Hewlett-packard Company

Berger Instruments, Inc.

Agilent Technologies, Inc.

Hewlett-packard Corporation

Mettler-toledo Autochem, Inc.

Aurora Sfc Systems, Inc.

Terry A Berger

Kimber D Fogelman

Mark A Nickerson

L Thompson Staats, Iii

Paul F Bente, Iii

Kenneth Klein

Edwin E Wikfors

Samuel O Colgate

Michael Casale

Tak Kui Wang

William H Wilson

James W Baker

Paul Bente

Hans-Georg Haertl

L Thomson Staats, Iii

L Thompson Iii Staats

Thompson L Staats

Michael A Casale

An apparatus, process, and system are disclosed that effectively provide separation of a combined gas/liquid flow stream into its separated gas and liquid factions. The invention is primarily directed to the fields of preparative supercritical fluid chromatography (SFC) and supercritical fluid extraction (SFE), but will have other utilization and applicability where phases of dramatically different density, viscosity and volumetric flow require separation.

Self cleaning gas-liquid separator for serial or parallel collection of liquid fractions

Methods and systems for pumping compressible fluids in high pressure applications such as high-pressure liquid chromatography (HPLC) or supercritical fluid chromatography (SFC) applications are disclosed. An improved cooling device for a pump head for use in a supercritical fluid chromatography (SFC) system is described. A system for chilling a pumping system, includes a Peltier cooling element in thermal contact with a pump head, wherein the cooling element chills the pump head and a mobile phase fluid flowstream prior to the mobile phase fluid entering the pump; a fluid-cooled heat exchanger, attached to the Peltier cooling element, which removes heat from the cooling element using a circulating fluid; and a second heat exchanger which cools the circulating fluid.

Efficient chiller for a supercritical fluid chromatography pump

A system for chilling a pumping system includes a Peltier cooling element, and first and second heat exchangers. The Peltier element is arranged near a pump head of a pump such that the Peltier element and the pump head are in thermal contact, where the Peltier element chills the pump head and a mobile phase flowstream prior to fluid from the mobile phase flowstream entering the pump. The first heat exchanger is attached to the Peltier element, and removes heat from the Peltier element using a circulating fluid. The second heat exchanger cools the circulating fluid, where the Peltier element and the pump head are arranged in an area that is isolated from the second heat exchanger.

A drive mechanism for back pressure regulator used in liquid chromatography, supercritical fluid chromatography, or supercritical fluid extraction allows very fine automated control over a very wide range of pressures by combining a linear actuator compressing a spring, pushing a pin. The nozzle assembly of the regulator comprises a flow through chamber containing a diaphragm and a seat, in which the pin pushes the diaphragm against the seat, together with an upstream pressure sensor and electronic feedback control to the motor of the actuator. The BPR of the embodiments exhibits high pressure stability and extremely low pressure noise, even at moderate to high pressures. The exemplary BPR can be use at either constant pressure or to generate pressure programs where the pressure is varied versus time. Further, the nozzle assembly has a field-replaceable head, requiring no mechanical adjustment on replacement.

Low noise back pressure regulator for supercritical fluid chromatography

An apparatus, system, and process of converting a standard, high performance liquid chromatography (HPLC) flow path to a flow path suitable for supercritical fluid chromatography (SFC) are described. This reversible technique is applied to a variety of flow configurations including binary, high pressure solvent mixing systems and quaternary, low pressure solvent mixing systems than can be conventionally operated or automated. The technique is generally applied to the fields of supercritical fluid chromatography and high pressure liquid chromatography, but users skilled in the art will find utility for any flow system where pressurization components must be periodically applied to and removed from both ends of a flow stream in an automated manner.

Automated conversion between SFC and HPLC

A device includes a gas-liquid separator that receives and separates a biphasic pressurized flow stream and delivers flow to at least one exit port enriched in vapor phase composition and at least one exit port enriched in liquid phase composition. The device further includes a low restriction inlet conduit in communication with the separator exit port enriched in liquid phase composition, and a positive displacement pump having an inlet port in communication with the inlet conduit to receive flow from the gas-liquid separator and an outlet port in communication with an outlet conduit.

