Abstract: To stabilize flow rate in a single-stroke, syringe-type high pressure pump to a constant value after turn-on, a control system; (1) in one embodiment, senses the maximum rate of change of pressure, detects a pressure when the rate of change is two-thirds of the maximum, increases the pump rate until the pressure is three times that at the value of the detected pressure and begins pumping at the preset constant flow rate; and (2) in another embodiment operates a pump system at a flow rate ten times the preset flow rate and, when the time derivative of the pressure has dropped to nine tenths of its maximum, the pump motor speed is reduced to the preset flow rate.

Abstract: 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.

Abstract: An active material is disclosed which comprises a metal oxide/hydroxide surface having chemically bonded to reactive sites thereon a substantially monomolecular layer of organic acid molecules. Each organic acid molecule is chemically bonded to a reactive site on the oxide/hydroxide surface through a phosphorus-containing acid group selected from the group consisting of a phosphonic acid group and a phosphinic acid group. Each organic acid molecule also comprises an unreacted acid group oriented away from the metal oxide/hydroxide surface and selected from the class consisting of a phosphonic acid group, a phosphinic acid group, a sulfonic acid group, and a carboxylic acid group.

Abstract: An equilibrated percent solids waveform is established in a simulated moving bed process. A contraction phase of the waveform is monitored as it rotates through a circulation loop including a plurality of resin bed compartments. The contraction phase is followed by a desorbent phase. A slurry of resin is added to each compartment between the contraction and desorbent phases.

Abstract: There is disclosed herein an apparatus and method for performing liquid chromatography analysis with a stable baseline. The apparatus utilizes positive displacement means on each of two flow paths and a control system to regulate the flow such that the flow in both flow paths is identical. Only one flow path has sample injected therein. Each flow path is passed through a separate liquid chromatography column and a common detector at the output end of each column. Since flow path contains solvent only and the flow path contains both solvent and sample, any changes in the characteristics of the output streams of the liquid chromatography columns caused by changes in the solvent composition itself have a common mode. Therefore, only the difference signal is output from the detector which indicates changes in the characteristics of the output stream of the sample flow path caused solely by the presence of the sample components.

Abstract: A chromatographic separation process employing fewer beds packed with an adsorbent, while enabling separation of feedstock fluid, containing a plurality of components which have different degrees of affinity for the adsorbent, into constituent fractions which are withdrawn separately. According to at least one preferred embodiment, a step of supplying feedstock fluid to the simplified separation apparatus is preceded and followed by a step of circulating the fluid through the apparatus, a cycle of supply-desorbing-circulation being carried out repeatedly.

Abstract: A high pressure liquid chromatography jacket includes a rectangular, fluid-tight enclosure which has a removable cover on which a pair of tubing seal fittings are mounted. The fittings form a fluid-tight seal around the inlet and discharge tubes of a chromatographic column which is mounted in the enclosure. The enclosure is connected to a source of temperature controlled fluid which circulates through the enclosure and controls the temperature of the chromatographic column.In an alternative embodiment of the invention, a valve is provided which allows sample materials being loaded to enter a sample storage loop, which is exposed to the temperature controlled fluid. The sample, whose temperature has been controlled by the temperature controlled fluid, is then injected into a chromatographic column under high pressure.

Abstract: A chiral two-phase system for resolution of racemic mixtures, or for separation of diastereomers, is disclosed. The system comprises two immiscible liquid phases and one or more enantioselectively binding chiral components, each of which is substantially in one of said phases.Also disclosed is a method for chiral resolution of racemic mixtures, or for separation of diastereomers. Use is here made of the fact that different enantiomers are partitioned differently between the phases in the above-mentioned two-phase system in that one of the enantiomers is selectively bound to one of the chiral components which is substantially in one of said phases.

Abstract: A method and apparatus for determining, by use of ion chromatography, a microconstituent contained in a major constituent as impurities present in the major constituent. The invention causes only that portion of the effluent from the detector, shown on an ion chromatograph, that corresponds to the neighborhood of the microconstituent to be led again to the collecting valve. Thus, the microconstituent of the solution can be determined quickly and easily, without reference to the kind of microconstituent being tested.

