Apparatus, systems, and methods for oxygenating distillate spirits

Abstract

Ageing distilled spirits in wood barrels matures the spirit into a more balanced and complex final product. Disclosed are assemblies and methods for improving distilled spirit maturation. Particularly, the present invention is directed to oxygenating a distilled spirit using a container and an oxygen reservoir or air gate, thereby reducing, minimizing, or eliminating evaporation losses, while improving product sensory attributes.

Description

APPARATUS, SYSTEMS, AND METHODS FOROXYGENATING DISTILLATE SPIRITSCROSS-REFERENCE TO RELATED APPLICATIONS

[0001] The present application claims the benefit of priority of U.S. Provisional Application No. 63 / 562,398, filed March 7, 2024, which is incorporated herein by reference in its entirety.TECHNICAL FIELD

[0002] The present invention generally relates to distilled spirits. Aspects of the invention relate to improved ageing of distilled spirits.BACKGROUND OF THE INVENTION

[0003] The flavor, aroma, color and texture of a newly distilled whiskey, brandy or rum is quite different from that of the final aged spirit. Newly distilled whiskey typically has a raw and harsh quality, with a sharp and fiery taste, lacking the smoothness and complexity consumers look for in a mature spirit. Ageing in wood barrels is where many of the desirable changes occur, as the spirit interacts with the wood, undergoes chemical reactions, and matures into a more balanced and complex final product.

[0004] For centuries, wooden barrels have been used to store and carry foods and other valuable products. They were specifically designed to be as air-tight and leak-free as possible to prevent spoilage and damage of the goods they held. As storage of wine, spirits and beer was common practice, over time it was discovered that longer storage imparted favorable flavors and aromas to the liquid, modifying its harsh taste.

[0005] Unfortunately, a consequential amount of a spirit’s volume is lost as the spirit ages. Maturation of distilled spirits in standard barrels takes many years to complete and is accompanied by a slow evaporative loss of ethanol and water through the porous wood and small gaps into the surrounding air, the so-called angel’s share. The annual loss is considerable, amounting to around 3.5% - 4% at the beginning of the ageing process andthen slowing down to about 2% annually (www.theglenlivet.com / en-us / articles / angels- share-meaning). At the end of a 20 year-long ageing process, a standard barrel would typically lose about a third of its initial liquid volume, a considerable loss the spirits industry has long endured. This loss continues over time and a highly valued 50-year-old whiskey may only have about a third of its original liquid volume left inside the barrel.

[0006] Distilleries in Kentucky store more than 12.6 million Bourbon barrels (Kentucky Distillers’ Association, 2023) in warehouses holding an estimated 1.9 billion liters of barrel strength Bourbon (assuming -53-gallon barrels with an average fill level of 75%). At an annual evaporation loss of 2%, about 80 million bottles of Bourbon would be lost annually (assuming cask strength of 62.5%, bottle strength of 40%, bottle size of 750 ml), an annual retail revenue loss of around $3 billion (at $40 per bottle). In Scotland, some 22 million Scotch barrels are maturing in warehouses around the country (The Scotch Whiskey Association, 2022), accruing similar annual losses.

[0007] While evaporation losses are economic burdens for distilleries, they also constitute environmental burdens. A black ethanol -fueled fungus called Baudoinia compniacensis grows on whiskey warehouse buildings and near-by properties, becoming an environmental nuisance for neighboring communities, and upsetting residents who demand compensation from distilleries (New York Times, March 1, 2023). The emission of non-methane volatile organic compounds (NMVOC) by whisky distilleries might have an impact on ozone formation and the climate and could pose a public-relation risk for the industry (Review of the Human Health and Environmental Impacts of Non -Methane Volatile Organic Compound Emissions from Malt Whisky Maturation in Scotland. Final report prepared for the Scottish Government by Aether Ltd., August 2023).

[0008] For over a century, the distilling industry has invested considerable resources to reduce, minimize, or eliminate evaporation losses, while improving product sensory attributes and accelerating spirit maturation. The slow progress made so far reflects the complexity of the physicochemical processes involved in spirit maturation and how these affect the sensory attributes of the finished product. There remains a need to improve spirit maturation.SUMMARY OF THE INVENTION

[0009] Described are novel assemblies, apparatus, systems, methods, and processes for ageing a distilled spirit under an oxygen atmosphere.

[0010] Further described are novel assemblies, apparatus, systems, methods and processes for ageing a distilled spirit in a container using an excess supply of oxygen, including but not limited to, a supply of oxygen that is greater that the supply of oxygen provided using traditional ageing. An excess supply of oxygen may be provided by a substantially continuous, unhindered, unrestricted, unlimited, and / or consistent supply of oxygen atmosphere to improve and / or accelerate its sensory attributes.

[0011] The described invention discloses systems, methods, processes, assemblies, and apparatus for oxygenating a spirit during ageing, reducing evaporation losses, accelerating maturation, and / or improving product sensory attributes. Disclosed herein are methods for ageing a distilled spirit comprising the steps of: (a) providing a substantially increased amount of oxygen for the spirit, and (b) preventing evaporation loss from the spirit.

[0012] Advantages of the present disclosure include, but are not limited to, reducing evaporation losses, accelerating maturation, and improving product sensory attributes. For example, the process and apparatus improve smoothness and complexity that consumers seek in a matured spirit. Advantages also include improved removal of a spirit’s raw or harsh quality, such as sharp or fiery taste, or lack of smoothness and complexity. The disclosed invention advances oxidation of chemical compounds that detract from the spirit’s quality. Another advantage is the reduced risk of over-oaking.

[0013] In one aspect, the invention comprises a method for improving sensory attributes of an alcoholic beverage by exposing the alcoholic beverage in a container to a supply of oxygen. In another aspect, the invention comprises a method for improving sensory attributes of an alcoholic beverage by exposing the alcoholic beverage in a container to an excess supply of oxygen. In various aspects, the supply of oxygen is an amount that is greater that the supply of oxygen provided using traditional ageing. In various aspects, the supply of oxygen is an unrestricted amount of oxygen.

