN106885774B - A kind of thin-layer spectral electrochemical detection device with sandwich structure - Google Patents
A kind of thin-layer spectral electrochemical detection device with sandwich structure Download PDFInfo
- Publication number
- CN106885774B CN106885774B CN201710025942.9A CN201710025942A CN106885774B CN 106885774 B CN106885774 B CN 106885774B CN 201710025942 A CN201710025942 A CN 201710025942A CN 106885774 B CN106885774 B CN 106885774B
- Authority
- CN
- China
- Prior art keywords
- layer
- electrode
- window
- thin
- detection device
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 230000003595 spectral effect Effects 0.000 title claims abstract description 34
- 238000000835 electrochemical detection Methods 0.000 title claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 claims abstract description 32
- 239000002184 metal Substances 0.000 claims abstract description 32
- 230000001681 protective effect Effects 0.000 claims abstract description 30
- 229920000642 polymer Polymers 0.000 claims abstract description 25
- 238000003487 electrochemical reaction Methods 0.000 claims abstract description 18
- 125000006850 spacer group Chemical group 0.000 claims abstract description 15
- 238000013461 design Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- 230000005611 electricity Effects 0.000 claims description 5
- 230000003287 optical effect Effects 0.000 claims description 5
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 3
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 3
- 238000009434 installation Methods 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 29
- 238000011065 in-situ storage Methods 0.000 abstract description 5
- 239000007795 chemical reaction product Substances 0.000 abstract description 3
- 230000005518 electrochemistry Effects 0.000 abstract description 3
- 239000013067 intermediate product Substances 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 238000002347 injection Methods 0.000 description 7
- 239000007924 injection Substances 0.000 description 7
- 239000002608 ionic liquid Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 229910052697 platinum Inorganic materials 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000011160 research Methods 0.000 description 6
- 238000002484 cyclic voltammetry Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 238000002329 infrared spectrum Methods 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004070 electrodeposition Methods 0.000 description 3
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-phenylethanol Chemical compound OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Natural products CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- 240000000233 Melia azedarach Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000007806 chemical reaction intermediate Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- DLRJIFUOBPOJNS-UHFFFAOYSA-N phenetole Chemical compound CCOC1=CC=CC=C1 DLRJIFUOBPOJNS-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000000411 transmission spectrum 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
-
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
-
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N2021/0325—Cells for testing reactions, e.g. containing reagents
- G01N2021/0328—Arrangement of two or more cells having different functions for the measurement of reactions
Abstract
The thin-layer spectral electrochemical detection device with sandwich structure that the invention discloses a kind of.Rubber spacer, upper layer window, polymer washer and lower layer's window are successively arranged between this detection device upper layer metal decking and lower metal panel；Polymer washer is arranged between upper layer window and lower layer's window；Form the multilayered structure of similar sandwich；Working electrode, reference electrode and auxiliary electrode are set in thin layer, constitute the electrochemical reaction cell of three electrodes；Lower layer's window periphery is equipped with protective case；Through-hole is equipped among protective case, through-hole can just place lower layer's window and polymer washer；Electrode connects jack and is arranged on the outside of protective case；The present invention has good air-tightness, and thickness of thin layer can be adjusted according to polymer washer, and then provides the purpose for having outstanding thin layer electrochemistry response feature, it can be achieved that electrochemical reaction product and intermediate product In situ spectroscopic detect.
Description
Technical field
The present invention relates to electrochemical in-situs and spectrum analysis field, have three for in-situ study more particularly to a kind of
The thin-layer spectral electrochemical detection device of Mingzhi's structure.
Background technique
Spectroelectrochemistry combines electrochemistry and spectral technique, for research and accurately concludes electrochemical reaction product and centre
Product provides a kind of new method.Controlled by voltage, make electrochemical reaction in spectroelectrochemistry detection device smoothly into
Row, while the spectral information of these substances is obtained, and then obtain electrochemical reaction dynamics and thermodynamic parameter, it is that research electricity is living
Inorganic, organic, organism electrochemical reaction mechanism the important means of property.The key of spectroelectrochemistry research is spectroelectrochemistry
Detection device.
