Introducing samples into supercritical fluid chromatography systems

Patent metadata

Field	Value
Publication number	US-9764251-B2
Application number	US-201314383239-A
Country	US
Kind code	B2
Filing date	Mar 5, 2013
Priority date	Mar 8, 2012
Publication date	Sep 19, 2017
Grant date	Sep 19, 2017

Abstract

A supercritical fluid chromatography system is provided with an injection valve subsystem for introducing a sample into a flow of mobile phase fluid. The injection valve subsystem includes an auxiliary valve and an inject valve. The operations of the auxiliary and inject valves are coordinated in such a manner as to reduce sample carry-over and system pressure perturbations occurring during sample injection.

First claim

What is claimed is:

1. A method comprising;
pressurizing a flow path connected to a separation column with a mobile phase fluid comprising liquefied CO 2 ; then
pressurizing fluidic tubing and a sample loop containing a sample with the mobile phase fluid; and then
establishing fluidic communication between the fluidic tubing and the separation column and thereby introducing the sample into the pressurized flow path;
wherein the flow path fluidically connects an auxiliary value and the separation column, and wherein the fluidic tubing fluidically connects the auxiliary valve and an inject value;
wherein the auxiliary valve comprises:
an auxiliary valve stator comprising a first plurality of stator ports; and
an auxiliary valve rotor comprising a first plurality of grooves wherein the auxiliary valve rotor is rotatable, relative to the auxiliary valve stator, between a plurality of discrete positions to form different fluidic passageways within the auxiliary valve;

wherein the inject valve comprises:
an inject valve stator comprising a second plurality of stator ports; and
an inject valve rotor comprising a second plurality of grooves, wherein the inject valve rotor is rotatable, relative to the inject valve stator, between a plurality of discrete positions to form different fluidic passageways within the inject valve;

wherein the respective position of the auxiliary valve rotor and the inject valve rotor are coordinated to form plurality of discrete configurations for performing the step of pressurizing the flow path, pressurizing the fluidic tubing and the sample loop, and establishing fluidic communication between the fluidic tubing and the separation column; and
wherein the step of establishing the fluidic communication between the fluidic tubing and the separation column is performed while the auxiliary valve rotor is in an inject position and the inject valve rotor is an inject position such that the mobile phase fluid flows from the one or more pumps to the auxiliary valve, then from the auxiliary valve to the inject vlave, and then back to the auxiliary valve, and then to the flow path.

2. The method claim 1 , further comprising venting the fluidic tubing and the sample loop to atmospheric pressure.

3. The method of claim 1 , further comprising venting the sample loop and the fluidic tubing to atmospheric pressure prior to pressurizing the fluidic tubing and the sample loop containing the sample.

4. The method of claim 1 , wherein the step of pressurizing the fluidic tubing and the sample loop is performed while the inject valve rotor is in an inject position which places the sample loop in fluidic communication with the fluidic tubing.

5. The method of claim 1 , wherein the step of pressurizing the fluidic tubing and the sample loop is performed while the auxiliary valve rotor is in a fill position which inhibits flow of the mobile phase fluid between the auxiliary valve and the column.

6. The method of claim 1 , wherein pressurizing the flow path comprises delivering the mobile phase fluid from one or more pumps to the separation column through the auxiliary valve.

7. The method of claim 6 , further comprising venting the sample loop and the fluidic tubing to atmospheric pressure prior to pressurizing the fluidic tubing and the sample loop containing the sample, wherein the venting step is performed while the mobile phase fluid is being delivered to the separation column.

8. The method of claim 1 , wherein the step of pressurizing the flow path is performed while the auxiliary valve rotor is in a load position which allows the mobile phase fluid to flow from one or more pumps to the separation column through the auxiliary valve.

9. The method of claim 8 , further comprising venting the sample loop and the fluidic tubing to atmospheric pressure while the auxiliary valve rotor is in the load position.

10. The method of claim 9 , wherein the step of venting the sample loop is performed while the inject valve rotor is in an inject position which places the sample loop in fluidic communication with the fluidic tubing.

11. An injection valve subsystem for introducing a sample into a mobile phase fluid flow in a supercritical fluid chromatography system, the subsystem comprising:
I) an auxiliary valve comprising:
A) an auxiliary valve stator comprising a first plurality of stator ports; and
B) an auxiliary valve rotor comprising a first plurality of grooves,

II) an inject valve comprising:
A) an inject valve stator comprising a second plurality of stator ports; and
B) an inject valve rotor comprising a second plurality of grooves,

III) a sample loop fluidically connected to the inject valve stator for receiving the sample to be introduced into the mobile phase fluid flow; and
IV) fluidic tubing fluidically connecting the auxiliary valve stator and the inject valve stator,
wherein the auxiliary valve rotor is rotatable, relative to the auxiliary valve stator, between a plurality of discrete positions to form different fluidic passageways within the auxiliary valve;
wherein the inject valve rotor is rotatable, relative to the inject valve stator, between a plurality of discrete positions to form different fluidic passageways within the inject valve, and
wherein the respective positions of the auxiliary valve rotor and the inject valve rotor are coordinated in such a manner as to allow the sample loop and the fluidic tubing to be pressurized to a high system pressure before they are placed in fluidic communication with a separation column fluidically connected to the auxiliary valve;
wherein the respective positions of the auxiliary valve rotor and the inject valve rotor are coordinated to provide;
a first configuration that allows the fluidic tubing and the sample loop to vent to atmospheric pressure via the auxiliary valve;
a second configuration that allows the sample loop to be loaded with the sample while the fluidic tubing vents to atmosphere;
a third configuration that allows first and second fluidic tubing and the sample loop to be pressurized via a flow of a mobile phase fluid one or more pumps connected to the auxiliary valve; and
a fourth configuration that allows the sample to be delivered from the sample loop to a separation column fluidically connected to the auxiliary valve.

12. A supercritical fluid chromatography (SFC) system comprising:
I) a separation column;
II) one or more pumps for delivering a flow of a mobile phase fluid comprising CO2 to the separation column; and
III) an injection valve subsystem according to claim 11 , in fluidic communication with the one or more pumps and the separation column, wherein the auxiliary valve stator is in fluidic communication with the one or more pumps and the separation column.

13. The injection valve subsystem of claim 11 , wherein the first plurality of ports comprises:
a first port fluidically connected to the first fluidic tubing;
a second port for venting to atmospheric pressure;
a third port for venting to atmospheric pressure;
a fourth port fluidically connected to the fluidic tubing;
a fifth port for fluidically connecting the auxiliary valve to a pump; and
a sixth port for fluidically connecting the auxiliary valve to a separation column; and
wherein the second plurality of ports comprises:
a seventh port fluidically connected to the sample loop;
an eighth port for fluidically connecting the inject valve to a metering syringe;
a ninth port for fluidically connecting the inject valve to a needle for aspirating the sample;
a tenth port fluidically connected to the seventh port via the sample loop;
an eleventh port fluidically connect

Assignees

• Waters Technologies Corp

Inventors

• Berg Emily J
• Shreve Joshua A
• Usowicz James E
• Wittmer Douglas P
• Lebeau Aaron

Classifications

• B01D15/40

  using supercritical fluid as mobile phase or eluent · CPC title

• G01N30/16

  Injection (G01N30/24 takes precedence) · CPC title

• B01D15/14 Primary

  relating to the introduction of the feed to the apparatus · CPC title

• G01N30/32

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

• G01N30/28

  Control of physical parameters of the fluid carrier · CPC title