IP Library Granted Patent US 9,441,996
Granted Patent B2
US 9,441,996 · App. 14/511,636 · Granted Sep 13, 2016

Phase detection in multi-phase fluids

Inventors: Ryan Hill (Watertown, MA); Joshua A. Shreve (Franklin, MA); Robert Dumas (Upton, MA); Sylvain Cormier (Mendon, MA); Edwin Denecke (North Attleboro, MA); Kenneth R. Plant (Leominster, MA); Kurt D. Joudrey (Chelmsford, MA)
Assignee: WATERS TECHNOLOGIES CORPORATION
G01F1/74G01N21/41G01N30/74
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Quick Facts
Patent No.
US 9,441,996
App. No.
14/511,636
Granted
Sep 13, 2016
Kind
B2
Abstract

The present disclosure relates to phase detection in multi-phase fluids where two fluid phases can be present in the fluid. Phase detection apparatus and methods are disclosed for determining the phase(s) (e.g., supercritical, liquid, and/or gas) of a fluid in a multi-phase fluid system, such as carbon dioxide based separation and chromatography system.

Claims (31)

1. An apparatus for detecting the phase of a fluid in a multi-phase fluid system comprising:

a conduit defining a fluid flow path;

a circuit comprising an optical radiation source and a photo detector;

a housing fixing the relative position of the conduit and the circuit, the housing comprising a first aperture adjacent to the optical radiation source and a second aperture adjacent to the photo detector, wherein the first aperture is sized and shaped to filter optical radiation from the optical radiation source to the fluid flow path, wherein the second aperture is sized and shaped to filter the optical radiation from the fluid flow path to the photo detector, and wherein the circuit measures the refractive index of a fluid in the fluid flow path, thereby determining the phase of the fluid; and

a controller in communication with the fluid phase detector, the controller being capable of modulating at least one variable affecting the physical state of the fluid flow based upon the fluid phase detected by the fluid phase detector.

2. The apparatus of claim 1 , wherein the controller modulates at least one variable affecting the physical state of the fluid flow, to bias the fluid flow to the liquid state, when the fluid phase detector detects a gas or mixed gas-liquid phase in the fluid flow.

3. The apparatus of claim 1 , wherein the housing flexibly fixing the relative position of the conduit and the circuit, thereby preventing damage to the circuit while maintaining the relative position of the conduit and the circuit.

4. The apparatus of claim 1 , wherein the circuit delivers a signal change when the phase of the fluid changes between a gas, a liquid, or a mixed gas-liquid phase.

5. The apparatus of claim 1 , wherein the housing prevents rotation of the conduit, thereby preventing damage to the conduit.

6. The apparatus of claim 1 , wherein the conduit is substantially transparent to the optical radiation.

7. The apparatus of claim 1 , wherein the fluid comprises CO 2 .

8. The apparatus of claim 1 , wherein the optical radiation source comprises an IR diode and the photo detector comprises a photodiode.

9. The apparatus of claim 1 , wherein the first aperture is configured to prevent optical radiation that is not incident on the center of the fluid flow path from reaching the conduit.

10. The apparatus of claim 1 , wherein the second aperture is configured to prevent optical radiation that does not pass through the center of the fluid flow path from reaching the photo detector.

11. A separation system comprising:

a fluid flow source, a separation device in fluid communication with the fluid flow source, and a phase detection apparatus for detecting the phase of the fluid in at least one region of the separation system, wherein the phase detection apparatus comprises:

a conduit defining a fluid flow path,

a circuit comprising an optical radiation source and a photo detector, and

a housing fixing the relative position of the conduit and the circuit, the housing comprising a first aperture adjacent to the optical radiation source and a second aperture adjacent to the photo detector, wherein the first aperture is sized and shaped to filter optical radiation from the optical radiation source to the fluid flow path, wherein the second aperture is sized and shaped to filter the optical radiation from the fluid flow path to the photo detector, and wherein the circuit measures the refractive index of a fluid in the fluid flow path, thereby determining the phase of the fluid.

12. The system of claim 11 , wherein the phase detection apparatus is disposed upstream of the separation device.

13. The system of claim 11 , wherein the phase detection apparatus is disposed downstream of the separation device.

14. The system of claim 11 , wherein the separation device comprises supercritical fluid chromatography or supercritical phase extraction.

15. The system of claim 11 , wherein the phase detector apparatus is integrated between the fluid flow source and the separation device by fittings on each end of the conduit to minimize disruption of the fluid flow.

16. A method for detecting the phase of a fluid in a separation system, comprising:

flowing a fluid through a conduit defining a fluid flow path, wherein the conduit is fixed in a position relative to a circuit comprising an optical radiation source and a photo detector by a housing defining a first aperture and a second aperture;

directing optical radiation from the optical radiation source through the first aperture onto the fluid flow path;

directing the optical radiation from the fluid flow path through the second aperture onto the photo detector;

measuring the refractive index of a fluid in the fluid flow path, thereby determining the phase of the fluid; and

modulating at least one variable affecting the physical state of the fluid flow, to bias the fluid flow to the liquid state, when the fluid phase detector detects a gas or mixed gas-liquid phase in the fluid flow.

17. The method of claim 16 , wherein the fluid comprises CO 2 .

18. The method of claim 16 , further comprising performing a supercritical phase chromatography or separation on a sample.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 12, 2014
From: HILL, RYAN; SHREVE, JOSHUA; DUMAS, ROBERT; CORMIER, SYLVAIN; DENECKE, EDWIN; PLANT, KENNETH R.; JOUDREY, KURT D.
To: WATERS TECHNOLOGIES CORPORATION
Reel/Frame 034486/0302 →
Continuity (2)
Provisional Application 61889716 · Oct 11, 2013
Related Publication 20150101419A1 · Apr 16, 2015