By Use Of A Karl Fischer Reagent Patents (Class 436/42)
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Patent number: 4874709Abstract: 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: GrantFiled: July 12, 1988Date of Patent: October 17, 1989Assignee: Merck Patent Gesellschaft mit Beschrankter HaftungInventors: Wolfgang Fischer, Karl D. Krenn
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Patent number: 4851352Abstract: 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: GrantFiled: June 13, 1986Date of Patent: July 25, 1989Assignee: Merck Patent Gesellschaft Mit Beschrankter HaftungInventors: Wolfgang Fischer, Edda Arlt, Karl D. Krenn
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Patent number: 4802957Abstract: 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: GrantFiled: April 10, 1986Date of Patent: February 7, 1989Assignee: Mitsubishi Chemical Industries LimitedInventors: Sinichi Kuwata, Hiromasa Katoh, Mitsumasa Ono
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Patent number: 4786602Abstract: 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: GrantFiled: May 15, 1986Date of Patent: November 22, 1988Inventor: Harald Dahms
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Patent number: 4748126Abstract: 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: GrantFiled: March 19, 1981Date of Patent: May 31, 1988Assignee: Riedel-de Haen AGInventors: Wolfgang Fischer, Karl-Dieter Krenn
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Patent number: 4740471Abstract: 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: GrantFiled: December 5, 1983Date of Patent: April 26, 1988Assignee: Riedel-De Haen AktiengesellschaftInventor: Eugen Scholz
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Patent number: 4725552Abstract: 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: GrantFiled: May 21, 1984Date of Patent: February 16, 1988Inventor: Harald Dahms
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Patent number: 4720464Abstract: 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: GrantFiled: November 26, 1984Date of Patent: January 19, 1988Assignee: Mitsubishi Chemical Industries, LimitedInventors: Sinichi Kuwata, Hiromasa Katoh, Mitsumasa Ono
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Patent number: 4703014Abstract: 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: GrantFiled: February 27, 1985Date of Patent: October 27, 1987Assignee: Merck Patent Gesellschaft mit beschrankter HaftungInventors: Wolfgang Fischer, Karl-Dieter Krenn
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Patent number: 4664756Abstract: 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: GrantFiled: December 27, 1984Date of Patent: May 12, 1987Assignee: Kyoto Electronics Manufacturing Co., Ltd.Inventors: Toshiyuki Shimizu, Yoshitomo Furukawa
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Patent number: 4647542Abstract: 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: GrantFiled: March 27, 1985Date of Patent: March 3, 1987Assignee: Merck Patent Gesellschaft mit beschrankter HaftungInventors: Wolfgang Fischer, Karl-Dieter Krenn
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Patent number: 4619900Abstract: 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: GrantFiled: August 6, 1984Date of Patent: October 28, 1986Assignee: Hoechst AktiengesellschaftInventor: Eugen Scholz
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Patent number: 4550083Abstract: 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: GrantFiled: February 14, 1983Date of Patent: October 29, 1985Assignee: Merck Patent Gesellschaft mit beschrankter HaftungInventors: Wolfgang Fischer, Georg Seitz, Karl-Dieter Krenn
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Patent number: 4429048Abstract: 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: GrantFiled: August 27, 1982Date of Patent: January 31, 1984Assignee: Riedel-de Haen Ag.Inventor: Eugen Scholz
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Patent number: 4416997Abstract: 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: GrantFiled: December 21, 1981Date of Patent: November 22, 1983Assignee: Merck Patent Gesellschaft mit beschrankter HaftungInventors: Wolfgang Fischer, Karl-Dieter Krenn
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Patent number: 4385124Abstract: 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: GrantFiled: January 13, 1982Date of Patent: May 24, 1983Assignee: J. T. Baker Chemicals B.V.Inventors: Antonie E. Verbeek, Jozef M. J. Mattheij
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Patent number: 4378972Abstract: 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: GrantFiled: November 26, 1980Date of Patent: April 5, 1983Assignee: Riedel-De Haen AktiengesellschaftInventor: Eugen Scholz