CN106885801A - A kind of method for monitoring electrochemical luminescence intensity and wavelength - Google Patents

A kind of method for monitoring electrochemical luminescence intensity and wavelength Download PDF

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CN106885801A
CN106885801A CN201710115635.XA CN201710115635A CN106885801A CN 106885801 A CN106885801 A CN 106885801A CN 201710115635 A CN201710115635 A CN 201710115635A CN 106885801 A CN106885801 A CN 106885801A
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electrode
electrochemical
wavelength
electrochemical luminescence
working electrode
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张袁健
吕燕芹
周志新
沈艳飞
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Southeast University
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    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/76Chemiluminescence; Bioluminescence
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    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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Abstract

The invention provides a kind of method for monitoring electrochemical luminescence intensity and wavelength, it is connected in electrochemical reaction cell and respectively with electrochemical measurement system by working electrode, to electrode and reference electrode assembling, the working face of working electrode is directed at the detector of spectroanalysis instrument;Spectroanalysis instrument is Raman spectrometer, ultraviolet-uisible spectrophotometer or sepectrophotofluorometer;To adding electrolyte solution in electrochemical reaction cell;Electrochemical luminescence material to be measured is modified on the working electrode (s or is added in electrolyte solution liquid;By electrochemical workstation to working electrode applied voltage, electrochemical luminescence material to be measured is electrically excited, electrochemical luminescence intensity and wavelength are gathered using spectroanalysis instrument.The present invention can be by the intensity of easy Instrument crosslinking method real-time monitoring electrochemical luminescence and wavelength, with detection sensitivity and wavelength resolution higher, the analysis detectability of electrochemical luminescence is greatly improved, has the advantages that quick, simple, accurate and sensitivity is high.

Description

A kind of method for monitoring electrochemical luminescence intensity and wavelength
Technical field
The present invention relates to Electrochemiluminescence technology, and in particular to a kind of side for monitoring electrochemical luminescence intensity and wavelength Method.
Background technology
Electrochemical luminescence (ECL) technology has device simple, favorable reproducibility, can to carry out luminous, sensitivity in situ high etc. excellent Point, reaches its maturity with to ECL study on mechanism, and its application on analytical chemistry is just being increasingly subject to the attention of people. Although current Electrochemial luminescence detecting instrument can detect the luminescent behavior of the material of electrochemical luminescence better performances, right In the weaker material of electrochemical luminescence signals, the sensitivity of Electrochemial luminescence detecting instrument needs further to improve.Additionally, existing Some electrochemical luminescence instrument wavelength resolution abilities are relatively low, it is difficult to which the electrochemical luminescence wavelength to sample carries out real-time monitoring, this limit The research to electrochemical luminescence materials optical behavior is made.
Existing Raman spectrometer collection equipment uses fibre-optical probe, and its effect is collection of scattered light, by light Signal sends into beam splitting system, and optical signal is separately introduced detector by beam splitting system according to different wavelength, under detector recording not Photon intensity representated by co-wavelength spectral line.The detector that it is used is silicon substrate CCD-detector, is multi-channel photon detector, With the development of silicon substrate CCD-detector, CCD-detector instead of the single channel detector (pole of collapse light two of photomultiplier Pipe), it can be detected simultaneously by 400 to the spectral line between 1100nm, in full spectral region can fast continuous scan, without connecing spectrum, Analysis time (analysis time is generally less than 30 seconds) is dramatically saves on, spectral resolution is higher than 0.2nm.UV, visible light light splitting light Degree meter technology is very ripe, can arbitrarily detect the light of different wave length in ultraviolet light, visible ray and near-infrared region, its detection model Enclose wider, wavelength accuracy is good (0.3nm), and repeatable accuracy is (≤0.1nm) high, and spectral resolution reaches 0.1nm.Analysis field with And there is absolute flexibility in the design of portable equipment.Photodiode reference detector that sepectrophotofluorometer is utilized and Selected R928P photomultipliers, photon-counting detector is swashed in detector (photomultiplier) by differentiating single photon The photoelectronic pulse for issuing, is extracted optical signal in digitized mode from thermal noise, and this system has good Long-time stability and detectivity very high, spectral resolution 1nm is the powerful for detecting atomic dim light.
