CN201514393U - Thin layer long optical path light spectrum electrochemical cell with capillary tube interface - Google Patents
Thin layer long optical path light spectrum electrochemical cell with capillary tube interface Download PDFInfo
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- CN201514393U CN201514393U CN2009201875556U CN200920187555U CN201514393U CN 201514393 U CN201514393 U CN 201514393U CN 2009201875556 U CN2009201875556 U CN 2009201875556U CN 200920187555 U CN200920187555 U CN 200920187555U CN 201514393 U CN201514393 U CN 201514393U
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Abstract
The utility model relates to a thin layer long optical path light spectrum electrochemical cell with a capillary tube interface. A cell body of the electrochemical cell is a quartz luminous pool of 1cm and is internally assembled with a fixed clapboard with a capillary tube connecting channel, as well as a three-electrode system formed by a working electrode plate, an auxiliary electrode and a reference electrode. The thin layer long optical path light spectrum electrochemical cell realizes the connection between a thin layer cavity of the electrochemical cell and a capillary electrophoresis apparatus for a first time, the volume of the thin layer cavity is not more than 50 microliters, reactant can be rapidly electrolyzed in a way of exhaustion, and the reaction products can be quickly separated and detected in an on-line way by the capillary electrophoresis apparatus. The electrochemical cell has another characteristic that the light spectrum electrochemical cell can be used for not only separating and detecting the electrode products in an on-line way, but also in situ light spectrum electrochemical testing. The device is simple in structure and easy to control in operation, the electrodes are conveniently assembled, disassembled and replaced, and the working electrode material can be selected. The electrochemical cell can be used for separation and detection of the complicated electrode reaction products as well as reaction kinetics study in the field of electrochemistry and related fields.
Description
Technical field
The utility model belongs to analytical chemistry and electrochemical field, is specifically related to spectrum electrochemical pool.
Background technology
The spectroelectrochemistry method combines galvanochemistry with spectroscopy, in the record electrochemical signals, electrode surface or near it liquid layer place in-situ acquisition can reflect and the spectral information of each species and number change effectively promoted the dynamic (dynamical) research of electrochemical reaction.The enforcement of this method must be adopted special thin-layer spectral electrochemical pond, and the microelectrolysis liquid in the thin layer chamber can be consumed apace by electrode reaction, thereby but finishes the collection of data within a short period of time.
Because the complicated electrode reaction produces multiple product and intermediate usually, except the original position spectral information, it also is that Reactive Mechanism of Electrode and dynamics research are needed that each species in the reaction system are carried out separation detection.The method that electrolysate is separated mainly contains high performance liquid chromatography (HPLC) (Electrochim Acta both at home and abroad; Bandeira M C E, Maia G; 2008,53 (13): 4512-4519), gas chromatography (Talanta; Turch á n M, Jara-Ulloa P, Bollo S, et al.; 2007,73 (5): 913-919) and thin-layer chromatography (Electrochim Acta; Iwakura C, M.Tsunaga, Tamura H; 1972,17 (8): 1391-1400) etc.The electrolytic solution volume is generally got 10～100mL, even adopted broad-area electrode, whole electrolysis time also reaches a few hours even more than tens hours, the association problem that is difficult to overcome below also existing simultaneously:
(1) organic or biomolecule can be adsorbed on electrode surface usually, and when the electrolysis duration is longer, the reaction product that accumulates on the electrode surface will seriously hinder the carrying out of reaction, cause required time longer.For eliminating this obstacle, some researchers take out (J Braz Chem Soc with electrode at regular intervals; Timbola AK, Souza C D, Giacomelli C, etal.; 2006,17 (1): 139-148.), the ultrasonic activation electrode surface had both brought the inconvenience of operation, again because of electrolysis interrupt repeatedly make the data lose the value of dynamic analysis.
(2) long-time electrolysis causes the forfeiture of reactive intermediate information.Intermediate is very common in organic reaction, if adopt the thin layer electrochemical cell and the broad-area electrode of micro updating, the electrolysis process is accelerated greatly, just can detect the higher intermediate of reactivity.
(3) long-time electrolysis also will make course of reaction be subjected to the interference of environmental factor more, as oxygen dissolve in, temperature fluctuation, trace impurity, table vibration etc.If the electrolysis process can finish in several minutes even tens seconds, be subjected to annoyance level very little, data will can be used for dynamic analysis.