[0014] In another aspect, the invention comprises a method for improving sensory attributes of an alcoholic beverage by exposing the alcoholic beverage in a container to a substantially continuous supply of oxygen. In another aspect, the method comprises exposure of the alcoholic beverage in a container to a periodic supply of oxygen under an oxygen atmosphere for a specified time. In another aspect, the method comprises exposure of the alcoholic beverage in a container to a substantially continuous supply of oxygen under an oxygen atmosphere for a specified time. A substantially continuous operation allows for temporary pauses for periodic sampling or testing of the spirit. In various aspects, the method further comprises minimizing, reducing, or substantially eliminating or substantially preventing evaporation loss of ethanol and / or water.

[0015] In another aspect, the invention comprises methods, systems, processes, apparatus, and assemblies for ageing a spirit using a headspace greater than the headspace that would be in place for traditional ageing, such as the headspace in a standard oak barrel. In another aspect, the invention comprises methods and assemblies for increasing headspace.

[0016] In one aspect, the invention comprises an assembly for use in ageing a distilled spirit. In various embodiments, the assembly comprises a closed system. In other various embodiments, the system is an open system. In one aspect, the assembly comprises a container comprising a distilled spirit, and an oxygen supply reservoir. In one nonlimiting example, the assembly is a closed system, wherein the oxygen supply reservoir is an object or container containing a supply of oxygen gas. In another non-limiting example, the assembly is an open system, wherein the oxygen supply reservoir is ambient air. In one such example of an open system, an oxygen-permeable film is attached to the container containing the distilled spirit, wherein the oxygen permeable film allows the passage of oxygen into the container from ambient air.

[0017] In one aspect, the invention comprises an assembly comprising a container having an opening to allow a continuous supply of oxygen enter the inside of the container while minimizing evaporation losses from the alcoholic beverage.

[0018] In one aspect, the invention comprises an assembly comprising a container having an opening sealed with a material penetrable to oxygen but non-penetrable to vapors from the alcoholic beverage.

[0019] In one aspect, the invention comprises an assembly comprising a container connected to a material permeable to oxygen but non-permeable to vapors or aromas from the distilled spirit.

[0020] In another aspect of the invention, the container is connected to the surrounding atmosphere via a conduit between the top of the container and a gate containing a film. The film is permeable to oxygen, maintaining an atmosphere inside the container equal to or similar to the surrounding atmosphere over a specified time but non- permeable to vapors or aromas from the distilled spirit.

[0021] In another aspect, the invention comprises an improved bung, wherein the bung is an oxygen-selective bung. In one aspect the bung comprises an air gate. Advantages of the oxygen- selective bung include but is not limited to allowing oxygen to enter the headspace of a barrel while blocking the escape of alcohol, water and volatile aroma compounds. An improved bung may increase oxygen ingress to a container such as a barrel. Such a bung may increase oxygen ingress by at least 2-fold compared to the natural oxygen uptake of a barrel.

[0022] In another aspect, the invention comprises an air gate comprising a holder and a semi-permeable film, wherein the film is permeable to oxygen and is impermeable to ethanol, water and aromas. In various aspects, the air gate is attached to a container, including but not limited to a barrel or bottle. The air gate may be optionally attached directly to the container. The air gate may be optionally attached to a container through a stopper or a bung.

[0023] In various embodiments, the air gate is attached in line between a container and an oxygen source, including but not limited to, ambient air or an oxygen supply reservoir.

[0024] In another aspect of the invention, the gate has an opening allowing oxygen from the surrounding oxygen atmosphere to enter the gate, pass through the film and enter the container, optionally via conduit.

[0025] In another aspect of the invention, the diameter of the gate is chosen to be wider than the diameter of the conduit to increase the amount of oxygen that can enter the container via the gate and the conduit.

[0026] In another aspect of the invention, the gate holder and the conduit independently comprise an impermeable material. Optionally, the holder comprises a material impermeable to ethanol and water. Optionally, the conduit comprises a material impermeable to ethanol and water.

[0027] In another aspect of the invention, the container is a barrel or a bottle.

[0028] In one aspect, the invention comprises an assembly comprising a wood container connected to an oxygen reservoir via a closed system.

[0029] In another aspect, the invention comprises a container sealed with an air-tight material. In another aspect, the invention comprises a container inside an air-tight reservoir. In another aspect of the invention, the wood container is sealed with a material non-penetrable to vapors from the distilled spirit or oxygen.

[0030] In another aspect of the invention, the wood container is an oak barrel connected to a reservoir of pure or diluted oxygen via a conduit such as a tube between the top of the barrel and the reservoir. The system is closed, maintaining a constant oxygen atmosphere inside the oak barrel over a specified time. In one non-limiting example, the tube is a stainless— steel tube.

[0031] In another aspect of the invention, the oak barrel is filled with an alcoholic beverage, allowing continuous oxidation of the alcoholic beverage to occur over a specified time. The invention comprises an oxygen reservoir made of stretchable or non- stretchable material attached airtight to the oak barrel via a tube using material non- penetrable to vapors from the alcoholic beverage or oxygen.

[0032] In another aspect of the invention, the oxygen reservoir can be attached to one, two, three or more wood containers. In one form of the invention, one oxygen reservoir is connected to one wood container via the top of the wood container with a conduit. In another form of the invention, one oxygen reservoir is connected to two or more wood containers via a conduit.

[0033] In another aspect of the invention, the wood container is inside a sealed airtight reservoir container. For example, this may be understood as a container-within-a- container. The sealed air-tight reservoir container is filled with oxygen. An opening, e.g., a hole, in the wood container allows oxygen to enter the wood container.

[0034] In various embodiments, the invention provides an assembly for ageing a distilled spirit comprising: (a) a container holding the distilled spirit to be aged; and (b) an oxygen supply reservoir.

[0035] In certain embodiments, the container comprises wood. In exemplary embodiments, the container is an oak cask. In certain embodiments, the container is sealed from the outside to prevent the liquid from permeating through the walls of the container, or to prevent oxygen escaping from the barrel.

