Volumetric flow regulation in multi-dimensional liquid analysis systems

Patent metadata

Field	Value
Publication number	US-9683975-B2
Application number	US-201514620924-A
Country	US
Kind code	B2
Filing date	Feb 12, 2015
Priority date	Feb 12, 2014
Publication date	Jun 20, 2017
Grant date	Jun 20, 2017

Abstract

A multi-dimensional liquid analysis system includes a first dimension system and a second dimension system, wherein outflow from the first dimension system is separated at a flow splitter under controlled conditions. The flow splitter separates the first dimension outflow into first and second split outlet flows, with one of the split outlet flows being metered to a designated flow rate with a flow metering device disposed downstream from the flow splitter. The flow metering device selectively closes or opens an outlet flow path to define a volumetric flow rate along that outlet flow path, so that the other split outlet flow is correspondingly controlled.

First claim

What is claimed is:

1. A multi-dimensional liquid analysis system, comprising:
a first dimension analysis system including a first separation column for chromatographically separating a liquid mobile phase into a first dimension outflow having a first dimension outflow rate;
a flow splitter for separating said first dimension outflow into a first split outlet flow and a second split outlet flow having a first pressure;
a second dimension analysis system including a second separation column for chromatographically separating said second split outlet flow into a second dimension outflow, and an injection valve for directing samples from said second split outlet flow into said second separation column, said injection valve having an inlet port for receiving said second split outlet flow, an outlet port, and first and second discrete sample loops comprising flow channels alternately positionable into fluid communication with said second split outlet flow or said second separation column; and
a flow metering device for receiving said second split outlet flow from said outlet port of said injection valve along an outlet flow path, said flow metering device comprising a valve for selectively closing or opening said outlet flow path in response to a control signal from a metering controller that is programmed to permit said second split outlet flow from said flow splitter at a predetermined second split outlet flow rate, as determined by a volume of said second split outlet flow permitted through said flow metering device along said outlet flow path within a designated period of time, said valve having:
(i) a stator having a stator face, a first inlet stator passage extending along said outlet flow path through said stator and opening to said stator face through a first stator port, a first discharge passage extending along said outlet flow path through said stator and opening to said stator face through a second stator port that is spaced from said first stator port, and a second discharge passage extending along a discharge path through said stator and opening to said stator face through a third stator port; and
(ii) a rotor having a rotor face in fluid-tight contact with said stator face at an interface, said rotor face including a shuttle configured to receive a liquid aliquot in fluid communication with said interface, wherein said rotor is rotatable with respect to said stator about an axis of rotation to sequentially move said shuttle into a plurality of circumaxially spaced stations, a first station aligning said shuttle in fluid communication with said outlet flow path at said first stator port, and a second station aligning said shuttle in fluid communication with said outlet flow path at said second stator port wherein said second and third stator ports are in fluid communication with each other at least when said shuttle is positioned at said second station.

2. A multi-dimensional liquid analysis system as in claim 1 , including a discharge means for discharging the liquid aliquot from said shuttle through said first discharge passage.

3. A multi-dimensional liquid analysis system as in claim 1 wherein said first and second sample loops each define respective first and second sample loop volumes that are each equal to or greater than an injection volume of said second split outlet flow needed for analysis by said second separation column.

4. A multi-dimensional liquid analysis system as in claim 1 wherein said first pressure is at least one kilopascal.

5. A multi-dimensional liquid analysis system as in claim 4 wherein said first pressure is between 1-10,000 kilopascals.

6. A multi-dimensional liquid analysis system as in claim 1 wherein said first sample flow channel is in fluid communication with said second separation column when said second sample flow channel is in fluid communication with said second split outlet flow.

7. A multi-dimensional liquid analysis system as in claim 1 wherein a first split outlet flow rate from said flow splitter is defined as the difference between said first dimension outflow rate and said second split outlet flow rate.

8. A method for analyzing a liquid sample, comprising:
(a) pumping the liquid sample with a first pump to a first dimension analysis system for identifying a chemical component of the liquid sample, said first dimension analysis system yielding a first dimension liquid outflow at a first dimension outflow rate;
(b) separating the first dimension liquid outflow into a first split outlet flow and a second split outlet flow having a first pressure of at least one kilopascal, wherein said second split outlet flow is motivated by said first pump;
(c) metering said second split outlet flow along an outlet flow path to a second split outlet flow rate by selectively closing or opening said outlet flow path with a flow metering device, wherein said flow metering device includes
(i) a stator having a stator face, a first inlet stator passage extending along said outlet flow path through said stator and opening to said stator face through a first stator port, a first discharge passage extending along said outlet flow path through said stator and opening to said stator face through a second stator port that is spaced from said first stator port, and a second discharge passage extending along a discharge path through said stator and opening to said stator face through a third stator port; and
(ii) a rotor having a shuttle configured to receive a liquid aliquot, said rotor being movable to correspondingly move said shuttle to a plurality of spaced apart stations, a first station aligning said shuttle to receive the liquid aliquot from said second split outlet flow along said outlet flow path, and a second station aligning said shuttle to discharge the liquid aliquot to said second split outlet flow along said outlet flow path, wherein said second and third stator ports are in fluid communication with each other at least when said shuttle is positioned at said second station; and
(d) directing said second split outlet flow through a second dimension analysis system having an analysis device for identifying a chemical component of the liquid sample, said second dimension analysis system including an injection valve having an inlet port for receiving said second split outlet flow, an outlet port, and first and second discrete sample loops comprising flow channels alternately positionable into fluid communication with said second split outlet flow or said analysis device, each of said first and second sample loops defining respective first and second sample loop volumes, wherein said second split outlet flow rate is sufficient to permit said second split outlet flow to fill a respective one of said first and second sample loop volumes within a designated time period that is the sum of an analysis time and an equilibration time of said analysis device.

9. A method as in claim 8 wherein said second split outlet flow is discontinuously connected at said flow metering device by said shuttle.

10. A method as in claim 8 wherein said outlet flow path is opened by positioning said shuttle at said first station.

11. A method as in claim 8 , including directing said second split outlet flow from said outlet port of said injection valve to said flow metering device.

12. A method as in claim 8 , including discharging the liquid aliquot from said shuttle by displacing the liquid aliquot with a gas.

13. A method as in claim 8 , including displacing the liquid aliquot from said shuttle under an applied vacuum pressure.

Assignees

• Idex Health & Science Llc

Inventors

• Sims Carl

Classifications

• G01N30/32 Primary

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

• G01N2030/207

  with metering cavity, e.g. sample loop · CPC title

• G01N30/20

  using a sampling valve · CPC title

• G01N2030/208

  with more than one cavity · CPC title

• B01D15/424

  Elution mode · CPC title