Therefore, the present invention has the advantage of detection sensitivity and wavelength resolution higher using these spectroanalysis instruments, By simple Instrument crosslinking, the signal response of the material weaker to electrochemical luminescence signals is not only drastically increased, and Realize the real-time monitoring to sample electrochemical luminescence wavelength.
The content of the invention
Goal of the invention:It is an object of the present invention to provide a kind of method for monitoring electrochemical luminescence intensity and wavelength, the method exists With sensitivity higher during the detection weaker material of electrochemical luminescence signals, and the electrochemical luminescence wavelength of sample can be carried out Real-time monitoring.
Technical scheme:One aspect of the present invention provides a kind of method for monitoring electrochemical luminescence intensity and wavelength, bag Include following steps:
1) by working electrode, to electrode and reference electrode assembling in electrochemical reaction cell and respectively with electrochemical workstation It is connected, the working face of working electrode is directed at the detector of high-resolution spectra analyzer;High-resolution spectra analyzer is Raman spectrum Instrument, ultraviolet-uisible spectrophotometer or sepectrophotofluorometer;
2) to electrolyte solution is added in electrochemical reaction cell, make working electrode, electrode and reference electrode are immersed respectively In the electrolyte solution;Contain coreagent and electrochemical luminescence material to be measured in electrolyte solution;
3) electrochemical luminescence material to be measured is electrically excited to working electrode applied voltage by electrochemical workstation, Electrochemical luminescence intensity and wavelength are gathered using high-resolution spectra analyzer.
The method that another aspect of the present invention provides another monitoring electrochemical luminescence intensity and wavelength, including with Lower step:
1) electrochemical luminescence material to be measured is modified in working electrode surface, obtains the working electrode modified;To modify Working electrode, electrode and reference electrode be assemblied in electrochemical reaction cell and respectively with electrochemical workstation be connected, will repair The working face containing electrochemical luminescence material to be measured is directed at the detector of high-resolution spectra analyzer in the working electrode adornd;It is high Resolved spectroscopy analyzer is Raman spectrometer, ultraviolet-uisible spectrophotometer or sepectrophotofluorometer;
2) to electrolyte solution is added in electrochemical reaction cell, make working electrode, electrode and reference electrode are immersed respectively In the electrolyte solution;Contain coreagent in electrolyte solution;
3) electrochemical luminescence material to be measured is electrically excited to working electrode applied voltage by electrochemical workstation, Electrochemical luminescence intensity and wavelength are gathered using high-resolution spectra analyzer.
Step 1) in, working electrode can use any one inert electrode, it is preferable that working electrode be glass-carbon electrode, Gold electrode, platinum electrode or graphite electrode;Can be using common to electrode to electrode, it is preferable that be to electrode platinum electrode or Carbon electrode;Reference electrode can use common reference electrode, it is preferable that reference electrode is that silver/silver chloride electrode or saturation are sweet Mercury electrode.
Step 2) in, coreagent be oxalic acid, hydrogen peroxide, oxygen, triethylamine, potassium peroxydisulfate and sodium peroxydisulfate in one kind or It is various;Supporting electrolyte in electrolyte solution is KCl that concentration is 0.001~1M, the NaCl that concentration is 0.001~1M, dense Spend is 0.001~1M PBSs or Tris-HCl cushioning liquid.
Step 3) in, constant potential is applied by electrochemical workstation or voltammetric scan is carried out, electrochemical luminescence material is entered Row is electrically excited.
The above method can be used to monitor the wavelength and intensity of single electrochemical luminescence material, it can also be used to while two kinds of monitoring Or the wavelength and intensity of two or more electrochemical luminescence materials.