Currently, reported spectroelectrochemistry detection device is all based on respective design, exist in practical applications very much
Problem, and then limit application of the spectroelectrochemistry in electrochemical research field.Comparing distinct issues includes:
(1) working electrode problem.Under the conditions of complicated electrochemical reaction, reaction product or intermediate product can be adsorbed on work
Electrode surface causes the pollution of electrode, and (see Britain Specac public affairs in some existing spectroelectrochemistry detection device designs
Take charge of the thin-layer spectral electrochemical detection device of production), electrode especially working electrode is all fixed non-exchange, therefore can not
The cleaning and reuse for carrying out electrode, cause huge waste.
(2) sample introduction problem.In existing some designs, sample introduction need to first inject a sample into liquid storage tank or electrode cell, after by
Liquid storage tank or electrode cell enter detection device, and sample size needed for this input mode is more, and it is biggish not to be suitable for viscosity
Sample (such as: ionic liquid).
(3) air-tightness problem.For containing the system of multiple electrochemical reaction processes, electrochemistry intermediate product is to oxygen
It is extremely sensitive with humidity, while the time for being used to complete the measurement of whole system spectroelectrochemistry is longer, it is therefore necessary to guarantee detection
Device in measurement process No leakage and have good air-tightness.
(4) construction problem.Every time measurement after spectroelectrochemistry detection device will be cleaned, some detection devices by
It is complicated in construction, thus dismantle, assembling process it is comparatively laborious, especially electrode position is corrected in an assembling process,
Limit the quick reuse of detection device.
(5) Problem of Universality.The special designing of detection device will limit it and match with general commercial spectral instrument, need
Light path calibration is carried out by special sample holder, is restricted the universality of spectroelectrochemistry.
The solution of problem above has important meaning to the application of promotion and universal spectroelectrochemistry method in daily research
Justice.
Summary of the invention
The problem of present invention is generally directed to the uses of current spectroelectrochemistry detection device provides a kind of with Sanming City
The thin-layer spectral electrochemical detection device of structure is controlled, the detection device function admirable is easy to operate, can be with current most of commercial
Ultraviolet-visible light and infrared spectrometer combination, and do not need additional sample bracket.
The object of the invention is realized by following technological means:
A kind of thin-layer spectral electrochemical detection device with sandwich structure, which is characterized in that including upper layer metal covering
Plate, rubber spacer, upper layer window, protective case, lower metal panel, polymer washer, lower layer's window, working electrode, ginseng
Than electrode and auxiliary electrode；Upper layer metal decking and lower metal panel are fixed by bolt spacings, and upper layer metal decking is under
Rubber spacer, upper layer window, polymer washer and lower layer's window are successively arranged between layer metal decking；
Upper layer window, lower layer's window and the polymer washer for being equipped with through-hole fit closely a group straticulation；Polymer pad
Circle is arranged between upper layer window and lower layer's window；Form the multilayered structure of similar sandwich；Set in thin layer working electrode,
Reference electrode and auxiliary electrode constitute the electrochemical reaction cell of three electrodes；
Lower layer's window periphery is equipped with protective case；Through-hole is equipped among protective case, through-hole can just place lower layer's window
With polymer washer；Electrode connects jack and is arranged on the outside of protective case；
It is all provided on upper layer metal decking, rubber spacer and upper layer window into sample outlet hole, between sample outlet hole and thin layer
Form U-shaped channel design；It is equipped with sample holes and sample outlet hole into sample outlet hole, two holes are located at the two sides of thin layer, and structure is identical, disengaging
Sample hole forms U-shaped channel design；
Protective case and upper layer metal decking are designed with bolt hole, lower metal panel together with bolt welding, rubber every
Pad 2 and window are fixed by being fitted close, bolt passing through bolt hole and nut cooperation fastening installation；
Working electrode, reference electrode and auxiliary electrode are connect with electrode cable respectively；Electrode cable is being protected with setting respectively
Three jacks in electrode connection jack on sheath are connected, and separately take three conducting wires, and three in electrode connection jack are inserted into one end
A jack, other end working electrode electrode holder corresponding with electrochemical workstation, reference electrode electrode holder and auxiliary electrode electrode
Folder is connected.
