With Automated Titrator Patents (Class 436/51)
  • Patent number: 5340541
    Abstract: Automation of the coulometric Karl Fischer titration has allowed for the accurate, precise determination of moisture content of lyophilized hGH formulations. The system of the present invention utilizes a vented, two-hole sampling/dispensing probe that dispenses titrant and withdraws sample solution through the closed container rubber septum into the Karl Fischer titration reaction vessel. This approach eliminates erroneous results due to environmental moisture contamination or loss of material during the sample transfer process. The system of the present invention is also equipped with a fixed loop valving system, which facilitates the precise measurement of a defined amount of water as a standard. This allows for an accurate accessment of system suitability that was lacking with commercial water standards due to inaccurate moisture content presumably from moisture contamination of the standard under storage and/or at the time of manufacture.
    Type: Grant
    Filed: March 5, 1993
    Date of Patent: August 23, 1994
    Assignee: Eli Lilly and Company
    Inventors: David A. Jackson, Ralph M. Riggin, John K. Towns
  • Patent number: 5302253
    Abstract: A method and apparatus for automatically measuring the acidity of overhead water in an oil refinery, and dispensing a neutralizing agent into the refinery system at a rate responsive to that measurement. A sample of overhead water is collected and passed through a filter and cation exchange resin. The acid concentration of the sample is then automatically measured and a signal generated based on the concentration. The signal goes to a controller which controls the dispensation rate of neutralizing agent into the refinery system, thus reducing the acidity of the overhead water and limiting the corrosive effects of such acidity.
    Type: Grant
    Filed: April 13, 1992
    Date of Patent: April 12, 1994
    Assignee: Nalco Chemical Company
    Inventors: Ronald B. Lessard, Paul Fearnside
  • Patent number: 5291418
    Abstract: Automatic titration method and apparatus provides for adjustment of the electric potential of a solution. A programmed computer responsive to iterative measurements of the potential regulates a two-phase adjustment process which approaches the desired electric potential (overall aim) using sub-aims thereby preventing overshoot of the overall aim.
    Type: Grant
    Filed: July 5, 1991
    Date of Patent: March 1, 1994
    Assignee: Eastman Kodak Company
    Inventors: James M. Sanders, Ming-Jye Lin, Michael P. Lionti, Michael C. Schrader
  • Patent number: 5260220
    Abstract: An automated analysis system for the determination of impurities in a liquified hydrocarbon stream. The system employs a hydrocarbon capture vessel for capturing a hydrocarbon sample, a water scrubbing vessel for extracting impurities from the hydrocarbon sample and a titration zone for analyzing the amount of impurities in the aqueous extract.
    Type: Grant
    Filed: November 19, 1991
    Date of Patent: November 9, 1993
    Assignee: Arco Chemical Technology, L.P.
    Inventors: W. Richard Dougherty, Donald J. Skahan
  • Patent number: 5192509
    Abstract: An automatic titration device for use in either batch processing or a continuous processing mode to identify quantitative fluid properties. The device consists of a plurality of reservoirs each connected to a respective plurality of pumps. A central computer controls individual pump speeds and therefore the pump output mix through a delivery tube that delivers fluid mixture through an ultrasonic mixer to a mixing tube whereupon a color detector is disposed to detect indicator color changes of the liquid for providing indication back to the central computer for calculation of fluid presence, fluid equivalent points, and related fluid properties.
    Type: Grant
    Filed: August 22, 1991
    Date of Patent: March 9, 1993
    Assignee: Halliburton Company
    Inventors: Jim B. Surjaatmadja, Clyde L. Lee
  • Patent number: 5186895
    Abstract: An automatic analytical apparatus in which a series of operations ranging from the sampling into a treating receptacle, pretreatment, analysis and discharge of a fluid sample to the preparation for the next analysis are repeated automatically in order, wherein the time-dependent variation of the composition is traced successively. This permits the presence of the composition variation or the course of the composition variation to be confirmed or the composition variation to be controlled, automatically.
