Including Liquid Flow Diversion Patents (Class 210/659)
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Patent number: 5422007Abstract: An apparatus and process for fractionation of component mixtures by chromatography or adsorption on a simulated mobile bed comprising three, four or five zones is described. A compressed gas is injected as eluent (IE, IR) using a compressor or pump, the pressure being lower than the critical pressure of the gas. At any point in at least one zone and preferably at any point in at least two zones from the eluent injection point (IR), the gas has a compressibility coefficient substantially different to 1. A supercritical fluid or a subcritical liquid may equally be injected as the eluent. The pressure between each zone may be altered.Type: GrantFiled: December 27, 1993Date of Patent: June 6, 1995Assignee: Institut Francais du Petrole & SeparexInventors: Roger Nicoud, Michel Perrut, Gerard Hotier
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Patent number: 5413762Abstract: A device for the purification of synthetic oligonucleotides, characterized by comprising means for switching between purification with an affinity column which recognizes trityl groups, in cases where trityl groups are bonded, and purification with a disposable stepwise reverse phase chromatography column in cases where no trityl groups are bonded. The device makes it possible for any person to easily perform high-degree purification, simply by setting the synthesized oligonucleotides. Furthermore, it accomplishes both a method using an affinity column cartridge and a method for purification by HPLC.Type: GrantFiled: November 29, 1993Date of Patent: May 9, 1995Assignees: Hideyasu Hirano, Astec Co., Ltd.Inventors: Hideyasu Hirano, Takayuki Emura
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Patent number: 5403386Abstract: An improvement to a sample concentrator apparatus for extracting and concentrating trace organic components from an aqueous sample for subsequent analysis; and a method for concentrating trace organics.Type: GrantFiled: October 14, 1993Date of Patent: April 4, 1995Assignee: Rohm and Haas CompanyInventors: Ledelle Collier, Wayne A. Thompson, Jr.
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Patent number: 5397467Abstract: A liquid chromatography system has a reservoir for the mobile phase with a cap which provides for effective control of charging the reservoir with the mobile phase, sparging the mobile phase while it is in the reservoir, feeding the mobile phase to the chromatograph, returning the mobile phase to the reservoir after it has passed through the chromatograph, venting or vacuumization of the reservoir and providing for automatic release of overpressure within the reservoir, all while maintaining the sparged environment in the reservoir.Type: GrantFiled: August 12, 1993Date of Patent: March 14, 1995Assignee: Kontes Glass CompanyInventors: Ned R. Morgan, John C. Bonino
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Patent number: 5393434Abstract: A liquid chromatography system including a liquid pump having a pumping chamber, an inlet port, an outlet port, and a purge port, all communicating with the pumping chamber; a separation column; an outlet valve connected between the outlet port and the separation column and adapted to control liquid flow therebetween; a source of mobile phase; an inlet valve connected between the inlet port and the source and adapted to control liquid flow therebetween; and a purge valve connected to the purge port.Type: GrantFiled: November 22, 1993Date of Patent: February 28, 1995Assignee: Zymark CorporationInventors: Burleigh M. Hutchins, Raymond R. Dunlap, Timothy J. Conklin, Bruce A. Swanson, John Petracca, Louis Abrahams, Ronald A. Kimball
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Patent number: 5391299Abstract: The present invention provides a process for production of starch sugars, wherein starch is subjected to liquefaction and saccharification to prepare a mixture containing 10-50% by weight, based on the total solid content, of glucose and 30-50% by weight, also based on the total solid content, of maltose and the mixture is concentrated so as to have a total solid content of 40-70% by weight; and the resulting mixture is subjected to component separation using a chromatographic separator of simulated moving bed type capable of fractionating the mixture into at least three fractions, to produce a glucose fraction with a glucose purity of at least 97% by weight, a maltose fraction with a maltose purity of at least 80% by weight and a high-purity oligosaccharide fraction at a high efficiency in one operation.Type: GrantFiled: February 9, 1994Date of Patent: February 21, 1995Assignee: Organo CorporationInventors: Takayuki Masuda, Kuniaki Kawano, Isamu Miyawaki
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Patent number: 5387347Abstract: The invention disclosed is a method and apparatus for moving-bed or simulated-moving-bed continuous chromatographic separation, in which some solvent is removed from the elution liquid at a point between the two zones where fractionation takes place. The resulting product streams have higher recovery and purity than without such solvent removal.Type: GrantFiled: September 15, 1993Date of Patent: February 7, 1995Inventor: Ronald D. Rothchild
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Patent number: 5382294Abstract: The object of the present invention is to chromatographically separate the higher and lower molecular weight components of juices, liquors, syrups and/or molasses (e.g., inorganic-organic complexes and organic non-sugars), thereby permitting the lower molecular weight sugar and soluble salt-containing fraction(s) to be further processed into natural sweetener products.Type: GrantFiled: July 29, 1993Date of Patent: January 17, 1995Inventors: Nicholas T. Rimedio, Li Fu Chen
