By Use Of A Karl Fischer Reagent Patents (Class 436/42)
  • Patent number: 4874709
    Abstract: The invention relates to a solvent for the Karl-Fischer determination of water and to a process for the determination of water using a solvent system which contains at least one higher alcohol as well as the customary Karl-Fischer solvents.
    Type: Grant
    Filed: July 12, 1988
    Date of Patent: October 17, 1989
    Assignee: Merck Patent Gesellschaft mit Beschrankter Haftung
    Inventors: Wolfgang Fischer, Karl D. Krenn
  • Patent number: 4851352
    Abstract: A solvent composition useful for the determination of water by the Karl Fischer method, comprises an ethylene glycol monoalkyl ether and a tetraalkylated ammonium salt.
    Type: Grant
    Filed: June 13, 1986
    Date of Patent: July 25, 1989
    Assignee: Merck Patent Gesellschaft Mit Beschrankter Haftung
    Inventors: Wolfgang Fischer, Edda Arlt, Karl D. Krenn
  • Patent number: 4802957
    Abstract: An electrolytic solution for Karl Fischer's coulometric titation and a method for measuring the water content of a sample using the same are disclosed. The electrolytic solution contains iodine or an iodide, sulfur dioxide, an amine and a solvent, wherein the amine is a pyridine derivative, imidazole or an imidazole derivative and the solvent is a mixture of (a) a polyhydric alcohol or an ether compound thereof, (b) methanol and (c) a halogenated hydrocarbon or an aromatic hydrocarbon. The measurement method achieves a high precision with reduced measurement time and is suitable for making water content measurements using a water content vaporization method.
    Type: Grant
    Filed: April 10, 1986
    Date of Patent: February 7, 1989
    Assignee: Mitsubishi Chemical Industries Limited
    Inventors: Sinichi Kuwata, Hiromasa Katoh, Mitsumasa Ono
  • Patent number: 4786602
    Abstract: A method for the colorimetric determination of water content of an unknown sample, using the Karl Fischer reaction. The Karl Fischer reagent in a container has added to it a dye whose optical absorption preferably does not overlap with the optical absorption of the Karl Fischer reagent. Measurement of the optical absorption of the reagent/dye mixture is then made at two wavelengths, one wavelength being strongly absorbed by iodine in the reagent while the other wavelength is strongly absorbed by the dye. After the unknown sample is added, optical absorption measurements are again made at the two wavelengths. The measurements made at the wavelength where the dye strongly absorbs are used to correct the optical absorption measurements made at the wavelength where iodine strongly absorbs. This corrects for all factors affecting optical density other than the amount of water in the unknown sample.
    Type: Grant
    Filed: May 15, 1986
    Date of Patent: November 22, 1988
    Inventor: Harald Dahms
  • Patent number: 4748126
    Abstract: A pyridine-free Karl-Fischer reagent for the determination of water which comprises (a) a solvent solution containing sulfur dioxide and an amine in a Karl-Fischer reagent solvent, the amine being functionally equivalent to pyridine in a Karl-Fischer reagent, and (b) a titrating agent containing iodine in a Karl-Fischer solvent; the molar ratio of amine to sulfur dioxide being about 2:1 to about 1:1 and the reagent being essentially free of pyridine.
    Type: Grant
    Filed: March 19, 1981
    Date of Patent: May 31, 1988
    Assignee: Riedel-de Haen AG
    Inventors: Wolfgang Fischer, Karl-Dieter Krenn
  • Patent number: 4740471
    Abstract: For the titrimetric determination of small amounts of water, a Karl Fischer reagent is used which contains sulfur dioxide, iodine and a nitrogen base as essential components. The use of specific nitrogen bases in place of pyridine, which is conventionally used, is advantageous. Particularly suitable are selected aliphatic amines and nitrogen-containing heterocyclic compounds, especially imidazoles. The pyridine-free titration agent is distinguished by high storage stability and can be used as a bicomponent or monocomponent reagent.