To further realize the object of the invention, it is preferable that the material of the upper layer window and lower layer's window is all made of
CaF2。
Preferably, the through-hole of the polymer washer is hexagon.
Preferably, the working electrode is metallic mesh structure, between auxiliary electrode and reference electrode.
Preferably, the working electrode is placed in optical path Center position.
Preferably, the protective case is rectangular parallelepiped structure, and a rectangular through-hole has been dug in centre.
Preferably, the protective case is plastic material.
A kind of thin-layer spectral electrochemical detection device with sandwich structure of the invention, the detection device main body is by one
Window and the polymer washer being located between two pieces of windows with electrode are formed, upper layer window both ends respectively open one
Aperture is used for sample introduction, and lower layer's window is fixed by protective case, and electrode cable is pierced by from protective case one end and connect jack with electrode
It is connected.All structures mutually fasten layer by layer, are finally fixed again by two pieces of metal deckings by knob nut, that is, are assembled into similar three
Mingzhi's detection device with multi-layer structure.And be provided with inlet and outlet on the panel of upper layer, on the window of upper layer into sample outlet hole
Relatively, there is rubber spacer for pressure buffer between panel and window.
The present invention realizes that ne-leakage, high-air-tightness are suitable for air-sensitive and water-sensitive material and easy volatile solvent, and suitable
For measuring for a long time.
Thin layer design provides outstanding thin layer volt-ampere electrochemical characteristic, eliminates the influence of solution diffusion to the full extent, fits
It is reacted for fast electrochemical；Meanwhile sample waste is reduced, measurement only needs 0.1-0.2 milliliters of samples every time.
Window of the present invention is convenient for changing, and by the selection of window, spectrum can cover ultraviolet, visible light, near-infrared, red
Outside, far infrared range.
The present invention utilizes hydrodynamic injection, and by U-shaped sample intake passage, this detection device can be applied to the higher ionic liquid of viscosity
Measurement under concrete conditions in the establishment of a specific crime.
The present invention is suitable for all brand ultraviolet-visible light-near-infrareds and infrared spectrometer, does not need special bracket and light
It learns attachment and carries out light path calibration.
Electronic noise of the present invention is low, while being suitable for laser Raman spectroscopy and some Experiment of Laser Scattering.
Compared with the existing technology, the present invention just has the following advantages:
1) the thin-layer spectral electrochemical detection device size is according to commercial spectrometers sample groove structure design, and when measurement only needs
Spectroelectrochemistry detection device is inserted into sample cell, assembly operation is simple and easy to do, and optical path is easy calibration, measurement noise
It is small.
2) thickness of thin layer of the thin-layer spectral electrochemical detection device can be easily adjusted by changing membrane thicknesses,
Good thin layer volt-ampere electrochemical characteristic is provided, eliminates the influence of solution diffusion to the full extent, electrochemical reaction is quick, complete
Entirely, and the test sample amount of needs is less.
3) the thin-layer spectral electrochemical detection device window is convenient for changing, and the window of different materials keeps detection device suitable
For the spectral measurement under different wave length；Meanwhile electrode can also be replaced according to requirement of experiment, be suitable under different condition
Electrochemical reaction, expand the application range of spectroelectrochemistry detection device.
4) the thin-layer spectral electrochemical detection device ne-leakage has high-air-tightness, is suitable for air-sensitive and water sensitive material
Material and easy volatile solvent and the electrochemical reaction of long period.
5) allow to carry out hydrodynamic injection by U-shaped sample intake passage, the biggish ionic liquid of viscosity can be used to carry out spectrum electricity
Chemical measurement.
