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US3896659A Expired / Lapsed US ⏱️ 0.0 years remaining

Method for determining the ethanol content of alcoholic beverages

Assignee: Bacardi and Co Ltd
•
Filing: 1973-10-04
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Granted: 1975-07-29
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Expires: 1993-10-04
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Abstract

Abstract The volumetric ethanol content of a liquid mixture containing water and ethanol (e.g., an alcoholic beverage) is determined by gas-solid chromatography using aqueous ethanol of known composition as an external calibration standard. A pre-determined volume of sample mixture to be analyzed is injected into a gas chromatographic column containing a solid hydrophobic microporous adsorbent and chromatographed. The adsorbent is a non-polar organic copolymer derived from divinyl benzene as a cross-linking agent and a hydrocarbon monomer possessing a polymerizable CH CH2 substituent (e.g., styrene, ethylvinyl benzene). An external calibration standard prepared by mixing a known volume of water with a known volume of ethanol is likewise separately chromatographed. The components of each injected sample are separated as they travel through the column and then detected by a thermal conductivity detector, thereby generating signals which are amplified and converted to digital form. The digital values corresponding to the amplified detector signals are transmitted to an integrator. Concurrently, analog signals can be transmitted to a chart recorder which registers the signals on a chromatogram as a series of peaks corresponding to the water and ethanol components of the sample mixture and external standard. The integrator provides a report of the numerical areas under the peaks, which is subjected to mathematical treatment to arrive at the volumetric content of ethanol in the sample mixture.

Inventors

  • 👤 Donald E Goodman

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-09 05:04
CPC Classifications
G; G01; G01N; G01N33/00; G01N33/02; G01N33/14; G01N33/146; G01N30/00; G01N30/02; G01N30/88