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Patent number: 5376277Abstract: An on-line multidimensional system which includes a liquid chromatograph having an on-line connection to a pyrolysis probe, which in turn has on-line connection to a gas chromatograph. Preferred applications use a size-exclusion chromatograph coupled to a pyrolysis probe coupled to a gas chromatograph to simultaneously produce composition as a function of molecular weight/size information for polymeric materials.Type: GrantFiled: May 28, 1993Date of Patent: December 27, 1994Assignee: The Dow Chemical CompanyInventors: Hernan J. Cortes, Curtis D. Pfeiffer, Steven J. Martin, Charles G. Smith, Gary L. Jewett
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Patent number: 5372721Abstract: A method is disclosed for determining the distribution according to size of particles which make up a noncontinuous phase dispersed within a matrix which is not completely soluble in an aqueous solution. The method involves dissolving the matrix containing the particles in an essentially nonaqueous liquid causing the particles to be suspended. The suspension is then eluted through a separating medium which sorts the particles according to size. A detector monitors the effluent from the separating medium and creates a record of the data. This record is then compared to data obtained from known standards in order to estimate the size distribution in the sample.Type: GrantFiled: October 19, 1993Date of Patent: December 13, 1994Assignee: The Dow Chemical CompanyInventors: Martin A. Langhorst, Joseph B. Henry
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Patent number: 5372716Abstract: The present invention is a collection system for use with supercritical fluid extraction. The system comprises a device for collecting analyte from a fluid having the same. There is also a restrictor for controlling flow of analyte to the collecting device. The restrictor converts the fluid with analyte from a first pressure to a second pressure. The second pressure is less than the first pressure. The first pressure is a supercritical pressure. The restrictor is in fluidic communication with the collecting device. There is also a device for deabsorbing the analyte from the collecting device. The deabsorbing device is in fluidic communication with the collecting device. The collection system also includes a chromatograph for analyzing the analyte. The chromatograph is in fluidic communication with the collecting device to receive deabsorbed analyte. The chromatograph is remote from the collecting device. The chromatograph can be either a gas chromatograph or a liquid chromatograph.Type: GrantFiled: August 13, 1992Date of Patent: December 13, 1994Assignee: Suprex CorporationInventors: Joseph M. Levy, Raymond K. Houck
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Patent number: 5363886Abstract: The invention also relates to a method of packing an analytical column with packing particles. The method comprises the steps of pressurizing a first reservoir having packing particles disposed therein, with a solvent until the density of the solvent equals the density of the particles and forms a slurry where the particles are suspended in the solvent. Then, there is the step of fluidically connecting the first reservoir to an analytical column at essentially the same pressure as the first pressure such that the slurry flows into a chamber of the analytical column.Type: GrantFiled: August 25, 1993Date of Patent: November 15, 1994Assignee: Suprex CorporationInventor: Mehdi Ashraf-Khorassani
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Patent number: 5346622Abstract: Methods of separating and classifying the relative amounts of two or more classes of hydrocarbon molecules in a sample are disclosed wherein an input stream comprising a mobile phase and the sample is injected into a chromatographic column, and an effluent stream exiting a chromatographic column is split into a first effluent stream and a second effluent stream. The mass of carbon in each of the classes of hydrocarbons in the first effluent stream is determined, preferably using a flame ionization detector, and the second effluent stream is directed through a variable restrictor, allowing the pressure and mass flow rate of the input stream to be independently controlled and improved results obtained. In a preferred embodiment the present invention also includes identifying the hydrocarbon molecules in the second effluent stream in order to verify the analysis or provide additional data, preferably by using an ultraviolet detector.Type: GrantFiled: March 4, 1993Date of Patent: September 13, 1994Assignee: Hewlett-Packard CompanyInventors: Matthew S. Klee, Mu Z. Wang
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Patent number: 5340475Abstract: An on-line supercritical fluid extraction multidimensional chromatographic system and method is described which provides a cell for extracting a target compound in a supercritical fluid, and a restrictor interface for trapping the extracted target compound while decompressing and venting the supercritical fluid. A pump and valve arrangement is provided to convey the trapped target compound through a micro LC column for separating (and detecting) constituents of interest from interfering species, and ultimately introducing constituent of interest into a gas chromatograph for analysis. The system is characterized as being "on-line" in that fluid communication is provided between all of the system components and the process is continuous. Similarly, the system is characterized as being "multidimensional" in that both liquid and gas chromatographic techniques can be employed in tandem to provide analysis, selectivity and sensitivity in the parts per billion range.Type: GrantFiled: March 10, 1993Date of Patent: August 23, 1994Assignee: The Dow Chemical CompanyInventors: Hernan J. Cortes, Robert M. Campbell