[0036] In certain embodiments, the oxygen supply reservoir holds an inert gas - oxygen mixture. In exemplary embodiments, the oxygen supply reservoir holds an inert gas - oxygen mixture comprising an oxygen content ranging from about 1% to about 100%, ranging from about 10% to about 100% oxygen, ranging from about 21% to about 100% oxygen, ranging from about 50% to about 100%, ranging from about 75% to about 100%. In exemplary embodiments, the oxygen supply reservoir holds a volume ranging from about 0.1 L to about 10.0 L of oxygen - inert gas mixture for each 1 L of liquid. In exemplary embodiments, the oxygen supply reservoir maintains a pressure ranging from about 0.1 to about 100 atm, ranging from about 0.1 to about 10 atm, ranging from about 0.5 to about 2 atm, or of about 1 atm.

[0037] In certain embodiments, the container is attached directly or indirectly to the oxygen supply reservoir. In alternative embodiments, the container is placed inside the oxygen supply reservoir. In exemplary embodiments, the conduit is attached between the container and the oxygen supply reservoir. The conduit may optionally comprise a tube ora pipe. In exemplary embodiments, the conduit comprises an impermeable material. In exemplary embodiments, at least one container is connected to the same oxygen supply reservoir, or optionally, at least two containers are connected to the same oxygen supply reservoir. Figure 4 is an illustration showing three containers attached to a single oxygen supply reservoir and an oxygen supply tank.

[0038] In certain embodiments, the seal is a film that is impermeable to alcohol. In exemplary embodiments, the seal comprises a film or foil. In exemplary embodiments, the seal is a natural or synthetic product.

[0039] In various embodiments, the invention provides method for ageing a spirit, comprising the steps of (a) providing a container; (b) providing a reservoir; (c) adding a distilled spirit to the container; (d) adding oxygen gas or an oxygen-inert gas mixture to the reservoir; and (e) connecting the reservoir to the container.

[0040] In various embodiments, the invention provides method for oxygenating a spirit comprising the steps of (a) providing a container; (b) providing a reservoir; (c) adding a distilled spirit to the container; (d) adding oxygen gas or an oxygen-inert gas mixture to the reservoir; and (e) connecting the reservoir to the container.BRIEF DESCRIPTION OF THE DRAWINGS

[0041] FIG. 1 (A) is a drawing illustrating an example assembly comprising a container with distilled spirit attached to an oxygen supply reservoir. FIG. 1 (B) shows an example of a barrel holding a distilled spirit attached to an oxygen supply reservoir.

[0042] FIG. 2. is a drawing illustrating an example assembly comprising a container with distilled spirit attached to an oxygen supply reservoir and a pressurized oxygen tank via tubing.

[0043] FIG. 3 (A) and (B) are drawings illustrating exemplary assemblies comprising a barrel wrapped in an impermeable oxygen reservoir bag and attached to an oxygen tank.

[0044] FIG. 4 is a drawing illustrating a plurality of containers attached to a single reservoir.

[0045] FIG. 5 is a drawing illustrating an example assembly comprising three barrels enclosed within a reservoir bag.

[0046] FIG. 6 is a drawing illustrating an example assembly: (A) reservoir on top of a container connected via a tube, (B) reservoir on top of a container connected via conduit.

[0047] FIG. 7 is a drawing illustrating an example assembly: (A) barrel connected to a reservoir comprising an impermeable bag via a conduit; (B) container having an impermeable bag covering an open top of a barrel.

[0048] FIG. 8 is a flowchart illustrating an exemplary method of the present invention.

[0049] FIG. 9 (A) is a drawing illustrating an assembled view of an exemplary air gate. Fig 10 (B) shows an assembled air gate attached to a barrel. FIG. 9 (C) shows an air gate attached to a demijohn or bottle.

[0050] FIG. 10 (A) and (B) are drawings illustrating a cross-sectional view of an exemplary air gate.DETAILED DESCRIPTION OF THE INVENTION

[0051] Described are novel systems, processes, methods, assemblies, and apparatus for ageing a distilled spirit under an oxygen atmosphere to accelerate its ageing and improve its sensory attributes. Further described are novel processes to age a distilled spirit in a container such as a barrel or a bottle under a substantially continuous oxygen atmosphere to accelerate its ageing and improve its sensory attributes. Further described are systems, processes, methods, assemblies, and apparatus for oxygenating barrels or bottles during ageing of spirits, eliminating evaporation losses, accelerating maturation, and improving product sensory attributes.

[0052] Incorporation by reference

[0053] All publications, patents and other references mentioned herein are hereby incorporated by reference in their entireties.

[0054] Definitions

[0055] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which distilling and ageing a distilled spirit belongs. Terms used herein should be given a broad interpretation that also encompasses equivalent functions and features. In some cases, while several alternative terms or synonyms for structural or characteristic features are provided, such terms are not intended to be exhaustive. Descriptive terms should be given the broadest possible interpretation.

[0056] The following terms, unless otherwise indicated, shall be understood to have the following meanings:

[0057] Throughout this specification and claims, the word “comprise”, or variations such as “comprises”, or “comprising”, will be understood to imply the inclusion of a stated integer or group of integers but not the exclusion of any other integer or group of integers.

[0058] The term “a” and “an” refers to one or to more than one (i.e., to at least one) of the grammatical objects of the article. By way of example, “an element” means one element or more than one element. It is further noted that the claims may be drafted to exclude any optional element. As such, this statement is intended to serve as antecedent basis for use of such exclusive terminology as “solely”, “only”, and the like in connection with the recitation of claim elements, or use of a “negative” limitation.

[0059] Any directional terms such as “vertical”, “horizontal”, “up”, “down”, “upper”, “lower”, “on”, “under”, “above”, and “below,” may be used for convenience of explanation, and are not intended to be ultimately limiting if an equivalent function can be achieved with an alternative dimension and / or direction.

[0060] As used herein, “about” or “approximately” can mean within an acceptable error range, plus or minus less than 1 or 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 25, 30, or greater than 30 percent, depending upon the situation and known or knowable by one skilled in the art.

[0061] As used herein, units may be represented in metric or imperial. The term “mil” is a measurement that equals one-thousandth of an inch, or 0.001 inch. One mil also equals 0.0254 mm (millimeter).

[0062] As used herein, the term “assembly”, apparatus”, and “system” may be used interchangeably.