Claims Analysis

Total Claims: 9
Claim 1
Independent Claim 229 words
A HIGH-RESOLUTION METHOD FOR DETERMINING THE PROOF, PX, OF AN ALCOHOLIC BEVERAGE CONTAINING WATER AND ETHANOL, SAID METHOD COMPRISING THE STEPS OF: A. FORMING A SOLUTION OF A KNOWN VOLUME OF ETHANOL AND A KNOWN VOLUME OF WATER AND HAVING A KNOWN PROOF, P1, WHEREIN THE VOLUMETRIC RATIO OF ETHANOL-TO-WATER, R1, IS GREATER THAN THE VOLUMETRIC RATIO OF ETHANOL-TO-WATER, RX, IN THE BEVERAGE, B. FORMING A SOLUTION OF A KNOWN VOLUME OF ETHANOL AND A KNOWN VOLUME OF WATER AND HAVING A KNOWN PROOF, P2, WHEREIN THE VOLUMETRIC RATIO OF ETHANOL-TO-WATER, R2, IS LESS THAN THE VOLUMETRIC RATIO OF ETHANOL-TO-WATER IN THE BEVERAGE, C. SUBJECTING THE SOLUTION FORMED IN STEPS (A) AND (B) AND THE BEVERAGE TO GAS-SOLID CHROMATOGRAPHY IN A COLUMN CONTAINING A SOLID, MICROPOROUS, HYDROPHOBIC ORGANIC POLYMERIC ABSORBENT OF HIGH SURFACE AREA DERIVED FROM THE COPOLYMERIZATION OF DIVINYL BENZENE AND A VINYL HYDROCARBON MONOMER, D. PASSING THE BEVERAGE AND SOLUTIONS CHROMATOGRAPHED IN STEP (C) THROUGH A THERMAL CONDUCTIVITY DETECTOR TO GENERATE A SIGNAL CORRESPONDING TO EACH COMPONENT OF THE SOLUTIONS FORMED IN STEPS (A) AND (B) AND THE BEVERAGE, E. CONVERTING THE SIGNALS GENERATED IN STEP (D) TO NUMERICAL VALUES CORRESPONDING TO THE VOLUMES OF WATER AND ETHANOL IN THE SOLUTIONS FORMED IN STEPS (A) AND (B) AND THE BEVERAGE, AND F. SUBJECTING THE NUMERICAL VALUES OBTAINED IN STEP (E) TO MATHEMATICAL TREATMENT ACCORDING TO THE RELATIONSHIP
Claim 2
Dependent Claim 229 words
A HIGH-RESOLUTION METHOD FOR DETERMINING THE PROOF, PX, OF AN ALCOHOLIC BEVERAGE CONTAINING WATER AND ETHANOL, SAID METHOD COMPRISING THE STEPS OF: A. FORMING A SOLUTION OF A KNOWN VOLUME OF ETHANOL AND A KNOWN VOLUME OF WATER AND HAVING A KNOWN PROOF, P1, WHEREIN THE VOLUMETRIC RATIO OF ETHANOL-TO-WATER, R1, IS GREATER THAN THE VOLUMETRIC RATIO OF ETHANOL-TO-WATER, RX, IN THE BEVERAGE, B. FORMING A SOLUTION OF A KNOWN VOLUME OF ETHANOL AND A KNOWN VOLUME OF WATER AND HAVING A KNOWN PROOF, P2, WHEREIN THE VOLUMETRIC RATIO OF ETHANOL-TO-WATER, R2, IS LESS THAN THE VOLUMETRIC RATIO OF ETHANOL-TO-WATER IN THE BEVERAGE, C. SUBJECTING THE SOLUTION FORMED IN STEPS (A) AND (B) AND THE BEVERAGE TO GAS-SOLID CHROMATOGRAPHY IN A COLUMN CONTAINING A SOLID, MICROPOROUS, HYDROPHOBIC ORGANIC POLYMERIC ABSORBENT OF HIGH SURFACE AREA DERIVED FROM THE COPOLYMERIZATION OF DIVINYL BENZENE AND A VINYL HYDROCARBON MONOMER, D. PASSING THE BEVERAGE AND SOLUTIONS CHROMATOGRAPHED IN STEP (C) THROUGH A THERMAL CONDUCTIVITY DETECTOR TO GENERATE A SIGNAL CORRESPONDING TO EACH COMPONENT OF THE SOLUTIONS FORMED IN STEPS (A) AND (B) AND THE BEVERAGE, E. CONVERTING THE SIGNALS GENERATED IN STEP (D) TO NUMERICAL VALUES CORRESPONDING TO THE VOLUMES OF WATER AND ETHANOL IN THE SOLUTIONS FORMED IN STEPS (A) AND (B) AND THE BEVERAGE, AND F. SUBJECTING THE NUMERICAL VALUES OBTAINED IN STEP (E) TO MATHEMATICAL TREATMENT ACCORDING TO THE RELATIONSHIP
Claim 3
Dependent Claim 55 words
A method according to claim 1 wherein the solid adsorbent had an average pore diameter of less than about 100 Angstroms, a surface area of at least about 250 square meters per gram, and is derived from the copolymerization of divinyl benzene and a vinyl aromatic hydrocarbon monomer containing a single polymerizable -CH CH2 substituent.
Claim 4
Dependent Claim 19 words
A method according to claim 2 wherein the adsorbent is derived from the copolymerization of divinyl benzene and styrene.
Claim 5
Dependent Claim 20 words
A method according to claim 2 wherein the adsorbent is derived from the copolymerization of divinyl benzene and ethylvinyl benzene.
Claim 6
Dependent Claim 25 words
A method according to claim 1 wherein the solutions formed in steps (a) and (b) and the beverage are each diluted with a liquid diluent.
Claim 7
Dependent Claim 15 words
A method according to claim 5 wherein the diluent consists essentially of n-propanol and tetrahydrofuran.
Claim 8
Dependent Claim 46 words
A method according to claim 5 wherein; the column used in step (c) is operated at a temperature of between about 100*C. and about 200*C.; and the thermal conductivity detector used in step (d) is operated at a temperature of between about 150*C. and about 250*C.
Claim 9
Dependent Claim 42 words
A method according to claim 7 wherein: the column is operated in step (c) at a temperature between about 130*C. and about 150*C.; the thermal conductivity detector is operated in step (d) at a temperature of between about 190*C. and about 210*C.

References Cited (Backward Citations)

US3177138A Cited
US3306096A Cited
US3717028A Cited
US3557531A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1978-07-28 1979-01-27 1979-07-29 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1982-07-28 1983-01-27 1983-07-29 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1986-07-28 1987-01-27 1987-07-29 $7700.00 Window Closed / Lapsed

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