Detailed description of the invention
Fig. 1 spectroelectrochemistry thin layer transmits reaction unit main view direction explosive view；
Fig. 2 spectroelectrochemistry thin layer transmits reaction unit left view；
Fig. 3 is the structural schematic diagram of protective case in Fig. 1；
Fig. 4 is the structural schematic diagram of Fig. 1 metal decking at the middle and upper levels；
Fig. 5 is the cyclic voltammogram of ferrocene；
Fig. 6 is the in-situ ft-ir figure of 4- ethoxybenzene ethyl alcohol under 1.738V；A is background spectrogram in figure；B, c, d, e points
The variation of infrared spectrum after voltage 0min, 0.5min, 1.0min, 1.5min Wei not applied.
Shown in figure: upper layer metal decking 1, rubber spacer 2, upper layer window 3, protective case 4, electrode connection jack 5, under
Layer metal decking 6, into sample outlet hole 7, bolt 8, polymer washer 9, lower layer's window 10, nut 11, bolt hole 12, working electrode
13, thin layer 14, reference electrode 15, auxiliary electrode 16.
Specific embodiment
For a better understanding of the invention, below with reference to embodiment, the present invention will be further described, but reality of the invention
It is without being limited thereto to apply mode.
As shown in Figs 1-4, this thin-layer spectral electrochemical detection device has the multilayered structure of similar sandwich, including upper layer
Metal decking 1, rubber spacer 2, upper layer window 3, protective case 4, lower metal panel 6, polymer washer 9, lower layer's window
10, working electrode 13, reference electrode 15 and auxiliary electrode 16；Upper layer metal decking 1 and lower metal panel 6 pass through between bolt 8
Rubber spacer 2, upper layer window 3, polymer pad are successively arranged between fixation, upper layer metal decking 1 and lower metal panel 6
Circle 9 and lower layer's window 10.
According to the characteristics of infrared spectrometry and requirement, the material of upper layer window 3 and lower layer's window 10 is all made of
CaF2, and group straticulation 14 is fitted closely with the polymer washer 9 for being equipped with hexagon through-hole；Polymer washer 9 is arranged on upper layer
Between window 3 and lower layer's window 10；Thin layer 14 is folded between upper layer window 3 and lower layer's window 10, is formed similar
The multilayered structure of sandwich；Working electrode 13, reference electrode 15 and auxiliary electrode 16 are set in thin layer 14, constitute the electrification of three electrodes
Learn reaction tank；Wherein, metallic mesh working electrode 13 is between auxiliary electrode 16 and reference electrode 15, and is placed in optical path Center
Position, convenient for collecting the spectrum change information generated due to electrochemical reaction in electrode surface.
10 periphery of lower layer's window is equipped with protective case 4；Protective case 4 is cuboid, and the logical of a small cuboid has been dug in centre
Hole, through-hole can just place lower layer's window 10 and polymer washer 9.There are three electrode jack, protective case is 4 one end of protective case
Plastic material primarily serves fixed effect.Electrode connects the setting of jack 5 in 4 outside of protective case.
It is all provided on upper layer metal decking 1, rubber spacer 2 and upper layer window 3 into sample outlet hole 7, into sample outlet hole 7 and thin layer
U-shaped channel design is formed between 14；It is equipped with sample holes and sample outlet hole into sample outlet hole 7, two holes are located at the two sides of thin layer, structure phase
Together, as soon as from stomidium vertically down into thin layer 14, extra sample squeezes out sample vertically upward from the other end when sample introduction, disengaging
Sample hole forms U-shaped channel design, is used for 14 sample introduction of thin layer；Rubber spacer 2 is used for pressure buffer.
Protective case 4 and upper layer metal decking 1 are designed with bolt hole 12, and lower metal panel 6 and bolt 8 are closely welded on one
It rises, rubber spacer 2 and upper layer window, lower layer's window are fixed by being fitted close, and bolt 8 passes through bolt hole 12 and spiral shell
11 cooperation fastening installation of mother.
