Method and device for solvent evaporation from a liquid feed

Patent metadata

Field	Value
Publication number	US-9625427-B2
Application number	US-201314384943-A
Country	US
Kind code	B2
Filing date	Mar 12, 2013
Priority date	Mar 13, 2012
Publication date	Apr 18, 2017
Grant date	Apr 18, 2017

Abstract

The present invention relates to a device and an arrangement for selective solvent evaporation from a liquid feed, the feed comprising one or more components diluted in at least a first solvent or a solvent blend, comprising: a) a first tubular vessel having a distal end or a channel suitable for the formation of a droplet of a first volume, at an inflow rate n, at the tip or in the lumen of the tubular vessel, and b) means for subjecting the droplet to a solvent removal step at an evaporation rate r 2 to evaporate at least part of the first solvent or solvent blend, to accumulate the components in the feed in the droplet during the evaporation process at an accumulation rate r 3 , to obtain a concentrated feed volume in a concentrated droplet, wherein the evaporation and/or inflow rates are continuously adjusted to achieve a desired accumulation rate. The invention further relates to a method for selective solvent removal from an analyte mixture obtained in a chromatographic separation process.

First claim

The invention claimed is:

1. A device for selective solvent evaporation from a liquid feed, the feed comprising one or more components diluted in at least a first solvent or a solvent blend, comprising:
a) a first tubular vessel having a distal end or a channel suitable for the formation of a droplet of a first volume, at a rate of inflow rate r 1 , at the tip or in the lumen of the tubular vessel, and
b) means for subjecting the droplet to a solvent removal step at a solvent removal rate r 2 to evaporate at least part of the first solvent or solvent blend, to accumulate the components in the feed in the droplet during the evaporation process at a rate of accumulation r 3 , to obtain a concentrated feed volume in a concentrated droplet, wherein the evaporation and/or inflow rates are continuously adjusted to achieve a desired accumulation rate, and
means (c) to transfer the concentrated sample droplet into a second fluid to allow change of solvent composition and/or dilution and/or to allow transfer to another analysis method;
wherein at least one of r 1 , r 2 or r 3 are controlled by an automated system comprising a machine vision unit that sequentially acquires one or more images of the droplet, processes the acquired images to determine one or more droplet parameters; and communicates the parameters to a comparison means.

2. The device according to claim 1 , further comprising a means to determine at least two selected from the group consisting of r 1 , r 2 and r 3 .

3. The device according to claim 1 , wherein the device comprises at least one selected from the group consisting of; a means to adjust pressure, a means to adjust temperature and a means to adjust gas flow rate at the gas/liquid interface of the droplet.

4. The device according to claim 1 , wherein the automated system comprises at least one sensor, or at least one actuator or at least one sensor and at least one actuator.

5. The device according to claim 4 , wherein the comparison means correlates sensor data to a set point value, and delivers an adjustment signal to an actuator to adjust the magnitude of the parameter controlled by the actuator, wherein the actuator controls evaporation rate r 2 .

6. The device according to claim 1 , further comprising a means for dispensing the droplet from the distal end or within the capillary means.

7. The device according to claim 1 , further comprising a means to maintain the keeper solvent in a liquid phase during step b).

8. The device according to claim 7 , further comprising a means to add the keeper solvent to the first solvent or solvent blends, or to a sample droplet prior to, or during the evaporation process, or to both the first solvent or solvent blends and to a sample droplet prior to, or during the evaporation process.

9. An arrangement for the multi-dimensional separation of a liquid feed comprising one or more components, comprising:
i) at least a first separation device for the separation of compounds in the sample diluted in a first solvent or solvent blend in a first dimension into a first liquid feed comprising one or more components; and
ii) a device according to claim 1 , for selective solvent evaporation from the first liquid feed to obtain one or more concentrated droplets, and optionally
iii) at least a second separation device for the separation of the components in the concentrated sample droplets in a second dimension; and optionally
iv) a device for analyzing the components in the concentrated droplets.