Operation principle of the invention is:By electrochemical luminescence material in the case of electrically excited with electrolyte solution in Coreagent is had an effect, and sends fluorescence, and it is monitored by with the spectroanalysis instrument compared with high detection sensitivity and wavelength resolution Signal intensity and wavelength.
Beneficial effect:The present invention divides Electrochemiluminescence technology and Raman spectrometer, ultraviolet-uisible spectrophotometer, fluorescence The spectral analysis techniques such as light photometer are combined, and connection is simple between instrument, can be by easy method real-time monitoring electrification Luminous intensity and wavelength is learned, with detection sensitivity and wavelength resolution higher, electrochemical luminescence is greatly improved Analysis detectability;For the material all under same potential with electrochemical luminescence performance, detected with conventional electrochemical luminescence Instrument is difficult to distinguish its launch wavelength, and the electrochemical luminescence wavelength of different electrochemical substances can be distinguished by the method for the present invention, This is beneficial to expand the detection application of electrochemical luminescence material.Meanwhile, the present invention has expanded the application of different spectroanalysis instruments Field, electrochemical luminescence field is applied to by Raman spectrometer, ultraviolet-uisible spectrophotometer and sepectrophotofluorometer, this The method of Instrument crosslinking has widened thinking to solve Similar Problems.The present invention can not only realize technical breakthrough, Er Qieneng The development of Electrochemiluminescence technology is greatly facilitated, promotes the research to electrochemical substance luminescent behavior.
Brief description of the drawings
Fig. 1 is the ruthenium bipyridyl electrochemical luminescence spectrogram that embodiment 1 is measured;
Fig. 2 is the ruthenium bipyridyl electrochemical luminescence spectrogram that embodiment 2 is measured;
Fig. 3 is the Particles in Electrochemiluminescofce ofce Luminol spectrogram that embodiment 3 is measured;
Fig. 4 is the Particles in Electrochemiluminescofce ofce Luminol spectrogram that embodiment 4 is measured;
Fig. 5 is that comparative example 1 takes the spectrogram that a detection ruthenium bipyridyl electrochemical luminescence intensity is drawn;
Fig. 6 is that comparative example 2 takes the spectrogram that a detection Particles in Electrochemiluminescofce ofce Luminol intensity is drawn;
Fig. 7 is the electrochemical luminescence spectrum schematic diagram of the CNNS that embodiment 5 is measured and S-CNNS;
Fig. 8 is the ruthenium bipyridyl electrochemical luminescence spectrogram that embodiment 6 is measured;
Fig. 9 is the ruthenium bipyridyl electrochemical luminescence spectrogram that embodiment 7 is measured;
Figure 10 is the ruthenium bipyridyl electrochemical luminescence spectrogram that embodiment 8 is measured;
Figure 11 is electrochemical reaction cell of the present invention and its external sample pool structure schematic diagram.
Specific embodiment
Embodiment 1
Combined apparatus for monitoring electrochemical luminescence intensity and wavelength, including electrochemical reaction cell, electrochemical workstation And Raman spectrometer;Electrochemical reaction cell is three-electrode system, and wherein working electrode is commercialization L-type glass-carbon electrode, to electricity Extremely platinum electrode, reference electrode is Ag/AgCl electrodes, and three electrodes are connected with electrochemical workstation respectively, working electrode Working face is directed at the detector of Raman spectrometer.The installation step of device is as follows:First, Raman spectrometer is covered with shadow shield to swash Light emitting source.Then, electrode, reference electrode and polished, carrying out washing treatment working electrode will be assembled in electrochemical reaction cell, The working face of working electrode is directed at the detector of Raman spectrometer.By three electrodes electrode wires corresponding with electrochemical workstation respectively Connection, obtains final product combined apparatus.
