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In-situ electrochemical infrared spectroscopic-mass spectrometric detection system and method

An in-situ electrochemical and infrared spectroscopy technology, applied in the direction of material electrochemical variables, measuring devices, scientific instruments, etc., can solve the problem that mass spectrometry can only target volatile intermediate products and adsorption intermediate products, and achieve complete and accurate test information. Improved accuracy and wide-ranging effects

Active Publication Date: 2016-02-24
HARBIN INST OF TECH
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  • Claims
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Problems solved by technology

However, both types of in situ techniques have their own drawbacks: mass spectrometry can only target volatile intermediates, while infrared spectroscopy can only target surface-adsorbed and soluble intermediates
However, due to various technical obstacles, there is no research on the combination of the two at home and abroad, using in situ mass spectrometry and in situ infrared on the same electrode at the same time.

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  • In-situ electrochemical infrared spectroscopic-mass spectrometric detection system and method

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specific Embodiment approach 1

[0032] Specific implementation mode one: as figure 1 As shown, the in-situ electrochemical infrared spectroscopy-mass spectrometry detection system provided in this embodiment consists of four parts: a three-electrode electrolytic cell, a surface-enhanced infrared reflection spectroscopy analysis device, an in-situ mass spectrometer and an in-situ infrared transmission spectroscopy analysis device. ,in:

[0033] Described three-electrode electrolytic cell is made up of counter electrode electrolytic cell 3, research electrode electrolytic cell 5 and reference electrode electrolytic cell 4 and ion exchange membrane 14, and research electrode electrolytic cell 5 is connected with opposite electrode electrolytic cell 3 and reference electrode electrolytic cell respectively. 4 connected, the ion exchange membrane 14 is set in the research electrode electrolytic cell 5, the ion exchange membrane 5 allows the exchange of specific conductive ions, and isolates the penetration of othe...

specific Embodiment approach 2

[0042] Specific embodiment two: in order to detect the reaction mechanism of sample catalyst 16 to ethanol electrooxidation, research electrode electrolytic cell 5 injects 0.5MH 2 SO 4 +0.1MCH 3 CH 2 OH, counter electrode electrolytic cell 3 and reference electrode electrolytic cell 4 inject 0.5MH 2 SO 4 , so that the three-electrode electrolytic cell Unicom. The ion exchange membrane 14 is fixed in the research electrode electrolytic cell 5, allowing the exchange of hydrogen ions and isolating the penetration of other ions. The attenuated total reflection infrared transmitter 11, the ZnSe prism 10 and the reflection infrared signal receiver 9 in the surface-enhanced infrared reflection spectroscopy analysis device are fixed in proper positions, and the optical path is adjusted, wherein the diameter of the ZnSe prism is 25mm. A PTFE membrane 15 with an average pore diameter of 50 nm is located under the ion exchange membrane 14 , and the PTFE membrane 15 is closely connec...

specific Embodiment approach 3

[0043] Specific implementation mode three: In order to detect the reaction mechanism of the sample catalyst to the electro-oxidation of ethanol, the electrode electrolytic cell 5 is injected with 0.5MH 2 SO 4 +0.2MCH 3 CH 2 OH, counter electrode electrolytic cell 3 and reference electrode electrolytic cell 4 inject 0.5MH 2 SO 4 , so that the three-electrode electrolytic cell Unicom. The ion exchange membrane 14 is fixed in the research electrode electrolytic cell 5, allowing the exchange of hydrogen ions and isolating the penetration of other ions. The attenuated total reflection infrared emitter 11, the ZnSe prism 10 and the reflection infrared signal receiver 9 in the surface-enhanced infrared reflection spectroscopy analysis device are fixed in proper positions, and the optical path is adjusted, wherein the diameter of the ZnSe prism is 40mm. A PTFE membrane 15 with an average pore diameter of 220 nm is located under the ion exchange membrane 14 , and the PTFE membrane...

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Abstract

The invention discloses an in-situ electrochemical infrared spectroscopic-mass spectrometric detection system and method. The system is composed of a three-electrode electrolytic bath, a surface-enhanced infrared reflectance spectroscopic analysis apparatus, an in-situ mass spectrometer and an in-situ infrared transmission spectroscopic analysis apparatus, wherein the three-electrode electrolytic bath is composed of a counter electrode electrolytic bath, a working electrode electrolytic bath, a reference electrode electrolytic bath and an ion exchange membrane; the surface-enhanced infrared reflectance spectroscopic analysis apparatus is composed of an attenuated total reflection infrared ray emitter, a ZnSe prism and a reflected infrared signal receiver; the in-situ mass spectrometer is composed of a mass spectrometric rod, a vacuum pump, a glass capillary and a PTFE membrane; and the in-situ infrared transmission spectroscopic analysis apparatus is composed of an electrolyte storage tank, a waste electrolyte tank, a peristaltic pump, a CaF2 capillary glass tube, an infrared transmission light emitter and an infrared transmission light receiver. The system and method provided have the advantages of complete and accurate test information, high sensitivity, a wide application scope, capacity of realizing arbitrary combination, easiness in manufacturing, etc.

Description

technical field [0001] The invention belongs to the technical field of electrochemical detection, and relates to an in-situ electrochemical infrared spectrum-mass spectrometry detection system and method. Background technique [0002] In the development of electrochemical science, modern electrochemical analysis techniques for studying the products or intermediate products of electrochemical reactions have played a very important role. Among the numerous electrochemical spectroscopy techniques, in situ electrochemical mass spectrometry and in situ electrochemical infrared spectroscopy have received widespread attention. [0003] In situ electrochemical mass spectrometry has the ability to analyze volatile products and intermediate products with the change of electrode potential, and the analysis results are intuitive and reliable, making in situ electrochemical mass spectrometry a very effective on-site analysis method. In-situ electrochemical infrared spectroscopy has the ...

Claims

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Application Information

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IPC IPC(8): G01N21/552G01N27/42G01N27/62
CPCG01N21/552G01N27/423G01N27/62
Inventor 高云智屈云腾王龙李灿尹鸽平
Owner HARBIN INST OF TECH
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