Therefore, exhaust electrolysis time long be a bottleneck of restriction complicated electrode reaction product separation detection and reaction kinetics research.The paper of delivering from Electrochimica Acta amounts to from year March in January, 2000 to 2009 and to adopt chromatographic process that electrode product has been carried out about 63 pieces of the paper of separation detection in more than the 6000 piece of paper, only accounts for less than 1%.As seen, to detect be organic and the pressing for of bioelectrochemistry research to the ON-LINE SEPARATION of the quick conversion of realization response thing and product.Early stage Ceng Youyong mercury thin layer electrode (Anal Chem both at home and abroad; Hanley J L, Peters D G; 1976,48 (13): 2036-2038) or sampling valve electrochemical cell (analytical chemistry; Lin Xiangqin, Yan Chuanwei, Xu Zhengyan; 1996,24 (5): 613-618.) the preparation electrolysate is for online gas chromatography separation detection.There is the online galvanochemistry of report/HPLC to separate work (the J Am SocMass Spectr of electrolysate in recent years; Lohmann W,
R, G ü tter G, et al.; 2009,20 (1): 138-145), obtaining better effects aspect the separation of electrolysate and the qualitative evaluation, but coupling arrangement is still complicated, the electrolysis of exhaustion property is still quick inadequately.
The utility model content
The purpose of this utility model is the needs at complicated electrochemical reaction research, design a kind of thin-layer long optical distance spectrum electrochemical pool, make it to possess the test of original position spectroelectrochemistry and produce the dual-use function that the microelectrolysis sample detects for capillary electrophoresis separation with capillary interface.
It is the quick conversion that A/V comes the realization response thing than very big thin layer electrochemical cell that the utility model adopts the ratio of electrolytic solution volume " electrode area with ".The thin layer pond only produces the sample size of μ L level, considers the singularity of taking a sample from the thin layer chamber, needs to select a kind of adaptive with it method for separating and detecting.The sampling volume of HPLC method commonly used generally all surpasses thin layer chamber volume generally at 5-500 μ L; Even get its lower limit, also be difficult to accomplish in drawing the thin layer chamber, do not suck auxiliary electrode chamber solution in the considerable part solution, and to realize sample from the thin layer chamber to the online transfer of HPLC difficulty more just, thereby be not suitable for as with the separation means of thin layer pond coupling.The sample size of Capillary Electrophoresis only needs the nL level, and as carrier of separating, kapillary is easy to link to each other with the thin layer chamber by the microchannel, thereby realizes online sample introduction, separation and detection with the elastic quartz capillary tube of superfine internal diameter.Therefore, selecting the preceding thin layer electrochemical cell coupling of Capillary Electrophoresis and post is a kind of quite reasonable coupling.
Concrete structural design scheme is as follows:
A kind of thin-layer long optical distance spectrum electrochemical pool with capillary interface comprises quartzy luminosity pond 1, is provided with stationary barrier 2 and working electrode plate 8 side by side in the described quartzy luminosity pond 1;
A side adjacent with quartzy luminosity pond 1 pool wall is provided with the groove that connects its top on the stationary barrier 2, and described groove is auxiliary electrode chamber 6, is inserted with auxiliary electrode 7 in the auxiliary electrode chamber 6; The bottom of stationary barrier 2 and working electrode plate 8 adjacent sides is provided with the thin layer chamber 3 of indent, and described thin layer chamber 3 is the light path slit, evenly is laid with the current channel hole 4 that connects more than two in it; Stationary barrier 2 is provided with the capillary channel 5 that is communicated with thin layer chamber 3;
A side adjacent with quartzy luminosity pond 1 pool wall is provided with the groove that connects its top on the working electrode plate 8, and described groove is contrast electrode chamber 12, is inserted with contrast electrode 13 in the contrast electrode chamber 12; Be provided with copper-foil conducting electricity 11 in the working electrode plate 8; Working electrode plate 8 sides adjacent with the thin layer chamber 3 of stationary barrier 2 are provided with working electrode groove 9, are filled with electrode material in the working electrode groove 9; A side at working electrode groove 9 places is provided with the reference channel 10 of perforation on the working electrode plate 8, and it is outer as contact conductor that the upper end of described copper-foil conducting electricity 11 extends quartzy luminosity pond 1, and its lower end is positioned at working electrode groove 9 bottoms.
Described quartzy luminosity pond 1 is the quartzy luminosity of 1cm pond.
Described auxiliary electrode material is solid carbon paste or graphite or platinized platinum or other solid electrode material.