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Patent number: 5340404Abstract: D-Allose, a sweet non caloric sugar, is recovered from an aqueous solution containing at least on other monosaccharide by adsorptive separation using a calcium loaded ion exchange resin as the adsorbent.Type: GrantFiled: May 12, 1993Date of Patent: August 23, 1994Assignee: UOPInventor: Beth McCulloch
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Patent number: 5322627Abstract: A method and device are disclosed for performing supercritical fluid chromatography in packed columns of at least about 0.5 mm inside diameter. The column provides at least 50,000, preferably at least 100,000, theoretical plates with pressure drop across the column of at least 25 bar. The outlet pressure is controlled by the back pressure regulator. The column may comprise a plurality of individual columns in series. Separation is performed at a rate of at least 25 plates/min, preferably at least 100 plates/min.Type: GrantFiled: June 17, 1993Date of Patent: June 21, 1994Assignee: Hewlett-Packard CompanyInventors: Terry A. Berger, William H. Wilson
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Patent number: 5322626Abstract: Methods and apparatus for extracting sample components from complex matrices using supercritical fluid as the principal extracting solvent are disclosed. The invention takes advantage of the fact that the solvent power of a supercritical fluid is stepwise settable by the parameters of density, modifier concentration, and temperature. Accordingly, methods and apparatus for extracting a component from a sample using fluid flow system having a variable and controllable flow restriction are disclosed. The methods of the present invention comprise the steps of inserting the sample into the sample container section, inputting temperature, pressure, flow rate and extraction time set points. Flow rate is controlled and system pressure regulated by the variable flow restriction. The output stream from the extraction is then expanded through a nozzle and into a trap. In certain embodiments, the trap is filled with chemically active packing material.Type: GrantFiled: February 5, 1993Date of Patent: June 21, 1994Assignee: Hewlett-Packard CompanyInventors: Lenore R. Frank, Christopher M. Wurm, Paul C. Dryden, Steven J. Engel, Mark A. Nickerson, Ernest H. Zerenner
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Apparatus for coupled liquid chromatography and nuclear magnetic resonance spectroscopy measurements
Patent number: 5283036Abstract: Apparatus is provided for coupled liquid chromatography and nuclear magnetic resonance (NMR) spectroscopy measurements. The apparatus includes a liquid chromatograph, an intermediate storage device for intermediately storing of components of a probe eluent and an NMR spectrometer. Selected intermediately stored components are fed to an NMR measurement unit. The intermediate storing device includes a number of capillary tubes, which are switchable by an automatically controlled valve arrangement for selectively receiving and delivering desired eluent components.Type: GrantFiled: February 5, 1992Date of Patent: February 1, 1994Assignee: Bruker Analytische Messtechnik GmbHInventors: Martin Hofmann, Manfred Spraul -
Patent number: 5266205Abstract: A method of separating solute material from a polar fluid in a first polar fluid phase is provided. The method comprises combining a polar fluid, a second fluid that is a gas at standard temperature and pressure and has a critical density, and a surfactant. The solute material is dissolved in the polar fluid to define the first polar fluid phase. The combined polar and second fluids, surfactant, and solute material dissolved in the polar fluid is maintained under near critical or supercritical temperature and pressure conditions such that the density of the second fluid exceeds the critical density thereof. In this way, a reverse micelle system defining a reverse micelle solvent is formed which comprises a continuous phase in the second fluid and a plurality of reverse micelles dispersed in the continuous phase. The solute material is dissolved in the polar fluid and is in chemical equilibrium with the reverse micelles. The first polar fluid phase and the continuous phase are immiscible.Type: GrantFiled: July 1, 1992Date of Patent: November 30, 1993Assignee: Battelle Memorial InstituteInventors: John L. Fulton, Richard D. Smith
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Patent number: 5248426Abstract: A method of streamlining and lowering the cost of operation of ion chromatography as well as improving detection limits is disclosed. The apparatus includes chromatographic separating means through which a sample is eluted in an eluent solution including an electrolyte. The apparatus includes suppressor means having a chromatography effluent compartment means separated from a detector effluent compartment means by an ion exchange membrane, forming a chromatography effluent flow channel and a detector effluent channel, respectively. Electrode means are disposed in communication with both flow channels for passing an electric current transverse to the solution that is passing through them. The chromatography effluent flows through the chromatography effluent flow channel of the suppressor and through detector means which detects resolved ionic species therein.Type: GrantFiled: October 29, 1992Date of Patent: September 28, 1993Assignee: Dionex CorporationInventors: John R. Stillian, Victor M. Barreto, Keith A. Friedman, Steven B. Rabin, Mahmood Toofan