Abstract: Ion chromatograms are prepared with a chromatograph including a separation column and a conductivity measuring ion detection unit which are adapted to be selectively placed in communication with separate reservoirs for diluted and undiluted samples of a fluid to be analyzed. A control unit switches the reservoirs into communication with an eluent pump for displacing fluid samples through the detection unit in timed relationship such that the most concentrated ion is measured in the diluted sample prior to measurement by the detection unit of the last of the lesser concentrated ions. A pump having a controllable flow rate is connected to a mixing conduit through control valves which switch the flow to and from the reservoirs so that the reservoirs may be simultaneously filled with diluted and undiluted samples of fluid. The diluted sample may be prepared by mixing the undiluted fluid with the eluent.

Abstract: A stable baseline is achieved in a gradient ion chromatographic analysis by adding a nonionic modifier to the electrolytic eluent. The addition of the modifier may occur at any point upstream of the detector. The nonionic modifier has the effect of shifting the equilibrium of unsuppressed effluent electrolyte towards it nonionic form. For example, the addition of the nonionic modifier shifts both bicarbonate and carbonate towards the nonionic, nonconductive carbonic acid form.

Abstract: 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.

Abstract: A chromatographic method for the determination of individual phenols in water by adding a halogenating agent to the water, e.g., using the bromate-bromide reaction to generate tribromide ions which react with the phenols to form bromo-derivatives of the phenols, then to permeate the bromo-derivatives across a membrane, e.g., a silicone rubber membrane, into a liquid extractant, e.g., a dilute aqueous solution of sodium hydroxide and acetonitrile, and then determining the permeated bromo-derivatives in the liquid extractant by chromatography, e.g., by injecting the liquid extractant containing the permeated bromo-derivatives into a reverse phase liquid chromatographic system.

Abstract: A process for readily isolating and recovering highly pure erythritol at a high crystallization yield from an erythritol-containing culture medium, which contains erythritol together with various impurities such as salts, coloring materials and polysaccharides, through chromatographic separation with the use of a strongly acidic cation exchange resin. The process of the present invention can be continuously operated, since the lowered separation capability of said cation exchange resin can be readily restored by treating the same with a warm alkali solution.

Abstract: Disclosed is a chromatographic trapping assembly suitable for use with supercritical fluids. The apparatus includes means suitable for electronic control of the expansion of pressurized fluid through an orifice into a fluid trapping assembly using an axially movable column to regulate fluid through the orifice.

Abstract: A device for monitoring the release of a substance from a substrate, e.g., the release of ions through membranes, are disclosed.

Abstract: To prevent the solvents forming a gradient from mixing at the wrong place and to provide for accurate composition at start of the gradient in spite of solvent pressure variations, a microliquid or supercritical fluid chromatograph includes a combined mixer and pressure detector in which equal pressures of the two solvents in the gradient are detected by displacement of a ferromagnetic poppet in the mixing chamber. The poppet serves as a stop for the final solvent until the pressures are substantially equal and then its movement is detected by a circuit related to a linear variable differential transformer. The signal energizes a circuit which drives one of the sensing coils to drive the poppet during the gradient to provide mixing.

Abstract: To stablize flow rate in a single-stroke, syringe-type high pressure pump to a constant value after turn-on, a control system: (1) in one embodiment, the control system senses the maximum rate of change of pressure, detects a pressure when the rate of change is two-thirds of the maximum, increases the pump rate until the pressure is three times that at the value of the detected pressure and begins pumping at the preset constant flow rate and (2) in another embodiment, operates a pump system at a flow rate ten times the preset flow rate and, when the time derivative of the pressure has dropped to nine tenths of its maximum, the pump motor speed is reduced to the preset flow rate.

