Method for detecting hydrogen peroxide and nitrite by electrochemical sensor based on dual-metal porphyrin coordination polymer

A technology of coordination polymer and bimetalloporphyrin is applied in the field of electrochemical detection, which can solve the problems of few reports of bifunctional electrochemical sensors, and achieve the effects of good electrocatalytic performance, fast detection speed and improved performance.

Inactive Publication Date: 2015-09-09
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The electrochemical detection of hydrogen peroxide and nitrite involves electrocatalytic reduction and oxidation, respectivel...

Method used

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  • Method for detecting hydrogen peroxide and nitrite by electrochemical sensor based on dual-metal porphyrin coordination polymer
  • Method for detecting hydrogen peroxide and nitrite by electrochemical sensor based on dual-metal porphyrin coordination polymer
  • Method for detecting hydrogen peroxide and nitrite by electrochemical sensor based on dual-metal porphyrin coordination polymer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Embodiment 1 double metal coordination polymer [Cu 2 (Co-TCPP)(H 2 O)2 ]·0.5DMF·5H 2 Preparation of O(CoTCPP-Cu)

[0075] Weigh CoTCPP 3mg (0.01mmol), add DMF 3mL to dissolve it; meanwhile weigh excess Cu(NO 3 ) 2 .3H 2 O 100mg (0.4mmol), add DMF 2mL to dissolve it. The prepared Cu(NO 3 ) 2 The solution was added to the CoTCPP solution, and HNO was added while stirring 3 (1M) 1-4 mL, and finally a mixed solution with red flocs precipitated was obtained. The mixed solution was placed in an oven at 65-100° C. for 5 days to obtain a purple-red powder. Filtration, respectively with DMF, H 2 O and EtOH washed, and dried at room temperature.

[0076] The synthesis of CoTCPP can refer to literature: (a) Lindsey, J.S., H.C.Hsu, and I.C.Schreiman, SYNTHESIS OF TETRAPHENYLPORPHYRINS UNDER VERY MILD CONDITIONS. Tetrahedron Letters, 1986.27(41): 4969-4970. (b) Kumar, A., et al., One-pot general synthesis of metalloporphyrins. Tetrahedron Letters, 2007.48(41): 7287-7290....

Embodiment 2

[0078] Preparation of Embodiment 2 Electrochemical Sensor-I

[0079] (1) Polishing and cleaning of bare glassy carbon electrodes

[0080] Wash the glassy carbon electrode with secondary deionized water and ultrasonically for one minute, then polish it with alumina powder with a diameter of 0.3um for five minutes, wash the grinding cloth and the slurry on the electrode with secondary deionized water, and Put the glassy carbon electrode in the secondary deionized water for one minute, after repeated grinding and cleaning, finally dry the glassy carbon electrode for later use.

[0081] (2) Electrode modification

[0082] Ultrasonic dispersion of 5 mg of CoTCPP-Cu in 400 μL deionized water to form a suspension, 6 μL of the suspension was drop-coated on the surface of the glassy carbon electrode obtained in step (1), and dried; then drop-coated 2 μL of 1% nafion solution on the electrode surface , and dried to obtain the CoTCPP-Cu modified electrode, which is denoted as electric ...

Embodiment 3

[0083] Embodiment 3 Electrochemical sensor-1 is applied to the cyclic voltammetry scanning of hydrogen peroxide detection

[0084] (1) Preparation of hydrogen peroxide standard solution

[0085] Take 84μL of 30% hydrogen peroxide solution, and dilute it to 4mL. That is to prepare 0.2mol L -1 Hydrogen peroxide solution, other concentrations were prepared in the same way.

[0086] (2) Cyclic voltammogram for hydrogen peroxide detection

[0087] The C-V curves of the bare electrode and the electrochemical sensor-I with or without hydrogen peroxide in PBS electrolyte at pH = 7, as shown in the attached Figure 5A Shown, a is naked GCE, b is naked GCE plus 0.5mmolL -1 h 2 o 2 , the comparison between a and b shows that the bare GCE has an effect on H 2 o 2 No response. c-d are electrochemical sensor-I adding different concentrations of H 2 o 2 0 and 0.5 mmol L -1 , with the addition of hydrogen peroxide, the response of the reduction current is gradually enhanced, indica...

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Abstract

The invention discloses a method for detecting hydrogen peroxide and nitrite by an electrochemical sensor based on a dual-metal porphyrin coordination polymer. A dual-metal porphyrin coordination polymer (CoTCPP-Cu or CoTCPP-Cu/CNTs) composite material modification electrode is used as a working electrode; hydrogen peroxide or nitrite is detected by a timing current method; CoTCPP-Cu is a coordination polymer assembled by dual metals Co and Cu and tetra-(p-carboxyphenyl) porphyrin. The electrochemical sensor adopted in the method is a current type sensor, has unique dual-metal activity and is high in sensitivity; the method has the advantages of convenience in detection and wide application range; the detection limit for hydrogen peroxide can reach 5.0*10<-7>M and the detection limit for nitrite can reach 2.5*10<-6>. The detection method disclosed by the invention has the characteristics of quick on-site detection, high sensitivity, low cost and the like.

Description

technical field [0001] The invention relates to an electrochemical detection method, in particular to a method for detecting hydrogen peroxide or nitrite with an electrochemical sensor based on a double metal porphyrin coordination polymer. Background technique [0002] Coordination polymers are a class of organic-inorganic hybrid materials that link metal ions or clusters with organic ligands through coordination bonds. , gas storage and separation, optical materials, magnetic materials, etc. (see: (a) SR Batten, SM Neville, DR Turner, Coordination Polymers: Design, Analysis and Application, 2008. (b) Chemical Society Reviews, 38 (2009 ).).). However, there are few studies on the use of coordination polymers as electrocatalysts for electrosensing (see: (a) Zhang, W., Wang, L.L., Zhang, N., Wang, G.F., Fang, B., 2009 .Functionalization of Single-Walled Carbon Nanotubes with Cubic Prussian Blue and Its Application for Amperometric Sensing. Electroanalysis 21(21), 2325-2330....

Claims

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Application Information

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IPC IPC(8): G01N27/48G01N27/30
Inventor 周泊史丽梅张英华
Owner NANJING NORMAL UNIVERSITY
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