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Patent number: 5241998Abstract: The present invention is related to an apparatus for packing an analytical chromatography column having a first opening and a second opening with packing particles. The apparatus comprises means for providing solvent at a density essentially equal to the density of the packing particles. The providing means is in fluidic communication with the first opening of the column. The apparatus also comprises a first reservoir for containing the packing particles. The reservoir is in fluidic communication with the providing means such that solvent can mix with the particles in the first reservoir to form a slurry where the particles are suspended in the solvent and agglomeration of the packing particles is essentially absent when the slurry is introduced into the analytical chromatography column.Type: GrantFiled: October 30, 1991Date of Patent: September 7, 1993Assignee: Suprex CorporationInventor: Mehdi Ashraf-Khorassani
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Patent number: 5240604Abstract: An on-line multidimensional system which includes a liquid chromatograph having an on-line connection to a pyrolysis probe, which in turn has on-line connection to a gas chromatograph. Preferred applications use a size-exclusion chromatograph coupled to a pyrolysis probe coupled to a gas chromatograph to simultaneously produce composition as a function of molecular weight/size information for polymeric materials.Type: GrantFiled: November 25, 1992Date of Patent: August 31, 1993Assignee: The Dow Chemical CompanyInventors: Hernan J. Cortes, Curtis D. Pfeiffer, Steven J. Martin, Charles G. Smith, Gary L. Jewett
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Patent number: 5240603Abstract: Methods and apparatus for extracting sample components from complex matrices using supercritical fluid as the principal extracting solvent are disclosed. The invention takes advantage of the fact that the solvent power of a supercritical fluid is stepwise settable by the parameters of density, modifier concentration, and temperature. Accordingly, methods and apparatus for extracting a component from a sample using fluid flow system having a variable and controllable flow restriction are disclosed. The methods of the present invention comprise the steps of inserting the sample into the sample container section, inputting temperature, pressure, flow rate and extraction time set points. Flow rate is controlled and system pressure regulated by the variable flow restriction. The output stream from the extraction is then expanded through a nozzle and into a trap. In certain embodiments, the trap is filled with chemically active packing material.Type: GrantFiled: December 6, 1991Date of Patent: August 31, 1993Assignee: Hewlett-Packard CompanyInventors: Lenore R. Frank, Christopher M. Wurm, Paul C. Dryden, Steven J. Engel, Mark A. Nickerson, Ernest H. Zerenner
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Patent number: 5234599Abstract: An on-line multidimensional chromatographic system and method which couples a liquid chromatograph to a supercritical fluid chromatograph. The system includes an inlet column for depositing a fraction of interest eluting from the liquid chromatograph, an interface interposed between the inlet column and the supercritical fluid chromatograph for receiving and trapping an analyte from the deposited fraction on an impactor surface, and a valve arrangement for controlling fluid flow throughout the system. After the fraction of interest has been deposited in the inlet column, the liquid chromatograph solvent is removed from the inlet column, and then the deposited fraction is extracted from the inlet column in a supercritical fluid stream. The supercritical fluid stream is directed into the interface, where the analyte is trapped while the supercritical fluid is decompressed and vented.Type: GrantFiled: February 14, 1992Date of Patent: August 10, 1993Assignee: The Dow Chemical CompanyInventors: Hernan J. Cortes, Robert M. Campbell, R. Paul Himes, Curtis D. Pfeffer
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Patent number: 5223143Abstract: There is provided a process for efficient chromatographic separation of a plurality of components from a fluid feed containing the same, which process comprises repeating a cycle comprising the step (1) of substantially shutting off the internal fluid circulation at a position of endless, or continuous, circulatory system and withdrawing a fraction enriched with a component having a strong affinity for an adsorbent upstream of the shut-off position while feeding the fluid feed downstream of the shut-off position, and the step (2) of withdrawing a plurality of fractions enriched with the remaining components while feeding a fluid desorbent and circulating the internal fluid.Type: GrantFiled: June 12, 1992Date of Patent: June 29, 1993Assignee: Japan Organo Co., Ltd.Inventors: Takayuki Masuda, Tohru Sonobe, Kikuzo Kaneko, Fumihiko Matsuda
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Patent number: 5223435Abstract: Sequential degradation of peptides for sequencing purposes by successive cleavage of amino acids from one end of the peptide chain is performed in an adsorption column with flows of the degradation reagents and wash liquids passing through the column in both directions. Migration of the peptide in one direction is thereby compensated by a subsequent migration in the other, and loss of peptide from the column over repeated cleavages is avoided. In preferred embodiments, the column contains two serially arranged adsorbent zones with differing adsorption characteristics, and the directions of flow of the various system components through the column are selected with a view toward a difference in peptide partitioning between the stationary and mobile phases in one zone vs. the other. The result is that any migration of the peptide occurring at any stage of a given cycle of the procedure occurs at a greater rate toward the zone interface than away from it.Type: GrantFiled: October 25, 1991Date of Patent: June 29, 1993Assignee: Genetech, Inc.Inventor: William J. Kohr