10. The arrangement according to claim 9 , wherein the device for analyzing the compounds in the concentrated droplets comprises a physical, biochemical and/or chemical analysis tool.

11. The arrangement of claim 9 , further comprising a means to add a keeper solvent to the first solvent or solvent blends, and/or to a sample droplet prior to or during the evaporation process.

12. A process for the selective solvent removal from a liquid feed comprising one or more components diluted in at least a first solvent or a solvent blend, comprising the steps of:
a) forming an amount of the feed derived from a first separation device into a droplet with a first defined volume at the distal end or within a tubular vessel at a defined rate of inflow r 1 at the tip of the capillary or in the channel, and
b) subjecting the droplet to a solvent removal step to remove at least part of the solvent or solvent blend at a defined rate of solvent removal r 2 to remove at least part of the first solvent or solvent blend, and accumulation of components in the sample in the droplet during the solvent removal process at a rate of the accumulation r 3 , to obtain a concentrated feed droplet,

wherein rates r 1 and r 2 depend on the rate of accumulation r 3 , and
c) rediluting the concentrated droplet in a second solvent or solvent blend;
wherein the defined droplet surface area is monitored by machine vision.

13. The process according to claim 12 , wherein the droplet has a defined volume with a first defined surface area.

14. The process according to claim 12 , wherein the loss of solvent through evaporation is equal or higher to the amount of fluid sample added to the droplet through the capillary vessel.

15. The process according to claim 12 , wherein the defined droplet volume is kept constant.

16. The process according to claim 12 , wherein the concentrated droplet or a re-dissolved or re-diluted sample droplet is dispensed from the tubular vessel.

17. The process according to claim 12 , further subjecting the re-dissolved or re-diluted sample to a second separation process.

18. A process for the selective solvent removal from a liquid feed comprising one or more components diluted in at least a first solvent or a solvent blend, comprising the steps of:
a) forming an amount of the feed derived from a first separation device into a droplet with a first defined volume at the distal end or within a tubular vessel at a defined rate of inflow r 1 at the tip of the capillary or in the channel, and
b) subjecting the droplet to a solvent removal step to remove at least part of the solvent or solvent blend at a defined rate of solvent removal r 2 to remove at least part of the first solvent or solvent blend, and accumulation of components in the sample in the droplet during the solvent removal process at a rate of the accumulation r 3 , to obtain a concentrated feed droplet, wherein the droplet comprises a keeper solvent;
wherein the keeper solvent is a solvent or solvent blend that will essentially not evaporate during the process step b), and wherein the keeper solvent is at least present in an amount sufficient to retain the components in the analyte samples in a liquid state, either dissolved, dispersed and/or suspended; during and after the evaporation process, thereby preventing the sample concentration process from going to dryness.

19. The process according to claim 18 , wherein the keeper solvent comprises one or more normally solid compounds, one or more normally liquid compounds, and/or one or more normally gaseous compounds, which are liquid under the process conditions.

20. The process according to claim 19 , wherein the normally liquid solvent is selected from carbonaceous compounds of low normal volatility, including ethylene glycol, glycerol, propylene glycol, DMF, DMSO, 1-hexanol, 1-octanol, hydrocarbons, preferably n-alkanes, more preferably octane, decane or tetradecane, waxes; silicone waxes and/or silicone oils.

21. The process according to claim

Assignees

• Univ Leiden

Inventors

• Hankemeier Thomas
• Schoonen Jan-Willem
• Van Der Linden Heiko Jan
• Vulto Paul

Classifications

• G01N1/4022

  by thermal techniques; Phase changes · CPC title

• G01N30/12 Primary

  by evaporation · CPC title

• G01N1/2273

  Atmospheric sampling · CPC title

• G01N2030/027

  Liquid chromatography · CPC title

• G01N2030/126

  evaporating sample · CPC title