[0063] As used herein, the term “gate” or “air gate” refers to a barrier controlling the passage of oxygen and air in between, to and / or from the surrounding air and the inside of a container. A gate may also be referred to as a port or passage. In one aspect, the gate comprises a film. In another aspect, the gate comprises a film and a holder. In one aspect, an air gate refers to an oxygen-permeable film attached to a container containing distilled spirit. In another aspect, an air gate refers to an assembly comprising an oxygen- permeable film and a holder for attaching the oxygen-permeable film to the container. In one aspect, an air gate refers to an oxygen-permeable and ethanol substantially impermeable film attached to a container containing distilled spirit. In another aspect, an air gate refers to an assembly comprising an oxygen-permeable and ethanol substantially impermeable film and a holder for attaching the oxygen-permeable and ethanol substantially impermeable film to the container. In various embodiments, an air gate comprises a modified bung.

[0064] As used herein, the term “film” may refer to a sheet, foil or coating. An “air gate film” refers to a sheet that is included as a component of an air gate. In one aspect, a film comprises a thin sheet or foil of semi-permeable material. In another aspect, a film comprises a substantially non-porous sheet or substantially non-porous membrane. A “seal film” may refer to a sheet, foil, or coating acting as a barrier used to minimize or prevent liquid vapor or gas from passing into or out of a container. In one aspect, a seal comprises a thin sheet, foil, or coating of impermeable material.

[0065] Typically, a substantially non-porous film is a dense thin film. A film may also be referred to as a substantially non-porous membrane. Typically, transport through non-porous membranes, at a molecular level, is by a solution-diffusion mechanism in which separation is achieved by differences in solubility and / or diffusivity of solutes (Scott K. 1995. Handbook of Industrial Membranes (2ndEd.)).

[0066] In various embodiments, the non-porous film comprises a density of at least about 100 kg / m3, at least about 1000 kg / m3, at least about 2,000 kg / m3, or at least about 3,000 kg / m3. In various embodiments, the non-porous film comprises a density ranging from about 1000 kg / m3to at least about 2,000 kg / m3. In various embodiments, the non- porous film comprises a density ranging from about 2000 kg / m3to about 3,000 kg / m3. In various embodiments, the non-porous film comprises a density of about 2000 kg / m3. In various embodiments, the non-porous film comprises a density of about 2150 kg / m3.

[0067] As used herein, the term “oxygen transfer rate” (OTR) refers to the transfer of oxygen from the surrounding air to the inside of a container. In gas-liquid systems, oxygen transfer rate is typically expressed in units of g / (m2day), w / v oxygen mass per surface area per time. As a non-limiting example, an annual rate of oxygen entry into a barrel is the amount of oxygen that enters a barrel full of distilled spirit over the course of a year; the unit of measure being mg / L / year. One study using French oak estimates that a typical oxygen transfer rate to be about 14 mg oxygen / L / year (Junqua, R., Zeng, L., Pons, A. (2021). OENE One, 3, 53-65).

[0068] Atmospheric oxygen enters the barrel during ageing. The first mention of this phenomenon was reported by Ribereau-Gayon in 1931 (Ribereau-Gayon J 1931.Contribution A L’ etude Des Oxydations Et Reductions Dans Les Vins. Universite de Bordeaux, Bordeaux). This and subsequent studies found the oxygen transfer rate (OTR) of wine oak barrels to be between 0.7 and 97 mg / L year (Del Alamo-Sanza M, Nevares I. 2019. Oak Wine Barrel as an Active Vessel: A Critical Review of Past and Current Knowledge. Crit Rev Food Sci Nut. 58(16): 2711-2726). Accordingly, between 0.1575 and 21.825 g oxygen would enter a 225 L (59 gallon) standard wine barrel in a year. A standard wine barrel has a height of about 88-95 cm, a diameter at the widest point of about 70 cm, and a diameter at the heads of around 56-60 cm. With an average stave thickness of 2.5 cm, the inner surface area would be between 19,423 square centimeters and 21,821 square centimeters. The permeability would then be between 3.7 (mL mm) / (m2 atm day) and 513.3 (mL mm) / (m2atm day), assuming an oxygen partial pressure difference of 0.105 atm between both sides of the film. In a more recent study, the OTR in a wine barrel with a stave thickness of 2.7 cm was found to be 26 mL / L year,equivalent to a permeability of 137.6 (mL mm) / (m2atm day). The total oxygen ingress into a standard wine barrel of 225 L would therefore be 225 L x 26 mL / L = 5,850 mL.

[0069] As used herein, the term “oxygen dissolution rate” (ODR) refers to the rate at which oxygen dissolves into a spirit. For example, the ODR is the rate at which oxygen gas from a barrel’s headspace dissolves into a distilled spirit. The term “oxygenation”, in general, refers to the process of increasing concentrations of oxygen within a material. The term “oxygen dissolution”, in general, refers to the rate at which oxygen, as a solute in gaseous form, dissolves into a solvent to form part of a solution. The oxygen concentration at saturation of an alcohol water mixture at 62.5% alcohol -by-volume (ABV) is estimated at about 25 mg / L (Shchukarev SA, Tolmacheva TA. 1968. Solubility of Oxygen in Ethanol - Water Mixtures. Zh Strukt Khim 9(1): 21-28).

[0070] As used herein, the terms “spirit,” “distillate spirit”, and “distilled spirit,” may be used interchangeably. A distilled spirit may refer to a spirit at any time point in the manufacturing and bottling process. For example, a distilled spirit includes, but is not limited to, a raw spirit, a new make spirit, a spirit undergoing an ageing process, a matured spirit, and a distilled beverage product. A distilled beverage product may also be referred to as a final beverage for bottling ready for commercial sale and consumption. Typically, the term distilled spirit is used to distinguish a beverage from other alcoholic or non-alcoholic beverages such as wine or beer.

[0071] Distilled spirits are generally understood as types of beverages with a significantly higher alcoholic content than wine or beer. Also known as “distilled liquor” or “hard liquor,” this class of alcoholic drink encompasses brandy, rum, tequila, vodka, whiskey, and gin, among others. Distilled spirits are typically produced through yeast- driven fermentation of plants, fruit juice, or other carbohydrate-rich grains, followed by boiling or “distilling” (e.g., selective boiling and condensation).

