Interdigitated Electrode Assembly for High-Resolution In Situ EC-NMR

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Solution Overview

Problem

Nuclear magnetic resonance (NMR) spectroscopy is underutilized in organic chemistry during electrochemical reactions due to the adverse effects of conducting electrodes and electrolytes on the magnetic field, which compromises the sensitivity of conventional NMR probes.

Innovation Solution

An electrochemical NMR (EC-NMR) system with a cylindrical symmetric interdigitated electrode assembly, comprising conductive metals like gold or platinum on a polyimide support, that can be inserted into an NMR sample tube without modifying commercial NMR probes, allowing for high-resolution in situ NMR spectroscopy during electrolysis.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Adaptability or versatility

If conventional NMR probes are used with conducting electrodes and electrolytes, then electrochemical reactions can be performed, but the magnetic field becomes warped and sensitivity is compromised

Engineering Contradiction:

Improveability to perform electrochemical reactionsVSAvoidNMR sensitivity

Core Design Contradiction:

Adaptability or versatilityVSMeasurement precision

Solution Approach 1:

The electrode assembly is segmented into multiple thin interdigitated electrodes (working electrode and counter electrode) separated by insulating material. This segmentation distributes the magnetic field distortion across multiple small elements rather than one large electrode, reducing overall warping effects while maintaining electrochemical functionality

Inventive Principle:

Principle #1Segmentation

Solution Approach 2:

An insulating support structure (such as a cylindrical rod or substrate) is introduced as an intermediary between the electrodes and the NMR detection region. This intermediary physically separates the conducting electrodes from the sensitive NMR detection area, allowing electrochemical reactions to proceed while minimizing magnetic field warping that would otherwise compromise NMR sensitivity

Inventive Principle:

Principle #24Intermediary (Mediator)

2Ease of operation

If electrodes are placed in the NMR detection region, then in situ monitoring is enabled, but the magnetic field homogeneity deteriorates

Engineering Contradiction:

Improvein situ monitoring capabilityVSAvoidmagnetic field homogeneity

Core Design Contradiction:

Ease of operationVSStability of the object's composition

Solution Approach 1:

The electrode assembly is designed with a specific three-dimensional geometry (such as a cylindrical configuration with interdigitated electrodes arranged around the circumference) that positions the conducting elements in dimensions away from the central detection region, allowing in situ monitoring while preserving magnetic field homogeneity in the detection zone

Inventive Principle:

Principle #17Another dimension (Dimensionality change)

3Ease of manufacture

If simple electrode designs are used, then setup is quick and inexpensive, but high-resolution NMR features are compromised

Engineering Contradiction:

Improvesetup simplicity and costVSAvoidhigh-resolution NMR features

Core Design Contradiction:

Ease of manufactureVSManufacturing precision

Solution Approach 1:

The electrodes are constructed as thin flexible films or coatings deposited on a support structure. This allows the electrodes to be easily manufactured using simple deposition techniques while the thin profile minimizes their impact on the magnetic field, preserving high-resolution NMR features. The flexibility also enables easy insertion and removal from NMR tubes

Inventive Principle:

Principle #30Flexible shells and thin films

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

The EC-NMR system enables robust, high-resolution NMR spectroscopy during electrochemical reactions, maintaining sensitivity and allowing for the determination of sample composition and intermediate species, while minimizing the impact on the magnetic field.

Implementation Method 1

an electrode assembly comprising a plurality of interdigitated electrodes that comprise conductive metals deposited on a support

Methodology Applied

Scientific EffectElectrical conduction: Conduction (electrical)

Implementation Method 2

the presence of the electrodes and electrolytes in electrochemical reactions is known to warp the magnetic field

Methodology Applied

Scientific EffectMagnetic field interaction: Magnetic Field

Implementation Method 3

Nuclear magnetic resonance (NMR) spectroscopy is a powerful analytic technique for determining the composition of unknown samples. NMR utilizes the magnetic properties of atomic nuclei

Methodology Applied

Scientific EffectNuclear magnetic resonance: Magnetism

Implementation Method 4

electrolysis is a firmly established fundamental technique for driving non-spontaneous chemical reactions in organic chemistry

Methodology Applied

Scientific EffectElectrolysis: Electrolysis

Data Source

PatentUS10948441B2High-resolution in situ electrochemical NMR with interdigitated electrodes

Publication Date: 2021.03.16 GEORGETOWN UNIV

AI summary

A system for carrying out electrochemical nuclear magnetic resonance spectroscopy (EC-NMR) is disclosed, along with methods of manufacturing the EC-NMR system, and methods of using the EC-NMR system to monitor electrochemical reactions. The system comprises interdigitated electrodes arranged in a cylindrically symmetric manner. The system allows for nuclear magnetic resonance spectroscopy to be carried out on a sample during electrolysis with minimal effect to its sensitivity.