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Patent number: 5198120Abstract: A process for chromatographic fractional separation of a ternary or more fluid feed into at least three fractions according to a simulated moving bed procedure in a system wherein the simulated moving bed packed with an adsorbent is provided with a circulatory channel having a shutoff position where the circulation of the system can be shut off, comprises step (1) of feeding fresh fluid feed into the system on the downstream side of the shutoff position while withdrawing a fraction(s) of a component(s) having a medium affinity for the adsorbent from an adsorption zone(s) located upstream of the shutoff position, which step (1) is repeated alternately with step (2) of separately withdrawing fractions of components fractionated into respective adsorption zones remaining after the step (1) by feeding a fluid desorbent into the system with sequentially shifting the position of feeding the fluid desorbent and the positions of withdrawing enriched fractions, corresponding to the migration of the respective adsorptiType: GrantFiled: December 18, 1990Date of Patent: March 30, 1993Assignee: Japan Organo Co., Ltd.Inventors: Takayuki Masuda, Tohru Sonobe, Fumihiko Matsuda, Masaharu Horie
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Patent number: 5183604Abstract: A method is disclosed for determining the distribution according to size of particles which make up a noncontinuous phase dispersed within a matrix which is not completely soluble in an aqueous solution. The method involves dissolving the matrix containing the particles in an essentially nonaqueous liquid causing the particles to be suspended. The suspension is then eluted through a separating medium which sorts the particles according to size. A detector monitors the effluent from the separating medium and creates a record of the data. This record is then compared to data obtained from known standards in order to estimate the size distribution in the sample.Type: GrantFiled: January 24, 1992Date of Patent: February 2, 1993Assignee: The Dow Chemical CompanyInventors: Martin A. Langhorst, Joseph B. Henry
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Patent number: 5180487Abstract: It is an object to provide a recycle chromatograph with supercritical fluid mobile phase for separating a sample into components by recycling a mobile phase which includes modifier solvent for the purpose of taking a desired component.It is structured in such a manner that a recycling pump (10), a column (14), a detector (16), and a three-way valve (18) are connected in a sequential order as described above to form a closed loop which acts as a recycle flow line. A back-pressure regulator (20) is connected to the remainder port (C) of this three-way valve (18), and a mobile phase supplying and pressurizing device (30, 38, 30A, 48) for supplying the mobile phase under a predetermined pressure is connected to a flow line between the three-way valve (18) and the recycling pump (10).By means of this mobile phase supplying and pressurizing device and the recycle closed loop, (the column pressure drop .DELTA.p)/(column plate number) can be reduced, whereupon the column effective plate number can be increased.Type: GrantFiled: June 17, 1991Date of Patent: January 19, 1993Assignee: Nihon Bunko Kogyo Kabushiki KaishaInventors: Muneo Saito, Yoshio Yamauchi
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Patent number: 5178767Abstract: A solenoid driven valve is disclosed which is adaptable for controlling the introduction of a high pressure fluid into a fluid trapping assembly having an absorption column topped with an annular orifice expansion nozzle. The valve has an inlet port to introduce high pressure fluid, an axially moving solenoid driven pin which engages means to restrict fluid flow into said column. A diaphragm is located within the valve to direct fluid into the column and which separates the fluid in a region of high pressure from ambient pressures.Type: GrantFiled: February 22, 1991Date of Patent: January 12, 1993Assignee: Hewlett-Packard CompanyInventors: Mark A. Nickerson, John S. Poole, Lenore G. R. Frank
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Patent number: 5160625Abstract: An apparatus for flow field flow (FFF) fractionation comprises: a porous hollow fiber (1) which extends longitudinally between end-fittings (2, 3) of a tube (4), one end of said fiber (1) being connected to a first pump (5) for pumping a first carrier liquid into said fiber (1) via a valve (9) for introducing a liquid sample to be fractionated, the other end of said fiber (1) being connected to a container for a second carrier liquid via a flow-through detector (11), for detecting fractions of said sample; a second pump (12) which is connected to the interspace between the tube (4) and the fiber (1) to pump out carrier fluid through the porous fiber wall; and a control unit (6) which is adapted to control said first pump (5) to have a flower flow rate than said second pump (12) during injection and relaxation of the sample, and a higher flow rate than said second pump (12) to elute the sample; and a method for FFF fractionation in a hollow fiber utilizing the steps of sample application, relaxation, flow restType: GrantFiled: December 6, 1991Date of Patent: November 3, 1992Assignee: Pharmacia LKB Biotechnology ABInventors: Jan A. Jonsson, Alf Carlshaf