[0072] All forms of alcohol undergo a fermentation phase, but at some point (generally between about 14-18%), the alcohol concentration becomes toxic to the yeast and thus further fermentation is halted. The distillation step is unique to spirits and is used primarily to increase the alcohol percentage in the final product to 30 percent and higher. The mixture is optionally given additives, filtered, sterilized, and packaged or bottled(Visual Encyclopedia of Chemical Engineering Equipment, University of Michigan, Department of Chemical Engineering).

[0073] As used herein, the terms “new make spirit”, “raw spirit”, “fresh spirit”, “fresh malt spirit”, “new spirit”, or “unrefined spirit” may refer to spirit e.g. obtained by mashing of malt or equivalent raw material followed by lautering, fermentation and distillation before maturation in contact with wood. However, it is noteworthy that a spirit may be treated according to the invention at any appropriate stage of production. For example, a spirit may be removed from a wooden barrel for transfer to another and be treated during the transition or at any other time to assist in ageing of the spirit before human consumption.

[0074] As used herein the terms “matured” or “aged spirits” may be used interchangeably. A matured spirit may refer to spirits that have been transitioned from raw (or unrefined) spirits toward a state having one or more selected profile characteristics, such as flavor, aroma, texture, etc. Such transition may be referred to as “maturation” or “maturing”. Typically, such maturation of spirits has been achieved by barrel-based ageing processes. Matured spirits may also sometimes be referred to as “aged spirits”. As discussed herein, a matured spirit (or maturation or maturing) may be achieved in different time frames, and the term matured (or maturation or maturing) as used in reference to the various embodiments is not intended to imply any specific time period and is not intended to limit the various embodiments or claims to any specific time period.

[0075] As used herein, the term “solution” is afforded the meaning as typically understood in the art. In particular, a solution in the chemical art is understood as a homogeneous mixture composed of two or more substances. In such a mixture, a solute is a substance dissolved in another substance, known as a solvent. As a non-limiting example, a spirit may be a solution comprising water and ethanol. The terms “spirit” and “solution” may be used herein interchangeably.

[0076] As used herein, the term “beverage” is afforded the meaning generally understood in the art as a liquid intended for human consumption. Typically, a beveragecomprising ethanol may also be called an alcoholic beverage, adult beverage, alcoholic drink, strong drink, or simply a drink.

[0077] As used herein, the term “container” refers to an object used to hold a solution. In a non-limiting example, a container holds a distilled spirit. A container may also be referred to as a “vessel.” Examples of suitable containers include, but are not limited to, barrels, casks, tanks, jugs, demijohns, carboys, drums and bottles.

[0078] As used herein, the term “reservoir” refers to an object used to hold a gas. In a non-limiting example, a reservoir is used to hold a gas comprising oxygen, e.g., an oxygen / nitrogen gas mixture or substantially pure oxygen. A reservoir comprising oxygen gas may also be referred to as an “oxygen reservoir” or “oxygen supply reservoir”.

[0079] As used herein, the term “barrel” and “cask” may be used interchangeably. A “cask” as understood in the art, is typically a barrel-shaped vessel comprising staves, heads, and hoops. A cask may refer to the cask itself. A cask may also refer to the cask plus its contents collectively. A cask may also refer to the quantity of contents contained within the cask.

[0080] A “barrel” is afforded the meaning as typically understood in the art. Alternatively, a barrel may also be referred to as a drum. A cask may be a new cask or a used cask. A “used cask” as used herein refers to a cask, which has previously been used for ageing an alcoholic beverage. As a nonlimiting example, a used cask may have been used for ageing wine, rum, whisky, port, or sherry.

[0081] As used herein, the term “opening” in reference to a container such as a barrel, cask, or air gate, may refer to any one or more access point, opening, portal, or hole that may allow oxygen gas or oxygen-inert gas mixture through, into, or out of a container or air gate. Suitable openings may be used to connect a container to a reservoir and / or a gate. Openings may be any shape, including but not limited to circles, ellipses, or polygons. Examples of suitable openings include, but are not limited to, a bung hole, any other hole bored through a barrel, or a barrel with one of its heads removed. In various embodiments, the opening is threaded.

[0082] As used herein, the terms “bung”, “bung plug”, and “stopper”, may be used interchangeably, A bung can be any suitable bung as typically understood in the art to cap, close, or seal a bunghole, opening, or any other access point to a barrel. Examples of suitable bungs include, but are not limited to, wood, plastic, cork and cork-like stoppers. In various embodiments, the bung comprises natural, synthetic or a combination of natural and synthetic materials. In various embodiments, the bung is a silicone stopper. In various embodiments, the bung is a wooden stopper. In various embodiments, the bung comprises oak, acacia, chestnut, cherry, mulberry, elm, beech, ash, juniper, black locust, apple, maple, hickory, cedar, juniper, pine, spruce, or bamboo. In various embodiments, the bung is a rubber stopper. A bung may be tapered, or untampered. In various embodiments, the bung is threaded. A bung may be solid or comprise a hole. In various embodiments, the bung comprises a stopper comprising a hole to which a conduit is attached or passed though from top to bottom or otherwise outside to inside a container. In a non-limiting example, a stainless-steel pipe conduit is inserted through a hole in a silicone stopper. In a non-limiting example, a plastic or rubber hose conduit is inserted through a hole in a silicone stopper. In a non-limiting example, an air gate is inserted through a hole in a bung or silicone stopper. In various embodiments, the bung comprises an opening and a cover. Optionally, the cover comprises a hinge attachment to the bung opening. Optionally, the bung comprises a hinged cupola lid.

[0083] In various embodiments, a bung comprises a cap or lid. The cap or lid may be threaded or non-threaded. Alternatively, the cap comprises a flip-top, or flip lock snap handle. In various embodiments, the bung further comprises a gasket or seal. In one nonlimiting example, the bung comprises a steel cap and a gasket.

[0084] As used herein, the term “housing” describes a component that supports or substantially encloses another component. In one aspect, a housing encloses or supports a container. A housing may comprise one or more parts or components. A housing may comprise a rigid or flexible material.

[0085] In another aspect, a housing, in reference to an air gate, is a component of the air gate, wherein the housing holds, encloses or supports a film. As used herein, the term “gate housing” or “air gate housing” may refer to a support means or a holder for a film.

