CN106885774A - A kind of thin-layer spectral electrochemical detection means with sandwich structure - Google Patents
A kind of thin-layer spectral electrochemical detection means with sandwich structure Download PDFInfo
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- CN106885774A CN106885774A CN201710025942.9A CN201710025942A CN106885774A CN 106885774 A CN106885774 A CN 106885774A CN 201710025942 A CN201710025942 A CN 201710025942A CN 106885774 A CN106885774 A CN 106885774A
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- 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
- 238000012856 packing Methods 0.000 claims abstract description 28
- 229920000642 polymer Polymers 0.000 claims abstract description 25
- 238000003487 electrochemical reaction Methods 0.000 claims abstract description 19
- 125000006850 spacer group Chemical group 0.000 claims abstract description 15
- 238000010276 construction Methods 0.000 claims abstract description 9
- 238000013461 design Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 11
- 230000005611 electricity Effects 0.000 claims description 5
- 238000003780 insertion Methods 0.000 claims description 5
- 230000037431 insertion Effects 0.000 claims description 5
- 239000000203 mixture Substances 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
- 239000004033 plastic Substances 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 32
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 230000005518 electrochemistry Effects 0.000 abstract description 3
- 239000013067 intermediate product Substances 0.000 abstract description 3
- 239000007795 chemical reaction product Substances 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 10
- 210000004027 cell Anatomy 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 230000008859 change Effects 0.000 description 7
- 238000002347 injection Methods 0.000 description 7
- 239000007924 injection Substances 0.000 description 7
- 238000002329 infrared spectrum Methods 0.000 description 6
- 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
- 238000002474 experimental method Methods 0.000 description 5
- 238000011160 research 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
- 238000002484 cyclic voltammetry Methods 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
- 230000003670 easy-to-clean Effects 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
- 239000000047 product Substances 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 206010068052 Mosaicism Diseases 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 210000003765 sex chromosome Anatomy 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- CNMVSNTVPZWQMI-UHFFFAOYSA-N 2-(4-ethoxyphenyl)ethanol Chemical compound CCOC1=CC=C(CCO)C=C1 CNMVSNTVPZWQMI-UHFFFAOYSA-N 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- 238000004566 IR spectroscopy Methods 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004140 cleaning Methods 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
- 150000002118 epoxides Chemical class 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000010249 in-situ analysis Methods 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical class [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 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
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 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
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000000126 substance Substances 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
- 230000007306 turnover Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—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
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a kind of thin-layer spectral electrochemical detection means with sandwich structure.Rubber spacer, upper strata window, polymer packing ring and lower floor's window are sequentially provided between this detection means upper strata metal decking and lower metal panel；Polymer packing ring is arranged between upper strata window and lower floor's window；Form the sandwich construction of similar sandwich；Working electrode, reference electrode and auxiliary electrode are set in thin layer, the electrochemical reaction cell of three electrodes is constituted；Lower floor's window periphery is provided with protective case；Through hole is provided with the middle of protective case, through hole can just place lower floor's window and polymer packing ring；Electrode connection jack is arranged on protective case outside；The present invention has good air-tightness, and thickness of thin layer can be adjusted according to polymer packing ring, and then provides with outstanding thin layer electrochemistry response feature, is capable of achieving the purpose of electrochemical reaction product and the detection of intermediate product In situ spectroscopic.
Description
Technical field
The present invention relates to electrochemical in-situ and spectrum analysis field, it is more particularly to a kind of for in-situ study with three
The thin-layer spectral electrochemical detection means of Mingzhi's structure.
Background technology
Spectroelectrochemistry combines electrochemistry and spectral technique, for research and accurately concludes electrochemical reaction product and centre
Product provides a kind of new method.By voltage control, electrochemical reaction is set smoothly to enter in spectroelectrochemistry detection means
OK, while obtaining the spectral information of these materials, and then electrochemical reaction dynamics and thermodynamic parameter are obtained, is that research electricity is living
Inorganic, organic, organism electrochemical reaction mechanism the important means of property.What spectroelectrochemistry was studied it is critical only that spectroelectrochemistry
Detection means.
