Operation of an injector of a sample separation device

Inventors

Ortmann, Thomas • Seifried, Martin • Wouters, Sam • Spuling, Irina

Assignees

Agilent Technologies Inc

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Publication Number

US-12313607-B2

Patent

Publication Date

2025-05-27

Expiration Date


Abstract

A sample separation device includes a separation path and a control unit. The separation path is between a fluid drive and a sample separation unit, and is configured to inject a fluidic sample in an injector path into a mobile phase in the separation path driven by the fluid drive to the sample separation unit for chromatographically separating the fluidic sample. The control unit is configured to control blocking the injector path or at least a partial path thereof, generating an overpressure in the blocked injector path or the partial path thereof by a pressure source, and subsequently fluidically coupling the injector path or the partial path thereof to a region of lower pressure than the overpressure to generate an expansion stroke for releasing unwanted components from the injector path.

Core Innovation

The invention relates to a sample separation device configured for chromatographically separating a fluidic sample by injecting the fluidic sample in an injector path into a mobile phase in a separation path driven by a fluid drive to a sample separation unit. A control unit blocks the injector path or at least a partial path thereof, generates an overpressure in the blocked injector path or the partial path thereof by a pressure source, and subsequently fluidically couples the injector path or partial path to a region of lower pressure than the overpressure to generate an expansion stroke for releasing unwanted components.

The disclosed concept addresses unwanted components in the injector path, including components released during the expansion stroke. The region of lower pressure is lower than the generated overpressure and includes ambient pressure and a waste conduit. Unwanted components comprise one or more particles, one or more sample residues, and/or one or more bubbles.

The description further includes operating the sample separation device in method form, in which the injector path or at least a partial path is blocked, overpressure is generated by a pressure source, and the injector path or partial path is fluidically coupled to a region of lower pressure to generate an expansion stroke. In this operation, the injector path is rinsed to discharge unwanted components to the region of lower pressure simultaneously with and/or after generating the expansion stroke.

Claims Coverage

The partial content provides two independent claim families with the same core sequence: injecting a fluidic sample into a mobile phase, blocking an injector path, generating overpressure, and fluidically coupling to a lower-pressure region to generate an expansion stroke that releases unwanted components. The coverage also includes refinements for injection type, pressure selection, lower-pressure region, and rinsing behavior.

Expansion-stroke releasing from a blocked injector path via overpressure and lower-pressure coupling

The control unit blocks the injector path or at least a partial path thereof, generates an overpressure in the blocked injector path or the partial path thereof by a pressure source, and subsequently fluidically couples the injector path or the partial path thereof to a region of lower pressure than the overpressure to generate an expansion stroke for releasing unwanted components from the injector path.

Operating a sample separation device with overpressure-coupled expansion stroke cleanup

The method comprises providing a separation path between a fluid drive and a sample separation unit configured to inject a fluidic sample in an injector path into a mobile phase for chromatographically separating the fluidic sample, blocking the injector path or at least a partial path thereof, generating an overpressure in the blocked injector path or the partial path thereof by a pressure source, and subsequently fluidically coupling the injector path or the partial path thereof to a region of lower pressure than the overpressure to generate an expansion stroke for releasing unwanted components from the injector path.

Flow-through injection by connecting a sample reception volume into the separation path

The control unit controls flow-through injection by connecting a sample reception volume containing the fluidic sample into the separation path between the fluid drive and the sample separation unit.

Feed injection via connection at a fluidic T-point

The control unit controls feed injection such that the injector path connects to the separation path at a fluidic T-point to combine the fluidic sample with the mobile phase.

Overpressure selection using bar ranges

The control unit generates the overpressure at a pressure selected from 400–2000 bar or 700–1500 bar.

Lower-pressure region defined as ambient pressure

The region of lower pressure is at ambient pressure.

Unwanted components released from the injector path

The unwanted components comprise at least one of one or more particles, one or more sample residues, or one or more bubbles.

Waste conduit as the region of lower pressure

The region of lower pressure comprises a waste conduit.

Injector path rinsing tied to the expansion stroke

Simultaneously with and/or after generating the expansion stroke, the injector path is rinsed to discharge unwanted components to the region of lower pressure.

The claim set focuses on an injector-path cleanup mechanism in chromatographic HPLC separation: block the injector path, create overpressure, then couple to a lower-pressure region to generate an expansion stroke that releases unwanted components from the injector path. The coverage further specifies injection architectures, pressure constraints, definitions of the lower-pressure region, and optional rinsing behavior associated with the expansion stroke.

Stated Advantages

Enables releasing unwanted components from the injector path by generating an expansion stroke after blocking and overpressure generation.

Includes rinsing of the injector path to discharge unwanted components to the region of lower pressure simultaneously with and/or after generating the expansion stroke.

Reduces carryover via an injection/needle-seat architecture that enables backward rinsing of the needle seat using the analytical pump without a separate rinsing pump.

Documented Applications

Detecting and quantifying gas bubbles via compressibility measurements in an injector path before injection and performing expansion-stroke cleanup when gas is excessive.

Performing chromatographic separation by injecting a fluidic sample into a mobile phase in a separation path driven by a fluid drive to a sample separation unit, while releasing unwanted components from the injector path.

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