System and method for monitoring phase-separation and mutual miscibility of fluid mixtures

Patent metadata

Field	Value
Publication number	US-11604174-B2
Application number	US-201916684930-A
Country	US
Kind code	B2
Filing date	Nov 15, 2019
Priority date	Nov 16, 2018
Publication date	Mar 14, 2023
Grant date	Mar 14, 2023

Abstract

Exemplary embodiments are directed to methods and systems for controlling fluid parameters within a detector. A first and second fluid pump manager control the flow of a first and second fluid to one or more heating/cooling devices, and a mixer receives and mixes the first and second fluids. An optical detector flow cell receives the fluid mixture from the mixer, and a pressure regulator controls the pressure at the optical detector flow cell. Thus, the composition, temperature, and pressure of a fluid mixture entering an optical detector flow cell can be controlled in real time.

First claim

The invention claimed is:

1. A system for controlling fluid parameters within a detector comprising:
a first fluid pump manager configured to control a flow of a first fluid;
a second fluid pump manager configured to control a flow of a second fluid;
a fluid heating/cooling device configured to receive the first fluid from the first fluid pump manager and receive the second fluid from the second fluid pump manager;
a mixer configured to receive the first fluid and the second fluid from the fluid heating/cooling device;
an optical detector flow cell configured to receive a fluid mixture directly from the mixer, wherein the optical detector flow cell is connected with the mixer through a conduit without any intervening structures comprising a chromatographic separation column between the mixer and the optical detector flow cell; and
a pressure regulator located downstream of the optical detector flow cell and configured to actively control a pressure at the optical detector flow cell, wherein the first fluid pump manager and the second fluid pump manager are programmed to actively adjust a proportion of the first fluid and the second fluid directed to the mixer in real time.

2. The system of claim 1 , wherein the first fluid pump manager includes at least two fluid pumps and is programmed to direct specified proportions of at least two fluids to the fluid heating/cooling device via a second mixer.

3. The system of claim 1 , wherein the second fluid pump manager includes at least two fluid pumps and is programmed to direct specified proportions of at least two fluids to the fluid heating/cooling device via a third mixer.

4. The system of claim 1 , wherein the first fluid pump manager or the second fluid pump manager is configured to direct compressed CO 2 to the fluid heating/cooling device.

5. The system of claim 1 , wherein the fluid heating/cooling device includes a separate first and second fluid heating/cooling device located downstream of the first fluid pump manager and the second fluid pump manager, respectively, the system further comprising:
a third fluid heating/cooling device located downstream of the mixer configured to control a temperature of the fluid mixture prior to entering the optical detector flow cell.

6. The system of claim 5 , wherein the third fluid heating/cooling device comprises a heat exchanger.

7. The system of claim 1 , wherein the optical detector flow cell is a component of a UV-vis detector utilizing a wavelength selected based on a scattering efficiency through immiscible fluids and a scattering or absorption of light through miscible fluids.

8. The system of claim 1 , further comprising:
a controller configured to control the operation of the first pump manager, the second pump manager, the first and second fluid heating/cooling devices, and the pressure regulator in order to measure the miscibility of various fluid compositions in real time under different temperature and pressure conditions.

9. The system of claim 1 , wherein the fluid heating/cooling device comprises a heat exchanger.

10. The system of claim 1 , wherein the fluid heating/cooling device comprises an oven or a preheater.

11. A method for controlling fluid parameters within a detector comprising:
controlling a flow of a first fluid to a first preheater using a first fluid pump manager;
controlling a flow of a second fluid to a second preheater using a second fluid pump manager;
heating the first fluid and the second fluid to a specified temperature using the first and second preheaters, respectively;
receiving the first fluid and the second fluid at a mixer located downstream of the first and second preheaters;
directing a fluid mixture from the mixer directly to an optical detector flow cell, wherein the optical detector flow cell is connected with the mixer through a conduit without any intervening structures comprising a chromatographic separation column between the mixer and the optical detector flow cell; and
actively controlling a pressure at the optical detector flow cell using a pressure regulator wherein controlling the flow of the first fluid and controlling the flow of the second fluid include actively adjusting a proportion of the first fluid and the second fluid directed to the mixer in real time.

12. The method of claim 11 , wherein the first fluid pump manager includes at least two fluid pumps and is programmed to direct specified proportions of at least two fluids to the first preheater via a second mixer.

13. The method of claim 11 , wherein the second fluid pump manager includes at least two fluid pumps and is programmed to direct specified proportions of at least two fluids to the second preheater via a third mixer.

14. The method of claim 11 , wherein the first fluid pump manager or the second fluid pump manager is configured to direct compressed CO 2 to the first or second preheater.

15. The method of claim 11 , further comprising:
controlling a temperature of the fluid mixture prior to entering the optical detector flow cell using a third preheater located downstream of the mixer and upstream of the optical detector flow cell.

16. The method of claim 11 , wherein the optical detector flow cell is a component of a UV-vis detector utilizing a wavelength selected based on a scattering efficiency through immiscible fluids and a scattering or absorption of light through miscible fluids.

17. The method of claim 11 , further comprising:
controlling the operation of the first pump manager, the second pump manager, the first and second preheaters, and the pressure regulator; and measuring the miscibility of various fluid compositions in real time under different temperature and pressure conditions.

18. A system for monitoring miscibility and phase separation of fluid mixtures comprising:
a first fluid pump manager configured to control a flow of a first fluid;
a second fluid pump manager configured to control a flow of a second fluid;
a first preheater configured to receive the first fluid from the first fluid pump manager and heat the first fluid to a predetermined temperature;
a second preheater configured to receive the second fluid from the second fluid pump manager and heat the second fluid to a predetermined temperature;
a mixer configured to receive the first fluid and the second fluid from the preheater and create a fluid mixture;
an optical detector flow cell configured to receive the fluid mixture directly from the mixer, wherein the optical detector flow cell is connected with the mixer through a conduit without any intervening structures comprising a chromatographic separation column between the mixer and the optical detector flow cell;
a pressure regulator located downstream of the optical detector flow cell and configured to actively control a pressure at the optical detector flow cell; and
a controller configured to control operation of the first fluid pump manager, the second fluid pump manager, the first preheater, the second preheater, and the pressure regulator in order to control a temperature, pressure, and composition of the fluid mixture within the optical detector flow cell, wherein the first fluid pump manager and the second fluid pump manager are programmed to actively adjust a proportion of the first fluid and the second fluid directed to the mixer in real time.

Assignees

• Waters Technologies Corp

Inventors

• Tarafder Abhijit
• Besner Sebastien
• Basile Mark
• Gilar Martin

Classifications

• G01N30/74 Primary

  Optical detectors {(measurement of intensity, velocity, spectral content, polarisation, or phase of infrared, visible or ultraviolet light G01J)} · CPC title

• G01N30/34

  of fluid composition, e.g. gradient (G01N30/36 takes precedence) · CPC title

• G01N2030/347

  mixers · CPC title

• G01N21/33 Primary

  using ultraviolet light (G01N21/39 takes precedence) · CPC title

• G01N30/32

  of pressure or speed (G01N30/36 takes precedence) · CPC title