    Type: Grant
    Filed: December 5, 1983
    Date of Patent: April 26, 1988
    Assignee: Riedel-De Haen Aktiengesellschaft
    Inventor: Eugen Scholz
  • Patent number: 4725552
    Abstract: Improved Karl Fischer reagents of the two-component type are described which eliminate problems such as inaccurate results and false end-points during titrations to determine the water content of a sample. The two-component reagent includes a vessel solution and a titrant solution, where the sample is added to the vessel solution and is titrated with the titrant in order to determine the water content of the sample. The improved vessel solution is one containing an amine such as diethanolamine or imidazole, a reducing ion such as SO.sub.2, alcohol, and iodide in an amount between 0.002 and 0.4 mol/liter. The titrant is an iodine-containing solution.
    Type: Grant
    Filed: May 21, 1984
    Date of Patent: February 16, 1988
    Inventor: Harald Dahms
  • Patent number: 4720464
    Abstract: An electrolyte for Karl Fischer coulometric titration, which contains(a) iodine or an iodine compound,(b) sulfur dioxide,(c) a halogenated hydrocarbon or an aromatic hydrocarbon,and(d)(i) an amine of the following general formula (I), an amine of the following general formula (II) and a monohydric alcohol, or(ii) an amine of the following general formula (I) and/or an amine of the following general formula (II) and a polyhydric alcohol or an ether compound thereof of the following general formula (III):General formula (I): ##STR1## wherein R.sup.1 and R.sup.2 each represent a hydrogen atom, an alkyl group, a pyridyl group or a pyrrolidinyl group;General formula (II): ##STR2## wherein R.sup.3 -R.sup.10 each represent a hydrogen atom or an alkyl group, and m is an integer of 1-5;General formula (III):R.sup.11 O--(CH.sub.2).sub.n --OR.sup.12 (III)wherein R.sup.11 and R.sup.12 each represent a hydrogen atom or an alkyl group, and n is 2 or 3.
    Type: Grant
    Filed: November 26, 1984
    Date of Patent: January 19, 1988
    Assignee: Mitsubishi Chemical Industries, Limited
    Inventors: Sinichi Kuwata, Hiromasa Katoh, Mitsumasa Ono
  • Patent number: 4703014
    Abstract: A Karl-Fischer reagent useful in a process for the determination of water contains a pyridine substitute, sulfur dioxide and iodine. As the pyridine substitute, the reagent contains at least one compound from the group comprising the guanidines, amidines, imido-esters, isoureas, cyanamide, or salts thereof with a weak organic acid.
    Type: Grant
    Filed: February 27, 1985
    Date of Patent: October 27, 1987
    Assignee: Merck Patent Gesellschaft mit beschrankter Haftung
    Inventors: Wolfgang Fischer, Karl-Dieter Krenn
  • Patent number: 4664756
    Abstract: A method of detecting an electrode potential in a Karl Fischer moisture meter comprises the step of subtracting an electrode potential which is caused by a liquid resistance of a liquid sample from an electrode potential which is generated in an end point detecting electrode in the Karl Fischer moisture meter, to thereby obtain a true polarization potential.
    Type: Grant
    Filed: December 27, 1984
    Date of Patent: May 12, 1987
    Assignee: Kyoto Electronics Manufacturing Co., Ltd.
    Inventors: Toshiyuki Shimizu, Yoshitomo Furukawa
  • Patent number: 4647542
    Abstract: A new Karl Fischer reagent contains as a pyridine substitute at least one compound of the general formula ##STR1## in which R.sup.1 and R.sup.2, which can be identical or different, =hydrogen or alkyl having 1-6 C atoms,R.sup.3 =alkyl having 1-6 C atoms,X=alkali metal ion or one equivalent of an alkaline earth metal ion,n=0 or a number from 1 to 4 andm=a number from 1 to 4.
