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Electrochemical analysis device adopting nano boron-doped diamond film electrode and its uses

An electrochemical analysis, boron-doped diamond technology, applied in the field of electrochemical analysis device, high-sensitivity detection of heavy metal ions, can solve problems such as insufficient detection sensitivity of metal ions, achieve good anti-oxidative interference ability, simple equipment, and sample dosage less effect

Inactive Publication Date: 2008-03-26
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to disclose a highly sensitive qualitative and quantitative detection device for trace heavy metal ions, which effectively avoids the use of toxic mercury-containing electrodes, and greatly improves the lack of detection sensitivity of conventional BDD electrodes for metal ions disadvantages, up to 10 -9 mol / L order of magnitude, and good reproducibility for the analysis of one or more trace and ultra-trace heavy metal ions

Method used

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  • Electrochemical analysis device adopting nano boron-doped diamond film electrode and its uses

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Experimental program
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Embodiment 1

[0019]The nanometer boron-doped diamond film electrode that the present invention adopts refers to people such as Greg M.Swain in literature (Direct Electrochemistry of Cytochrome c at Nanocrystalline Boron-Doped Diamond, Shannon Haymond, Gerald T.Babcock, and Greg M.Swain, J .AM.CHEM.SOC.2002, 124, 10634-10635) reported in the microwave-assisted chemical vapor deposition method (adjusted in specific parameters) prepared. Specifically as solid B 2 o 3 As a boron doping source, the silicon substrate is placed in the reaction chamber after conventional treatment, and after being evacuated, the CH 4 (2%) and Ar (98%) mixed gas is input to the vicinity of the tungsten wire installed in the tube, and the tungsten wire is heated to above 2000°C with a DC stabilized voltage power supply, the substrate temperature is about 500-900°C, and the indoor gas pressure The temperature is 103-105Pa, and the growth time is 1h; then the sample is transferred to the microwave CVD reaction chamb...

Embodiment 2

[0022] Adopt the electrochemical analysis device of embodiment 1, put into the H of 1.0mol / L in electrolytic cell 5 earlier 2 SO 4 The solution is used as the electrolyte 6, and the working electrode 2 (nano-BDD electrode) is placed in the H 2 SO 4 The solution was electrolyzed at a potential of 2.8V (Vs.SCE) for 15s, and then, the working electrode 2 was 2 SO 4 The cyclic voltammetry scan was carried out in the solution, the potential range was -2.0 to +3.0V, and the scan rate was 50mV / s until a stable cyclic voltammogram was obtained.

[0023] Next, prepare 0.01mol / L Cd(NO 3 ) 2 , 0.01mol / LPb(NO 3 ) 2 , 0.01mol / LCu(NO 3 ) 2 , 0.01mol / L Ag(NO 3 ), 0.20mol / L HAC-NaAC (pH=4.6) solution. And according to the needs of the experiment, use 0.20mol / L HAC-NaAC (pH=4.6) buffer solution to dilute the metal nitrate solution prepared above step by step to obtain a series of metal ion salt solutions with different concentrations. And replace the H in the electrolytic cell 5 in...

Embodiment 3

[0029] The first step is the same as example 2, at first adopting constant potential electrolysis, the nano-boron-doped diamond film electrode is in the H of 1.0mol / L 2 SO 4 The solution was electrolyzed at a potential of 2.8V (Vs.SCE) for 15s, and then the electrode was placed in H 2 SO 4 The cyclic voltammetry scan was carried out in the solution, the potential range was -2.0 to +3.0V, and the scan rate was 50mV / s until a stable cyclic voltammogram was obtained.

[0030] Then, use double distilled water to prepare 0.01mol / L SnCl 2 , 0.01mol / L Cu(NO 3 ) 2 , 0.01mol / LAg(NO 3 ), 0.03mol / L HNO 3 solution. And according to the experimental needs, use 0.03mol / L HNO 3 The above prepared 0.01mol / L SnCl 2 , 0.01mol / L Cu(NO 3 ) 2 , Ag(NO 3 ) solution was diluted step by step to obtain a series of metal ion salt solutions with different concentrations. And replace the H in the electrolytic cell 5 in sequence 2 SO 4 solution as electrolyte 6.

[0031] Using anodic stri...

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Abstract

The electrochemical analysis device and its application of the diamond membrane electrode of the nanometer mixed with the boron are used to detect the heavy metal ion with high sensitivity. It includes the electrolysis, the working station and data collecting and controlling system. The electrolysis system is made up of the electrolysis pool with the single room structure, the electrode frame and the working electrode fixed on the electrode frame, the assistant electrode, the reference electrode. The working electrode is the diamond membrane electrode of the nanometer mixed with the boron. The three electrodes are connected with the electrochemical analyzer by the electrode line. The data collecting and controlling system is the computer installed with the electrochemical analyzer. The device has avoided using the electrode containing the hydrargyrum and improved the detection sensitivity, the detection limit can reach 10-9mol / L and it has good repeatability. The detection process does not need to remove oxygen by giving nitrogen; also it can reach the renovation on the electrode surface. The invention can detect many trace metal ion in sample at the same time.

Description

technical field [0001] The invention relates to an electrochemical analysis device using a nanometer boron-doped diamond film electrode and its application, relating to an electrochemical analysis device, and further relates to a method for highly sensitive detection of heavy metal ions by the device. Specifically, a three-electrode system using nano-boron-doped diamond film electrodes as working electrodes, combined with anodic stripping voltammetry or pulsed anode stripping voltammetry, can detect one or more trace and ultra-trace heavy metal ions in samples with high sensitivity. The device belongs to the technical fields of nanometer material, electrochemical analysis and environmental monitoring. Background technique [0002] Heavy metal ions such as Pb 2+ 、Cd 2+ , Hg 2+ 、Cu 2+ 、Cd 6+ , Mn 5+ 、As 3+ , Fe 3+ etc. Once it enters the human body, it will endanger health and even life. Therefore, the quantitative detection of heavy metals is of great significance in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/48
Inventor 赵国华刘梅川肖小娥
Owner TONGJI UNIV
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