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Patent number: 5156736Abstract: An apparatus and process for concentrating a selected component from a multi-component liquid using a sorbent bed having a preferential sorption rate for the selected component. The sorbent bed is enclosed in a single vessel and is operated in a simulated moving bed technique whereby the flow profile of the liquid is continually moved downwardly through the sorbent bed. Recirculation is continuous but variable and is accompanied by the injection of eluent and feedstock and the removal of extract and raffinate at preselected times, locations, and amounts as a function of the kinetics and voidage of the sorbent bed. Extract purity and operational efficiency of the sorbent bed are the result of this novel apparatus and process.Type: GrantFiled: May 7, 1991Date of Patent: October 20, 1992Inventor: Karlheinz W. R. Schoenrock
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Patent number: 5151178Abstract: A solenoid driven valve is disclosed which is adaptable for controlling the introduction of a high pressure fluid into a fluid trapping assembly having an absorption column topped with an annular orifice expansion nozzle. The valve has an inlet port to introduce high pressure fluid, an axially moving solenoid driven pin which engages means to restrict fluid flow into said column. A diaphragm is located within the valve to direct fluid into the column and which separates the fluid in a region of high pressure from ambient pressures.Type: GrantFiled: February 22, 1991Date of Patent: September 29, 1992Assignee: Hewlett-Packard CompanyInventors: Mark A. Nickerson, John S. Poole, Lenore G. R. Frank
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Patent number: 5149436Abstract: Chromatographic species are continuously separated by displacement chromatography using an apparatus that comprises an inlet distribution manifold, a particulate bed, and a plurality of collector receptacles. The particulate bed is moved with respect to the inlet distributor manifold and the collector receptacles.Type: GrantFiled: October 25, 1991Date of Patent: September 22, 1992Assignee: Union Oil Company of CaliforniaInventors: Vernon T. Taniguchi, Allen W. Doty
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Patent number: 5147538Abstract: A field-portable supercritical fluid extraction apparatus uses an SFE solvent delivery means, SFE solvent cooling means, and reciprocating high pressure liquid chromatography pump having a cooled pumphead. A solid matrix sample is contained within an extraction cell. The SFE solvent is preheated in the extraction cell oven before it is introduced into the extraction cell. After contact with the solid matrix the extraction effluent passes through a heated restriction tube before passing into a collection flask assembly having a collection solvent tube and a collection solvent condenser to condense collection solvent vapors entrained by escaping SFE solvent. The analytes are collected in the collection solvent. The SFE solvent cooling means, pumphead and collection solvent condenser are all cooled by the combination of a single stage thermoelectric device, liquid-cooled heat exchanger and convective heat sink.Type: GrantFiled: November 8, 1991Date of Patent: September 15, 1992Assignee: Electric Power Research Institute, Inc.Inventors: Bob W. Wright, Jonathan S. Fruchter
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Patent number: 5139681Abstract: An on-line multidimensional chromatographic system and method which couples a liquid chromatograph to a supercritical fluid chromatograph. The system includes an inlet column for depositing a fraction of interest eluting from the liquid chromatograph, an interface interposed between the inlet column and the supercritical fluid chromatograph for receiving and trapping an analyte from the deposited fraction on an impactor surface, and a valve arrangement for controlling fluid flow throughout the system. After the fraction of interest has been deposited in the inlet column, the liquid chromatograph solvent is removed from the inlet column, and then the deposited fraction is extracted from the inlet column in a supercritical fluid stream. The supercritical fluid stream is directed into the interface, where the analyte is trapped while the supercritical fluid is decompressed and vented.Type: GrantFiled: October 9, 1990Date of Patent: August 18, 1992Assignee: The Dow Chemical CompanyInventors: Hernan J. Cortes, Robert M. Campbell, R. Paul Himes, Curtis D. Pfeiffer
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Patent number: 5135718Abstract: A method for analyzing vanillylmandelic acid, homovanillic acid and creatinine by fast liquid chromatography, which includes a step of introducing a test solution containing vanillylmandelic acid, homovanillic acid and creatinine to a cation exchange resin column and separating creatinine from vanillylmandelic acid and homovanillic acid; a step of separating by a separation column vanillylmandelic acid and homovanillic acid in the test solution from which creatinine has been separated; and a step of detecting each component.Type: GrantFiled: March 11, 1991Date of Patent: August 4, 1992Assignee: Tosoh CorporationInventors: Seiji Kawaguchi, Hiroaki Takahashi, Yuji Saito
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Patent number: 5133869Abstract: Chromatographic species are continuously separated by either elution or displacement HPLC using an apparatus that comprises a stationary inlet distribution manifold, a stationary chromatographic bed, and mobile collector receptacles.Type: GrantFiled: October 4, 1991Date of Patent: July 28, 1992Assignee: Union Oil Company of CaliforniaInventors: Vernon T. Taniguchi, Paula J. Bosserman, Allen W. Doty