Abstract: Disclosed is a method of separating organic or organometallic materials under supercritical fluid conditions, the method comprising the steps of providing a bed of packing material selected from a metal oxide/hydroxide support material having phsophorous-containing organic molecules bonded to reactive sites on said support material, alumina and alumina-containing mixtures. The materials are introduced to the bed and a fluid is added to the bed under supercritical fluid conditions. The fluid removes one of the materials from the bed.

Abstract: Ion chromatograms are prepared with a chromatograph including a separation column and a conductivity measuring ion detection unit which are adapted to be selectively placed in communication with separate reservoirs for diluted and undiluted samples of a fluid to be analyzed. A control unit switches the reservoirs into communication with an eluent pump for displacing fluid samples through the detection unit in timed relationship such that the most concentrated ion is measured in the diluted sample prior to measurement by the detection unit of the last of the lesser concentrated ions. A pump having a controllable flow rate is connected to a mixing conduit through control valves which switch the flow to and from the reservoirs so that the reservoirs may be simultaneously filled with diluted and undiluted samples of fluid. The diluted sample may be prepared by mixing the undiluted fluid with the eluent.

Abstract: The invention is a method of group type separation of whole oils and bitumen by high performance liquid chromatography into fractions of asphaltenes, resins, aromatics, and saturated hydrocarbons. A multistep process is involved wherein the oil is initially solvated with a three part solvent mixture of methanol, acetone, and choroform. The solvated oil mixture is injected with a mobile phase into a cyano bonded phase column which will retain asphaltenes and resins, and pass through aromatics and saturated hydrocarbons. The unretained aromatics and saturated hydrocarbons are then injected into a silica column which will retain aromatics and pass through saturated hydrocarbons. Saturated hydrocarbons are recovered as they pass through the silica column. The resins, asphaltenes, and aromatics are recovered from the columns by a displacement material.

Abstract: A process and an apparatus for separating industrially a large amount of a biopolymer-containing sample by ion-exchange type column chromatography using the gradient elution method, wherein at least two precursor liquids for a mobile phase from liquid baths 3a and 3b are introduced into a mixing device 14 while the flow rate thereof is controlled over a wide range to obtain a mobile phase liquid. The mobile phase liquid thus obtained is introduced into the columns 1a and 1b so that the sample is separated in the columns and the biopolymer is collected in a fraction collector 6. The columns 1a and 1b are alternately regenerated.

Abstract: A system for chromatography using horizontal (radial) flow columns is disclosed. The system provides rapid separation of complex biological or organic mixtures at low operating pressures. The system may be used in a variety of applications, such as in the analysis of the constituents of a mixture, or in large pilot or plant scale operations where the isolation of one or more purified components of a mixture or fluid is required for further testing or for commercial purposes. The system is designed to accommodate separation via a variety of routes including ion-exchange, affinity, hydrophobic, chiral, hydroxylapatite, reverse phased as well as rapid desalting techniques.

Abstract: A plurality of analytes are analyzed by liquid chromatography in a liquid biological sample containing many components which can interfere with analysis by liquid chromatography. The sample, containing the analytes of interest, are passed to a first passage of a dialyzer which removes molecules in the sample which interfere with analysis. A diluent is passed through a second passage of the dialyzer in which the two liquids are separated from each other by a semipermeable membrane having holes large enough to permit the analytes of interest to pass into the diluent but holes small enough to prevent passage of sample components which interfere with analysis. The analyte-containing diluent is passed to a retaining element for temporarily retaining the analytes of interest by adsorption and/or partition. The analytes of interest are removed from the retaining element by a second diluent which is then passed through a chromatography column with a detector and the analytes are analyzed chromatographically.

Abstract: This invention concerns analysis by high performance liquid chromatography HPLC) of crude oils and petroleum products.In one embodiment of the invention a sample is quantitatively separated into saturates, alkyl benzenes and polynuclear aromatics using a system comprising a column packed with a porous silica packing material having a polar amino-cyano bonded phase in tandem with a column packed with a tetranitrofluorenimino packing material, and a dielectric constant detector.In another embodiment of the invention a sample is qualitatively separated into saturates, olefins, and total aromatics using a system employing an olefin-selective column and a dielectric constant detector.