Working electrode 13, reference electrode 15 and auxiliary electrode 16 are connect with electrode cable respectively；Electrode cable respectively with set
Three jacks set in electrode connection jack 5 on the protective sleeve are connected, and separately take three conducting wires, one end is inserted into electrode and connects jack
Three jacks in 5, other end working electrode electrode holder corresponding with electrochemical workstation, reference electrode electrode holder and auxiliary electricity
Pole electrode holder is connected, to realize that spectrometer and electrochemical workstation are combined.
The present invention has each component part of thin-layer spectral electrochemical detection device of sandwich structure simple and relatively independent,
It only needs mutually to fasten layer by layer, then is fixed by knob nut seal, can be formed with multi-level sandwich structure, therefore tear open
It unloads, is easy to assembly, being readily cleaned.Reaction detection thin layer is by polymer washer 9, upper layer window 3 and lower layer with three electrodes
Window 10 seals composition under impressed pressure, and without special designing reaction pond body and electrode cell, and thickness of thin layer can be by polymerizeing
Object washer is adjusted, and provides faster electrochemical reaction speed；Device sample introduction is not necessarily to liquid storage tank, direct using U-shaped sample intake passage
It is connected with thin layer, the present invention is made to be more suitable for the higher sample measurement of viscosity；Electrode is integrated with washer, reduces external site,
Improve the airtight effect of device.
The above-mentioned thin-layer spectral electrochemical detection device with sandwich structure overcomes the prior art to deposit in the following manner
The problem of:
(1) working electrode problem.Working electrode is easy to clean, and replacement working electrode need to be only bumped into polymer washer
9, and one end is connect with electrode cable, electrode replacement can be realized.
(2) sample introduction problem.Apparatus of the present invention sample introduction is not necessarily to liquid storage tank, is directly connected with thin layer using U-shaped sample intake passage, is made
The present invention is more suitable for the higher sample measurement of viscosity.General spectroelectrochemistry detection device is made by the mobility of sample
Sample voluntarily flows into detection device from liquid storage tank, and ionic liquid biggish for viscosity, due to its poor fluidity, sample enters
Detection device there is difficulty, and the present invention carries out hydrodynamic injection by U-shaped sample intake passage can overcome the problems, such as this completely.Pass through
The mode of syringe pressing, as soon as sample from the stomidium into sample outlet hole 7 vertically into thin layer 14, extra sample is vertical from the other end
It is straight to squeeze out.Meanwhile the input mode can reduce sample waste, measurement only needs 0.1-0.2 milliliters of samples every time.
(3) air-tightness problem.Reaction detection thin layer is by polymer washer 9, upper layer window 3 and lower layer with three electrodes
Window 10 seals composition under impressed pressure, and without special designing reaction pond body and electrode cell, and thickness of thin layer can be by polymerizeing
Object washer is adjusted, and provides faster electrochemical reaction speed；Electrode is integrated with washer, reduces external site, improves device
Airtight effect.
(4) construction problem.Each component part of apparatus of the present invention is simple and relatively independent, only needs mutually to fasten layer by layer, then lead to
It crosses knob nut seal to fix, can be formed with multi-level sandwich structure, therefore dismantle, is easy to assembly, be readily cleaned.
And since electrode position is fixed, therefore the quick of detection device is realized without being corrected to electrode position in an assembling process
It reuses.
(5) Problem of Universality.Detection device size of the invention is not needed according to commercial spectrometers sample groove structure design
Special sample holder, directly will test device insertion optical spectrometer sample slot can be realized measurement.
