High-resolution in situ electrochemical nmr with interdigitated electrodes

Patent metadata

Field	Value
Publication number	US-2018284042-A1
Application number	US-201615764811-A
Country	US
Kind code	A1
Filing date	Sep 30, 2016
Priority date	Oct 2, 2015
Publication date	Oct 4, 2018
Grant date	—

Abstract

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.

First claim

1 . An electrochemical nuclear magnetic resonance (EC-NMR) system comprising:
an interdigitated electrode acting as a working electrode; an interdigitated electrode acting as a counter electrode; and an NMR sample tube,
wherein the interdigitated electrodes are positioned inside the NMR sample tube such that the electrodes are in the NMR detection region of the NMR sample tube.

2 . The EC-NMR system of claim 1 , wherein the electrodes are cylindrically symmetric.

3 . The EC-NMR system of claim 1 , wherein the interdigitated electrodes comprise gold or platinum deposited on a support.

4 . The EC-NMR system of claim 1 , wherein the interdigitated electrodes comprise a support, wherein the support is a glass, ceramic, or polymer support.

5 . The EC-NMR system of claim 1 , further comprising an electrocatalyst, wherein the electrocatalyst is applied to one or both interdigitated electrodes.

6 . The EC-NMR system of claim 1 , wherein interdigitated electrodes are deposited on a flexible support.

7 . The EC-NMR system of claim 1 , wherein the thickness of the electrodes is in a range of 5-100 nanometers.

8 . The EC-NMR system of claim 7 , wherein the thickness of the electrodes is in a range of 5-50 nanometers.

9 . The EC-NMR system of claim 7 , wherein the thickness of the electrodes is in a range of 5-25 nanometers.

10 . The EC-NMR system of claim 1 , further comprising an electrical feed-through cap that fits on the NMR sample tube.

11 . The EC-NMR system of claim 10 , wherein the electrical feed-through cap comprises:
a working electrode metal finger extending through the cap, a counter electrode metal finger extending through the cap; wherein, when fitted to the NMR sample tube, the electrical fingers make sliding contact with the corresponding interdigitated electrodes; electrical connectors attached to each metal finger, wherein the electrical connectors allow each metal finger to be connected to a potentiostat; and a reference electrode positioned through the cap.

12 . The EC-NMR system of claim 3 , wherein the working electrode and the counter electrode are symmetrically shaped on the support.

13 . The EC-NMR system of claim 12 , wherein the symmetry is maintained when the support is rolled into a cylinder.

14 . A method of performing nuclear magnetic resonance spectroscopy during an electrochemical reaction comprising:
supplying an interdigitated electrode acting as a working electrode; supplying an interdigitated electrode acting as a counter electrode; and supplying an NMR sample tube, wherein the interdigitated electrodes are positioned inside the NMR sample tube such that the electrodes are in an NMR detection region of the NMR sample tube; and performing nuclear magnetic resonance spectroscopy in the NMR detection region.

15 . The method of performing nuclear magnetic resonance spectroscopy during an electrochemical reaction of claim 14 , wherein the working and counter electrodes are located on a support.

16 . The method of performing nuclear magnetic resonance spectroscopy during an electrochemical reaction of claim 15 , wherein the working and counter electrodes are symmetrically shaped on the support.

17 . A method of manufacturing an electrochemical nuclear magnetic resonance (EC-NMR) system comprising:
(a) cutting a support such that it will fit, when rolled into a cylinder, into an NMR tube; (b) applying a mask to the support; (c) depositing electrodes on the support; and (d) removing the mask to reveal an interdigitated electrode pattern.

Assignees

• Univ Georgetown

Inventors

• Tong Yuye J
• Sorte Eric G

Classifications

• C25B1/00

  Electrolytic production of inorganic compounds or non-metals · CPC title

• G01N24/088 Primary

  Assessment or manipulation of a chemical or biochemical reaction, e.g. verification whether a chemical reaction occurred or whether a ligand binds to a receptor in drug screening or assessing reaction kinetics · CPC title

• G01R33/30

  Sample handling arrangements, e.g. sample cells, spinning mechanisms · CPC title

• G01R33/46

  NMR spectroscopy · CPC title

• C25B1/01

  Products · CPC title