Freeze drying for gas chromatography stationary phase deposition

1. A process for introducing a chromatographic medium into a chromatography column, comprising:

contacting a column with a composition comprising a solvent and a chromatography medium, wherein said composition is in the liquid phase;

allowing the composition to solidify; and

removing at least a portion of the solvent by vacuum sublimation.

2. The process according to claim 1 , wherein the column is contacted with the composition at a first temperature, and the solvent is removed by vacuum sublimation at a second temperature.

3. The process according to claim 1 , wherein the chromatographic medium is chosen from bead packings, film coatings, and expanded polymeric structures.

4. The process according to claim 1 , wherein the solvent is chosen from maleic anhydride, dimethyl sulfone, cyclohexanol, p-dichlorobenzene, norcamphor, dimethyl formamide, 1-methyl-2-pyrrolidone, and succinonitrile.

5. The process according to claim 1 , wherein the chromatography column is a gas chromatography column.

6. The process according to claim 1 , wherein the column has a length ranging from 10 cm to 2 m, and a footprint ranging from 0.5 cm 2 to 2 cm 2 .

7. The process according to claim 6 , wherein the column is sealed with a cover layer by at least one of adhesion bonding, diffusion bonding, anodic bonding, welding, soldering, thermal fusion bonding, and deformation sealing.

8. The process according to claim 1 , wherein at least some structures of the column are etched into a wafer.

9. The process according to claim 8 , wherein said column is a gas chromatography column, and said wafer comprises a plurality of gas chromatography columns.

10. The process according to claim 1 , wherein the column is sealed prior to removal of the solvent by vacuum sublimation.

11. The process according to claim 1 , wherein the solvent is removed in a vacuum oven at a temperature below the melting point of the composition.

12. The process according to claim 1 , wherein the column is contacted with the composition by at least one of spin-coating a composition onto a wafer comprising the column, suctioning the composition into the column, spray-coating the composition onto a wafer comprising the column, and submerging a wafer comprising the column into the composition.

13. A process for filling an elongated groove with a chromatographic medium, wherein the elongated groove comprises part of an unassembled miniaturized chromatographic column, said process comprising:

exposing said elongated groove to a composition comprising a solvent and a chromatographic medium; and

removing at least a portion of the solvent from the elongated groove by vacuum sublimation.

14. The process according to claim 13 , wherein the groove is sealed prior to removing solvent from the groove by vacuum sublimation.

15. The process according to claim 14 , wherein the groove is sealed by at least one of adhesion bonding, diffusion bonding, and anodic bonding of a cover layer.

16. The process according to claim 13 , wherein the elongated groove is exposed to the composition by applying centrifugal forces to pack and retain the composition into the elongated groove.

17. The process according to claim 13 , wherein the elongated groove contains an input aperture, and said groove is filled by inserting the composition through the input aperture.

18. The process according to claim 17 , wherein the elongated groove contains an output aperture, and a vacuum is applied to the output aperture, such that the composition is suctioned from the input aperture.

19. The process according to claim 13 , wherein the elongated groove is exposed to the composition at a first temperature, and the solvent is removed by vacuum sublimation at a second temperature.

20. A process for deposition of a stationary phase in a microfabricated gas chromatography column, comprising:

combining the stationary phase with a solvent to form a composition, wherein the solvent is suitable for removal by vacuum distillation;

filling at least a portion of the microfabricated gas chromatography column with the composition; and

removing at least a portion of the solvent in the composition by vacuum sublimation.