Embodiment 1
Platinum guaze working electrode, platinum guaze auxiliary is respectively adopted in the embodiment working electrode 13, reference electrode 15, auxiliary electrode 16
Electrode, platinum filament reference electrode, remaining same Fig. 1-4.In use, preparing the acetonitrile solution of 0.1mol/L lithium perchlorate as electrolysis
Liquid is added 0.9mg ferrocene (about 1mmol/L) into 5mL electrolyte, 0.2mL solution is taken with syringe, using hydrodynamic injection
Mode injects thin layer 14 from sample holes, covers tightly and takes three conducting wires by the thin-layer spectral electrification with sandwich structure into sample outlet hole 7
Learning detection device, (model CHI660E, electrochemical workstation can provide electricity of the molecule on electrode interface with electrochemical workstation
The information such as redox electronics transfer information and solution diffusive migration) connection, cyclic voltammetry scan is carried out to sample.Experiment
Method choice cyclic voltammetry, experiment parameter are provided that take-off potential -1V, maximum potential 0.95V, sweep speed 5mV/s,
2 sections of number of segment of scanning；Cyclic voltammogram if Fig. 5 is ferrocene (electrode cable Lian Haohou, opens electrochemical workstation and matches
Software, select cyclic voltammetry, be arranged experiment parameter, click determine i.e. starts to scan), the interval of oxidation peak and reduction peak
For 16mV, illustrate that the thin-layer spectral electrochemical detection device with sandwich structure is capable of providing outstanding thin layer volt-ampere electrification
Feature is learned, eliminates the influence of solution diffusion to the full extent, is suitable for fast electrochemical and reacts.
Embodiment 2
Platinum guaze working electrode, platinum guaze auxiliary is respectively adopted in the embodiment working electrode 13, reference electrode 15, auxiliary electrode 16
Electrode, platinum filament reference electrode, remaining same Fig. 1-4.In use, taking 0.2mL1- butyl -3- methylimidazole fluoroform with syringe
Sulfonate ([bmim] CF3SO3) ionic liquid, thin layer is injected from sample holes by the way of hydrodynamic injection, is covered tightly into sample outlet hole 7,
Thin-layer spectral electrochemical detection device insertion Fourier Transform Infrared Spectrometer with sandwich structure is subjected to infrared spectroscopy
Background channel scans, and sample channel scanning is clicked after background scans to get the curve a into Fig. 6, with [bmim] CF3SO3As back
The infrared spectrum of scape, the spectrogram is more steady, illustrates that the detection device has the characteristics that light measurement noise is small.And by it is U-shaped into
Sample channel carry out hydrodynamic injection, can overcome the biggish ionic liquid of viscosity be applied to transmission spectra electrochemical measurement when, due into
Sample is difficult and is unable to get the problem of application.
To 5mL [bmim] CF3SO3Middle addition 20.8mg4- ethoxybenzene ethyl alcohol (about 25mmol/L), is taken with syringe
0.2mL solution injects thin layer from sample holes by the way of hydrodynamic injection, covers tightly into sample outlet hole 7, take three conducting wires that will have three
The thin-layer spectral electrochemical detection device of Mingzhi's structure is connect with electrochemical workstation, by the thin-layer spectral with sandwich structure
Electrochemical detection device is placed in Fourier Transform Infrared Spectrometer sample cell.Fig. 6, which is shown, to be applied under 1.738V voltage, 4- second
The variation of the infrared spectrum of oxygroup benzyl carbinol, and with [bmim] CF3SO3Infrared spectrum as background spectrogram.Wherein b, c, d, e
The variation of infrared spectrum after respectively application voltage 0min, 0.5min, 1.0min, 1.5min.Become every 0.5min spectral signal
Change obviously, illustrates that thin layer without diffusion, reflects that electrochemical reaction is quick；Spectral signal no longer changes after 1.5min, illustrates electrification
Learn fully reacting.Through electrochemical oxidation reactions, 1723cm-1、1691cm-1There is new infrared absorption peak in place, it was demonstrated that 4- ethyoxyl
Major oxidation product of the benzyl carbinol under the voltage of 1.738V is 4- acetophenone, this process also makes benzene ring structure simultaneously
Changed, 1614cm-1Place's characteristic peak shifts to lower wave number to 1602cm-1.Result of study shows: this has sandwich knot
The thin-layer spectral electrochemical detection device of structure is controlled by voltage, keeps electrochemical reaction smooth in spectroelectrochemistry detection device
It carries out, while being capable of providing preferable In situ spectroscopic information, data supporting is provided for analysis reaction intermediate, is particularly suitable for
In the research of reaction mechanism.