    Type: Grant
    Filed: February 15, 1991
    Date of Patent: February 16, 1993
    Assignee: Mitsui Toatsu Chemicals, Incorporated
    Inventors: Mitsuo Onofusa, Nobuyoshi Hashimoto, Kimiteru Tagawa, Michiro Hagiwara
  • Patent number: 5132233
    Abstract: The sample injection cell comprises a body and a bore through the body for receiving a probe to pass fluid sample into the bore. A transverse passageway into the body permits a diluent to enter the bore and be mixed with a sample in a predetermined ratio and be dispensed directly into the flow cell. The diluent simultaneously washes the probe when the probe is located in the bore. A waste basin forms part of an integral unit and is adjacent the bore so that fluid from a flow cell can enter the waste basin and then exit under gravity to a waste drain.
    Type: Grant
    Filed: March 13, 1989
    Date of Patent: July 21, 1992
    Assignee: Beckman Instruments, Inc.
    Inventors: Delbert D. Jackson, Samuel G. Ricchio
  • Patent number: 5108929
    Abstract: Efficient control of the pH of a flowing alkaline wastewater stream is accomplished by monitoring the pH of the flowing stream, generating a signal in response to the pH monitored, and injecting CO.sub.2 as necessary to reduce the pH. High pressure liquid CO.sub.2 is supplied to a proportional control valve which is operated in response to the signal to change the high pressure CO.sub.2 fluid to an intermediate pressure CO.sub.2 fluid in a manner so as to significantly reduce its density by creating a significant gaseous fraction. This lower density CO.sub.2 fluid is supplied to a spring-loaded injector having an orifice in communication with the flowing stream. The intermediate pressure is above the pressure at which the injector opens whereby the lower density CO.sub.2 fluid is injected into the flowing stream, allowing particularly precise control to be achieved.
    Type: Grant
    Filed: August 14, 1989
    Date of Patent: April 28, 1992
    Assignee: Liquid Carbonic Corporation
    Inventors: John S. Segura, David M. Forstrom
  • Patent number: 5104527
    Abstract: A process and apparatus for automatically monitoring or adjusting, or both, the concentration of total reducers (i.e. reduced sulfur-containing constituents which consume iodine) in an aqueous medium (e.g. waste water stream) whereby the time period for iodine titration of an untreated sample of the aqueous medium is automatically measured by measuring a time of light being transmitted through a titration sample cell and this time measurement is automatically translated into an output signal to either a monitoring means or a process adjustment means (e.g. oxidant chemical feed pump) or both.
    Type: Grant
    Filed: November 27, 1990
    Date of Patent: April 14, 1992
    Assignee: Ashland Oil, Inc.
    Inventor: Jack L. Clinkenbeard
  • Patent number: 5080866
    Abstract: A method of analysis in which a first fluid is delivered to a sensing position at a controlled first rate of flow through a fluid junction. Fluid including this first fluid is pumped to the sensing position at a rate of flow greater than the first rate, whereby to aspirate further fluid into the first fluid at the fluid junction. A condition of the fluid is sensed at the sensing position. Associated analytic apparatus includes first and second pumps (1, 2). The first pump has a pair of ports and the second pump has at least one port. A conduit (4, 5) provides fluid flow communication from a first of the ports of the first pump (1) to the port of the second pump (2). A fluid junction (3) in the conduit (4, 5) is spaced from the second pump for admitting a further fluid to the conduit. A sensor (13) is associated with the conduit (5) to sense a condition of the fluid in the conduit at least at a sensing position between the fluid junction (3) and the second pump (2).
    Type: Grant
    Filed: December 19, 1990
    Date of Patent: January 14, 1992
    Inventors: John D. Petty, Russell M. Peachey, Denis R. Sweatman
  • Patent number: 5006312
    Abstract: A gravimetric method for determining the iodine adsorption number of carbon black is disclosed. The concentration of an accurately weighed iodine solution is determined by titrating with a standardized titrant and determining the concentration of the iodine solution by the weight of the standardized titrant needed to reach the titration endpoint. An appropriate amount of accurately weighed iodine solution is mixed with an accurately weighed amount of carbon black, and the mixture is equilibrated. The concentration of the resulting supernatant is determined by determining the weight of the standardized titrant needed to reach the titration endpoint. The iodine adsorption number is then determined based on the gravimetrically determined concentrations of the solutions. Preferably, the method is semi-or fully automated, and an apparatus for accomplishing the same is disclosed.
    Type: Grant
    Filed: June 18, 1990
    Date of Patent: April 9, 1991
    Inventor: Lawrence J. Murphy, Jr.
  • Patent number: 5004696
    Abstract: A process and apparatus for automatically monitoring or adjusting, or both, the concentration of total reducers (i.e. reduced sulfur-containing constituents which consume iodine) in an aqueous medium (e.g. waste water stream) whereby the time period for iodine titration of an untreated sample of the aqueous medium is automatically measured and this time measurement is automatically translated into an output signal to either a monitoring means or a process adjustment means (e.g. oxidant chemical feed pump) or both.
    Type: Grant
    Filed: March 24, 1988
    Date of Patent: April 2, 1991
    Assignee: Ashland Oil, Inc.
    Inventor: Jack L. Clinkenbeard
  • Patent number: 5002892
    Abstract: A gravimetric method for determining the iodine adsorption number of carbon black is disclosed. The concentration of an accurately weighed iodine solution is determined by titrating with a standardized titrant and determining the concentration of the iodine solution by the weight of the standardized titrant needed to reach the titration endpoint. An appropriate amount of accurately weighed iodine solution is mixed with an accurately weighed amount of carbon black, and the mixture is equilibrated. The concentration of the resulting supernatant is determined by determining the weight of the standardized titrant needed to reach the titration endpoint. The iodine adsorption number is then determined based on the gravimetrically determined concentrations of the solutions. Preferably, the method is semi-or fully automated, and an apparatus for accomplishing the same is disclosed.
    Type: Grant
    Filed: August 31, 1989
    Date of Patent: March 26, 1991
    Assignee: Cabot Corporation
    Inventor: Lawrence J. Murphy, Jr.
  • Patent number: 4950610
    Abstract: Titration apparatus includes two cells that receive and contain liquids and are transparent to light. A liquid having an unknown characteristic and mixed with an indicator that is optically responsive to a titrant is disposed in the cells. Light is transmitted through each cell to separate photosensors. The photosensor signals are compared and a titrant is added to one of the cells in known-volume increments until the difference between the signals reaches or exceeds a prescribed threshold. The characteristic of the liquid is calculated from the quality of known concentration titrant added in order to reach or exceed the prescribed threshold.
    Type: Grant
    Filed: September 28, 1987
    Date of Patent: August 21, 1990
    Assignee: Man-Gill Chemical Company
    Inventor: Douglas L. Tittle
  • Patent number: 4920056
    Abstract: Apparatus and method for automatic microbatch reaction including a reactor having a reaction chamber, such as a 1.5 milliliter plastic centrifuge tube having a conical bottom. An automatically actuated injection valve is used to inject less than 1 milliliter of a sample into the reaction chamber. One or more automatically actuated reagent valves are used to introduce respective pressurized reagents into the reaction chamber to process the sample. The volume of the reagent(s) introduced into the reaction chamber is less than 1 milliliter and controlled by the on time of the respective reagent valve. The automatically actuated valves are controlled by a computer based timer. A sensor positioned in the chamber, such as a pH electrode, can be used to analyze the processed sample in place or the processed sample can be analyzed by flowing it from the reaction chamber through a flow-through detector, such as a flow-through spectrophotometer.
    Type: Grant
    Filed: February 19, 1988
    Date of Patent: April 24, 1990
    Assignee: The Dow Chemical Company
    Inventor: Purnendu K. Dasgupta
  • Patent number: 4910151
    Abstract: An apparatus and method for on-line monitoring of a characteristic of a process liquid stream includes a cell for isolating a precise volume of the liquid. A sample chamber is over filled and the excess removed from the chamber by using a downwardly extending drain line which terminates at a precisely positioned, downwardly facing inlet negative pressure is applied to the drain line to draw the excess liquid upwardly from the captured volume until the liquid level reaches the inlet and entry of air disrupts the liquid draining effect. The embodiment shown employs a closed volume, a vent, a conduit for delivery of process liquid into the cell under pressure and a syphon/drain line for removing excess liquid from the cell volume until there remains only a sample of accurately repeatable volume.
    Type: Grant
    Filed: April 14, 1987
    Date of Patent: March 20, 1990
    Assignee: Tytronics, Incorporated
    Inventor: Moses Platt
  • Patent number: 4876206
    Abstract: This invention relates to methods for quickly and accurately detecting the presence of rare earth minerals which can be performed in the field. An ore sample to be tested for the presence of rare earth minerals is contacted with both a basic reagent, preferably containing an alkali metal, and with a halide acid such as hydrochloric acid. Once the treated ore sample is dry, it is examined under a shortwave ultraviolet light for fluorescence of a red-orange color. If rare earth minerals are present, fluorescence of a red-orange color will occur. If no rare earth minerals are present, no red-orange fluorescence is observed. The sensitivity of the disclosed methods to rare earth minerals may be varied by altering the basic reagent to permit the user to "zero in" on the most concentrated source of rare earth minerals.
    Type: Grant
    Filed: February 10, 1989
    Date of Patent: October 24, 1989
    Inventor: Wayne L. Sayer
  • Patent number: 4873057
    Abstract: The sample and the reagent required for titration are fed into a titration vessel (1), the reagent and/or sample being supplied intermittently in the form of pulses of liquid. Toward this end, a controlled valve (9) is provided in the supply line (4) for the reagent. The opening and closing times of this valve (9) and, hence, the frequency and duration of the pulses of liquid, are chosen such that the ratio of the average sample flow to the average reagent flow is sufficient to achieve the ratio of sample to the reagent at the equivalence point. This renders continuous titration possible, for which only one pump (7) is needed, which does not require any complex servo system and, therefore, has a low energy consumption.
    Type: Grant
    Filed: March 10, 1987
    Date of Patent: October 10, 1989
    Assignee: Zellweger Uster Ltd
    Inventors: Peter M. Robertson, Erwin Suter
  • Patent number: 4865992
    Abstract: A system and method for quantitative analysis of a solution to determine the concentration of a chemical species in the solution. The system includes a reaction vessel; a source of at least one liquid reagent for reacting with the chemical species being tested for; a conduit leading from the reagent source to the reaction vessel; pneumatic pressure for forcing the reagent through the conduit; controls for controlling the amount of reagent added to the reaction vessel; and a detection device for detecting reaction between the reagent and the chemical species.
    Type: Grant
    Filed: August 28, 1986
    Date of Patent: September 12, 1989
    Assignee: Hach Company
    Inventors: Clifford C. Hach, John G. Wasson
  • Patent number: 4749552
    Abstract: Automatic titration analysis apparatus includes a sampling mechanism, a titration mechanism, an analysis mechanism and a control mechanism. The sampling mechanism takes a prescribed quantity of a sample for analysis in accordance with a first signal. The titration mechanism titrates a prescribed quantity of a reagent for analysis of the sample and provides a titer at an end point of the titration according to second signals. The analysis mechanism receives the sample from the sampling mechanism, analyzes the sample and converts a change in the physical properties of the sample caused by the titration into an electrical quantity.
    Type: Grant
    Filed: August 6, 1986
    Date of Patent: June 7, 1988
    Assignee: Ebara Densan Ltd.