[0086] As used herein, the term “holder” describes a component that holds, houses, encloses, carries, retains, or otherwise supports a film. In various embodiments, the holder comprises a casing, support, carrier, retainer, bracket, mount, frame or fixture. In various embodiments, the holder is a means of supporting or protecting the film. In various embodiments, the holder is a protective exterior for the film. A housing may comprise one or more parts or components. A housing may comprise a rigid material, flexible material, or a combination thereof. A housing may comprise a semi-permeable material, impermeable material or a combination thereof. In one aspect the holder is a component of an air gate.

[0087] As used herein, the term “system” includes, but is not limited to, objects that together form an assembly, or perform the methods described herein. In various embodiments, the system is an assembly or apparatus. A “closed system” is a system comprising substantially impermeable materials. Typically, a closed system substantially does not allow transfer of matter into or out of the system. In various embodiments, a closed system is impermeable to oxygen, ethanol, and / or water. In one aspect, an assembly comprising a container and an oxygen reservoir is a non-limiting example of a closed system. An “oxygen-permeable system” is a system comprising one or more oxygen-permeable materials. In one aspect, “oxygen-permeable system” comprises materials that are not permeable to liquids, vapors or aromas, including but not limited to water and ethanol liquids and vapors. An “open system” is a system comprising one or more semi-permeable materials. In one aspect, an open system is a system comprising one or more semi-permeable materials and one or more substantially impermeable materials. In another aspect an open system is a system comprising one or more oxygen- permeable materials. In another aspect an open system is a system comprising one or more oxygen-permeable materials, and one or more materials substantially impermeable to liquid or vapors of ethanol and liquid or vapors of water. In one aspect, an assembly comprising a container and an oxygen-permeable film is a non-limiting example of an open system. In one aspect, an assembly, wherein the oxygen supply reservoir comprises ambient air, is a non-limiting example of an open system. An assembly comprising a container and an air gate, is a non-limiting example of an open system. In one such example, the air gate comprises an oxygen-permeable film that allows oxygen from ambient air to pass from outside to inside a container. An assembly comprising acontainer and an air gate, is also a non-limiting example of an “oxygen-permeable system.”

[0088] As used herein, the term “sensory attributes” include, but are not limited to, flavor, aroma, texture, color, clarity, balance, and complexity.

[0089] The terms “impermeable” or “non-permeable” are used as typically understood in the art. Typically, an impermeable material is a material that does not allow substantially any substance to pass through the material. An impermeable material may also be referred to as a “non-penetrable” material. The terms impermeable, non-permeable, and nonpenetrable may be used interchangeably. In particular, the non- permeable material is air-tight, vapor-tight, liquid-tight, or any combination thereof. In various embodiments, a non-permeable material may not allow passage of oxygen from a system. For example, non-permeable material does not allow passage of oxygen into or out of a system. In another example, non-permeable material does not allow passage of ethanol, liquid or vapor out of a system. The term impermeable may be used in reference to a particular chemical, liquid, vapor or gas. For example, a material may be impermeable with respect to water or alcohol, while being permeable with respect to oxygen gas. Such material, as used herein, is referred to as a semi-permeable material.

[0090] Impermeability may be quantified in that a material has an extremely low, minimal, or negligible permeability, making it effectively resistant to the passage of liquids, gases, or vapors. Impermeable materials typically have gas permeability below 10'3Barrer. For liquids, impermeable materials typically have Vapor Transfer Rate values below 0.1 g / m2 / day.

[0091] As used herein, the term “semi-permeable” is used as typically understood in the art. A semi-permeable material may also be referred to a “semi-penetrable” material. A semi-permeable material can be a material that allows certain substances to pass through it but not other substances. The term “semi-permeable material” may be used when the term impermeable is used in reference to one or more particular chemicals, liquids, vapors or gases, or any combinations thereof. For example, a material may be a semi-permeable material when the material is impermeable to one substance while being permeable to another substance. In various embodiments, a semi-permeable material maybe impermeable with respect to water or alcohol, while being permeable with respect to oxygen gas. A suitable semi-permeable material should not allow passage of vapor or aromas from a system. A suitable semi-permeable material should not allow passage of vapor, such as water or alcohol vapor, from a system. In various embodiments, the semi- permeable material is permeable to oxygen, an oxygen-inert gas mixture, or both. For example, a semi-permeable material allows oxygen into or out of a system. In another example, semi-permeable material does not allow passage of ethanol liquid or vapor out of a system. In another example, the semi-permeable material allows oxygen into or out of the system while not allowing ethanol out of the system. In another example, the semi- permeable material is selective for small, non-polar molecules, but not larger, polar molecules.

[0092] A “skived” material or a “skived sheet” is typically produced by slicing or cutting thin layers from larger blocks of compressed resin using specialized skiving machines. This results in thinner and optionally wider sheets compared to molded sheets. One advantage of skived sheets are their flexibility and conformability properties. Skiving allows precise control over sheet thickness variations across different sections or areas. This flexibility in thickness enables engineers and designers to tailor the sheet according to specific requirements, making it ideal for intricate applications where a customized fit is necessary. Also, skived sheets may have excellent surface smoothness and uniformity, which can be attributed to the slicing process.

[0093] As used herein, the term “mini-stave” or “micro-stave” may refer to a smaller piece of wood rendered (e.g., cut, chopped, chiseled, etc.) from a larger piece of wood. In various embodiments, mini-staves comprise wood chips. Any suitable size of mini-stave may be used. Typical mini-staves, used in wine or spirit barrels, are on the order of 10 mm x 60 mm x 1000 mm, or larger. In various embodiments, a mini-stave comprises cubic dimensions ranging from about 0.05 mm x 0.05 mm x 0.05 mm to about 100 mm x 200 mm x 1000 cm. In various embodiments, the mini-staves comprise dimensions of about 5-20 mm x 5-20 mm x 20-200 mm. In various embodiments, the mini-staves comprise dimensions of about 0.1-5 mm x 0.1-5 mm x 0.1-5 mm. In various embodiments, the mini-staves comprise dimensions of about 10 mm x 60 mm x 1000 mm. In various embodiments, the mini-staves comprise dimensions of about 10 mm x 100 mm x 200 mm. In various embodiments, the mini-staves comprise dimensions ofabout 10 mm x 10 mm x 100 mm. Mini-staves or micro-staves may be rendered (e.g., cut, chopped, chiseled, etc.) from a larger piece of wood such that the volume and surface area of the wood piece that is the mini-stave is controlled to achieve a selected volume and surface area thereby enabling controlled and uniform extraction of the wood components by a spirit. While referred to herein using the term “micro” as part of “micro-stave” the term “micro” is not used in its metric system prefix meaning as part of “micro-stave” but is rather a general descriptor indicating that the “micro-staves” as described herein are small.

