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Method for immobilization of metal iridium complexes with silicon nanoparticles being coated on electrode

A technology of silicon nanoparticles and immobilized metals, which is applied in the direction of electrodes, electrochemical variables of materials, chemiluminescence/bioluminescence, etc., can solve the problems of long time consumption, easy contamination, unresolved reproducibility and service life, and achieve Effect of small particle size and improved sensitivity

Inactive Publication Date: 2014-01-22
JIANGNAN UNIV
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Problems solved by technology

However, since the metal iridium complex is exposed on the electrode surface and is easily polluted, the above two sensors do not solve the problems of reproducibility and service life
Song Qijun et al. disclosed the patent of a sensor based on iridium complex electroluminescence and molecular imprinting recognition technology [15], which uses polyvinyl alcohol (PVA) / CNT immobilized metal iridium complex to modify the electrode, but the preparation process of this method is time-consuming longer

Method used

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  • Method for immobilization of metal iridium complexes with silicon nanoparticles being coated on electrode
  • Method for immobilization of metal iridium complexes with silicon nanoparticles being coated on electrode
  • Method for immobilization of metal iridium complexes with silicon nanoparticles being coated on electrode

Examples

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example 1

[0017] Example 1. Preparation of sensor: Add 0.44g AOT and 800 μL n-BuOH to 20ml ultrapure water, and stir magnetically to completely dissolve AOT until clear. Pipette 10.08mmol / L (pq) with a pipette 2 Add 100 μl of Ir(acac) in DMSO to the micellar system, and stir magnetically. Add 500 μL of vinyltrimethoxysilane to the micellar system, and stir for 1 h under magnetic force. Finally, 20 μl of concentrated ammonia water was added and magnetically stirred for 20 h to obtain a red silica nanoparticle emulsion doped with iridium complexes. Dialyze with a dialysis bag with a molecular weight cut-off of 12-14KDa for 50 hours, and remove the dialysate obtained by removing AOT and n-BuOH. After dialysis, the silica nanoparticles are evenly dispersed. Use a micro-sampler to pipette 10 μL of the dispersion liquid, drop-coat it on the surface of the glassy carbon electrode, place the electrode in the air to evaporate the solvent, and form a uniform particle on the electrode surface. ...

example 2

[0018] Example 2. Preparation of sensor: 0.44g AOT, 800 μl n-BuOH were added to 20ml ultrapure water, and magnetically stirred to completely dissolve AOT until clear. Pipette 10.08mmol / L (pq) with a pipette 2 100 μl of Ir(acac) in DMSO was added to the micellar system, and magnetically stirred for 1 h. Add 500 μL of vinyltriethoxysilane to the micellar system, and stir magnetically for 20 h. Finally, 20 μl of concentrated ammonia water was added and magnetically stirred for 20 h to obtain a red silica nanoparticle emulsion doped with iridium complexes. Dialyze with a dialysis bag with a molecular weight cut-off of 12-14 KDa for 50 h, and filter the dialysate obtained by removing AOT and n-BuOH with a 0.2 μl microporous membrane. After dialysis, the silica nanoparticles are evenly dispersed. Use a micro-sampler to pipette 10 μL of the dispersion liquid, drop-coat it on the surface of the glassy carbon electrode, place the electrode in the air to evaporate the solvent, and for...

example 3

[0019] Example 3. Preparation of sensor: 0.33g AOT, 600 μl n-BuOH were added to 20ml ultrapure water, and magnetically stirred to completely dissolve AOT until clear. Pipette 10.08mmol / L (pq) with a pipette 2 100 μl of Ir(acac) in DMSO was added to the micellar system, and magnetically stirred for 1 h. Add 500 μL of phenyltrimethoxysilane to the micellar system, and stir for 1 h under magnetic force. Finally, 0.042 g of sodium carbonate was slowly added and magnetically stirred for 20 h to obtain a red silica nanoparticle emulsion doped with iridium complexes. Dialyze with a dialysis bag with a molecular weight cut-off of 12-14 KDa for 50 h, and filter the dialysate obtained by removing AOT and n-BuOH with a 0.2 μl microporous membrane. After dialysis, the silica nanoparticles are evenly dispersed. Use a micro-sampler to pipette 10 μL of the dispersion liquid, drop-coat it on the surface of the glassy carbon electrode, place the electrode in the air to evaporate the solvent,...

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Abstract

The invention relates to a method for immobilization of metal iridium complexes with silicon nanoparticles being coated on an electrode, belongs to the electrochemiluminescence detection field, aims to immobilize water-insoluble metal iridium complexes on an electrode surface and achieves direct detection of coreactants. Organic silicon nanoparticles loaded with oil-soluble metal metal iridium complexes di(2-phenychinoline)(acetylacetone) iridium((pq)2Ir(acac)) are prepared by a positive phase microemulsion method. A micro emulsion system is di(2-ethylhexyl) succinic acid ester sodium sulfonate (AOT) / n-butyl alcohol (n-BuOH) / water. A solution of (pq)2Ir(acac) is added in the micro emulsion system. Then organic silicon monomers are added. Finally alkali is added as catalysts and organic silicon nanoparticles loaded with metal metal iridium complexes are synthesized. The scanning electron microscope results show that the synthesized organic silicon nanoparticles are monodisperse and spherical. The fluorescence spectra shows that the fluorescence properties of metal iridium complexes loaded in the organic silicon nanoparticles do not change. The synthesized silicon nanoparticles are dropped and painted on the surface of a glassy carbon electrode, and a solid-phase electrochemiluminescence electrode is prepared. The electrode has high sensitivity and measurement reproducibility to a typical coreactant di(2-butyl) ethanolamine (DBAE).

Description

technical field [0001] The invention relates to the synthesis of organosilicon nanoparticles loaded with metal iridium complexes and the development of a modified electrode-solid-phase electrochemiluminescent electrode. The modified electrode can be used for rapid detection of various organic amine substances. Background technique [0002] Electrochemiluminescence (Electrochemiluminescence or ECL) is mainly through electrochemical means, using certain compounds in the system to be measured to generate an unstable electronically excited intermediate state in an electrochemical reaction, which is generated when the substance in the excited state transitions back to the ground state light radiation. The intensity of the optical radiation produced by this electrochemical reaction can be used to determine the substance content. Since ECL uses electrolysis technology to produce chemiluminescence caused by certain redox substances on the electrode surface, this method has the adva...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/30G01N21/76C25B11/00
Inventor 宋启军刘艳丽韩超峰孙自淑
Owner JIANGNAN UNIV
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