In the combined apparatus, there is no particular/special requirement to the structure of electrochemical reaction cell, as long as making the working face of working electrode Alignment detector.As an example of electrochemical reaction cell of the present invention, as shown in figure 11, the outside of electrochemical reaction cell Include wriggling pump discharge 5 successively from top to bottom, electrode interface 3, working electrode interface 1, reference electrode interface 2 and peristaltic pump are connect Mouth 4;Sample room is provided with outside electrochemical reaction cell, sample room is be made up of preposition baffle plate 6, base 7 and backboard 9 Hemi-closure space, sets notch 8 on base 7, electrochemical reaction cell is placed on the notch 8 in sample room, and preposition baffle plate 6 is taken up an official post Meaning sets 5 interfaces and is respectively:Working electrode connection jaws 10, reference electrode connection jaws 11, to electrode connection mouthfuls 12, peristaltic pump tube Import 13, peristaltic pump tube outlet 14.Electrochemical reaction cell is made up of quartz material.The length of electrochemical reaction cell is 4cm, a width of 4cm, a height of 4cm.Backboard is highly 10cm, and a width of 12cm, thickness is 1cm.Base a length of 14cm, a width of 12cm, thickness It is 0.7cm.Sample room is opaque iron and steel material quality and is made.
The method that electrochemical luminescence intensity and wavelength are monitored using said apparatus, is comprised the following steps:
1) to addition 0.05M pH in electrochemical reaction cell 9.0 PBS (KCl, 0.15M containing 0.05M Ru(bpy)3 2+With 100mM oxalic acid);
2) constant potential (+1.3V), under the current potential, the ruthenium bipyridyl dead electricity of electrode surface are applied by electrochemical workstation Son, and reacted with the coreagent (oxalic acid) in electrolyte solution, finally cause ruthenium bipyridyl to send fluorescence, by Raman Spectrometer collection launches collection of illustrative plates, and the ruthenium bipyridyl of gained launches collection of illustrative plates as shown in figure 1, can be real-time by the Instrument crosslinking method The electrochemical luminescence wavelength and intensity of ruthenium bipyridyl are monitored, its wavelength resolution reaches 0.2nm.
Embodiment 2
Using device monitoring electrochemical luminescence intensity in the same manner as in Example 1 and wavelength, comprise the following steps:
1) to addition 0.05M pH in electrochemical reaction cell 9.0 PBS (KCl, 0.15M containing 0.05M Ru(bpy)3 2+With 100mM oxalic acid);
2) volt-ampere curve is circulated by electrochemical workstation and scans (0~+1.3v), gathered by Raman spectrometer and sent out Collection of illustrative plates is penetrated, the ruthenium bipyridyl of gained launches collection of illustrative plates as shown in Fig. 2 being capable of real-time monitoring ruthenium bipyridyl by the Instrument crosslinking method Electrochemical luminescence wavelength and intensity, its wavelength resolution reach 0.2nm.
Embodiment 3
Using device monitoring electrochemical luminescence intensity in the same manner as in Example 1 and wavelength, comprise the following steps:
1) luminol is dissolved with 0.1M NaOH, it is 1.0 × 10 to be configured to concentration-2The luminol solution of M;By the luminol Solution and H2O2Solution, KCl are added in PBS, prepared pH be 7.4 electrolyte solution (containing 1.0 × 10-4M Luminol, 10mM H2O2With 0.1M KCl);
2) to adding 10mL steps 1 in electrochemical reaction cell) obtained in electrolyte solution;
3) constant potential (0.5V) is applied by electrochemical workstation.Under the current potential, the luminol betatopic of electrode surface, And with electrolyte solution in coreagent (H2O2) react, finally cause luminol that fluorescence occurs, by Raman spectrometer Collection transmitting collection of illustrative plates, the luminol of gained launches collection of illustrative plates as shown in figure 3, being capable of real-time monitoring Rumi by the Instrument crosslinking method The electrochemical luminescence wavelength and intensity of promise, its wavelength resolution reach 0.2nm.