[0094] In some embodiments, micro-staves may be created from the desired wood material, such as a hardwood (e.g., oak, ash, beech, etc.), softwood (e.g., cedar, juniper, pine, spruce, etc.), wood-like grass (e.g., bamboo, etc.), etc. In some embodiments, microstaves may be inspected for desired wood characteristics. In some embodiments, microstaves may be toasted. In some embodiments, micro-staves may be charred. In some embodiments, micro-staves may be toasted and charred.

[0095] In various embodiments, micro-staves may be added to a container. In exemplary embodiments, the container is an oak cask. In various embodiments, microstaves provide additional wood surface area within a cask. In certain embodiments, micro-staves comprise one or more species of wood. In certain embodiments, microstaves comprise one or more species of wood that is different from the wood from which the cask is comprised.

[0096] As used herein, the term “toasted” refers to a state of a wood product, such as a micro-stave or barrel, in which the wood product has been exposed to heat thereby causing thermal decomposition of the cellulose, hemicellulose and lignin in the wood forming the wood product without any resulting visible char accumulation on the external surface of the wood. Toasted wood products may have been heated such that some decomposition of the wood surface occurred without combustion reactions at the surface of the wood resulting in visible carbon residues (e.g., char layers). Toasting as described herein may be performed such that the entire volume of the wood is transformed and decomposed uniformly. Toasting may be done in an oven and may take a time period from minutes to hours or days to achieve a toasted state of a wood product.

[0097] As used herein, the term “charred” refers to a state of a wood product, in which the wood product has been exposed to heat thereby causing thermal decomposition of the cellulose, hemicellulose and lignin in the wood to at least a point where visible char accumulates on the external surface of the wood. Such resulting visible carbon residues (e.g., char layers) may be as thin as only a few microns (e.g., 2 microns) thick on the surface of the charred wood product. The entire surface of a wood product need not show visible carbon residues (e.g., charring) for the wood product to be considered a charred wood product, such that as long as a portion of the surface of the wood product shows visible carbon residues (e.g., charring) the wood product is a charred wood product. In contrast, a toasted wood product may show no visible carbon residues (e.g., charring). Charring as described herein may be performed such that there is a gradient in wood transformation and decomposition due to very high temperatures at the surface that is being charred. Charring may be done with a heat source, such as a gas flame / torch, IR heater, etc., and may take a period of time from seconds to minutes to achieve a charred state of a wood product.

[0098] Although any compositions, assemblies, apparatuses, kits, and methods similar or equivalent to those described herein can also be used in the practice or testing of the invention, described herein are representative illustrative, compositions, assemblies, apparatuses, kits, and methods.

[0099] It is appreciated that certain features of the compositions, assemblies, apparatuses, kits, and methods, which are, for clarity, described in the context of separate embodiments, may also be provided in combination in a single embodiment. Conversely, various features of the compositions, assemblies, apparatuses, kits, and methods, which are, for brevity, described in the context of a single embodiment, may also be provided separately or in any suitable sub combination. All combinations of the embodiments are specifically embraced by the present disclosure and are disclosed herein just as if each and every combination was individually and explicitly disclosed, to the extent that such combinations embrace operable processes and / or compositions. In addition, all subcombinations listed in the embodiments describing such variables are also specifically embraced by the present invention and are disclosed herein just as if each and every such sub-combination was individually and explicitly disclosed herein. Isolated features mayfunction independently as an invention from other features and not necessarily require implementation as a complete combination to have advantages.

[0100] As will be apparent to those of skill in the art upon reading this disclosure, each of the individual embodiments described and illustrated herein may have discrete components and features which may be readily separated from or combined with the features of any of the other several embodiments without departing from the scope or spirit of the present methods. Any recited method can be carried out in the order of events recited or in any other order that is logically possible.

[0101] Each of the various elements disclosed herein may be achieved in a variety of manners. This disclosure should be understood to encompass each such variation, be it a variation of an embodiment of any apparatus embodiment, a method or process embodiment, or even merely a variation of any element of these. Particularly, it should be understood that the words for each element may be expressed by equivalent apparatus terms or method terms even if only the function or result is the same. Such equivalent, broader, or even more generic terms should be considered to be encompassed in the description of each element or action. Such terms can be substituted where desired to make explicit the implicitly broad coverage to which this invention is entitled.

[0102] As a non-limiting example, it should be understood that all action may be expressed as a means for taking that action or as an element which causes that action. Similarly, each physical element disclosed should be understood to encompass a disclosure of the action which that physical element facilitates. As a non-limiting example, a disclosure of an “attachment mechanism” should be understood to encompass disclosure of the act of “attaching,” whether explicitly described or not, and, conversely, were there only disclosure of the act of “attaching”, such a disclosure should be understood to encompass disclosure of an “attaching mechanism”. Such changes and alternative terms are to be understood to be explicitly included in the description.

[0103] Barrel -ageing

[0104] Barrel-ageing is complex and dynamic involving additive, subtractive, and interactive physicochemical processes that take place in the gas (oxygen) - solid (wood) - liquid (spirit / wine) reaction system of a barrel (Liebmann AJ, Rosenblatt M. 1943.Changes in whiskey while maturing. Ind Eng Chem 35: 994-1002). These processes occur simultaneously and contribute to the transformation of the spirit in the following way (Piggott JR, Sharp R, Duncan REB. 1989. The Science and Technology of Whiskies, Longman, Harlow).

[0105] Additive: Direct extraction of wood components and carry-over extractives from previous use of the cask. Decomposition of the wood macromolecules lignin, cellulose and hemicellulose followed by elution into the spirit.