Abstract: Disclosed is a method of separating organic or organometallic materials under supercritical fluid conditions, the method comprising the steps of providing a bed of packing material selected from a metal oxide/hydroxide support material having phosphorous-containing organic molecules bonded to reactive sites on said support material, alumina and alumina-containing mixtures. The materials are introduced to the bed and a fluid is added to the bed under supercritical fluid conditions. The fluid removes one of the materials from the bed.

Abstract: In one embodiment of the invention supercritical fluid chromatographic separation may be accomplished by apparatus which includes a column, an oven for maintaining the temperature of a sample in the oven, an injector for delivering a sample containing fluid to the column and a pump for delivering carrier fluid to the injector. A discharge outlet for receiving processed fluid from the column contains one or two restrictors and a nozzle for discharge of processed fluid. The pump also delivers fluid which is the carrier fluid not containing the sample to a position in the pressure control inlet so as to alter the linear velocity of the sample containing fluid through the column. A controller controls operation of the oven and pump. A valve and a transducer may be positioned in the line between the pump and the discharge outlet in order to permit adjustment of the pressure of the unprocessed carrier fluid being introduced into the discharge outlet by the controller.

Abstract: A method and apparatus for supplying a preset amount of sample solution to a liquid chromatographic column wherein (1) a first piston, which moves along the axis of a piston container sealingly contacting the side walls of said piston container, is moved a preset distance so as to draw a fixed amount of driving solution from the driving solution chamber of a piston cylinder into the piston container, thus displacing a second piston which moves along the axis of said piston cylinder sealingly contacting the side walls of said piston cylinder and dividing said piston cylinder into a sample solution chamber and a driving solution chamber, said displacement of said second piston serving to cause sample solution to be drawn from a sample solution reservoir into the sample solution chamber of the piston cylinder in a fixed amount equal to the fixed amount of driving solution drawn into the piston container; and (2) driving solution is pumped into said driving solution chamber in order to displace said second piston

Abstract: Desired components can be simply and economically separated and recovered from a sample solution having a complicated composition through a liquid chromatography by passing the sample solution through a separation column, thereby separating components contained therein in the separation column, then selectively passing the eluate from the separation column through a trapping column according to a desired component, thereby trapping the desired component in the trapping column, while discarding or recycling the effluent eluate from the trapping column, and then passing another eluting solution composed of a volatile substance when dried under reduced pressure through the trapping column, thereby recovering eluate containing the desired component from the trapping column.

Abstract: Apparatus and method for extracting a component from a sample across a membrane into an extractant and then injecting the extracted sample component into a chromatographic eluent and onto a chromatographic column to chromatographically analyze the extracted sample component. In essence, the advance provided by this invention is that the extractant and the eluent are the same and only one pump is used for pumping the eluent and extractant. In prior apparatus and methods in this field, the extractant and the eluent were separate and each had its own pump.

Abstract: Packing tube membranes or membrane channels for Ion Chromatography with inert or charged ion exchange beads greatly increases overall suppressor efficiency. The length of membrane required is reduced, e.g. from 20 feet to 5 feet and bandspreading is reduced from 870 .mu.l to 200 .mu.l. This significant increase in efficiency is attributed to the mixing action of the packing on the flow stream which results in convective radial transport much more rapid than the diffusion controlled transport observed in unpacked membranes. The technique is also described for developing more efficient liquid chromatographic post-column reactors for adding reagent to the column effluent to increase detection sensitivity.

Abstract: Apparatus and method for automatically detecting and quantitatively determining the presence of metals. The apparatus includes a sample collecting device for locating in an effluent and means to inject the sample into a chromatographic column to separate out the various metal ions present. Two analysing devices, namely, spectrophotometric detector and an electrochemical detector are used. These elements are monitored and controlled by a microprocessor which monitors the delay from injection of the sample and controls the conditions in the electrochemical detector to ensure maximum effectiveness in measuring metal presence. The microprocessor also controls the production of data output from the detectors and controls the frequency of the sample collection.