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Patent number: 5133859Abstract: Methods and apparatus for extracting sample components from complex matrices using supercritical carbon dioxide as the principal extracting solvent are disclosed. The present invention takes advantage of the fact that the solvent power of a supercritical fluid is stepwise settable by the parameters of density, modifier concentration, and temperature. Accordingly, methods and apparatus for extracting a component from a sample using flow system having a variable and controllable flow restriction are disclosed. The methods of the present invention comprise the steps of inserting the sample into the sample container section, inputting temperature, pressure, flow rate and extraction time setpoints. The flow rate is controlled and the system pressure regulated by the variable flow restriction.Type: GrantFiled: March 2, 1990Date of Patent: July 28, 1992Assignee: Hewlett-Packard CompanyInventors: Lenore R. Frank, Christopher M. Wurm, Paul C. Dryden, Steven J. Engel
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Patent number: 5126055Abstract: A process for separating optical isomers in a simulated moving bed system, which comprises introducing a solution containing an optical isomer mixture and a desorbing liquid into a packed bed containing an optical resolution packing therein and having front and rear ends thereof connected to each other endlessly via a fluid passage to circulate a fluid unidirectionally and at the same time drawing out a solution containing one of the separated isomers and another solution containing the other isomer from the packed bed, wherein a port 13 for introducing a desorbing liquid, a port 14 for drawing out a solution containing a strongly adsorbable optical isomer, i.e. an extract, a port 15 for introducing a solution containing a mixture of optical isomers, and a port 16 for drawing out a solution containing a weakly adsorbable optical isomer, i.e.Type: GrantFiled: August 21, 1991Date of Patent: June 30, 1992Assignee: Daicel Chemical Industries, Ltd.Inventors: Akira Yamashita, Fumihiko Shoji
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Patent number: 5124023Abstract: Fused polynuclear aromatic compounds (PNAs) are continuously removed from a recycle oil stream in a hydrocracking process. An adsorption bed removes the PNAs from the recycle oil, a desorbing reagent removes the PNAs from the bed, and a regenerating agent regenerates the bed, all steps being performed simultaneously and continuously.Type: GrantFiled: May 22, 1990Date of Patent: June 23, 1992Assignee: Union Oil Company of CaliforniaInventors: Paula J. Bosserman, Vernon T. Taniguchi
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Patent number: 5124042Abstract: A three step flow injection analysis method for determining the degree of neutralization of phenol in solution. The first step is to flow a stream of a carrier liquid, such as water, along one side of a two sided semipermeable membrane, such as a silicone rubber membrane. The second step is to flow a stream of water along the other side of the membrane to a detector, such as a flow through ultraviolet spectrometer, the detector being responsive to the concentration of the phenol in the flowing stream of water. The third step is to add a volume of the solution to the flowing stream of carrier liquid so that the solution is carried to the first side of the membrane where a portion of the phenol permeates across the membrane into the flowing stream of water to be detected by the detector, the degree of neutralization of the phenol in the solution being a function of the response of the detector. The results of the method are substantially unaffected by variations in the concentration of the phenol.Type: GrantFiled: August 1, 1991Date of Patent: June 23, 1992Assignee: The Dow Chemical CompanyInventors: Robert A. Bredeweg, Richard G. Melcher
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Patent number: 5122275Abstract: A method and apparatus for separation of an extract component from a raffinate component in a simulated moving bed chromatographic separation train system. The system includes a plurality of beds, packed with a sorbent material, connected to form a closed recycle loop. Inlets to the train are provided for a feed stream and a desorbent stream along with outlets for removal of a raffinate stream and an extract stream. Increased product throughput and yield are obtained by intermittantly introducing and withdrawing the various streams to the train while continuously recycling a portion of the fluid in the system.Type: GrantFiled: September 5, 1989Date of Patent: June 16, 1992Assignee: A. E. Staley Manufacturing CompanyInventor: John F. Rasche
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Patent number: 5102553Abstract: The flow rates through the individual compartments of the sorbent bed of a simulated moving bed are controlled in accordance with time variable functions in each step to maintain an improved steady state waveform for the process.Type: GrantFiled: April 1, 1991Date of Patent: April 7, 1992Assignee: The Amalgamated Sugar CompanyInventors: Michael M. Kearney, Kathleen L. Hieb
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Patent number: 5094741Abstract: Methods and apparatus for extracting sample components from complex matrices using supercritical fluid as the principal extracting solvent are disclosed. The invention takes advantage of the fact that the solvent power of a supercritical fluid is stepwise settable by the parameters of density, modifier concentration, and temperature. Accordingly, methods and apparatus for extracting a component from a sample using fluid flow system having a variable and controllable flow restriction are disclosed. The methods of the present invention comprise the steps of inserting the sample into the sample container section, inputting temperature, pressure, flow rate and extraction time set points. Flow rate is controlled and system pressure regulated by the variable flow restriction.Type: GrantFiled: May 18, 1990Date of Patent: March 10, 1992Assignee: Hewlett-Packard CompanyInventors: Lenore R. Frank, Christoper M. Wurm, Paul C. Dryden, Steven J. Engel, Mark A. Nickerson, Ernest Zerenner