Embodiment 4
Using device monitoring electrochemical luminescence intensity in the same manner as in Example 1 and wavelength, comprise the following steps:
1) luminol is dissolved with 0.1M NaOH, it is 1.0 × 10 to be configured to concentration-2The luminol solution of M;By the luminol Solution and H2O2Solution, KCl are added in PBS, are obtained the electrolyte solution that pH is 7.4 and (are contained 1.0 × 10-4M Luminol, 10mM H2O2With 0.1M KCl);
2) to adding 10mL steps 1 in electrochemical reaction cell) obtained in electrolyte solution;
3) volt-ampere curve is circulated by electrochemical workstation and scans (0~+0.5V), gained luminol transmitting collection of illustrative plates is such as Shown in Fig. 4, electrochemical luminescence wavelength and the change of intensity of real-time monitoring luminol, its ripple are capable of by the Instrument crosslinking method Resolution ratio long reaches 0.2nm.
Comparative example 1
Ruthenium bipyridyl electrochemical luminescence is detected using the method for optical filter based on commercialization Electrochemial luminescence detecting instrument at present Intensity and wavelength, its specific steps are substantially consistent with embodiment 1, and difference is to be circulated by electrochemical workstation Volt-ampere curve scans (0~+1.3V), and detector is current commercialization Electrochemial luminescence detecting instrument.It is narrow that different wave length is placed respectively Band optical filter is mapped after must corresponding to ECL signal intensities, obtains Fig. 5.As shown in Figure 5, also can by using the method for optical filter The electrochemical luminescence wavelength and intensity of ruthenium bipyridyl are obtained, but because the method is to take a measurement, the method phase with embodiment 1,2 Than its wavelength resolution is relatively low, and sensitivity is relatively low.
Comparative example 2
Detect that Particles in Electrochemiluminescofce ofce Luminol is strong using the method for optical filter based on commercialization Electrochemial luminescence detecting instrument at present Degree and wavelength, its specific steps are substantially consistent with embodiment 3, and difference is that it is bent to be circulated volt-ampere by electrochemical workstation Line scans (0~+0.5V), and detector places different wave length narrow-band-filter respectively to be commercialized Electrochemial luminescence detecting instrument at present Piece is mapped after obtaining correspondence ECL signal intensities, obtains Fig. 6.It will be appreciated from fig. 6 that being also obtained in that by using the method for optical filter The electrochemical luminescence wavelength and intensity of luminol, but because the method is to take a measurement, its ripple compared with the method for embodiment 3,4 Resolution ratio long is relatively low, and sensitivity is relatively low.
Embodiment 5
Using device in the same manner as in Example 1, while the wavelength and intensity of two kinds of electrochemical luminescence materials of monitoring.Two kinds Electrogenerated chemiluminescence material is respectively the nitrogen carbide nanometer sheet of azotized carbon nano piece (CNNS) and the sulfur doping prepared at 550 DEG C (S-CNNS).Comprise the following steps that:
1) glass carbon plate electrode surface is divided into two regions first, CNNS and S-CNNS is added dropwise respectively, after air drying To the working electrode modified;
2) electrode, reference electrode and the working electrode modified will be assembled in electrochemical reaction cell, it is anti-to electrochemistry Ying Chizhong adds 10mL pH 7.4Tris-HCl buffer solutions (K containing 100mM2S2O8With 0.1M KCl).By electrochemical workstation Apply constant potential (- 1.6V).Under the current potential, the CNNS and S-CNNS of working electrode surface obtain electronics, and and electrolyte respectively Coreagent (K in solution2S2O8Or triethylamine) react, due to the most strong ECL launch wavelengths difference of CNNS and S-CNNS At 435nm and 522nm, send out intensity long eventually through two kinds of nitrogen carbide material electrochemicals of detector monitors of Raman spectrometer and The change of wavelength is as shown in fig. 7, the most strong ECL emissive porwers of CNNS and S-CNNS can be respectively obtained at 435nm and 522nm. Show by the Instrument crosslinking method in the technical scheme can while obtain the electrochemical luminescence intensity of two kinds of materials, and Two kinds of electrochemical luminescence wavelength of material are efficiently differentiated, its wavelength resolution reaches 0.2nm.
