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 splitter for a pressurized primary flowstream of a mobile phase is provided. The splitter comprises a first splitting stage that divides the primary flowstream between a major split flowstream and a minor split flowstream by means of a first and a second restrictive flow element; a first dilution stage that combines a dilution flow source with the minor split flowstream to create a diluted minor flowstream; a second splitting stage that divides the diluted minor flowstream between a secondary major diluted flowstream and a secondary minor diluted flowstream by means of a third restrictive element in the secondary minor diluted flow stream; and a second dilution stage wherein a conditioning flow source conditions the secondary minor diluted flow stream after the third restrictive element prior to outlet of the secondary minor diluted flowstream from the splitter.
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:
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.
摘要:
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.
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:
Methods and apparatus for collecting gasses from the sample headspace of a sealed sample container are disclosed. The gasses in the sample headspace are withdrawn by inserting a probe into the sample headspace and permitting the gasses to flow into an external headspace. The probe is then disconnected from the sample to seal the external headspace and the external headspace is then connected to an analytical instrument such as a gas chromatograph to permit the sample gasses to be transferred out of the external headspace and into the instrument. The step of transferring the gasses is preferably accomplished by connecting a source of carrier gas to an inlet port of the external headspace and sweeping the sample gasses from the external headspace. In certain preferred embodiments of the present invention, vibration is used to promote the formation of sample gasses either by vibrating the sample container itself or by moving the sample container relative to a stop to vibrate a septum which seals the sample container in certain embodiments. In these embodiments, the agitation created by such vibrations increases the rate of outgassing from the sample to the sample headspace. Also, in certain embodiments, the external headspace includes a flexible portion that is vibrated to agitate the external headspace and thereby promote uniform dispersion of sample gasses throughout the headspace.
摘要:
A device and process for separating liquid and gas phases in a flowstream containing a liquefied gas or supercritical fluid under pressure mixed with a liquid. A splitter vessel separates the liquid from gas phases and transfers liquid to a collection container while conducting the gas phase out of the splitter. Separation of liquid phase out of the flowstream is provided without additional pressure schemes or solvent extractions imposed on the stream.
摘要:
A device and process for separating liquid and gas phases in a flowstream containing a liquefied gas or supercritical fluid under pressure mixed with a liquid. A splitter vessel separates the liquid from gas phases and transfers liquid to a collection container while conducting the gas phase out of the splitter. Separation of liquid phase out of the flowstream is provided without additional pressure schemes or solvent extractions imposed on the stream.
摘要:
A depressurization process for a packed separation column is provided where the column system experiences a rapid and/or severe drop in pressure that could potentially damage column components. The process provides a safe de-pressurization of the column on the outlet side by decreasing the outlet pressure in controlled steps while allowing the inlet pressure of the column time to lower after each decreased step.