IP Library Granted Patent US 9,283,541
Granted Patent B2
US 9,283,541 · App. 13/035,645 · Granted Mar 15, 2016

Thin layer chromatography plates and related methods

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Quick Facts
Patent No.
US 9,283,541
App. No.
13/035,645
Granted
Mar 15, 2016
Kind
B2
Abstract

In an embodiment, a method for manufacturing a thin layer chromatography (“TLC”) plate is disclosed. The method includes forming a layer of elongated nanostructures (e.g., carbon nanotubes), and at least partially coating the elongated nanostructures with a coating. The coating includes a stationary phase and/or precursor of a stationary phase for use in chromatography. The stationary phase may be functionalized with hydroxyl groups by exposure to acidified water vapor or immersion in a concentrated acid bath (e.g., HCl and methanol). At least a portion of the elongated nanostructures may be removed after being coated. Embodiments for TLC plates and related methods are also disclosed.

Claims (29)

1. A method for manufacturing a thin layer chromatography plate, the method comprising:

forming a catalyst layer disposed on a substrate that includes a first portion and at least a second portion, each of the first and at least a second portions exhibiting a selected non-linear configuration;

forming a layer of elongated nanostructures on the first and at least a second portions of the catalyst layer, wherein the layer of elongated nanostructures includes a first portion grown on the first portion of the catalyst layer and at least a second portion grown on the at least a second portion of the catalyst layer;

at least partially coating the elongated nanostructures with a coating, the coating including at least one of a stationary phase or a precursor of a stationary phase for use in chromatography;

after the act of at least partially coating the elongated nanostructures with a coating, at least partially removing the elongated nanostructures; and

exposing the coating to an acid in order to bond hydroxyl groups to the coating.

2. The method as recited in claim 1 , wherein exposing the coating to an acid comprises immersing at least the coating of the thin layer chromatography plate in an acidic solution.

3. The method as recited in claim 2 , wherein the acidic solution comprises at least one acid selected from the group consisting of hydrochloric acid, nitric acid, hydrobromic acid, acetic acid, formic acid, and trifluoroacetic acid.

4. The method as recited in claim 2 , wherein the acidic solution comprises a concentrated bath of 50:50 vol/vol HCl and methanol.

5. The method as recited in claim 1 , wherein exposing the coating to an acid comprises exposing the coating to acidified water vapor.

6. The method as recited in claim 5 , wherein the coating is exposed to acidified water vapor by introducing the acidified water vapor into an oxidizing chamber containing the coating while the coating is being cooled.

7. The method as recited in claim 5 , wherein the coating is exposed to acidified water vapor by introducing the acidified water vapor into an oxidizing chamber containing the coating while maintaining the coating at an elevated temperature.

8. The method as recited in claim 1 , wherein the coating that at least partially coats the elongated nanostructures defines respective elongated structures that extend longitudinally away from the substrate.

9. The method as recited in claim 1 , wherein the substrate comprises a backing layer on which the catalyst layer is disposed, the backing layer including at least one material selected from the group consisting of silica, silicon, nickel, alumina, borosilicate glass, and steel.

10. The method as recited in claim 1 , wherein forming the layer of elongated nanostructures on the first and at least a second portions of the catalyst layer comprises growing a layer of carbon nanotubes.

11. The method as recited in claim 1 , wherein at least partially coating the elongated nanostructures with a coating comprises forming the coating to include at least one material selected from the group consisting of silicon, silicon dioxide, silicon nitride, aluminum, aluminum oxide, titanium, titanium oxide, zirconium, and zirconium oxide.

12. The method as recited in claim 11 , wherein forming the coating to include at least one material selected from the group consisting of silicon, silicon dioxide, silicon nitride, aluminum, aluminum oxide, titanium, titanium oxide, zirconium, and zirconium oxide comprises at least partially infiltrating the elongated nanostructures by low pressure chemical vapor deposition with an infiltrant.

13. The method as recited in claim 1 , wherein at least partially removing the elongated nanostructures comprises oxidizing the coating that at least partially coats the elongated nanostructures so that a plurality of stationary phase structures are formed and oxidizing the elongated nanostructures so that the elongated nanostructures are substantially removed.

14. The method as recited in claim 1 , wherein each of the first and at least a second portions of the catalyst layer form a zigzag pattern.

15. The method as recited in claim 14 , wherein the first and second portions of the zigzag pattern are at approximately 90° relative to one another.

16. A method for manufacturing a thin layer chromatography plate, the method comprising:

forming a catalyst layer disposed on a substrate that includes a first portion and at least a second portion, each of the first and at least a second portions exhibiting a selected non-linear configuration;

forming a layer of elongated nanostructures on the first and at least a second portions of the catalyst layer, wherein the layer of elongated nanostructures includes a first portion grown on the first portion of the catalyst layer and at least a second portion grown on the at least a second portion of the catalyst layer;

at least partially coating the elongated nanostructures with a coating, the coating including at least one of a stationary phase or a precursor of a stationary phase for use in chromatography;

after the act of at least partially coating the elongated nanostructures with a coating, at least partially removing the elongated nanostructures; and

exposing the coating to a solution in order to hydroxylate the coating.

17. The method as recited in claim 16 , wherein exposing the coating to a solution in order to hydroxylate the coating comprises exposing at least the coating of the thin layer chromatography plate to an acidic solution.

18. The method as recited in claim 16 , wherein at least partially removing the elongated nanostructures comprises oxidizing the coating that at least partially coats the elongated nanostructures so that a plurality of stationary phase structures are formed and oxidizing the elongated nanostructures so that the elongated nanostructures are substantially removed.

19. The method as recited in claim 16 , wherein each of the first and at least a second portions of the catalyst layer form a zigzag pattern.

Assignments (4)
RELEASE OF SECURITY INTEREST IN PATENTS Recorded Jul 17, 2025
From: JPMORGAN CHASE BANK, N.A.
To: CHAMPIONX LLC; APERGY ESP SYSTEMS, LLC; APERGY BMCS ACQUISITION CORP; HARBISON-FISCHER, INC.; NORRIS RODS, INC.,; NORRIS RODS, INC.,; NORRISEAL-WELLMARK, INC.; PCS FERGUSON, INC.; QUARTZDYNE, INC.; US SYNTHETIC CORPORATION
Reel/Frame 072004/0019 →
SECURITY AGREEMENT Recorded Nov 6, 2019
From: APERGY ESP SYSTEMS, LLC; APERGY BMCS ACQUISITION CORP.; PCS FERGUSON, INC.; QUARTZDYNE, INC.; THETA OILFIELD SERVICES, INC.; US SYNTHETIC CORPORATION; WINDROCK, INC.
To: JPMORGAN CHASE BANK, N.A.
Reel/Frame 050941/0695 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 25, 2015
From: SONG, JUN
To: BRIGHAM YOUNG UNIVERSITY
Reel/Frame 036410/0628 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 19, 2011
From: LINFORD, MATTHEW R.; DAVIS, ROBERT C.; VANFLEET, RICHARD R.; JENSEN, DAVID SCOTT; YANG, LI
To: BRIGHAM YOUNG UNIVERSITY
Reel/Frame 026151/0193 →