Embodiment 6
Combined apparatus for monitoring electrochemical luminescence intensity and wavelength, including electrochemical reaction cell, electrochemical workstation And sepectrophotofluorometer;Electrochemical reaction cell is three-electrode system, and wherein working electrode is commercialization L-type glass-carbon electrode, It is platinum electrode to electrode, reference electrode is Ag/AgCl electrodes, and three electrodes are connected with electrochemical workstation respectively, work electricity The working face of pole is directed at the photon-counting detector of sepectrophotofluorometer.
The installation step of device is as follows:First, the excitation source of sepectrophotofluorometer is covered with shadow shield.Then, will Electrode, reference electrode and polished, carrying out washing treatment working electrode are assemblied in electrochemical reaction cell, the work of working electrode In face of the photon-counting detector of quasi- sepectrophotofluorometer.By three electrodes, electrode wires corresponding with electrochemical workstation connect respectively Connect, obtain final product combined apparatus.
The method that electrochemical luminescence intensity and wavelength are monitored using said apparatus, is comprised the following steps:
1) to addition 0.05M pH in electrochemical reaction cell 9.0 PBS (KCl, 0.15M containing 0.05M Ru(bpy)3 2+With 100mM oxalic acid);
2) constant potential (+1.3V), under the current potential, the ruthenium bipyridyl dead electricity of electrode surface are applied by electrochemical workstation Son, and reacted with the coreagent (oxalic acid) in electrolyte solution, finally cause ruthenium bipyridyl to send fluorescence, by fluorescence Spectrophotometer collection transmitting collection of illustrative plates, the ruthenium bipyridyl of gained launches collection of illustrative plates as shown in figure 8, can by the Instrument crosslinking method The electrochemical luminescence wavelength and intensity of real-time monitoring ruthenium bipyridyl, its wavelength resolution reach 1nm.
Embodiment 7
Combined apparatus for monitoring electrochemical luminescence intensity and wavelength, including electrochemical reaction cell, electrochemical workstation And ultraviolet-uisible spectrophotometer;Electrochemical reaction cell is three-electrode system, and wherein working electrode is commercialization glass-carbon electrode, It is platinum electrode to electrode, reference electrode is Ag/AgCl electrodes, and three electrodes are connected with electrochemical workstation respectively, work electricity The working face of pole is directed at the detector of ultraviolet-uisible spectrophotometer.The installation step of device is as follows:Will be to electrode, reference electrode It is assemblied in electrochemical reaction cell with polished, carrying out washing treatment working electrode, the working face alignment UV, visible light of working electrode The detector of spectrophotometer.By the electrode wires connection corresponding with electrochemical workstation respectively of three electrodes, combined apparatus are obtained final product.
The method that electrochemical luminescence intensity and wavelength are detected using said apparatus, is comprised the following steps:
1) to addition 0.05M pH in electrochemical reaction cell 9.0 PBS (KCl, 0.15M containing 0.05M Ru(bpy)3 2+With 100mM oxalic acid);
2) constant potential (+1.3V), under the current potential, the ruthenium bipyridyl dead electricity of electrode surface are applied by electrochemical workstation Son, and reacted with the coreagent (oxalic acid) in electrolyte solution, finally cause ruthenium bipyridyl to send fluorescence, by ultraviolet The detector collection transmitting collection of illustrative plates of visible spectrophotometer, the ruthenium bipyridyl transmitting collection of illustrative plates of gained is as shown in figure 9, pass through the instrument Method for combined use is capable of the electrochemical luminescence wavelength and intensity of real-time monitoring ruthenium bipyridyl, and its wavelength resolution reaches 0.1nm.