Abstract: A method and apparatus for supplying a preset amount of sample solution to a liquid chromatographic column wherein (1) a first piston, which moves along the axis of a piston container sealingly contacting the side walls of said piston container, is moved a preset distance so as to draw a fixed amount of driving solution from the driving solution chamber of a piston cylinder into the piston container, thus displacing a second piston which moves along the axis of said piston cylinder sealingly contacting the side walls of said piston cylinder and dividing said piston cylinder into a sample solution chamber and a driving solution chamber, said displacement of said second piston serving to cause sample solution to be drawn from a sample solution reservoir into the sample solution chamber of the piston cylinder in a fixed amount equal to the fixed amount of driving solution drawn into the piston container; and (2) driving solution is pumped into said driving solution chamber in order to displace said second piston

Abstract: A separation process by liquid chromatography, which comprises sending a mixture sample in a large amount together with a liquid mobile phase to at least one column, into which a packing having a large particle size has been charged, to preliminarily fractionate the components of the mixture, taking out fractions containing objective components from the eluate from the first column, and recycling said fractions within a loop provided with at least one second column, into which a packing having a large particle size has been charged, to separate precisely the objective components.According to this process, it is possible to separate economically objective components from the sample loaded in a large amount.

Abstract: A method and apparatus for the simultaneous analysis of borate and chloride ions in a liquid sample, such as a sample of nuclear reactor water, by ion chromatographic techniques are disclosed. The ion chromatographic system employed includes an exclusion column, an anion exchange column, and means for alternately directing effluent from said exclusion column to refractive index detecting means or void volume from the exclusion column and second eluent through the anion exchange column to conductivity detecting means.

Abstract: In an apparatus for conducting solubilization chromatography wherein a solvent consisting of a buffer and ionized micells is allowed to flow through a capillary tube whose both ends are connected to the plus and minus sides, respectively, of a DC source, then a sample is introduced into the capillary tube, components of the sample are separated by combination of dissolution phenomenon of the sample in the ionized micells and capillary electro-phoresis, and qualitative and quantitative analysis of the components is carried out; a three way joint is provided having a first opening connected to the capillary tube, a second opening connected to tubing for feeding the solvent and sample, and a third opening serving as a discharge outlet for residue solution of solvent and sample not introduced into the capillary tube; and means are provided for controlling the time the sample contacts an inlet of the capillary tube within the three way joint, whereby the quantity of sample introduced into the capillary tube is con

Abstract: An ink production system constructed with a dyestuff solution producing unit, a dyestuff solution processing unit by execution of chromatographic operations on the dyestuff solution, and an ink preparation unit to effect preparation of ink with the refined dyestuff solution as discharged from the processing unit.

Abstract: A chromatograph sample homogenizer having a mixing chamber containing means for homogenizing a mixture therein and means of controlled ingress and/or controlled egress for (1) eluant from a chromatographic column, (2) wash solvent, (3) transport gas, (4) waste material, and (5) homogenized sample. Methods for manipulating the operation of the sample homogenizer to provide homogenized samples and homogenized diluted samples.

Abstract: Sulfite spent liquor is subjected to a two-step chromatographic separation to form substantially purified fractions of sugars and lignosulfonates. The process for the separation of sugars and lignosulfonates comprises the steps of(a) introducing sulfite spent liquor with a pH of 2.5 to 3.5 onto a chromatographic column containing a resin in metal salt form;(b) eluting the sulfite spent liquor from the column with water to recover a substantially sugar-free lignosulfonate-rich fraction and a sugar-rich fraction;(c) collecting the sugar-rich fraction for further purification;(d) adjusting the pH of the collected sugar-rich material to between 5.5 and 6.5 and introducing the material onto a second chromatographic column containing a resin in monovalent salt form; and(e) eluting the sugar-rich material from the second column with water, whereby a second sugar-rich fraction and a second lignosulfonate-rich fraction are formed.

