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Analysis system for in-situ electrochemistry-mass spectrometry combination

An in-situ electrochemical and analysis system technology, which is applied in the detection and analysis field of in-situ detection of electrochemical and mass spectrometry signals, can solve problems such as no solutions, and achieve easy installation and disassembly, easy collection, and broad application prospects Effect

Active Publication Date: 2018-07-27
上海零露仪器设备有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, currently known electrochemical mass spectrometry techniques do not have a solution that can simultaneously optimize the above situations

Method used

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  • Analysis system for in-situ electrochemistry-mass spectrometry combination
  • Analysis system for in-situ electrochemistry-mass spectrometry combination
  • Analysis system for in-situ electrochemistry-mass spectrometry combination

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] For the detection and research of the reaction mechanism of the electrodes for the electro-oxidation of formic acid, the electrochemical cell 7 and the liquid storage tank 11 were injected with 0.5 mol / L sulfuric acid + 0.5 mol / L formic acid. Turn on the sampling pump and the sampling pump, the pump flow rate is 100mL / min, keep the electrolyte flowing, so that the three electrodes are connected in the electrochemical cell. At the same time, after the mass spectrometer starts to scan the blank baseline and stabilizes, then perform electrochemical potential scanning, collect the product through the mass spectrometer inlet and analyze and detect its mass spectrum signal, such as figure 2 shown. figure 2 .From the in situ real-time mass spectrometry detection of the product of electrocatalyzed formic acid, in the process of cyclic voltammetry potential scanning, the mass spectrometry signal of carbon dioxide was detected in both positive scanning and negative scanning. Co...

Embodiment 2

[0032] For the detection and research of the reaction mechanism of the electrode to the electrooxidation of methanol, the electrochemical cell 7 and the liquid storage tank 11 were injected with 0.5 mol / L sulfuric acid + 0.5 mol / L methanol. Turn on the sampling pump and the sampling pump, the pump flow rate is 100mL / min, keep the electrolyte flowing, so that the three electrodes are connected in the electrochemical cell. At the same time, after the mass spectrometer starts to scan the blank baseline and stabilizes, then perform electrochemical potential scanning, collect the product through the mass spectrometer inlet and analyze and detect its mass spectrum signal, such as image 3 shown. image 3 From the in situ real-time mass spectrometry detection of the product of electrocatalyzed methanol, CO 2 The ion current is the largest, followed by CHOOH and CH 3 COOH, combined with other characterization techniques, it can be speculated that in the process of electrocatalytic o...

Embodiment 3

[0034] For detecting and studying the reaction mechanism of the electrode to the electrooxidation of ethanol, the electrochemical cell 7 and the liquid storage tank 11 are injected with 0.5 mol / L sulfuric acid + 0.5 mol / L ethanol. Turn on the sampling pump and the sampling pump, the pump flow rate is 100mL / min, keep the electrolyte flowing, so that the three electrodes are connected in the electrochemical cell. After the mass spectrometer starts to scan the blank baseline and stabilizes, then perform electrochemical potential scanning, collect the product through the mass spectrometer inlet and analyze and detect its mass spectrum signal, such as Figure 4 shown. Figure 4 From the in situ real-time mass spectrometry detection of the product of electrocatalytic ethanol, it can be seen that in the process of electrocatalytic oxidation of ethanol to carbon dioxide, there will be CH 3 COOH is generated, additional CH 3 CH 2 The OH signal is caused by the volatilization of a sm...

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Abstract

The invention discloses an analysis system for in-situ electrochemistry-mass spectrometry combination. The analysis system comprises an electrochemical cell, wherein electrolyte is arranged inside theelectrochemical cell; a work electrode, a reference electrode and an auxiliary electrode are arranged in the electrochemical cell; the work electrode is fixed in an inverted mode; a mass spectrometrysample feeding opening is fixed in an overhead mode and is arranged under the work electrode; the distance between the work electrode and the mass spectrometry sample feeding opening is regulated andcontrolled; the mass spectrometry sample feeding opening is arranged below the liquid level of the electrolyte. The analysis system has the advantages that the inverted mode structure of the work electrode and the overhead mode structure of the mass spectrometry sample feeding opening conform to the hydrodynamic principle of volatile products; the product collection is easy. Meanwhile, through the flow speed control of a sampling pump and a sample outlet pump, reaction liquid at the work electrode surface and the electrolyte of the whole electrochemical cell can be timely updated. The whole device can be easily mounted and dismounted. Wide application prospects are realized in the fields of catalysis, energy storage, adsorption, environment and the like.

Description

technical field [0001] The invention belongs to the technical field of electrochemical detection, and in particular relates to a detection and analysis method and system for integrating in-situ detection of electrochemical and mass spectrometry signals. Background technique [0002] Studying the electrochemical reaction products at the electrode interface plays a vital role in understanding and mastering the reaction mechanism of the entire reaction system. In-situ electrochemical mass spectrometry has the ability to detect and analyze volatile products and intermediate products produced in the electrochemical reaction process, and its analysis results have the advantages of intuition, reliability and punctuality, which has attracted widespread attention in related fields and Rapidly developed into a very effective analytical technique. For the electrochemical reaction system, the volatile products produced by it have floating properties due to their relatively small densit...

Claims

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Application Information

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IPC IPC(8): G01N27/48G01N27/62
CPCG01N27/48G01N27/62
Inventor 张峰王振王金锁
Owner 上海零露仪器设备有限公司
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