Embodiment 8
Using device monitoring electrochemical luminescence intensity in the same manner as in Example 6 and wavelength, comprise the following steps:
1) to addition 0.05M pH in electrochemical reaction cell 9.0 PBS (KCl, 0.15M containing 0.05M Ru(bpy)3 2+With 100mM oxalic acid);
2) voltammetric scan (0~+1.3V) is circulated by electrochemical workstation, then opens the test operation on computer Software, sets relevant parameter and elects standing wave long scan (620nm) as, and transmitting collection of illustrative plates is gathered by sepectrophotofluorometer, gained Ruthenium bipyridyl transmitting collection of illustrative plates as shown in Figure 10, the electrochemical luminescence of real-time monitoring ruthenium bipyridyl is capable of by the Instrument crosslinking method Wavelength and intensity, its wavelength resolution reach 1nm.

Claims (10)

1. a kind of method for monitoring electrochemical luminescence intensity and wavelength, it is characterised in that comprise the following steps:
1) by working electrode, to electrode and reference electrode assembling in electrochemical reaction cell and respectively with electrochemical workstation phase Even, the working face of working electrode is directed at the detector of high-resolution spectra analyzer;The high-resolution spectra analyzer is Raman light Spectrometer, ultraviolet-uisible spectrophotometer or sepectrophotofluorometer;
2) to electrolyte solution is added in electrochemical reaction cell, make working electrode, immerse described respectively to electrode and reference electrode In electrolyte solution;Contain coreagent and electrochemical luminescence material to be measured in the electrolyte solution;
3) electrochemical luminescence material to be measured is electrically excited to working electrode applied voltage by electrochemical workstation, is used The high-resolution spectra analyzer gathers electrochemical luminescence intensity and wavelength.
2. a kind of method for monitoring electrochemical luminescence intensity and wavelength, it is characterised in that comprise the following steps:
1) electrochemical luminescence material to be measured is modified in working electrode surface, obtains the working electrode modified;The work that will have been modified Make electrode, electrode and reference electrode are assemblied in electrochemical reaction cell and respectively with electrochemical workstation are connected, will modify Working electrode in containing electrochemical luminescence material to be measured working face be aligned high-resolution spectra analyzer detector;The height Resolved spectroscopy analyzer is Raman spectrometer, ultraviolet-uisible spectrophotometer or sepectrophotofluorometer;
2) to electrolyte solution is added in electrochemical reaction cell, make working electrode, immerse described respectively to electrode and reference electrode In electrolyte solution;Contain coreagent in the electrolyte solution;
3) electrochemical luminescence material to be measured is electrically excited to working electrode applied voltage by electrochemical workstation, is used The high-resolution spectra analyzer gathers electrochemical luminescence intensity and wavelength.
3. method according to claim 1 and 2, it is characterised in that the working electrode is glass-carbon electrode, gold electrode, platinum Electrode or graphite electrode.
4. method according to claim 1 and 2, it is characterised in that described is platinum electrode or carbon electrode to electrode.
5. method according to claim 1 and 2, it is characterised in that the reference electrode is silver/silver chloride electrode or saturation Calomel electrode.
6. method according to claim 1 and 2, it is characterised in that the coreagent is oxalic acid, hydrogen peroxide, oxygen, three second One or more in amine, potassium peroxydisulfate and sodium peroxydisulfate.
7. method according to claim 1 and 2, it is characterised in that the supporting electrolyte in the electrolyte solution is dense Spend the KCl for 0.001~1M, concentration be the NaCl of 0.001~1M, concentration be 0.001~1M PBSs or Tris- HCl cushioning liquid.
8. method according to claim 1 and 2, it is characterised in that step 3) in, permanent electricity is applied by electrochemical workstation Position carries out voltammetric scan, and electrochemical luminescence material is electrically excited.
9. method according to claim 1 and 2, it is characterised in that methods described is used to monitor single electrochemical luminescence thing The wavelength and intensity of matter.
10. method according to claim 1 and 2, it is characterised in that methods described be used for two kinds or two kinds of monitoring simultaneously with The wavelength and intensity of upper electrochemical luminescence material.
CN201710115635.XA 2017-03-01 2017-03-01 A kind of method for monitoring electrochemical luminescence intensity and wavelength Pending CN106885801A (en)

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