Embodiment of the present invention are not limited by the above embodiments, other any real without departing from spirit of the invention
Made changes, modifications, substitutions, combinations, simplifications under matter and principle, should be equivalent substitute mode, are included in the present invention
Protection scope within.
Claims (7)
1. a kind of thin-layer spectral electrochemical detection device with sandwich structure, which is characterized in that including upper layer metal decking,
Rubber spacer, upper layer window, protective case, lower metal panel, polymer washer, lower layer's window, working electrode, reference electricity
Pole and auxiliary electrode；Upper layer metal decking and lower metal panel are fixed by bolt spacings, upper layer metal decking and lower layer's gold
Belong to and is successively arranged rubber spacer, upper layer window, polymer washer and lower layer's window between panel；
Upper layer window, lower layer's window and the polymer washer for being equipped with through-hole fit closely a group straticulation；Polymer washer is set
It sets between upper layer window and lower layer's window；Form the multilayered structure of similar sandwich；Working electrode, reference are set in thin layer
Electrode and auxiliary electrode constitute the electrochemical reaction cell of three electrodes；
Lower layer's window periphery is equipped with protective case；Through-hole is equipped among protective case, through-hole can just place lower layer's window and gather
Close object washer；Electrode connects jack and is arranged on the outside of protective case；
It is all provided on upper layer metal decking, rubber spacer and upper layer window into sample outlet hole, into forming U between sample outlet hole and thin layer
Type channel design；It is equipped with sample holes and sample outlet hole into sample outlet hole, two holes are located at the two sides of thin layer, and structure is identical, into sample outlet hole
Form U-shaped channel design；
Protective case and upper layer metal decking are designed with bolt hole, and lower metal panel is together with bolt welding, 2 He of rubber spacer
Window is fixed by being fitted close, bolt passing through bolt hole and nut cooperation fastening installation；
Working electrode, reference electrode and auxiliary electrode are connect with electrode cable respectively；Electrode cable is respectively with setting in protective case
On electrode connection jack in three jacks be connected, separately take three conducting wires, be inserted into electrode connection jack three of one end insert
Hole, other end working electrode electrode holder corresponding with electrochemical workstation, reference electrode electrode holder and auxiliary electrode electrode holder phase
Even.
2. the thin-layer spectral electrochemical detection device according to claim 1 with sandwich structure, which is characterized in that institute
The material for stating upper layer window and lower layer's window is all made of CaF2。
3. the thin-layer spectral electrochemical detection device according to claim 1 with sandwich structure, which is characterized in that institute
The through-hole for stating polymer washer is hexagon.
4. the thin-layer spectral electrochemical detection device according to claim 1 with sandwich structure, which is characterized in that institute
Stating working electrode is metallic mesh structure, between auxiliary electrode and reference electrode.
5. the thin-layer spectral electrochemical detection device according to claim 1 or 4 with sandwich structure, feature exist
In the working electrode is placed in optical path Center position.
6. the thin-layer spectral electrochemical detection device according to claim 1 with sandwich structure, which is characterized in that institute
Stating protective case is rectangular parallelepiped structure, and a rectangular through-hole has been dug in centre.