System and process for an active drain for gas-liquid separators

An invention is claimed that enables the pumping of compressible fluids at high pressures when an accurate flow is desired. Two pressure sources, for example pumps plumbed in series, separate thermodynamic work, such as pressurization, at the first pressure source from a volumetric or matter metering function in the second pressure source. One example is a flowstream delivery for a chemical instrumentation system that is manufactured from relatively unsophisticated pumps yet delivers precise flows with low pulsation (&#x3c;1%) over pressures greater than 100 bar. An advantage of one embodiment allows the economical conversion of typical HPLC systems to state of-the-art supercritical fluid chromatography (SFC) systems with minimal modification to system components.

Compressible fluid pumping system for dynamically compensating compressible fluids over large pressure ranges

The invention is a device and method in a high-pressure chromatography system, such as a supercritical fluid chromatography (SFC) system, that uses a pump as a pressure source for precision pumping of a compressible fluid. The preferred exemplary embodiment comprises a pressure regulation assembly installed downstream from a compressible fluid pump but prior to combining the compressible flow with a relatively incompressible modifier flow stream. The present invention allows the replacement of an high-grade SFC pump in the compressible fluid flow stream with an inexpensive and imprecise pump. The imprecise pump becomes capable of moving the compressible fluid flow stream in a precise flow rate and pattern. The assembly dampens the damaging effects of an imprecise pump, such as large pressure oscillations caused by flow ripples and noisy pressure signals that do not meet precise SFC pumping requirements.

Pump as a pressure source for supercritical fluid chromatography

A system for collection of liquid phase sample fractions from a supercritical fluid chromatography system is disclosed. The system has different ways of gathering the liquid phase into a collection chamber and provides for automated removal of liquid phase from a collection chamber into separate collection container. A separate pressure scheme is invoked upon the collection chambers to move liquid phase out of a chamber and into the separate collection container. In addition, the invention provides a renewal system for the collection chambers where each chamber returns to an uncontaminated stated by washing with a cleaning solution after removal of collected liquid phase. Spent cleaner from a chamber is purged using the pressure system into a waste stream for disposal.

Automated sample collection in supercritical fluid chromatography

A fractionated sample collection process and device having at least one pressurized chamber used to gather and store liquid samples generated from a flow stream containing a mixture of highly compressed gas, compressible liquid, or supercritical fluid and a relatively incompressible liquid. A bank of multiple collection chambers is secured together in a frame to form a cassette unit. Each collection chamber may house a replaceable liner such as a test tube vial, to hold a fractionated liquid phase sample. After filling with sample, a collection chamber is returned to a clean state and ready for refilling with a new sample by manually or automatically replacing the liner.

Apparatus and method for preparative supercritical fluid chromatography

Pump as a pressure source for supercritical fluid chromatography involving pressure regulators and a precision orifice

A process and device for chromatography, such as preparative and analytical supercritical fluid chromatography, or supercritical fluid extraction for a liquid phase SFC collection system that separates and retains eluted components from sample injections. The process efficiently separates liquid and gas phases in the flow stream upstream of a collection vessel and without additional pressure schemes or solvent extractions imposed on the flowstream. Sample fractions are collected from sample component concentration peaks based upon the chromatographic elution of the sample components. Samples are repeatedly the injected into the mobile phase flow stream and collected into large volume collection containers, thereby allowing longer unattended run times and cost-efficient sample purification and recovery.

Rapid sample collection in supercritical fluid chromatography

An improved method of introducing sample into a low-pressure flow stream of a high-pressure chromatography system to improve efficiency and significantly shorten the time of the separation process through a chromatography column is described. The method comprises injecting samples in a modifier liquid flow stream upstream of a mixing column that combines two independent flow streams of a liquid modifier with a highly compressed solvating fluid. Focusing can be controlled at the column head by changing the ratios of the two flow streams. Total flow may also be adjusted to speed the application of the sample onto the column during injection. The method improves the timing and efficiency of a supercritical fluid chromatography system and can reduce the amount of modifier added to the mobile phase flow stream.

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Newark, DE, United States of America

Terry A Berger