Montmorillonite-based liquid chromatography column

Patent metadata

Field	Value
Publication number	US-2020246777-A1
Application number	US-201916267348-A
Country	US
Kind code	A1
Filing date	Feb 4, 2019
Priority date	Feb 4, 2019
Publication date	Aug 6, 2020
Grant date	—

Abstract

The montmorillonite-based liquid chromatography column is a chromatography column, which may be steel, packed with unmodified montmorillonite for use in normal phase liquid chromatography, particularly high-performance liquid chromatography (HPLC). The column may be prepared by sieving montmorillonite to achieve a desired particle size range, preferably in the micrometer range, i.e., montmorillonite microparticles, and more preferably between 5-10 μm. The montmorillonite microparticles are suspended in a solvent, for example, ethanol, and packed into a column for use in HPLC. Before packing, the montmorillonite microparticles may be dried by, for example, heating for a period of time, e.g., by heating preferably at about 100° C. for at least 2 hours. The packing may be performed at a pressure of at least 5000 psi, and more preferably, between 5000-7000 psi. The column may be used for separation of simple polar compounds under relatively low pressure conditions.

First claim

1 . A montmorillonite-based liquid chromatography column, comprising a high-performance liquid chromatography (HPLC) column packed with a stationary phase of montmorillonite, the montmorillonite being preheated before packing to remove water from silicon layers, wherein the montmorillonite stationary phase column has:
i) a uniform particle distribution size between 5 μm and 10 μm; ii) a BET surface area of 339 m 2 /g; iii) packing performed at a pressure of 5,000 psi; and iv) a back-pressure less than 500 psi at 25° C.-70° C. at flow rates ranging from 0.1 to 1.0 mL/min.

2 - 5 . (canceled)

6 . The montmorillonite-based liquid chromatography column according to claim 1 , wherein the HPLC column packed with the montmorillonite comprises a stainless steel column.

7 . A method of making a montmorillonite-based liquid chromatography column, comprising the steps of:
sieving raw montmorillonite to obtain a uniform distribution of micron-sized montmorillonite particles; drying the sieved montmorillonite; suspending the dried montmorillonite in a solvent to form a suspension; and packing a high-performance liquid chromatography column with the suspension of sieved montmorillonite to form a montmorillonite stationary phase in the column.

8 . The method of making a montmorillonite-based liquid chromatography column according to claim 7 , wherein the micron-sized montmorillonite particles have an average particle size between 5 μm and 10 μm.

9 . The method of making a montmorillonite-based liquid chromatography column according to claim 7 , wherein said step of drying the sieved montmorillonite comprises heating the sieved montmorillonite in an oven at 100° C. for two hours.

10 . The method of making a montmorillonite-based liquid chromatography column according to claim 7 , wherein the solvent is ethanol, the sieved montmorillonite being sonicated in the ethanol solvent for 10 minutes to form the suspension.

11 . The method of making a montmorillonite-based liquid chromatography column according to claim 7 , wherein the packing is performed at a pressure of 5,000 psi for 10 minutes.

12 . The method of making a montmorillonite-based liquid chromatography column according to claim 7 , wherein the high-performance liquid chromatography column comprises a stainless steel column.

Assignees

• Univ King Saud

Inventors

• Aqel Ahmad Ifseisi
• Ahmed Ayman Abdelghafar
• Badjah-Hadj-Ahmed Ahmed-Yacine
• Alothman Zeid Abdullah

Classifications

• B01J20/3092

  Packing of a container, e.g. packing a cartridge or column (of chromatography columns B01D15/206) · CPC title

• B01J20/3085

  Chemical treatments not covered by groups B01J20/3007 - B01J20/3078 · CPC title

• B01J20/3078

  Thermal treatment, e.g. calcining or pyrolizing · CPC title

• B01J20/30

  Processes for preparing, regenerating, or reactivating · CPC title

• B01J20/28011

  Other properties, e.g. density, crush strength · CPC title