Methods for injecting samples in liquid chromatography, particularly in high performance liquid chromatography

Patent metadata

Field	Value
Publication number	US-10031112-B2
Application number	US-201715596738-A
Country	US
Kind code	B2
Filing date	May 16, 2017
Priority date	Jan 25, 2008
Publication date	Jul 24, 2018
Grant date	Jul 24, 2018

Abstract

A sample injection method for liquid chromatography is performed with an injection valve having a waste port, two sample loop ports, and two high-pressure ports. One high-pressure port can be connected to a pump and the other high-pressure port can be connected to a chromatography column. A sample loop is connected to one of the sample loop ports on one end and to a pump volume of a sample conveying device on the other end. A section of the sample loop can be separated to facilitate receiving a sample fluid in the sample loop. A control unit controls the injection valve and the sample conveying device. The sample injector allows a sample to be loaded into the sample loop and then pressurized to an operating pressure prior to injecting the sample into the chromatography column. The sample loop may also be isolated from the operating pressure for facilitating depressurization of the loop.

First claim

The invention claimed is:

1. A method of operating a liquid chromatography system, the liquid chromatography system comprising a liquid chromatography column and an injection valve, the method comprising:
isolating a sample loop of the liquid chromatography system from a high-pressure fluidic path in fluid communication with the liquid chromatography column, wherein the high-pressure fluidic path is at a pump pressure, wherein the sample loop is in fluid communication with the injection valve and the sample loop comprises a sample conveying device, and isolating the sample loop comprises placing the injection valve in a PRESSURE COMPENSATION position, wherein a volume of the sample conveying device is defined by a cavity in which a movable element is slidably mounted;
calculating a distance for a movement of the movable element within the cavity from a first position to a second position to increase a pressure in the sample loop from an essentially ambient pressure to the pump pressure based on one or more of a compressibility of a fluid in the sample loop, an elasticity of the sample loop, and the pump pressure; and
while the sample loop is isolated from the high-pressure fluidic path, decreasing the volume of the sample conveying device to increase the pressure in the sample loop from the essentially ambient pressure to essentially correspond to the pump pressure of the high-pressure fluidic path,
wherein decreasing the volume includes sliding the movable element within the cavity by the calculated distance from the first position to the second position.

2. The method of claim 1 , wherein at the PRESSURE COMPENSATION position,
(i) first and second sample loop ports of the injection valve are closed so as to facilitate a pressurization of the sample loop, and
(ii) first and second high-pressure ports of the injection valve are connected so as to operatively connect a high-pressure pump in fluid communication with the high-pressure fluidic path to the liquid chromatography column.

3. The method of claim 2 further comprising:
determining the compressibility of the fluid with the high-pressure pump.

4. The method of claim 1 , wherein placing the injection valve in the PRESSURE COMPENSATION position includes rotating a rotor of the injection valve with respect to a stator of the injection valve.

5. The method of claim 1 further comprising:
operating the injection valve to connect the sample loop to the high-pressure fluidic path such that the pump pressure from a high-pressure pump of the liquid chromatography system is applied to the sample loop, and a sample in the sample loop flows from the sample loop into the high-pressure fluidic path and to the chromatography column.

6. The method of claim 5 further comprising:
after operating the injection valve to connect the sample loop, introducing the sample into the chromatography column;
isolating the sample loop from the high-pressure fluidic path by placing the injection valve back in the pressure compensation position; and
increasing the volume of the sample conveying device to reduce the pressure in the sample loop from the pump pressure of the liquid chromatography column to the essentially ambient pressure.

7. The method of claim 1 , in which the compressibility of the fluid and the elasticity of the sample loop are stored in a control unit of the liquid chromatography system.

8. The method of claim 1 , in which the moveable element includes a plunger.

9. The method of claim 2 , in which the sample loop includes a first connecting piece and a second connecting piece, in which the first connecting piece is connected to the first sample loop port of the injection valve and to the sample conveying device, in which the second connecting piece is connected to the second sample loop port of the injection valve and to the sample conveying device, in which the second connecting piece includes an intake segment and a feed segment, in which the intake segment and the feed segment are configured to be separated.

10. A method of injecting a sample in a liquid chromatography system, the method comprising:
isolating a sample loop of the liquid chromatography system from a high-pressure fluidic path of the liquid chromatography system, the high-pressure fluidic path at a pump pressure in fluid communication with a liquid chromatography column of the liquid chromatography system, wherein the high-pressure fluidic path is at a pump pressure, wherein the sample loop comprises a sample conveying device, wherein a volume of the sample conveying device is defined by a cavity in which a movable element is slidably mounted;
calculating a distance for a movement of the movable element within the cavity from a first position to a second position to increase a pressure in the sample loop from an essentially ambient pressure to the pump pressure based on one or more of a compressibility of a fluid in the sample loop, an elasticity of the sample loop, and the pump pressure;
placing the sample in the sample loop;
with the sample placed in the sample loop and with the sample loop remaining isolated from the high-pressure fluidic path, decreasing the volume of the sample conveying device to increase the pressure in the sample loop from the essentially ambient pressure to essentially correspond to the pump pressure of the high-pressure fluidic path, wherein the movable element within the cavity is moved by the calculated distance from the first position to the second position; and
connecting the sample loop to the high-pressure fluidic path so that the pump pressure from a high-pressure pump is applied to the sample loop to cause the sample in the sample loop to flow from the sample loop through a portion of the high-pressure fluidic path to the chromatography column.

11. The method of claim 10 further including:
isolating the sample loop from the high-pressure fluidic path of the liquid chromatography system after the sample has flowed into the high-pressure fluidic path; and
(b) increasing the volume of the sample conveying device to reduce the pressure in the sample loop to the essentially ambient pressure.

12. The method of claim 10 wherein isolating the sample loop from the high-pressure loop includes placing an injection valve in a PRESSURE COMPENSATION position in which
first and second sample loop ports of the injection valve are closed so as to facilitate pressurization of the sample loop, and
first and second high-pressure ports of the injection valve are connected so as to operatively connect the high-pressure pump to the liquid chromatography column.

13. The method of claim 12 wherein placing the injection valve in the PRESSURE COMPENSATION position includes rotating a rotor of the injection valve with respect to a stator of the injection valve.

14. The method of claim 12 further comprising:
determining the compressibility of the fluid with the high-pressure pump.

15. The method of claim 12 , in which the sample loop includes a first connecting piece and a second connecting piece, in which the first connecting piece is connected to the first sample loop port of the injection valve and to the sample conveying device, in which the second connecting piece is connected to the second sample loop port of the injection valve and to the sample conveying device, in which the second connecting piece includes an intake segment and a feed segment, in which the intake segment and the feed segment are configured to be separated.

16. The method of claim 10 wherein the movable element is connected to a drive device which is operable to move the movable e

Assignees

• Dionex Softron Gmbh

Inventors

• Hochgraeber Hermann

Classifications

• G01N30/24

  Automatic injection systems · CPC title

• G01N30/32

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

• G01N30/20 Primary

  using a sampling valve · CPC title

• G01N2030/201

  multiport valves, i.e. having more than two ports · CPC title

• G01N35/1097

  characterised by the valves (valves in general F16K) · CPC title