At present, the spectroelectrochemistry detection means reported is all based on respective design, in actual applications in the presence of a lot
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, product or intermediate product can be adsorbed in work
Electrode surface, causes the pollution of electrode, and (public see Britain Specac in some existing spectroelectrochemistry detection means designs
Take charge of the thin-layer spectral electrochemical detection means of production), especially working electrode all fixes non-exchange to electrode, therefore cannot
Cleaning and the reuse of electrode are carried out, huge waste is caused.
(2) sample introduction problem.It is existing some design in, sample introduction need to first inject a sample into liquid storage tank or electrode cell, after by
Liquid storage tank or electrode cell enter into detection means, and sample size needed for this input mode is more, and it is larger not to be suitable for viscosity
Sample is (for example：Ionic liquid).
(3) airtight sex chromosome mosaicism.For the system containing multiple electrochemical reaction processes, its electrochemistry intermediate product is to oxygen
It is extremely sensitive with humidity, while more long for completing the time of whole system spectroelectrochemistry measurement, it is therefore necessary to ensure detection
Device No leakage and with good air-tightness in measurement process.
(4) construction problem.Every time measurement after spectroelectrochemistry detection means will be cleaned, some detection means by
It is complicated in construction, therefore dismounting, assembling process are comparatively laborious, especially electrode position are corrected in an assembling process,
Limit the quick reuse of detection means.
(5) Problem of Universality.The particular design of detection means can limit its match with general commercial spectral instrument, it is necessary to
Light path calibration is carried out by special sample holder, the universality of spectroelectrochemistry is restricted.
The solution of problem above has important meaning to promoting and popularizing application of the spectroelectrochemistry method in daily research
Justice.
The content of the invention
Present invention is generally directed to problem present in current spectroelectrochemistry detection means use, there is provided one kind has Sanming City
The thin-layer spectral electrochemical detection means of structure is controlled, the detection means function admirable is simple to operate, can be with current most of commercial
Ultraviolet-visible light and infrared spectrometer are combined, and do not need additional sample support.
The object of the invention is realized by following technological means：
A kind of thin-layer spectral electrochemical detection means with sandwich structure, it is characterised in that including upper strata metal covering
Plate, rubber spacer, upper strata window, protective case, lower metal panel, polymer packing ring, lower floor's window, working electrode, ginseng
Than electrode and auxiliary electrode；Upper strata metal decking and lower metal panel are fixed by bolt spacings, and upper strata metal decking is with
Rubber spacer, upper strata window, polymer packing ring and lower floor's window are sequentially provided between layer metal decking；
Upper strata window, lower floor's window are brought into close contact composition thin layer with the polymer packing ring for being provided with through hole；Polymer pad
Circle is arranged between upper strata window and lower floor's window；Form the sandwich construction of similar sandwich；Set in thin layer working electrode,
Reference electrode and auxiliary electrode, constitute the electrochemical reaction cell of three electrodes；
Lower floor's window periphery is provided with protective case；Through hole is provided with the middle of protective case, through hole can just place lower floor's window
With polymer packing ring；Electrode connection jack is arranged on protective case outside；
All it is provided with into sample outlet hole on upper strata metal decking, rubber spacer and upper strata window, is entered between sample outlet hole and thin layer
Form U-shaped channel design；Enter sample outlet hole and be provided with sample holes and sample outlet hole, two hole positions are in the both sides of thin layer, and structure is identical, pass in and out
Sample hole forms U-shaped channel design；
Protective case and upper strata metal decking are designed with bolt hole, lower metal panel together with bolt welding, rubber every
Pad 2 and window are all that, by being fitted close fixation, bolt passing through bolt hole is fastened with nut screw connection and installed；
Working electrode, reference electrode and auxiliary electrode are connected with electrode cable respectively；Electrode cable respectively be arranged on guarantor
Three jacks in electrode connection jack on sheath are connected, and separately take three wires, in one end insertion electrode connection jack three
Individual jack, other end working electrode electrode holder corresponding with electrochemical workstation, reference electrode electrode holder and auxiliary electrode electrode
Folder is connected.