Described stationary barrier material is polytetrafluoroethylene (PTFE) or tygon (PE).
Described thin layer chamber 3 degree of depth are 0.05-0.5mm, and length is identical with stationary barrier 2 width, are 5-7mm highly, and its lower edge is apart from stationary barrier 2 bottom 7-9mm; Bottom, thin layer chamber evenly distributes 9 micropores as current channel hole (4).
Described current channel hole (4) diameter is 0.05-0.3mm.
Described capillary channel 5 diameters are 0.05-0.5mm.
Described contrast electrode 13 is to use the silver-silver chloride electrode of the glass capillary of Φ 1mm as sleeve pipe.
Useful technique effect of the present utility model is embodied in the following aspects:
(1) the utility model is simple in structure, is easy to processing and fabricating, the experiment easy operating.
(2) adopt the quartzy luminosity of common 1cm pond that the merchant sells as the pond body, need not to transform spectrophotometric specimen holder.
(3) three electrodes can insert fixing and the taking-up cleaning easily.
(4) adopt the parallel transmission mode of the long light path of 1cm, need not to use light air electrode, optional working electrode material.
(5) auxiliary electrode is parallel relative with working electrode by equally distributed 9 micropores on the stationary barrier, makes the distribution of current on the working electrode even relatively.
(6) thickness of thin layer is regulated and is controlled by the thin layer chamber of processing different depth on stationary barrier, need not the very high screw thread of requirement on machining accuracy, also need not to use thin barrier film.
(7) pull double duty, both can be applicable to the original position UV-Vis spectroelectrochemistry test of electrode reaction, also can be capillary electrophoresis apparatus the microelectrolysis sample is provided fast, be used for ON-LINE SEPARATION and detect electrolysate.
Description of drawings
Fig. 1 is the utility model structural representation.
Fig. 2 is the A-A cut-open view of Fig. 1.
Fig. 3 is the B-B cut-open view of Fig. 1.
Fig. 4 is the C-C cut-open view of Fig. 1.
Fig. 5 is the D-D cut-open view of Fig. 1.
Fig. 6 is the E-E cut-open view of Fig. 1.
The potassium ferricyanide [the K that Fig. 7 records for the utility model
3Fe (CN)
6] the thin layer cyclic voltammetry curve figure of solution.
Fig. 8 inhales curve map for the circulation volt that the utility model records.
The original position UV-Vis spectrogram of the permanent electromotive force oxidizing process of the catechin that Fig. 9 records for the utility model.
The online Capillary Electrophoresis spectrogram of the permanent electromotive force oxidation product of the catechin that Figure 10 records for the utility model.
Embodiment
Below in conjunction with accompanying drawing, the utility model is further described by embodiment.
Referring to Fig. 1, a kind of thin-layer long optical distance spectrum electrochemical pool with capillary interface comprises the quartzy luminosity of 1cm pond 1, be provided with stationary barrier 2 and working electrode plate 8 side by side in the quartzy luminosity pond 1, available (also can) a small amount of fluid sealant is fixed on stationary barrier 2 in the pond, and the stationary barrier material is polytetrafluoroethylene (PTFE) or tygon (PE).
The making of stationary barrier 2, referring to Fig. 1-Fig. 3, get the cube that a bar shaped PTFE plate carefully is polished into 10mm (length) * 5mm (wide) * 55mm (height), wherein long and wide dimensional requirement strictness, become 90 ° of right angles between each face, make its three energy and pond body inner edge driving fit.Be provided with the groove that connects its top with stationary barrier 2 sides of the relative side of quartzy luminosity pond 1 pool wall, described groove is auxiliary electrode chamber 6, its long 8mm * wide 3mm * high 48mm; Be fitted with auxiliary electrode 7 in the auxiliary electrode chamber 6, auxiliary electrode 7 is the gauze platinum electrode of 8mm * 8mm.Stationary barrier 2 bottoms adjacent with working electrode plate 8 are provided with the thin layer chamber 3 of indent, this thin layer chamber 3 is the light path slit, the thin layer chamber degree of depth is a 0.2mm (that is thin layer chamber thickness, depth range is 0.05-0.5mm,), length and the identical (10mm of stationary barrier 2 width, that is optical path length), highly be 7mm (altitude range is 5-7mm), its lower edge is apart from stationary barrier 2 bottom 9mm (scope is 7-9mm), be laid with nine in it and connect micropore as current channel hole 4, the current channel bore dia is 0.2mm (diameter range is 0.05-0.3mm); The capillary channel 5 that is communicated with thin layer chamber 3 is housed on the stationary barrier 2, and capillary channel 5 diameters are 0.3mm (diameter range is 0.05-0.5mm).
