摘要:
An improved method and apparatus for safely introducing sample into a flow stream of a supercritical fluid chromatography system is described. The sample injection method improves safety of injection by eliminating the risk of injecting sample into a high-pressure system containing liquids and gasses at or near supercritical ranges. The method improves the efficiency and significantly shortens the time of the injection process by using a check valve placed between a fill port on an injection valve and sample port where sample is injected by a syringe. After sample injection from a sample loop into a high-pressure flow stream, an injection valve is reset to receive a subsequent sample. High-pressure flow stream mixtures become trapped within the sample loop when the valve is reset. The check valve prevents the mixtures from expanding into the sample port and blowing out a syringe and flow stream mixtures from the fill lines. The trapped flow stream mixtures are directed to a waste port where they are safely contained. The technique can be applied equally as effective to preparatory SFC as well as to analytical SFC systems.
摘要:
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.
摘要:
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.
摘要:
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.
摘要:
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.
摘要:
In a system for analyzing a chemical sample by chromatographic separation of said sample into components a method and apparatus are provided for heating the mobile phase to a desired temperature prior to exiting the restrictor, while maintaining the density of the mobile phase at a desired level. Such heating and density maintenance being provided by the combination of a restrictor having a minimal taper length and a temperature zone immediately prior to the outlet end of the restrictor, which temperature zone has a minimum length. A second temperature zone spaced upstream from the first zone, and an intermediate thermally conductive member between the first and second zones can be provided as an alternative embodiment for establishing a thermal gradient. As the mobile phase passes through the second zone, the intermediate conductive member, and the first zone, the mobile phase is subjected to a thermal gradient.
摘要:
In a system for analyzing a chemical sample by chromatographic separation of said sample into components a method and apparatus are provided for maximizing detector resolution and minimizing duration by maintaining the linear velocity of the mobile phase at a desired level by affecting the viscosity and density characteristics of the mobile phase as it passes through a restrictor by programming the restrictor temperature.
摘要:
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.
摘要:
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.
摘要:
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.