Further to realize the object of the invention, it is preferable that the material of the upper strata window and lower floor's window is used
CaF2。
Preferably, the through hole of the polymer packing ring is hexagon.
Preferably, the working electrode is metallic mesh structure, between auxiliary electrode and reference electrode.
Preferably, the working electrode is placed in light path center.
Preferably, the protective case is rectangular 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 means with sandwich structure of the invention, the detection means main body is by one
To window and it is located between two pieces of windows the polymer packing ring with electrode and constitutes, upper strata window two ends respectively opens one
Aperture is used for sample introduction, and lower floor's window is fixed by protective case, and electrode cable is passed from protective case one end and is connected jack with electrode
It is connected.All structures are mutually fastened layer by layer, are finally fixed by knob nut by two pieces of metal deckings again, that is, be assembled into similar three
Mingzhi has the detection means of sandwich construction.And be provided with inlet and outlet on the panel of upper strata, with upper strata window on enter sample outlet hole
Relatively, there is rubber spacer between panel and window for pressure buffer.
The present invention realizes ne-leakage, and high-air-tightness is suitable to 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, and the influence of solution diffusion is eliminated to the full extent, fits
For fast electrochemical reaction；Meanwhile, sample waste is reduced, measurement every time only needs to 0.1-0.2 milliliters of sample.
Window of the present invention is convenient for changing, and by the selection of window, spectrum can cover ultraviolet, visible ray, near-infrared, red
Outward, far infrared scope.
The present invention utilizes hydrodynamic injection, and by U-shaped sample intake passage, this detection means can be applied to viscosity ionic liquid higher
Measurement under concrete conditions in the establishment of a specific crime.
The present invention is applied to all brand ultraviolet-visible light-near-infrareds and infrared spectrometer, it is not necessary to special support and light
Learning annex carries out light path calibration.
Electronic noise of the present invention is low, while being applied to laser Raman spectroscopy and some Experiment of Laser Scattering.
Relative to prior art, the present invention just has the following advantages：
1) the thin-layer spectral electrochemical detection means size is only needed according to commercial spectrometers sample cell structure design during measurement
Spectroelectrochemistry detection means is inserted into sample cell, assembly operation is simple and easy to do, and light path is easily calibrated, measurement noise
It is small.
2) thickness of thin layer of the thin-layer spectral electrochemical detection means can be easily adjusted by changing membrane thicknesses,
Good thin layer volt-ampere electrochemical characteristic is provided, the influence of solution diffusion is eliminated to the full extent, electrochemical reaction is quick, complete
Entirely, and need detection sample size it is less.
3) the thin-layer spectral electrochemical detection means window is convenient for changing, and the window of different materials fits detection means
For the spectral measurement under different wave length；Meanwhile, electrode can also be changed according to requirement of experiment, it is adaptable under different condition
Electrochemical reaction, expand the range of application of spectroelectrochemistry detection means.
4) the thin-layer spectral electrochemical detection means ne-leakage, with high-air-tightness, is suitable to air-sensitive and water sensitive material
Material and easy volatile solvent, and the long period electrochemical reaction.
5) allow to carry out hydrodynamic injection by U-shaped sample intake passage, the ionic liquid that can be used viscosity larger carries out spectrum electricity
Chemical measurement.
Brief description of the drawings
Fig. 1 spectroelectrochemistries thin layer transmission reaction unit main view direction explosive view；
Fig. 2 spectroelectrochemistries thin layer transmits reaction unit left view；
Fig. 3 is the structural representation of protective case in Fig. 1；
Fig. 4 is the structural representation of Fig. 1 metal deckings 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 ethanol under 1.738V；A is background spectrogram in figure；B, c, d, e point
Not Wei after applied voltage 0min, 0.5min, 1.0min, 1.5min infrared spectrum change.
Shown in figure：Upper strata metal decking 1, rubber spacer 2, upper strata window 3, protective case 4, electrode connection jack 5, under
Layer metal decking 6, enter sample outlet hole 7, bolt 8, polymer packing ring 9, lower floor's window 10, nut 11, bolt hole 12, working electrode
13rd, thin layer 14, reference electrode 15, auxiliary electrode 16.
Specific embodiment
To more fully understand the present invention, with reference to embodiment, the present invention will be further described, but reality of the invention
Apply mode not limited to this.
As Figure 1-4, this thin-layer spectral electrochemical detection means has the sandwich construction of similar sandwich, including upper strata
Metal decking 1, rubber spacer 2, upper strata window 3, protective case 4, lower metal panel 6, polymer packing ring 9, lower floor's window
10th, working electrode 13, reference electrode 15 and auxiliary electrode 16；Upper strata metal decking 1 and lower metal panel 6 are by between bolt 8
Rubber spacer 2, upper strata window 3, polymer pad are sequentially provided between fixation, upper strata metal decking 1 and lower metal panel 6
Circle 9 and lower floor's window 10.
According to the characteristics of infrared spectrometry and requirement, the material of upper strata window 3 and lower floor's window 10 is used
CaF2, and it is brought into close contact composition thin layer 14 with the polymer packing ring 9 for being provided with hexagon through hole；Polymer packing ring 9 is arranged on upper strata
Between window 3 and lower floor's window 10；Thin layer 14 is folded between upper strata window 3 and lower floor's window 10, forms similar
The sandwich construction of sandwich；Working electrode 13, reference electrode 15 and auxiliary electrode 16 are set in thin layer 14, the electrification of three electrodes is constituted
Learn reaction tank；Wherein, metallic mesh working electrode 13 is located between auxiliary electrode 16 and reference electrode 15, and is placed in light Lu Zhizheng
Position, is easy to collect the spectrum change information produced in electrode surface by electrochemical reaction.
The periphery of lower floor's window 10 is provided with protective case 4；Protective case 4 is cuboid, and the logical of small cuboid has been dug in centre
Hole, through hole can just place lower floor's window 10 and polymer packing ring 9.There are three electrode jacks the one end of protective case 4, and protective case is
Plastic material, primarily serves fixed effect.Electrode connection jack 5 is arranged on the outside of protective case 4.
All it is provided with into sample outlet hole 7 on upper strata metal decking 1, rubber spacer 2 and upper strata window 3, enters sample outlet hole 7 and thin layer
U-shaped channel design is formed between 14；Enter sample outlet hole 7 and be provided with sample holes and sample outlet hole, two hole positions are in the both sides of thin layer, structure phase
Together, during sample introduction sample from a stomidium vertically down into thin layer 14, unnecessary sample is just extruded vertically upward from the other end, turnover
Sample hole forms U-shaped channel design, for the sample introduction of thin layer 14；Rubber spacer 2 is used for pressure buffer.
Protective case 4 and upper strata metal decking 1 are designed with bolt hole 12, and lower metal panel 6 is closely welded on one with bolt 8
Rise, rubber spacer 2 and upper strata window, lower floor's window are all that, by being fitted close fixation, bolt 8 passes through bolt hole 12 and spiral shell
Female 11 coordinate fastening to install.
Working electrode 13, reference electrode 15 and auxiliary electrode 16 are connected with electrode cable respectively；Electrode cable respectively with set
Three jacks put in electrode connection jack 5 on the protective sleeve are connected, and separately take three wires, one end insertion electrode connection 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, so as to realize that spectrometer is combined with electrochemical workstation.
Thin-layer spectral electrochemical detection means each part of the present invention with sandwich structure is simple and relatively independent,
Only need mutually to fasten layer by layer, then fixed by knob nut seal, you being formed has multi-level sandwich structure, therefore tears open
Unload, it is easy to assembly, it is easy to clean.Reaction detection thin layer is by the polymer packing ring 9 with three electrodes, upper strata window 3 and lower floor
Window 10 seals composition under impressed pressure, and pond body and electrode cell are reacted without particular design, and thickness of thin layer can be by being polymerized
Thing packing ring is adjusted, there is provided electrochemical reaction speed faster；Device sample introduction is direct using U-shaped sample intake passage without liquid storage tank
It is connected with thin layer, the present invention is more suitable for viscosity sample higher and measure；Electrode is integrated with packing ring, reduces external site,
Improve the airtight effect of device.
The above-mentioned thin-layer spectral electrochemical detection means with sandwich structure overcomes prior art to deposit in the following manner
Problem：
(1) working electrode problem.Working electrode is easy to clean, and replacing working electrode need to be only bumped into polymer packing ring
9, and one end is connected with electrode cable, you can realize that electrode is changed.
(2) sample introduction problem.Apparatus of the present invention sample introduction is directly connected using U-shaped sample intake passage without liquid storage tank with thin layer, is made
The present invention is more suitable for viscosity sample measurement higher.General spectroelectrochemistry detection means is made by the mobility of sample
Voluntarily from liquid storage tank inflow detection means, and the ionic liquid larger for viscosity, due to its poor fluidity, sample enters sample
Detection means there is difficulty, and the present invention carries out hydrodynamic injection by U-shaped sample intake passage can overcome this problem completely.Pass through
The mode of syringe pressing, from a stomidium of sample outlet hole 7 is entered vertically into thin layer 14, unnecessary sample just hangs down sample from the other end
Straight extrusion.Meanwhile, the input mode can reduce sample waste, and measurement every time only needs to 0.1-0.2 milliliters of sample.
(3) airtight sex chromosome mosaicism.Reaction detection thin layer is by the polymer packing ring 9 with three electrodes, upper strata window 3 and lower floor
Window 10 seals composition under impressed pressure, and pond body and electrode cell are reacted without particular design, and thickness of thin layer can be by being polymerized
Thing packing ring is adjusted, there is provided electrochemical reaction speed faster；Electrode is integrated with packing ring, reduces external site, improves device
Airtight effect.
(4) construction problem.Each part of apparatus of the present invention is simple and relatively independent, only needs mutually to fasten layer by layer, then lead to
Knob nut seal is crossed to fix, you can formed have multi-level sandwich structure, therefore dismounting, it is easy to assembly, it is easy to clean.
And because electrode position is fixed, therefore realize the quick of detection means without being corrected to electrode position in an assembling process
Reuse.
(5) Problem of Universality.Detection means size of the invention is according to commercial spectrometers sample cell structure design, it is not necessary to
Special sample holder, is directly to be capable of achieving measurement by detection means insertion optical spectrometer sample groove.
Embodiment 1
The embodiment working electrode 13, reference electrode 15, auxiliary electrode 16 are respectively adopted platinum guaze working electrode, platinum guaze auxiliary
Electrode, platinum filament reference electrode, remaining same Fig. 1-4.When using, the acetonitrile solution of 0.1mol/L lithium perchlorates is prepared as electrolysis
Liquid, to 0.9mg ferrocene (about 1mmol/L) is added in 5mL electrolyte, takes 0.2mL solution, using hydrodynamic injection with syringe
Mode injects thin layer 14 from sample holes, covers tightly into sample outlet hole 7, takes three wires by the thin-layer spectral electrification with sandwich structure
(model CHI660E, electrochemical workstation can provide electricity of the molecule on electrode interface with electrochemical workstation to learn detection means
The information such as redox electro transfer information and solution diffusive migration) connection, voltammetric scan is circulated to sample.Experiment
Method choice cyclic voltammetry, experiment parameter sets as follows：Take-off potential -1V, maximum potential 0.95V, sweep speed 5mV/s,
2 sections of hop count of scanning；Such as Fig. 5 for the cyclic voltammogram of ferrocene (after electrode cable is connected well, is opened electrochemical workstation and matched
Software, select cyclic voltammetry, experiment parameter is set, clicks on and determine to start scanning), the interval of its oxidation peak and reduction peak
It is 16mV, illustrates that there is the thin-layer spectral electrochemical detection means of sandwich structure can provide outstanding thin layer volt-ampere for this electrochemical
Feature is learned, the influence of solution diffusion is eliminated to the full extent, it is adaptable to which fast electrochemical reacts.
Embodiment 2
The embodiment working electrode 13, reference electrode 15, auxiliary electrode 16 are respectively adopted platinum guaze working electrode, platinum guaze auxiliary
Electrode, platinum filament reference electrode, remaining same Fig. 1-4.When using, 0.2mL1- butyl -3- methylimidazole fluoroforms are taken with syringe
Sulfonate ([bmim] CF3SO3) ionic liquid, thin layer is injected from sample holes by the way of hydrodynamic injection, cover tightly into sample outlet hole 7,
Thin-layer spectral electrochemical detection means insertion FTIS with sandwich structure is carried out into infrared spectrum
Background channel is scanned, and sample channel scanning is clicked on after background scans, that is, curve a in Fig. 6 is obtained, with [bmim] CF3SO3As the back of the body
The infrared spectrum of scape, the spectrogram is more steady, illustrates the characteristics of detection means has photo measure noise small.And by it is U-shaped enter
Sample passage carries out hydrodynamic injection, when the ionic liquid that viscosity can be overcome larger is applied to transmission spectra electrochemical measurement, due to entering
The problem that sample is difficult and cannot be applied.
To 5mL [bmim] CF3SO3Middle addition 20.8mg4- ethoxybenzenes ethanol (about 25mmol/L), is taken with syringe
0.2mL solution, thin layer is injected by the way of hydrodynamic injection from sample holes, is covered tightly into sample outlet hole 7, and taking three wires will be with three
The thin-layer spectral electrochemical detection means of Mingzhi's structure is connected with electrochemical workstation, by the thin-layer spectral with sandwich structure
Electrochemical detection device is placed in FTIS sample cell.Fig. 6 is shown under applying 1.738V voltages, 4- second
The change of the infrared spectrum of epoxide benzyl carbinol, and with [bmim] CF3SO3Infrared spectrum as background spectrogram.Wherein b, c, d, e
The change of infrared spectrum respectively after applied voltage 0min, 0.5min, 1.0min, 1.5min.Become every 0.5min spectral signals
Change substantially, illustrate thin layer without diffusion, reflect that electrochemical reaction is quick；Spectral signal no longer changes after 1.5min, illustrates electrification
Learn reaction complete.Through electrochemical oxidation reactions, 1723cm-1、1691cm-1There is new infrared absorption peak in place, it was demonstrated that 4- ethyoxyls
Major oxidation product of the benzyl carbinol under the voltage of 1.738V is 4- acetophenones, and this process also makes benzene ring structure simultaneously
Change is there occurs, its 1614cm-1Place's characteristic peak shifts to lower wave number to 1602cm-1.Result of study shows：There should be sandwich knot
The thin-layer spectral electrochemical detection means of structure makes electrochemical reaction smooth in spectroelectrochemistry detection means by voltage control
Carry out, while preferable In situ spectroscopic information can be provided, data supporting is provided for analytical reactions intermediate, be particularly suitable for
In the research of reaction mechanism.
Embodiments of the present invention are simultaneously not restricted to the described embodiments, other any real without departing from spirit of the invention
Matter and the change, modification, replacement made under principle, combine, simplify, should be equivalent substitute mode, being included in the present invention
Protection domain within.
Claims (7)
1. a kind of thin-layer spectral electrochemical detection means with sandwich structure, it is characterised in that including upper strata metal decking,
Rubber spacer, upper strata window, protective case, lower metal panel, polymer packing ring, lower floor's window, working electrode, reference electricity
Pole and auxiliary electrode；Upper strata metal decking and lower metal panel are fixed by bolt spacings, and upper strata metal decking and lower floor are golden
Rubber spacer, upper strata window, polymer packing ring and lower floor's window are sequentially provided between category panel；
Upper strata window, lower floor's window are brought into close contact composition thin layer with the polymer packing ring for being provided with through hole；Polymer packing ring sets
Put between upper strata window and lower floor's window；Form the sandwich construction of similar sandwich；Working electrode, reference are set in thin layer
Electrode and auxiliary electrode, constitute the electrochemical reaction cell of three electrodes；
Lower floor's window periphery is provided with protective case；Through hole is provided with the middle of protective case, through hole can just place lower floor's window and gather
Compound packing ring；Electrode connection jack is arranged on protective case outside；
All it is provided with into sample outlet hole on upper strata metal decking, rubber spacer and upper strata window, enters and U is formed between sample outlet hole and thin layer
Type channel design；Enter sample outlet hole and be provided with sample holes and sample outlet hole, in the both sides of thin layer, structure is identical, enters sample outlet hole for two hole positions
Form U-shaped channel design；
Protective case and upper strata metal decking are designed with bolt hole, lower metal panel together with bolt welding, the He of rubber spacer 2
Window is all that, by being fitted close fixation, bolt passing through bolt hole is fastened with nut screw connection and installed；
Working electrode, reference electrode and auxiliary electrode are connected with electrode cable respectively；Electrode cable respectively be arranged on protective case
On electrode connection jack in three jacks be connected, separately take three wires, three in one end insertion electrode connection jack 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 means with sandwich structure according to claim 1, it is characterised in that institute
The material for stating upper strata window and lower floor's window uses CaF2。
3. the thin-layer spectral electrochemical detection means with sandwich structure according to claim 1, it is characterised in that institute
The through hole for stating polymer packing ring is hexagon.
4. the thin-layer spectral electrochemical detection means with sandwich structure according to claim 1, it is characterised in that institute
Working electrode is stated for metallic mesh structure, between auxiliary electrode and reference electrode.
5. the thin-layer spectral electrochemical detection means with sandwich structure according to claim 1 or 4, its feature exists
In the working electrode is placed in light path center.
6. the thin-layer spectral electrochemical detection means with sandwich structure according to claim 1, it is characterised in that institute
Protective case is stated for rectangular structure, a rectangular through hole has been dug in centre.
7. the thin-layer spectral electrochemical detection means with sandwich structure according to claim 1, it is characterised in that institute
Protective case is stated for plastic material.
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| 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 |
| CN109001271A (en) * | 2018-06-08 | 2018-12-14 | 中国科学技术大学 | A kind of thin liquid layer electrochemical reaction cell suitable for In-situ Infrared detection |
| CN111855767A (en) * | 2020-07-01 | 2020-10-30 | 安徽中医药大学 | Multifunctional flowing thin-layer electrochemical cell and application thereof |
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| CN102654477A (en) * | 2012-04-23 | 2012-09-05 | 华东理工大学 | Dark-field nano spectral electrochemical detection pool for plasma observation |
| CN103175876A (en) * | 2011-12-22 | 2013-06-26 | 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 |
| US8585880B2 (en) * | 2011-09-27 | 2013-11-19 | Battelle Memorial Institute | Method and apparatus for simultaneous spectroelectrochemical analysis |
| CN105403553A (en) * | 2015-12-31 | 2016-03-16 | 中国科学技术大学 | Thin-layer flow electrolytic cell applicable to electrochemical in-situ Raman spectrum detection |
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| US8585880B2 (en) * | 2011-09-27 | 2013-11-19 | Battelle Memorial Institute | Method and apparatus for simultaneous spectroelectrochemical analysis |
| CN103175876A (en) * | 2011-12-22 | 2013-06-26 | 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 |
| CN102654477A (en) * | 2012-04-23 | 2012-09-05 | 华东理工大学 | Dark-field nano spectral electrochemical detection pool for plasma observation |
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| 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 |
| CN109001271A (en) * | 2018-06-08 | 2018-12-14 | 中国科学技术大学 | A kind of thin liquid layer electrochemical reaction cell suitable for In-situ Infrared detection |
| 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 |
| CN111855767A (en) * | 2020-07-01 | 2020-10-30 | 安徽中医药大学 | Multifunctional flowing thin-layer electrochemical cell and application thereof |
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