Referring to Fig. 4-Fig. 6, be provided with the groove that connects its top with working electrode plate 8 sides of the relative side of quartzy luminosity pond 1 pool wall, described groove is contrast electrode chamber 12, the contrast electrode chamber size is identical with the auxiliary electrode chamber size.Be inserted with contrast electrode 13 in the contrast electrode chamber 12, contrast electrode 13 is to use the silver-silver chloride electrode (Ag/AgCl/KCl of the glass capillary of Φ 1mm as sleeve pipe
Sat).Be provided with copper-foil conducting electricity 11 in the working electrode plate 8; Working electrode plate 8 sides adjacent with the thin layer chamber 3 of stationary barrier 2 are provided with working electrode groove 9, the long 8mm of working electrode groove 9 * high 7mm * dark 1mm, its both sides respectively keep the 1mm edge with insulation, be filled with electrode material pyrolytic graphite sheet in the working electrode groove 9, its back side keeps well contacting with Copper Foil 11 with conducting resinl, and its front is through polishing and the equal working electrode surface that is of working electrode plate 8 plate faces; Working electrode plate 8 one sides at working electrode groove 9 places are provided with the reference channel 10 of perforation, and it is outer as contact conductor that the upper end of copper-foil conducting electricity 11 extends quartzy luminosity pond 1, and its lower end is positioned at working electrode groove 9 bottoms.
Referring to Fig. 7, show that electrochemical cell thin layer of the present utility model is functional.
Referring to Fig. 8, show that electrochemical cell of the present utility model can be used for the test of circulation volt suction method.
The thin layer character of the thin-layer long optical distance spectrum electrochemical pool of the band capillary interface that embodiment 1 is made is carried out cyclic voltammetric and is characterized, and original position measures the thin layer cyclic voltammetry curve simultaneously and the circulation volt is inhaled curve.Surveying instrument is UV-Vis 2550 type UV-Vis spectrophotometers (Tianjin, island company), CHI660B electrochemical workstation (Shanghai occasion China instrument company).Electrolytic solution is 1.0mmol L
-1K
3Fe (CN)
6+ 1mol L
-1KCl, potential scan speed 1mV s
-1, absorbance (A) detects wavelength 420nm, scanning 5 circles.Measured thin layer cyclic voltammetry curve and corresponding circulation volt are inhaled curve and are seen accompanying drawing 7 and 8.Fig. 7 shows that good thin layer exhausts the property electrolytic characteristic, and the ratio of negative electrode and anodic peak current is near 1, peak-to-peak electric potential difference 36mV (＜59mV), the cathodic reduction after-current approaches the background baseline, shows that edge effect is less; Fig. 8 of synchronous recording also shows good thin layer feature, and when electromotive force during near 0.0V, the level of absorbance line of below shows that electroactive component all has been converted into it basically and has gone back ortho states K
4Fe (CN)
6, and when electromotive force during near 0.5V, the horizontal line of top is corresponding to its oxidation state K
3Fe (CN)
6
Referring to Fig. 9, show that electrochemical cell of the present utility model can be used for original position UV-Vis spectrum test.
The thin-layer long optical distance spectrum electrochemical pool of the band capillary interface that embodiment 1 is made is applied to the UV-Vis spectrum of the permanent electromotive force oxidizing process of in site measurement catechin.Spectral instrument and electro-chemical systems are with embodiment 2.Catechin concentration 0.1mmol L
-1(pH 11.5), oxidation potential 0.15V writes down UV-Vis spectrum in the course of reaction repeatedly in the 600nm-200nm wavelength coverage, continues to spectral line and changes basicly stable (also writing down a spectral line before the electrolysis), and gained UV-Vis spectrum is seen accompanying drawing 9.
Referring to Figure 10, show that electrochemical cell of the present utility model can be used for the online capillary electrophoresis separation detection of electrolysate.