7. the thin-layer spectral electrochemical detection device according to claim 1 with sandwich structure, which is characterized in that institute
Stating protective case is plastic material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710025942.9A CN106885774B (en) | 2017-01-13 | 2017-01-13 | A kind of thin-layer spectral electrochemical detection device with sandwich structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710025942.9A CN106885774B (en) | 2017-01-13 | 2017-01-13 | A kind of thin-layer spectral electrochemical detection device with sandwich structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106885774A CN106885774A (en) | 2017-06-23 |
| CN106885774B true CN106885774B (en) | 2019-11-15 |
Family
ID=59176005
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710025942.9A Active CN106885774B (en) | 2017-01-13 | 2017-01-13 | A kind of thin-layer spectral electrochemical detection device with sandwich structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106885774B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107764881A (en) * | 2017-11-27 | 2018-03-06 | 民康医疗科技（天津）有限公司 | A kind of portable blood test kit device based on electrochemical method |
| CN109001271B (en) * | 2018-06-08 | 2024-03-29 | 中国科学技术大学 | Thin liquid layer electrochemical reaction pond suitable for infrared detection of normal position |
| CN111855767B (en) * | 2020-07-01 | 2022-10-11 | 安徽中医药大学 | Multifunctional flowing thin-layer electrochemical cell and application thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8585880B2 (en) * | 2011-09-27 | 2013-11-19 | Battelle Memorial Institute | Method and apparatus for simultaneous spectroelectrochemical analysis |
| CN103175876B (en) * | 2011-12-22 | 2014-09-17 | 中国科学院大连化学物理研究所 | Spectroelectrochemical in-situ pool and application thereof |
| CN103196963A (en) * | 2012-01-05 | 2013-07-10 | 中国科学院过程工程研究所 | Ionic liquid system electrochemical process in-situ research device |
| CN102654477B (en) * | 2012-04-23 | 2014-12-17 | 华东理工大学 | Dark-field nano spectral electrochemical detection pool for plasma observation |
| CN105403553B (en) * | 2015-12-31 | 2019-01-22 | 中国科学技术大学 | A kind of laminar flows electrolytic cell suitable for the detection of electrochemical in-situ Raman spectrum |
-
2017
- 2017-01-13 CN CN201710025942.9A patent/CN106885774B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN106885774A (en) | 2017-06-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| McKenzie et al. | Versatile tools for understanding electrosynthetic mechanisms | |
| Lee et al. | Electrochemical upgrade of CO2 from amine capture solution | |
| Elgrishi et al. | A practical beginner’s guide to cyclic voltammetry | |
| León et al. | Designing spectroelectrochemical cells: A review | |
| CN106885774B (en) | A kind of thin-layer spectral electrochemical detection device with sandwich structure | |
| Bond et al. | Changing the look of voltammetry | |
| Gregoire et al. | Scanning droplet cell for high throughput electrochemical and photoelectrochemical measurements | |
| Wightman | Microvoltammetric electrodes | |
| Zoski | Handbook of electrochemistry | |
| Nemes et al. | A terahertz-transparent electrochemical cell for in situ terahertz spectroelectrochemistry | |
| CN107389591A (en) | The dual-purpose in situ detection hermetic electrolyte pond of Raman and infrared spectra, use its method and application thereof | |
| CN105203527B (en) | The optical electro-chemistry detection means and its application method of a kind of double detection cells | |
| Yang et al. | Surface-enhanced infrared spectroscopic study of a CO-covered Pt electrode in room-temperature ionic liquid | |
| CN111721752A (en) | Raman and mass spectrum combined in-situ detection sealed electrolytic cell device and method | |
| Rastgar et al. | Characterization of photoactivity of nanostructured BiVO4 at polarized liquid–liquid interfaces by scanning electrochemical microscopy | |
| Corva et al. | Differential tafel analysis: A quick and robust tool to inspect and benchmark charge transfer in electrocatalysis | |
| Schlüter et al. | Nonlinear electrochemical analysis: worth the effort to reveal new insights into energy materials | |
| Ha et al. | Implementation of second-generation fourier transform electrochemical impedance spectroscopy with commercial potentiostat and application to time-resolved electrochemical impedance spectroscopy | |
| CN101424693B (en) | Portable plumbum ion concentration analyzer using disposable sensor | |
| Chen et al. | Parallel-opposed dual-electrode detector with recycling amperometric enhancement for capillary electrophoresis | |
| Giordano et al. | An integrated platform for gas-diffusion separation and electrochemical determination of ethanol on fermentation broths | |
| Tang et al. | Adsorption and Electrochemistry of Carbon Monoxide at the Ionic Liquid–Pt Interface | |
| Krempl et al. | Dynamic interfacial reaction rates from electrochemistry–mass spectrometry | |
| Ibañez et al. | Bipolar spectroelectrochemistry | |
| CN100406882C (en) | Method for capillary electrophoresis amperometric detection of amphetamines |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |