By Use Of A Karl Fischer Reagent Patents (Class 436/42)
  • Patent number: 11885782
    Abstract: A first method for determining an amount of water in a sample includes the step of providing a reagent including: sulfur dioxide or a derivative thereof; a base; an optional hydrogen halide or hydrogen halide donor; a solvent; and a sulfonic acid; and the step of titrating the sample with the reagent. A second method for determining an amount of water in a sample includes the step of providing the aforementioned reagent, combining the sample with the reagent; and adding a source of iodine to the sample and/or the reagent. The reagent may alternatively consist essentially of sulfur dioxide or a derivative thereof; imidazole and/or a derivative thereof; an optional hydrogen halide or hydrogen halide donor; acetonitrile; methane sulfonic acid; and methanol and/or ethanol.
    Type: Grant
    Filed: October 22, 2021
    Date of Patent: January 30, 2024
    Assignee: HONEYWELL INTERNATIONAL INC.
    Inventor: Roman Neufeld
  • Patent number: 11714072
    Abstract: A reagent composition for a Karl Fischer titration includes (1) sulfur dioxide or a derivative thereof, (2) a derivative of imidazole, (3) an alcohol, and (4) at least one amino acid that is present in an amount that is greater than zero and up to about 10 weight percent based on a total weight of the reagent composition. Moreover, a molar ratio of the derivative of imidazole to the sulfur dioxide or derivative thereof is greater than 1:1. Iodine is optionally included in a one-component reagent and excluded in a two-component reagent. This disclosure further provides a method for determining an amount of water in a sample via Karl Fischer titration. The method includes the step of providing the sample, providing the reagent composition, which optionally includes the iodine (I2), and titrating the sample with the reagent composition.
    Type: Grant
    Filed: March 23, 2020
    Date of Patent: August 1, 2023
    Assignee: HONEYWELL INTERNATIONAL INC.
    Inventors: Stefan Seekamp, Marco Konopatzki
  • Patent number: 11480552
    Abstract: The present invention provides a method for measuring moisture content in a separator of secondary battery by using a gas chromatograph equipped with a headspace sampler. The separator of secondary battery may be a safety reinforced separator (SRS) in which inorganic substance particles and a binder polymer are coated on a polyolefin substrate.
    Type: Grant
    Filed: January 3, 2018
    Date of Patent: October 25, 2022
    Inventors: Min-Jeong Lee, Jong-Mo Jung
  • Patent number: 11366652
    Abstract: The functionality offered through a game development application can be extended using a plurality of extension modules. A customer portal can expose information about the available modules to a developer, where the extension modules can include components such as a customer interface enabling an authorized entity to access or modify the functionality, as well as an application programming interface (API) or other interface for enabling the functionality to be accessed during gameplay. The API can be associated with various resources that can be allocated to the customer over a period of time, or that can be allocated dynamically in order to process discrete tasks. The allocation of resources can occur after release of the game and during live gameplay. Similar functionality can be accessed by a game administrator to trigger specific actions during gameplay.
    Type: Grant
    Filed: March 27, 2017
    Date of Patent: June 21, 2022
    Assignee: AMAZON TECHNOLOGIES, INC.
    Inventors: Anthony Pressacco, Michael Eric Deem
  • Patent number: 10626029
    Abstract: Anion exchange membranes may include a polymeric microporous substrate and a cross-linked anion exchange polymeric layer on the substrate. Anion exchange membranes may have a resistivity of less than about 1.5 Ohm-cm2 and an apparent permselectivity of at least about 95%. The anion exchange membranes may be produced by a unique, two step process.
    Type: Grant
    Filed: November 7, 2017
    Date of Patent: April 21, 2020
    Assignee: Evoqua Water Technologies LLC
    Inventor: Juchui Ray Lin
  • Patent number: 9157901
    Abstract: When measuring the liquid crystals to he measured, the present invention adding the liquid crystals under test to a mixed solvent to form a solvent to be measured; measuring the moisture in the liquid crystal measurement sample through a reaction reagent to achieve a measurement result; wherein the mixed solvent comprises a first solvent, and the first solvent is dissolved with the methanol of the reaction reagent mutually and dissolves the liquid crystals to be measured. In the present invention, the moisture in the liquid crystal can be fully released and achieve accurate measurements.
    Type: Grant
    Filed: November 22, 2013
    Date of Patent: October 13, 2015
    Assignee: SHENZHEN CHINA STAR OPTOELECTRONICS TECHNOLOGY CO., LTD.
    Inventor: Rui Xu
  • Publication number: 20150140667
    Abstract: When measuring the liquid crystals under test, the present invention adding the liquid crystals under test to a mixed solvent to form a solvent under test; measuring the moisture in the liquid crystal measurement sample through a reaction reagent to achieve a measurement result; wherein the mixed solvent comprises a first solvent, and the first solvent is dissolved with the methanol of the reaction reagent mutually and dissolves the liquid crystals under test. In the present invention, the moisture in the liquid crystal can be fully released and achieve accurate measurements.
    Type: Application
    Filed: November 22, 2013
    Publication date: May 21, 2015
    Inventor: Rui Xu
  • Publication number: 20140275135
    Abstract: Solid forms of chemical compounds that modulate kinase activity, including PI3 kinase activity, and compounds, pharmaceutical compositions, and methods of treatment of diseases and conditions associated with kinase activity, including PI3 kinase activity, are described herein. Also provided herein are processes for preparing compounds, solid forms thereof, and pharmaceutical compositions thereof.
    Type: Application
    Filed: March 13, 2014
    Publication date: September 18, 2014
    Applicant: Infinity Pharmaceuticals, Inc.
    Inventors: Daniel G. GENOV, Louis GRENIER, Andrew B. HAGUE, Alexander Redvers EBERLIN, Ludovic Sylvain Marc RENOU, Susana DEL RIO GANCEDO
  • Patent number: 8506387
    Abstract: A gaming machine connected in a gaming network or operating as a stand-alone machine, is capable of accepting two or more currencies for wager game play. The machine operates internally using a native monetary type and converts non-monetary bills to native amounts in the form of restricted or cashable credits. The multiple currency capability of the machine is utilized to encourage the use of restricted credits by adjusting conversion rates, payback tables, and the like. These features, combined with the use of restricted credits, also enable ways to monitor abuse and illegal activity on the gaming machine and implement ways to limit losses by a player. Certain post-conversion processes are used to ensure that the player is returned non-converted amounts. The gaming machine has additional hard and soft meters to process multiple monetary types.
    Type: Grant
    Filed: December 29, 2011
    Date of Patent: August 13, 2013
    Assignee: IGT
    Inventors: William R. Brosnan, Bryan D. Wolf, Stephen W. Morro, Terrence Lee McCreary, Jr., M. Ali Saffari, John W. Chamberlain
  • Publication number: 20130171734
    Abstract: Provided is a reagent composition for measuring moisture content in a lithium secondary battery electrolyte, more particularly, a reagent composition for measuring moisture content in a lithium secondary battery electrolyte, containing imidazole, iodine, sulfur dioxide, and an amide based solvent, so that the reagent composition can suppress side reactions to thereby accurately measure a small amount of moisture content.
    Type: Application
    Filed: December 17, 2012
    Publication date: July 4, 2013
    Applicant: SOULBRAIN CO., LTD.
    Inventor: Soulbrain Co., Ltd.
  • Publication number: 20130105741
    Abstract: The present disclosure relates to pastes and methods of making a moisture determination of the paste during manufacture; optionally, the pastes comprise carbon nanotubes.
    Type: Application
    Filed: October 31, 2011
    Publication date: May 2, 2013
    Applicant: CNANO TECHNOLOGY LIMITED
    Inventors: Caihong Xing, Yunwang Mei, Yan Zhang, Haimei Zang, Gang Xu, Jun Ma
  • Patent number: 8430747
    Abstract: A gaming system including a central server linked to a plurality of gaming machines and a plurality of bonus awards. The central server monitors wagers on the gaming machines. Based at least in part on the wagers the central server determines when bonus events will occur and which gaming machine(s) will provide the bonus awards. In one embodiment, the central server determines which gaming machine will provide a primary bonus award and any secondary bonus awards, wherein at least one gaming machine may be provided a plurality of bonus awards.
    Type: Grant
    Filed: July 30, 2007
    Date of Patent: April 30, 2013
    Assignee: IGT
    Inventors: Carl V. Kniesteadt, Anthony J. Baerlocher, James A. Vasquez, Tonja M. Ferry, Erick T. Ching
  • Patent number: 8429269
    Abstract: A solution for server-side rendering includes, at a server configured to store a video images representing states of users in a computer application, identifying future user actions based at least in part on a state of a user in the computer application. The solution also includes, responsive to the identifying, rendering video images for sending to a user device associated with the user. At the user device, a state of the user in a computer application is sent to the server. Responsive to the sending, video images are stored, each of the video images representing a future state of the user after the user performs a future action. Responsive to a user action, one of the video images is selected for display on a user display of the user device. According to one aspect, the future user actions identified by the server are limited to less than a possible number of user actions for users having the state.
    Type: Grant
    Filed: December 9, 2009
    Date of Patent: April 23, 2013
    Assignee: Sony Computer Entertainment Inc.
    Inventor: Michael Alan Kutner
  • Publication number: 20120322158
    Abstract: The present invention provide a water content measurement method for a hydrogen fluoride-containing compound represented by the general formula: XF.nHF (where X is either one of K, NH4, Na and Li; and n is a rational number greater than 0), including the steps of causing thermal decomposition of the hydrogen fluoride-containing compound, thereby generating a thermal decomposition gas, and then, determining the water content of the hydrogen fluoride-containing compound by quantification of the water content of the thermal decomposition gas.
    Type: Application
    Filed: February 21, 2011
    Publication date: December 20, 2012
    Applicant: Central Glass Company, Limited
    Inventors: Akiou Kikuchi, Nobuyuki Tokunaga
  • Patent number: 8216038
    Abstract: A gaming machine according to the present invention includes: a gaming portion in which a plurality of main dice roll and stop; a timer capable of measuring time; a station having an input device with which a player can place a normal BET and a side BET different from the normal BET, based on a prediction of the outcomes of dice; and a controller, the controller programmed to execute the processing of (A) starting acceptance of the normal BET and the side BET from the input device provided in the station, (B) measuring the time from when the acceptance was started in the processing (A) by using the timer, (C) terminating the acceptance of the normal BET and the side BET from the input device provided in the station, when the time measured in the processing (B) reaches a predetermined value, (D) determining whether or not the side BET has been placed by using the input device provided in the station, since the acceptance was started in the processing (A), (E) increasing the predetermined value when determining
    Type: Grant
    Filed: September 30, 2008
    Date of Patent: July 10, 2012
    Assignee: Universal Entertainment Corporation
    Inventor: Kazumasa Yoshizawa
  • Patent number: 8197322
    Abstract: Apparatuses and methods for facilitating access to a plurality of gaming activities via a processing arrangement involve facilitating player identification of a set of gaming activities selected from the plurality of gaming activities. A collection of references are assigned to the set of the gaming activities. Each of the references refers to at least one of gaming activities of the set of gaming activities identified by the player. The collection of references is stored in a computer-readable medium, and player access to the set of gaming activities is facilitated using the stored collection of references.
    Type: Grant
    Filed: April 27, 2007
    Date of Patent: June 12, 2012
    Assignee: King Show Games, Inc.
    Inventor: Bradley Berman
  • Patent number: 7419831
    Abstract: A method for calibrating an analysis instrument, e.g., a gas chromatograph, for water analysis that includes four steps. The first step is to continuously remove water from a liquid that contains water to produce a liquid containing a reduced amount of water such as by membrane pervaporation. The second step is to analyze the liquid containing a reduced amount of water for water by a reference water analysis method such as by Karl Fischer titration. The third step is to analyze the stream of liquid containing a reduced amount of water using the instrument to be calibrated, e.g., a gas chromatograph having a helium photoionization pulse discharge detector. The fourth step is to calibrate the instrument using the analysis of the second step. In a related embodiment, a system for normal phase chromatography.
    Type: Grant
    Filed: August 20, 2002
    Date of Patent: September 2, 2008
    Assignee: Dow Global Technologies, Inc.
    Inventors: Nile Nelson Frawley, Jeffrey Robert Larson, Mark William Beach, Mark Lindsay Dittenhafer, Steven Randall Erskine, Joseph J. Kiefer
  • Patent number: 7416894
    Abstract: The invention relates to water standards that are producible by grounding and mixing at least one component abounding in water and one water-free or low water component each. The inventive water standards are characterized by a good storage stability. They are suitable for the calibration or the inspection of devices to determine the water content after thermal release, especially for determining the water content according to Karl Fischer in combination with a Karl Fischer oven (Karl-Fischer oven technique).
    Type: Grant
    Filed: July 14, 2004
    Date of Patent: August 26, 2008
    Assignee: Merck Patent GmbH
    Inventors: Silke Gruenke, Stefanie Bauer
  • Publication number: 20080014641
    Abstract: A method and apparatus for determining a concentration of water in an oil mixture using both the Karl Fischer test method and spectrochemical analysis. The invention allows for chemical species that masquerade as water in an oil mixture to be identified and accounted for in determining a more accurate water concentration measurement than by using the Karl Fischer test method alone.
    Type: Application
    Filed: July 14, 2006
    Publication date: January 17, 2008
    Inventors: A. Andrew Carey, Anthony J. Hayzen
  • Patent number: 7247485
    Abstract: Karl Fischer reagent comprising iodide, sulphur dioxide with an initial concentration above 0.5 M, and imidazole/imidazole derivative dissolved in alcoholic solvent, whereby the molar ratio between the initial imidazole/imidazole derivative concentration and the initial sulphur dioxide concentration is above 10. The reagent contains a modifying substance that is an aliphatic hydrocarbon, or a primary or secondary alcohol, or a combination thereof. A method for the determination of water content by means of Karl Fischer coulometric titration in a diaphragm-free cell, whereby the Karl Fischer reagent is used, and the coulometric titration is carried out in a diaphragm-free cell. Use of the Karl Fischer reagent in a method for the determination of water content by means of coulometric titration.
    Type: Grant
    Filed: May 18, 2000
    Date of Patent: July 24, 2007
    Assignee: Teknikbrostiftelsen
    Inventors: Anders Cedergren, Ulrika Nordmark
  • Patent number: 7214537
    Abstract: A multicomponent fluid composition monitoring and compositional control system, in which a component analysis is effected by titration or other analytical procedure, for one or more components of interest, and a computational means then is employed to determine and responsively adjust the relative amount or proportion of the one or more components in the multicomponent fluid composition, to maintain a predetermined compositional character of the multicomponent fluid composition. The system is usefully employed in semiconductor manufacturing photoresist and post-etch residue removal, in which the cleaning medium is a semi-aqueous solvent composition, and water is the monitored and responsively adjusted component.
    Type: Grant
    Filed: October 4, 2002
    Date of Patent: May 8, 2007
    Assignee: Advanced Technology Materials, Inc.
    Inventors: Russell Stevens, Thomas Kloffenstein, Todd Aycock, Joseph W. Evans
  • Patent number: 7182912
    Abstract: An analyzer for performing automated assay testing. The analyzer includes a storage and conveyor system for conveying cuvettes to an incubation or processing conveyor, a storage and selection system for test sample containers, a storage and selection system for reagent containers, sample and reagent aspirating and dispensing probes, a separation system for separating bound from unbound tracer or labeled reagent, a detection system and date collection/processing system. All of the subunits of the machine are controlled by a central processing unit to coordinate the activity of all of the subunits of the analyzer. The analyzer is specifically suited for performing heterogeneous binding assay protocols, particularly immunoassays.
    Type: Grant
    Filed: May 29, 2002
    Date of Patent: February 27, 2007
    Assignee: Bayer Corporation
    Inventors: Glen Carey, Scott C. Lewis, Mary Beth Whitesel, Frank C. Klingshirn
  • Patent number: 7138240
    Abstract: Described are methods of detecting G-protein coupled receptor (GPCR) activity in vivo and in vitro; methods of assaying GPCR activity; and methods of screening for GPCR ligands, G Protein-coupled receptor kinase (GRK) activity, and compounds that interact with components of the GPCR regulatory process.
    Type: Grant
    Filed: May 9, 2002
    Date of Patent: November 21, 2006
    Assignee: Duke University
    Inventors: Lawrence S. Barak, Marc G. Caron, Stephen S. Ferguson, Jie Zhang
  • Patent number: 7122376
    Abstract: The invention relates to a formed tablet calibration standard-reagent for calibrating Karl Fischer reactions for determining water content in a substance, the reagent containing a first component, namely sodium tartrate dihydrate, and a second component, namely magnesium stearate. The invention further relates to a method for determining the water content of a substance using a Karl Fischer analysis. The invention further relates to a formed tablet calibration standard-reagent kit that includes a sealed package containing a formed tablet calibration standard-reagent for a Karl Fischer reaction.
    Type: Grant
    Filed: November 1, 2001
    Date of Patent: October 17, 2006
    Assignee: Facet Analytical Services and Technology, LLC
    Inventor: Scott Andrew Miller
  • Patent number: 7049146
    Abstract: The present invention relates to a formed tablet calibration standard-reagent for Karl Fischer reactions to determine the water content of substances, such as pharmaceuticals, food stuffs, and oils.
    Type: Grant
    Filed: March 5, 2004
    Date of Patent: May 23, 2006
    Assignee: Facet Analytical Services and Technology, LLC
    Inventor: Scott Andrew Miller
  • Patent number: 6946298
    Abstract: A reagent for the determination of water content of a sample according to the Karl Fischer method is disclosed. The reagent comprises a base component comprised of a mixture of imidazole and a substituted imidazole. Preferably, the Karl Fischer reagent is a one component reagent comprising imidazole and 2-methylimidazole.
    Type: Grant
    Filed: November 15, 2001
    Date of Patent: September 20, 2005
    Assignee: Sigma-Aldrich Co.
    Inventors: Helga Hoffmann, Katrin Schöffski
  • Publication number: 20040171161
    Abstract: The present invention relates to a formed tablet calibration standard-reagent for Karl Fischer reactions to determine the water content of substances, such as pharmaceuticals, food stuffs, and oils.
    Type: Application
    Filed: March 5, 2004
    Publication date: September 2, 2004
    Inventor: Scott Andrew Miller
  • Publication number: 20040110298
    Abstract: The invention relates to a formed tablet calibration standard-reagent for calibrating Karl Fischer reactions for determining water content in a substance, said reagent containing a first component, namely sodium tartrate dihydrate, and a second component, namely magnesium stearate. The invention further relates to a method for determining the water content of a substance using a Karl Fischer analysis. The invention further relates to a formed tablet calibration standard-reagent kit, comprising a sealed package containing said formed tablet calibration standard-reagent.
    Type: Application
    Filed: April 14, 2003
    Publication date: June 10, 2004
    Inventor: Scott Andrew Miller
  • Publication number: 20020137217
    Abstract: A disclosed gaming terminal data repository may be used to store game software components, game software component information and gaming transaction information for a plurality of gaming terminals owned by a plurality of gaming entities. The repository may store the game software component information and the gaming transaction information in a database partitioned according to the different gaming entities in a manner allowing a game software component configuration of a particular gaming machine to be easily analyzed and modified. Using various update triggers, game software components for gaming terminals connected to the gaming terminal data repository may be automatically updated. The gaming machines, configured or designed to receive game software components from the repository, may present game play using a combination of game software components residing on the gaming machine and the game software components received from the repository.
    Type: Application
    Filed: December 21, 2000
    Publication date: September 26, 2002
    Applicant: International Game Technology
    Inventor: Richard E. Rowe
  • Publication number: 20020127726
    Abstract: A reagent for the determination of water content of a sample according to the Karl Fischer method is disclosed. The reagent comprises a base component comprised of a mixture of imidazole and a substituted imidazole. Preferably, the Karl Fischer reagent is a one component reagent comprising imidazole and 2-methylimidazole.
    Type: Application
    Filed: November 15, 2001
    Publication date: September 12, 2002
    Applicant: Sigma-Aldrich Co.
    Inventors: Helga Hoffmann, Katrin Schoffski
  • Patent number: 6372505
    Abstract: In a process for titrating substances by adding increments of a titrant in time intervals, the course of the reaction is monitored in its approach toward the end point (EP), and the addition of titrant is controlled. At least one differential component is determined from the course of the reaction and used for controlling the addition of titrant. The process can be performed by an apparatus that includes a delivery unit for the titrant and suitable devices for performing the monitoring, differentiating and control functions.
    Type: Grant
    Filed: October 26, 1999
    Date of Patent: April 16, 2002
    Assignee: Mehler-Toledo GmbH
    Inventors: Albert Aichert, Gregor Amrein
  • Patent number: 6315888
    Abstract: A constant-current polarization voltage detecting method includes step of feeding to a detecting electrode a predetermined minute current in a pulse form, and detecting sequentially a polarization voltage at each time of feeding the pulsating current, in an electrochemical analysis in solution. The polarization voltage is detected after a lapse of a predetermined time from the initiation of feeding the pulsating current at each time. A Karl Fischer's moisture content analyzing apparatus can utilize such a method.
    Type: Grant
    Filed: April 18, 2000
    Date of Patent: November 13, 2001
    Assignees: Mitsubishi Chemical Corporation, Dia Instruments Co., Ltd.
    Inventors: Hiromasa Kato, Masafumi Nakatani
  • Patent number: 6131442
    Abstract: A method of determining the moisture content in wood in which a sample of the wood being tested is first frozen with liquid nitrogen, homogenized and a test sample is placed in a Karl Fischer titration system. The test sample is placed into a solvent solution and the reagent or titrant is progressively added to the solvent solution as the presence of moisture from the wood sample is detected. Once the moisture has been titrated from the solution the moisture content of the wood is determined based upon the amount of reagent dispensed into the titration solution.
    Type: Grant
    Filed: July 28, 1999
    Date of Patent: October 17, 2000
    Assignee: Riverwood International Corporation
    Inventor: Andrew M. Krause
  • Patent number: 5962328
    Abstract: An electrolytic solution for Karl Fischer coulometric titration is disclosed which consists mainly of an amine, sulfur dioxide, iodide ions, and a solvent which is a mixed solvent comprising (a) propylene carbonate and (b) a dialkylene glycol monoalkyl ether (wherein the alkylene groups and the alkyl group each have from 1 to 4 carbon atoms). The electrolytic solution, which is based on a less toxic solvent, has fewer side reactions with ketones and is useful in accurately determining the water content of ketones.
    Type: Grant
    Filed: June 25, 1997
    Date of Patent: October 5, 1999
    Assignee: Mitsubishi Chemical Corporation
    Inventors: Hiromasa Kato, Naoko Katayama
  • Patent number: 5750404
    Abstract: Novel reagents and the rapid technique were developed for the simultaneous determination of water and ene-diols or thiols in chemical products, drugs and other materials which are inaccessible for direct K. Fischer titration. The reagents include iodine, tetramethylammonium iodide or potassium iodide, non-toxic organic or inorganic base adapted to provide a pH in range of 5.5 to approximately 8.0 (diethanolamine, thriethanolamine, sodium acetate or/and urea) in methanol or another alcohol mixed with N,N-dimethyl-formamide, or with formamide, or with dimethyl sulfoxide and N,N dimethylformamide mixture as a solvent. The use of the reagents is based on the consecutive titration first a) of an ene-diol or thiol by the novel reagents and then b) of water by a conventional K. Fischer reagent in the same cell in a system protected from water vapour and oxygen, with the help of the double burette for electrometric location of the end point in both titrations (or a multistage titroprocessor).
    Type: Grant
    Filed: August 12, 1996
    Date of Patent: May 12, 1998
    Inventors: Felix Sherman, Ilya Kuselman, Avinoam Shenbar
  • Patent number: 5567618
    Abstract: The present invention relates to a Karl Fischer reagent for the determination of water, characterized in that it contains tetrahydrofurfuryl alcohol (THFA) as alcohol component.
    Type: Grant
    Filed: May 18, 1995
    Date of Patent: October 22, 1996
    Assignee: Riedel-De Haen Aktiengesellschaft
    Inventor: Eugen Scholz
  • Patent number: 5466606
    Abstract: The invention relates to the use of N-methylformamide as solvent in the determination of water by the Karl Fischer method.
    Type: Grant
    Filed: August 22, 1994
    Date of Patent: November 14, 1995
    Assignee: Riedel-De Haen Aktiengesellschaft
    Inventor: Eugen Scholz
  • Patent number: 5453377
    Abstract: Various methods are described for producing volumetric one-component iodine-free Karl Fischer reagents useful for determining the water content of a sample, the reagents containing triiodide as the dominant oxidizing species. The reagents contain a reducing agent such as SO.sub.2, a buffer such as amine, a solvent, and an oxidizing agent that is triiodide, generally in the form of triiodide ions. The molar amount of SO.sub.2 in these reagents is greater than the molar amount of triiodide. The characteristics of these methods generally include the formation of triiodide in a first solution having a first amine/SO.sub.2 ratio prior to obtaining a final solution having the final amine/SO.sub.2 ratio. These methods provide economies in the ingredients used, and yield reagents exhibiting good liter strength and enhanced reproducibility of properties from one production run to the next.
    Type: Grant
    Filed: June 21, 1994
    Date of Patent: September 26, 1995
    Inventor: Harald Dahms
  • Patent number: 5401662
    Abstract: In the method for the determination of water, the sample is admixed with a molar 1:1 adduct of sulphur dioxide with an amine having a pK.sub.A of more than 6, dissolved in an aprotic solvent, and is oxidized with iodine.
    Type: Grant
    Filed: September 13, 1993
    Date of Patent: March 28, 1995
    Assignee: Riedel-de Haen Aktiengesellschaft
    Inventors: Hermann Matschiner, Claus-Peter Maschmeier
  • Patent number: 5389545
    Abstract: An essentially iodine-free and pyridine-free single component reagent for volumetric water analysis using the Karl Fischer reaction, a process for making the reagent, and the use of the reagent to determine the water content of a sample. The reagent contains triiodide ions as an oxidizing agent, a buffer such as an amine, a reducing agent such as SO.sub.2, and a solvent. The presence of iodine, if any, is in an amount less than 1% of the amount of the triiodide ions.
    Type: Grant
    Filed: July 26, 1993
    Date of Patent: February 14, 1995
    Inventor: Harald Dahms
  • 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: 5292413
    Abstract: The present invention relates to a catholyte for the Karl Fischer coulometric water determination, which is characterized in that it is composed of a solution of one or more salts of an organic nitrogen base and acid in a solvent.
    Type: Grant
    Filed: July 6, 1992
    Date of Patent: March 8, 1994
    Assignee: Riedel-De Haen Aktiengesellschaft
    Inventor: Eugen Scholz
  • Patent number: 5246863
    Abstract: An improved technique and apparatus for automatic titration for determining the water content of a sample by a Karl Fischer (K.F.) reaction. Rather than requiring titration from one endpoint to another identical endpoint, each determination is made using a calibration relative to the water equivalent of a known amount of titrant together with the change in sensor output that occurs when a sample is added to the K.F. reagent. Improved accuracy and speed of analysis results.
    Type: Grant
    Filed: December 9, 1991
    Date of Patent: September 21, 1993
    Inventor: Harald Dahms
  • Patent number: 5187101
    Abstract: An electrolytic solution for Karl Fischer's coulometric titration comprising a iodide ion, sulfur dioxide, a basic compound and a solvent, and a method for measuring a water content using the same are disclosed. In the electrolytic solution, the basic compound is a mixture comprising an amino alcohol and a compound represented by formula (I): ##STR1## wherein n represents an integer of from 1 to 3, the amino alcohol is present at a molar ratio of not more than 1 to sulfur dioxide, and the amino alcohol and compound represented by formula (I) is present at a total molar ratio of from 1 to 5 to sulfur dioxide. The electrolytic solution is free from a pyridine odor, applicable either as an anolyte or as a catholyte, and capable of considerably reducing time required for water content measurement.
    Type: Grant
    Filed: May 23, 1991
    Date of Patent: February 16, 1993
    Assignee: Mitsubishi Kasei Corporation
    Inventors: Hiromasa Kato, Yuka Fujimoto, Akiyoshi Nozawa, Shinichi Kuwata
  • Patent number: 5179024
    Abstract: An improved K.F. solution for colorimetric analysis to determine the water content of an unknown sample, and an improved sealed vial or ampule containing this solution and a process for determining water content using this solution and the sealed vial. The ampule is designed so that it can be broken into discrete parts, where an air-tight seal is maintained by the presence of an elastic band located in the area where the vial is broken. A syringe needle is used to pierce the elastic band to inject a precisely controlled amount of unknown sample into the vial. The K.F. solution is optimally comprised of a reducing ion such as SO.sub.2, a buffer including imidazole or its derivatives, iodine, iodide, and a solvent which can include a halogenated hydrocarbon.
    Type: Grant
    Filed: May 30, 1991
    Date of Patent: January 12, 1993
    Inventor: Harald Dahms
  • Patent number: 5139955
    Abstract: Reagent for the coulometric determination of water in a membrane-free cell, composed of an alcoholic solvent or solvent mixture in which imidazole and/or an imidazole derivative and/or diethanolamine and/or triethanolamine and sulphur dioxide and an iodide or plurality of iodides and optionally a conducting salt or plurality of conducting salts are dissolved. A membrane-free cell and method for the coulometric determination of water using this reagent are also disclosed.
    Type: Grant
    Filed: February 7, 1990
    Date of Patent: August 18, 1992
    Assignee: Riedel-De Haen AG
    Inventor: Eugen Scholz
  • Patent number: 5102804
    Abstract: The invention relates to a Karl-Fischer reagent, kit and a process for the determination of water with the aid of this reagent, which contains, instead of iodine, an approximately equimolar amount of iodine halides and salts of aromatic nitrogen-containing heterocyclic compounds.
    Type: Grant
    Filed: December 26, 1990
    Date of Patent: April 7, 1992
    Assignee: Merck Patent Gellschaft mit beschrankter Haftung
    Inventors: Wolfgang Fischer, Gerhard Wieland, Karl-Dieter Krenn
  • Patent number: 5086000
    Abstract: The invention relates to a process for the preparation of alkylenebis(2-pyridylamine) compounds by reacting 2-halopyridine derivatives with alkylenediamines and to the use of these compounds in a Karl Fischer reagent as are indicated for the determination of water content.
    Type: Grant
    Filed: November 20, 1990
    Date of Patent: February 4, 1992
    Assignee: Merck Patent Gesellschaft mit beschrankter Haftung
    Inventors: Rolf Pohlke, Wolfgang Fischer
  • Patent number: 5055309
    Abstract: A kefir-like fermented milk is produced from a raw material, which contains lactose and at least one sugar, by subjecting the lactose to lactic acid fermentation with a lactic acid bacterium and the sugar to alcoholic fermentation with a yeast. The alcoholic fermentation is controlled, for example, by conducting same with a lactose non-fermenting and galactose non-fermenting yeast until all assimilable sugar sources are substantially eliminated. A gelatinous kefir-like fermented milk is also produced by controlling the alcoholic fermentation to start after addition of a gelling agent.
    Type: Grant
    Filed: June 15, 1989
    Date of Patent: October 8, 1991
    Assignee: Yakult Honsha Co., Ltd.
    Inventors: Taketsugu Saita, Yoshiharu Kuma, Norio Bukawa, Tomoko Saga
  • Patent number: 4929314
    Abstract: A high pressure coulometric titration apparatus features a pressure vessel for containing a titration vessel, which is capable of being subjected to a pressure above the vaporization pressure of the sample to be analyzed. A back pressure regulator is employed to maintain the internal chamber created by the pressure vessel at this predetermined pressure level, so that the sample will remain in a liquid phase throughout the analysis. A fluid control arrangement is also provided for sweeping the chamber with a dry, inert gas, as well as conveying a predetermined amount of the sample to the titration vessel. This fluid control arrangement in combination with the pressure vessel operates to insure that all of the water in the sample will be trapped in the solvent, as well as to prevent the introduction of extraneous water into the system.
    Type: Grant
    Filed: July 7, 1989
    Date of Patent: May 29, 1990
    Assignee: The Dow Chemical Company
    Inventors: Frederick Simonson, III, Timothy M. Gunn