The thin-layer long optical distance spectrum electrochemical pool of the band capillary interface that embodiment 1 is made is used for permanent electromotive force oxidation catechin, and preparation microelectrolysis sample carries out ON-LINE SEPARATION for capillary electrophoresis apparatus and detects.CL1020 efficient capillary electrophoresis apparatus (color land, Beijing scientific instrument company limited) is adopted in the electrophoresis test, joins UV-detector, fused quartz capillary inner diameter 50 μ m (Hebei light transmitting fiber Yongnian factory).Electro-chemical systems is with embodiment 2.Catechin concentration 1mmol L
-1(pH 11.5), runtime buffer solution 20mmol L
-1Na
2B
4O
7(pH 9.0)+10mmol L
-1KH
2PO
4, working voltage 20kV, discrepancy in elevation sample introduction detects wavelength 200nm, and gained Capillary Electrophoresis spectrogram is seen accompanying drawing 10 (an electrophoresis peak that has only catechin on the Capillary Electrophoresis spectrum before the electrolysis).
Claims (8)
1. thin-layer long optical distance spectrum electrochemical pool with capillary interface is characterized in that:
Comprise quartzy luminosity pond (1), be provided with stationary barrier (2) and working electrode plate (8) in the described quartzy luminosity pond (1) side by side;
Stationary barrier (2) is gone up a side adjacent with quartzy luminosity pond (1) pool wall and is provided with the groove that connects its top, and described groove is auxiliary electrode chamber (6), is inserted with auxiliary electrode (7) in auxiliary electrode chamber (6); The bottom of stationary barrier (2) and the adjacent side of working electrode plate (8) is provided with the thin layer chamber (3) of indent, and described thin layer chamber (3) is the light path slit, evenly is laid with the current channel hole (4) that connects more than two in it; Stationary barrier (2) is provided with the capillary channel (5) that is communicated with thin layer chamber (3);
Working electrode plate (8) is gone up a side adjacent with quartzy luminosity pond (1) pool wall and is provided with the groove that connects its top, and described groove is contrast electrode chamber (12), is inserted with contrast electrode (13) in contrast electrode chamber (12); Be provided with copper-foil conducting electricity (11) in the working electrode plate (8); Working electrode plate (8) side adjacent with the thin layer chamber (3) of stationary barrier (2) is provided with working electrode groove (9), and the working electrode groove is filled with electrode material in (9); The side that the last working electrode groove (9) of working electrode plate (8) is located is provided with the reference channel (10) of perforation, and it is outer as contact conductor that the upper end of described copper-foil conducting electricity (11) extends quartzy luminosity pond (1), and its lower end is positioned at working electrode groove (9) bottom.
2. a kind of thin-layer long optical distance spectrum electrochemical pool with capillary interface according to claim 1 is characterized in that: described quartzy luminosity pond (1) is the quartzy luminosity of 1cm pond.
3. a kind of thin-layer long optical distance spectrum electrochemical pool with capillary interface according to claim 1 is characterized in that: described auxiliary electrode material is solid carbon paste or graphite or platinized platinum or other solid electrode material.
4. a kind of thin-layer long optical distance spectrum electrochemical pool with capillary interface according to claim 1 is characterized in that: described stationary barrier material is teflon or tygon.
5. a kind of thin-layer long optical distance spectrum electrochemical pool according to claim 1 with capillary interface, it is characterized in that: described thin layer chamber (3) degree of depth is 0.05-0.5mm, length is identical with stationary barrier (2) width, highly is 5-7mm, and its lower edge is apart from stationary barrier (2) bottom 7-9mm; Bottom, thin layer chamber evenly distributes 9 micropores as current channel hole (4).
6. a kind of thin-layer long optical distance spectrum electrochemical pool with capillary interface according to claim 5 is characterized in that: described current channel hole (4) diameter is 0.05-0.3mm.
7. a kind of thin-layer long optical distance spectrum electrochemical pool with capillary interface according to claim 5 is characterized in that: described capillary channel (5) diameter is 0.05-0.5mm.
8. a kind of thin-layer long optical distance spectrum electrochemical pool with capillary interface according to claim 5 is characterized in that: described contrast electrode (13) is to use the silver-silver chloride electrode of the glass capillary of Φ 1mm as sleeve pipe.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507708A (en) * | 2011-10-21 | 2012-06-20 | 合肥工业大学 | Chip-type thin-layer electrolytic cell capillary electrophoresis microfluidic online sample feeding device |
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2009
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507708A (en) * | 2011-10-21 | 2012-06-20 | 合肥工业大学 | Chip-type thin-layer electrolytic cell capillary electrophoresis microfluidic online sample feeding device |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100623 Termination date: 20100916 |