Hewlett-packard Company

Berger Instruments, Inc.

Agilent Technologies, Inc.

Other

Mettler-toledo Autochem, Inc.

Mark A Nickerson

Terry A Berger

Kimber D Fogelman

L Thompson Staats, Iii

Paul F Bente, Iii

Kenneth Klein

John S Poole

Paul C Dryden

Ernest H Zerenner

Steven J Engel

Lenore R Frank

Lenore G Frank

Christopher M Wurm

Paul Bente

William E Barber

Frank Marsden Willis

Louis T Staats, Iii

W Dale Snyder

Clayton E Law

Michael S James

Frank J DeMonte

Christoper M Wurm

Rich White

Raymond J Bell

Dennis R Gere

Meliss A Powell

Thompson L Staats

A column for use in chromatography, the column having a tube with a bore that can contain a packing medium captured between two porous plugs positioned at opposite ends. End fittings are attached to the tube ends, the end fittings having a duct with a duct opening having a diameter at least as large as the diameter of the tube bore which it faces. The duct opening may be positioned within a recess in spaced apart relation to the porous plugs to prevent the end fitting from contacting the plug and burnishing its surface.

Chromatography column with large diameter end fitting openings

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

A method for converting a pump for use in a flow stream containing a mixture of highly compressed gas, compressible liquid or supercritical fluid wherein the pump delivers a compressible fluid against a back-pressure regulator which in turn delivers a controllable flow rate downstream of the regulator without performing variable compressibility compensation adjustments on the pump. By using a pressurized source of compressible fluid combined with isocratic conditions, the delivery pressure from the pump is controlled at a rate higher than the downstream gradient with the back-pressure regulator, and an inexpensive pump may be used in place of specialized, expensive pumps and compressibility compensation systems for use in stems operating at or near supercritical fluid levels of compressible fluids. Significant capital and operating laboratory costs are saved through a simpler and cheaper system for accurately delivering compressible fluids into mobile phase flow streams.

Converting a pump for use in supercritical fluid chromatography

An efficient and safe method and apparatus for collecting exhaust gasses in an open-air sample collection container in a supercritical fluid chromatography system is claimed. The invention uses a vacuum force to evacuate the gaseous phase and vapors separated from liquid mobile phase in a sample collection device. The invention is portable to use on a series of collection containers, such as test tubes or wells in a titration place. Embodiments are claimed for capture of gasses and vapors either internally or externally to a collection container. The invention removes the gasses from the collection container that are then safely vented to a waste collector, thereby creating a safer environment for the laboratory and properly removing and disposing potentially hazardous chemicals instead of venting these chemicals into the environment.

Exhaust gas collection system for supercritical fluid chromatography

A preferred sample introduction apparatus includes a wall that defines a channel, with the channel being configured to receive a sample and being adapted to engage in fluid communication with the separation column of a chromatographic apparatus. Preferably, a coating of semi-conductive material is arranged adjacent to at least a portion of the wall. Additionally, a heater controller is provided which electro-magnetically communicates with the coating. So configured, the coating, in response to receiving energy from the heater controller, increases in temperature, thereby increasing a temperature of the sample.

Sample introduction systems and methods

A method and apparatus for sample screening and sample preparation within a vessel sealed with a cap, the vessel having at least a portion of the inside surface coated with a stationary phase having an affinity for analytes of interest. A sample possibly containing such analytes is introduced into the vessel whereby the analytes of interest migrate out of the sample and into the stationary phase for detection by a screening device and for desorption.

Sample screening and preparation within a collection vessel

A method and apparatus for non-liquid solvent introduction of analyte into an analytical instrument and, more particularly, to a bonded liquid phase analyte trap with integral flow switching that may include a rapid solid-state heating and cooling device. The analyte trap includes a first wafer having a flow channel formed on its bottom side such that a second wafer attached to the bottom side of the first wafer encloses the flow channel and a stationary phase coating is chemically bonded to the walls of the flow channel to provide a mechanism for trapping analytes of interest.

Micromachined analyte trap for gas phase streams

Methods and apparatus for extracting an analyte from a sample using a field-portable extraction instrument. The preferred embodiment of the extraction instrument includes an extraction fluid source, a sample container, a valve element, a nozzle, and a collection trap vessel. The methods of the present invention include the steps of inserting the sample into the sample container, attaching the sample container to the instrument, and providing a quantity of pressurized extraction fluid from the pressurized extraction fluid source into the sample container to initiate the extraction process. Extraction is facilitated by directing the extraction fluid into the sample at a rapid flow rate such that the sample and extraction fluid are vigorously mixed and a sample/solvent mixture is created. The valve element is then operated to isolate the extraction fluid source and to fully close the sample container. As an optional step, heat may be applied to the closed sample container to create conditions for effecting supercritical fluid extraction. The valve element is then operated to direct a fluid/constituent mixture from the sample container section to the collection trap vessel. The analyte of interest that is present in the fluid/constituent mixture is thereby trapped.

Portable extraction instrument

Sample analysis in a portable analytical instrument, preferably in the form of a gas chromatograph, benefits from temperature control of one or more zones in the instrument by way of thermal energy developed from an energy reservoir. In a preferred embodiment, analytical instrument performs chromatographic analysis and the selected zone comprises a temperature-controlled thermal chamber, or oven (124) which includes a heating unit (118), a temperature sensor (128), and a cooling unit (130). A separation column column (118) is positioned within the oven (124). The energy reservoir comprises a first reservoir (125) of heating fluid in the form of a compressed light hydrocarbon, a second reservoir (126) of a compressed inert gas, or a combination thereof. A controlled temperature in the oven (124) resulting from the operation of the heating unit (118) and/or cooling unit (130) may be effected in response to a control signal generated by a computer (122). A sample mixture passing through the column (118) is thereby exposed to a desired temperature profile according to a selected program so that the sample (111) will separate into its components for subsequent detection by a detector (124).

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Landenberg, PA, United States of America

Mark A Nickerson