    Type: Grant
    Filed: March 27, 1985
    Date of Patent: March 3, 1987
    Assignee: Merck Patent Gesellschaft mit beschrankter Haftung
    Inventors: Wolfgang Fischer, Karl-Dieter Krenn
  • Patent number: 4619900
    Abstract: The determination of water by the Karl Fischer method is carried out using a reagent containing sulfur dioxide, iodine and a base. The determination is carried out in a liquid medium in which the sample under investigation has been dissolved. The solvents used are, above all, methanol and 2-methoxyethanol. The presence of a further solvent which enables the reaction to take place without interference is advantageous. Solvents suitable for this purpose are lower alkanols which are substituted by halogen atoms and/or phenyl radicals. These alkanols are also employed as the solvent in Karl Fischer reagents.
    Type: Grant
    Filed: August 6, 1984
    Date of Patent: October 28, 1986
    Assignee: Hoechst Aktiengesellschaft
    Inventor: Eugen Scholz
  • Patent number: 4550083
    Abstract: A Karl Fischer reagent useful in the determination of water, comprises sulfur dioxide, iodine and a salt which is a system compatible addition compound of a nitrogen-containing organic base having a pK.sub.b <10 with a weak aromatic carboxylic acid having a pK.sub.a >2.
    Type: Grant
    Filed: February 14, 1983
    Date of Patent: October 29, 1985
    Assignee: Merck Patent Gesellschaft mit beschrankter Haftung
    Inventors: Wolfgang Fischer, Georg Seitz, Karl-Dieter Krenn
  • Patent number: 4429048
    Abstract: For the titrimetric determination of small amounts of water, the Karl Fischer reagent is used which contains sulfur dioxide, iodine and pyridine as essential components. Replacement of pyridine by specific nitrogen bases is advantageous. Particularly suitable are selected aliphatic amines and nitrogen-containing heterocyclic compounds, especially imidazoles. The pyridine-free titration agent is distinguished by high storage stability; it can be used as bicomponent or monocomponent reagent.
    Type: Grant
    Filed: August 27, 1982
    Date of Patent: January 31, 1984
    Assignee: Riedel-de Haen Ag.
    Inventor: Eugen Scholz
  • Patent number: 4416997
    Abstract: An essentially pyridine-free Karl Fischer reagent useful in the determination of water, comprises a dissolving agent containing sulfur dioxide and a pyridine substitute in a Karl Fischer solvent, and a titrating agent containing iodine in a Karl Fischer solvent, wherein the pyridine substitute is an alkali or alkaline earth metal benzoate or ammonia, and the reagent is essentially free of pyridine.
    Type: Grant
    Filed: December 21, 1981
    Date of Patent: November 22, 1983
    Assignee: Merck Patent Gesellschaft mit beschrankter Haftung
    Inventors: Wolfgang Fischer, Karl-Dieter Krenn
  • Patent number: 4385124
    Abstract: Reagent for the quantitative determination of water, used together with an iodine-containing titrating solution, the reagent being free of pyridine and containing sulfur dioxide and an anhydrous alkali metal salicylate in methanol, 2-methoxyethanol or a mixture thereof in a volume ratio of at most 90 : 10 when a mixture of methanol and 2-methoxyethanol is used, which has been neutralized with an aliphatic amine for stabilizing the pH value.This reagent is distinguished in that the increase of the blind value is restricted to a very low value even at elevated temperatures.
    Type: Grant
    Filed: January 13, 1982
    Date of Patent: May 24, 1983
    Assignee: J. T. Baker Chemicals B.V.
    Inventors: Antonie E. Verbeek, Jozef M. J. Mattheij
  • Patent number: 4378972
    Abstract: For the titrimetric determination of small amounts of water, the Karl Fischer reagent is used which contains sulfur dioxide, iodine and pyridine as essential components. Replacement of pyridine by specific nitrogen bases is advantageous. Particularly suitable are selected aliphatic amines and nitrogen-containing heterocyclic compounds, especially imidazoles. The pyridine-free titration agent is distinguished by high storage stability; it can be used as bicomponent or monocomponent reagent.
    Type: Grant
    Filed: November 26, 1980
    Date of Patent: April 5, 1983
    Assignee: Riedel-De Haen Aktiengesellschaft
    Inventor: Eugen Scholz