    Inventors: Hitoshi Sakisako, Masashi Kimura
  • Patent number: 4741815
    Abstract: An apparatus for electrochemical indication of the final stage of a titration analysis has a first indication electrode located in an electrochemical titration container connected by a switch to a sampling current amplifier feeding a recorder. Both the amplifier and the switch are controlled by a timing circuit which causes the switch to connect and disconnect the electrode to the amplifier. By only connecting the electrode to the amplifier for a brief time and activating the amplifier for a brief time thereafter, the instantaneous value of indication current is obtained. During the remaining time period, the indication electrode is galvanically disconnected from the amplifier and consequently, no reduction of concentration of electroactive substance in the proximity of the electrode occurs and an extremely high current response is attained.
    Type: Grant
    Filed: April 13, 1987
    Date of Patent: May 3, 1988
    Assignee: Slovenska vysoka skola technicka
    Inventors: Juraj Bercik, Jan Dzurov, Leos Vyskocil
  • Patent number: 4671123
    Abstract: A hand held self-contained automated pipette for portable operation having an electrically operated digital linear actuator. The actuator preferably includes a stepper motor driving a rotor. A threaded screw is coaxially positioned within the rotor and is connected to an actuator shaft having elongate grooves slidable in a guide for preventing shaft rotation so that precise linear motion is imparted to the shaft. A pipetting displacement assembly having one of various sizes is removably attached for actuation by a common actuator including programmed movement of a displacing piston in a displacement cylinder to optimize air interface volume, neutralize variations in vacuum pipette effects, and provide an accommodated stroke and readout for improved accuracy while pipetting and/or titrating different ranges of volumes. A control circuit is provided so that the back EMF of the stepper motor coils is recirculated when power is duty-cycled off for power conservation.
    Type: Grant
    Filed: February 16, 1984
    Date of Patent: June 9, 1987
    Assignee: Rainin Instrument Co., Inc.
    Inventors: Haakon T. Magnussen, Jr., Gary L. Smith, Stephen J. Ruskewicz, Anthony K. Wingo
  • Patent number: 4554255
    Abstract: A method and an apparatus providing a simple and speedy determination of a slight amount of sulfurous acid contained in liquids by means of pH meters, based on the Modified Rankine's method in principle, and wherein the pH of a first sample of liquid is determined before and after adding an amount of hydrogen peroxide thereto, the pH of a second sample of liquid is determined before and after adding an amount of an acid or lower pH buffer solution thereto, and the concentration of sulfurous acid in the liquid is calculated from the measured pH values and an equation derived from the functional relationship:c=f(.DELTA.pH.sub.A, .DELTA.pH.sub.B)wherein c is the concentration of sulfurous acid.
    Type: Grant
    Filed: July 6, 1983
    Date of Patent: November 19, 1985
    Assignee: Sanwa Shoji Co., Ltd.
    Inventors: Katsuyoshi Ishii, Michio Kobori, Seiichi Morimoto
  • Patent number: 4476095
    Abstract: A fluorometric titrator has means to transfer a pipette between first and second positions and a buret for a chelating agent has a reversible drive powered either by a pulse generator or an oscillator. Valve controlled means are operable to place the buret in communication with the pipette or a reservoir. In the first position of the pipette, a precise sample volume is aspirated into it by the buret, then driven by the oscillator and in its second position and with the buret drive reversed but still powered by the oscillator, the sample volume is discharged from the pipette into a cuvette in the fluorometer. On the resulting fluorescence the fluorometer output drives the pulse generator to dispense chelating agent and to operate a counter until a selected end point is reached. The pipette is then returned to its second position with the buret drive again operated by the oscillator and during the return, the buret is refilled.
    Type: Grant
    Filed: April 12, 1974
    Date of Patent: October 9, 1984
    Inventors: Robert L. Scott, Samuel Nejame, Jr., Charles S. Jacobs, Jr., Charles A. Bell