Abstract: A process for chromatographic separation of dextrose from starch hydrolysate wherein the aqueous raffinate produced by contacting the starch hydrolysate with a chromatographic column or bed is treated with glucoamylase and recycled, at least in part, for use as an eluant for dextrose. An immobilized glucoamylase is used in the treatment to produce an aqueous dextrose-containing solution. It is this solution that is recycled and used, at least in part, as the eluant in the chromatographic column or bed used in the process.

Abstract: Methods of and apparatus for identifying peaks corresponding to the same chemical component in a series of liquid chromatograms to identify the peaks without foreknowledge of the chromatographic behavior of any component in the sample, or even the number of components in the sample.

Abstract: Method of separating A.sub.14 -.sup.125 I-insulin from heterogeneously labeled insulin molecules for biological studies which involves iodating insulin in a controlled manner, selectively absorbing the insulin from the iodination procedure in a tightly packed bed of octadecylsilane bonded to silica employing reverse phase liquid chromatography principles, thereafter eluting large and small radioactive and nonradioactive materials such as damaged insulin, various contaminants and polar materials from the bed with dilute trifluoroacetic acid, thereafter eluting the intact .sup.125 I-insulin from the bed with a mixture of acetonitrile and dilute trifluoroacetic acid and then separating the A.sub.14 -insulin by high performance liquid chromatography or ion exchange chromatography.

Abstract: A support material comprised of a substrate and a coating bound to the substrate made up of a polymer containing succinimide units or derivatives thereof. A method for preparing a support material comprising reacting a polymer containing succinimide units with surface amine groups on a substrate.

Abstract: Concentration of the solutes contained in a liquid solvent is effected by passing the solvent through a first trapping means that adsorbs them, flushing the first trapping means with supercritical fluid and reducing its solubility parameter in a second trapping means so that the latter can adsorb desired solutes.

Abstract: A process for separating an extract component from a raffinate component contained in a feed mixture. A unidirectional fluid flow system is maintained through a series of separating units through which the components travel at different rates. The units are interconnected in series so as to form a single closed loop. A component concentration distribution is established within the system of units so as to comprise a series of zones. Feed and displacement fluid are each mixed with a different intercolumn stream prior to being passed into the inlets of two of the units and extract and raffinate are taken only as portions of streams from outlets of two or more of the units at appropriate points on the component concentration distribution. At the appropriate times the inlets and outlets are shifted so as to simulate movement of the units in a direction downstream with respect to the direction of fluid flow and thereby enable the inlets and outlets to continually lie in the appropriate zones.

Abstract: The present invention concerns a fractionation process of a mixture by elution chromatography.It is characterized in that the collected eluent is purified, restored to supercritical state and recycled in the head of the column.It concerns a cracking process of mixtures by elution chromatography with liquid in the supercritical state and an installation for its operation.

Abstract: A process for separating an extract component from a raffinate component contained in a feed mixture. A unidirectional fluid flow system is maintained through a series of separating units through which the components travel at different rates. A component concentration distribution is established within the system of units and divided into specific zones. Feed and displacement fluid are passed into the inlets of two of the units and extract and raffinate are taken as the entire streams from outlets of two of the units all at appropriate points on the component concentration distribution. Other inlets and outlets of the various units lying in the same zone are interconnected. At the appropriate times the inlets and outlets are shifted so as to simulate movement of the units in a direction co-current with the fluid flow and thereby enable the inlets and outlets to continually lie in the appropriate zones. Zones may be combined as zone pairs, each such pair thereupon being considered a single continuous zone.

Abstract: A microprocessor-based analytical liquid chromatograph is programmed to run automatically a series of experiments on a sample mixture using four solvents to determine the solvent strengths and composition needed to optimize resolution.

Abstract: A method for increasing the capacity of a chromatographic system useful for the quantitative determination of at least one component of interest at a trace level concentration in a multi-component composition.

Abstract: A system for analyzing constituents of coal-derived materials comprises three adsorption columns and a flow-control arrangement which permits separation of both aromatic and polar hydrocarbons by use of two eluent streams.