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Patent number: 5093004Abstract: A description is given of a process and an apparatus for continuous separation in fluid phase of a mixture of at least three constituents into three fractions. A technique is used, known as the simulated countercurrent technique, in a separation column which is filled with sorbent and has 6 zones 6, 5, 4, 3, 2 and 1 which have different functions, and the following sequence of steps is carried out: strong solvent S.sub.2 is introduced, an extract E.sub.2 with strong solvent is removed, weak solvent S.sub.1 is introduced. The extract with weak solvent E.sub.1 is drawn off, the separating mixture is introduced, refined substance is drawn off with weak solvent R, rinsing solvent (S.sub.1) is introduced, a current Rcy is recycled alternatingly towards the feed of strong solvent S.sub.2 and then towards the feed of weak solvent S.sub.1. A current coming from zone 6 is sent alternatingly to an outlet for the extract with strong solvent E.sub.2, then towards the intake of the fifth zone.Type: GrantFiled: August 28, 1990Date of Patent: March 3, 1992Assignee: Institut Francais du PetroleInventors: Gerard Hotier, Jean-Michel Toussaint, Gabriel Terneuil, Daniel Lonchamp
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Patent number: 5089126Abstract: This invention provides an apparatus and method for the complete fractionation of submicron particles according to size by capillary hydrodynamic fractionation. This objective is achieved by using small diameter capillaries; introducing a minor fraction of a liquid dispersion of particles to be separated into at least one capillary fraction; passing the minor fraction through the capillary; and, at the exit of the capillary, diluting the minor fraction with the same liquid as is carrying the fractionated sample. These modifications in the flow patterns are essential to the use of capillaries with diameters smaller than 60 microns. This invention is especially adapted for rapid analytical separation of not only rigid colloidal particles but also of soft latexes.Type: GrantFiled: March 31, 1989Date of Patent: February 18, 1992Assignee: Lehigh UniversityInventors: Cesar A. Silebi, Jose D. Ramos
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Patent number: 5087360Abstract: A field-portable supercritical fluid extraction apparatus uses an SFE solvent delivery means, SFE solvent cooling means, and reciprocating high pressure liquid chromatography pump having a cooled pumphead. A solid matrix sample is contained within an extraction cell. The SFE solvent is preheated in the extraction cell oven before it is introduced into the extraction cell. After contact with the solid matrix the extraction effluent passes through a heated restriction tube before passing into a collection flask assembly having a collection solvent tube and a collection solvent condenser to condense collection solvent vapors entrained by escaping SFE solvent. The analytes are collected in the collection solvent. The SFE solvent cooling means, pumphead and collection solvent condenser are all cooled by the combination of a single stage thermoelectric device, liquid-cooled heat exchanger and convective heat sink.Type: GrantFiled: April 19, 1990Date of Patent: February 11, 1992Assignee: Electric Power Research Institute, Inc.Inventors: Bob W. Wright, Jonathan S. Fruchter
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Patent number: 5071547Abstract: The present invention involves a dual column chromatographic apparatus with column switching capability that is useful in any pressurized fluid chromatography system. The apparatus has at least a first and second chromatographic column, a detector, a fluid conveyance system having a multivalve arrangement, pressurizable fluid conduit assembly, and a controller.The columns are adapted for containing stationary phase or packing for separation of a multicomponent sample into one or more components. The multi-valve arrangement has a plurality of multi-port, multi-modal valves and can include an ingress-egress valve; a guard pre-column valve; detector isolation valve; a set of four, four-port, multi-modal valves; or a set of two four-port, multi-modal valves and one six-port, multi-modal valve or a first valve set and a second valve set. The two chromatographic columns, multi-valve arrangement, and detector are linked for pressurized fluid communication by the pressurized fluid conduit assembly.Type: GrantFiled: March 23, 1990Date of Patent: December 10, 1991Assignee: Separations Technology, Inc.Inventors: Frederick D. Cazer, Barry L. Scott, Garth E. Strobel
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Patent number: 5064539Abstract: In a method using a chromatographic separation apparatus consisting of plurality of unit packed beds each having a supply inlet/extraction outlet, wherein the apparatus is effectively divided into four zones; an adsorption zone, a refining zone, a desorption zone, and a concentration zone. A supply and extraction step is performed in which all of the fluid flowing out of the adsorption zone is extracted through the nonadsorbate fluid extraction outlet, and then a recycle step, in which no fluid is supplied to or extracted from the bed, is performed to move the concentration distributions in the bed to a desired position. As a result, the method requires fewer unit beds, and enables extraction of components of higher purity.Type: GrantFiled: October 31, 1990Date of Patent: November 12, 1991Assignee: Ryoka Techno Engineering & Construction Co.Inventors: Masatake Tanimura, Masao Tamura, Takashi Teshima