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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AI-Extracted Technical Summary

Problems solved by technology

However, currently known electrochemical mass spectrometry techniques do ...

Method used

Electrolytic cell is made of transparent glass, avoids the interference to line of sight, does not affect the observation to working electrode and mass spectrometry inlet;

[0021] The inverted structure of the working electrode and the upper structure of the mass spectrometry inlet are ...

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.

Application Domain

Material electrochemical variables

Technology Topic

Auxiliary electrodeMass spectrum analysis +8

Image

Examples

Experimental program(3)

Example Embodiment

[0029] Example 1

[0030] For detecting the reaction mechanism of the electro-oxidation of formic acid by the research electrode, the electrochemical cell 7 and the storage tank 11 are injected with 0.5 mol/L sulfuric acid + 0.5 mol/L formic acid. Turn on the injection pump and the output pump, the pump flow rate is 100mL/min, keep the electrolyte circulating, 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, perform electrochemical potential scanning, collect the product through the mass spectrometer inlet and analyze and detect its mass spectrometric signal, such as figure 2 Shown. figure 2.According to the in-situ real-time mass spectrometry detection of the product of electrocatalytic formic acid, during the cyclic voltammetric potential scan, both the positive scan and the negative scan detected the mass spectrum signal of carbon dioxide. Combined with other characterization techniques, it can be known that formic acid is generated by electrocatalytic oxidation Carbon dioxide follows the "dual path mechanism", namely, the "active intermediate path" (also known as the direct path or dehydrogenation path) and the "toxic intermediate path" (also known as the indirect path or dehydration path).

Example Embodiment

[0031] Example 2

[0032] For detecting the reaction mechanism of the electrode electro-oxidation of methanol, the electrochemical cell 7 and the storage tank 11 are injected with 0.5 mol/L sulfuric acid + 0.5 mol/L methanol. Turn on the injection pump and the output pump, the pump flow rate is 100mL/min, keep the electrolyte circulating, 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, perform electrochemical potential scanning, collect the product through the mass spectrometer inlet and analyze and detect its mass spectrometric signal, such as image 3 Shown. image 3 The product of electrocatalytic methanol in the medium is detected by in-situ real-time mass spectrometry, and CO 2 Has the largest ion current, followed by CHOOH and CH 3 COOH, combined with other characterization techniques, it can be inferred that in the process of electrocatalytic oxidation of methanol to carbon dioxide, there will be CHOOH and CH 3 The generation of COOH.

Example Embodiment

[0033] Example 3

[0034] For detecting the reaction mechanism of the electrode to the electro-oxidation of ethanol, the electrochemical cell 7 and the storage tank 11 are injected with 0.5 mol/L sulfuric acid + 0.5 mol/L ethanol. Turn on the injection pump and the output pump, the pump flow rate is 100mL/min, keep the electrolyte circulating, so that the three electrodes are connected in the electrochemical cell. After the mass spectrometer starts to scan the blank baseline and stabilizes, perform an electrochemical potential scan, collect the product through the mass spectrometer inlet and analyze and detect its mass spectrum signal, such as Figure 4 Shown. Figure 4 In situ real-time mass spectrometry of the product of electrocatalytic ethanol, it can be known that in the process of electrocatalytic oxidation of ethanol to carbon dioxide, CH 3 COOH generation, additional CH 3 CH 2 The OH signal is caused by the volatilization of a small amount of ethanol.

[0035] Through the above three examples, it can be seen that the in-situ electrochemical mass spectrometry analysis system is convenient to collect the gas generated during the reaction. It can not only analyze the final gas or volatile products, but also detect intermediate gases or volatile products. There are unique analytical advantages in the research of various electrochemical reaction mechanisms.

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Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

good collection
Simple installation and disassembly

Analysis system for in-situ electrochemistry-mass spectrometry combination

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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