[0106] Subtractive: Removal of compounds by evaporation and adsorption by the charred inner layer of the cask.

[0107] Interactive: Reactions between compounds of the wood and distillate.Chemical degradation reactions including oxidations. Masking of distillate flavors and aromas involving changes in the whiskey matrix. Without being bound by theory, the harshness of a distilled spirit is removed, in whole or in part, by eliminating sulfur compounds through oxidative reactions.

[0108] Warehouse conditions: In dry climates, more water than alcohol will evaporate from the barrel, increasing alcohol concentration inside the barrel. The opposite is true in humid climates. In colder climates, while evaporation rates are lower, maturation times are longer. The opposite is true in warmer climates. Climate controlled warehouses can be used to optimize ageing conditions while minimizing evaporation losses.

[0109] Barrel size: Some distilleries experiment with smaller barrels which have a higher surface area-to-volume ratio, resulting in faster maturation but also higher evaporation losses. In large barrels with lower surface area-to-volume ratios, maturation and evaporation rates are slowed down.

[0110] Barrels with increased surface area: Some barrel manufacturers offer charred barrels with increased inner surface areas obtained by cutting spirals or grooves throughout the inside of the barrel which significantly increases the surface area to allow ageing spirits access to alternating layers of charred and uncharred oak.

[0111] Wood barrels are semi-permeable. Air (oxygen) enters barrels slowly through pores and small gaps between staves, heads, and the bung plug, occupying headspace anddissolving in the spirit. Studies with wine barrels have shown Oxygen Transfer Rates (OTRs) of 5 to 45 mg / L per year depending on the experimental protocol and barrel type. Assuming spirit and wine barrels have similar OTRs and assuming they remain constant over time, 10 to 90 g oxygen would enter a 200 L barrel during a 10-year maturation period, equivalent of 7 to 63 L of pure oxygen at standard temperature and pressure.

[0112] Oxygenation of wine barrels has been well studied and a process called microoxidation was developed replicating barrel maturation in stainless steel vessels under more controlled conditions, over a shorter time period and at lower cost. The amount of added oxygen is carefully matched to the volume of wine and applied in a controlled manner via membranes or by slowly bubbling oxygen through a long column of wine. Depending on the wine and the process, between 0.75 to 3 cm3(1.1 to 4.3 mg) of oxygen is applied per liter of wine over a 4- to 8-month period. Too much oxygen can result in over-oxidation, whereas too little oxygen results in reduction, both yielding undesirable sensory attributes. Authorized by the European Commission in 1996, it is widely adopted by wine producers in Europe and the USA.

[0113] During barrel ageing of whiskey, oxidation reactions play an important role in breaking down lignin and hemicellulose, developing congener compounds and removing off flavor and aroma compounds. Interaction between hydrolysable tannins, dissolved oxygen and copper ions produces active oxygen and peroxide. These oxidants promote the formation of dimethyl sulfoxide from dimethyl sulfide and form the congeners vanillic and syringic acid from lignin degradation products. Ethanol is oxidized to acetaldehyde which establishes an equilibrium with hemiacetal and acetal. Further oxidation results in the formation of acetic acid which reacts with ethanol to form ethyl acetate (Russell I, Stewart G, Bamforth C. 2003. Whisky: Technology, Production and Marketing. Elsevier.

[0114] Studies suggest that oxygenation is a rate-limiting step in traditional barrelageing of whiskey. Withers et al. compared the sensory and chemical attributes of Scotch malt distillate matured in full-size uncharred, American white oak casks with distillate matured in smaller 6-liter casks of similar wood (Withers SJ, Piggott JR, Conner JM, and Paterson A. 1995. Comparison of Scotch malt whiskey maturation in oak miniature casks and American standard barrels, J Inst Brew. 101 : 359-364). Differences in the ratios ofconcentrations of extractives between both cask sizes were found, suggesting different oxidation rates. Furthermore, a publication by J.S. Swan describes maturation as a slow process of continuous oxidation (Swan JS. 1994. In: Campbell I. editor. Proceedings of the Fourth Aviemore Conference on Malting, Brewing and Distilling, Institute of Brewing, London).

[0115] Relatively little is known about the oxygen requirements of barrel-ageing spirits. In the absence of data, it is often assumed that ageing spirits should be exposed to controlled amounts of oxygen similar to wine and that micro-oxygenation is required to avoid over-oxidation of spirits (Spedding G. 2017. Eighty years of rapid maturation studies. Why are we not there yet?. American Distilling Institute). This view, however, seems at odds with the standard industry practice of maturing spirits in barrels over many years or even decades.

[0116] Over extraction of oak components (over-oaking) leads to undesirable sensory attributes often described as oaky or woody. Spirits in new barrels, barrels with high inner surface area and / or barrels stored for too long are at risk of over-oaking. Spirit oxygenation and subsequent oxidation reactions that are not in balance with oak extraction can lead to an unfavorable sensory profile.

[0117] As a spirit ages, alcohol and water evaporate, increasing the air (oxygen)-filled headspace inside the barrel. This air space provides a reservoir of oxygen to replenish the dissolved oxygen in the spirit that is used up in oxidation reactions during maturation (Russell I, Stewart G, Bamforth C. 2003. Whisky: Technology, Production and Marketing. Elsevier.). Unless the barrel is regularly rotated, barrel staves at the top of the barrel begin to dry, creating small gaps through which air (oxygen) can enter the barrel. (Singleton VL. 1974. Some aspects of the wooden container as a factor in wine maturation. In: Webb A. Chemistry of winemaking. Adv Chem. American Chemical Society, Washington, DC). Take the case of a 50-year-old Scotch whiskey. Only about a third of its original liquid volume is left inside the whiskey barrel. Everything else has evaporated and is now headspace, exposing the remaining spirit to a constant supply of oxygen (Conner, J. 2014. Maturation. In: Whisky: Technology, Production and Marketing; Elsevier). In the context of micro-oxidation, this would have to be considered over-oxidation. Interestingly, a 50-year-old Scotch whiskey is highly sought after for itsastonishing depth and rich notes of oxidation products like dark chocolate, cinnamon, and treacle toffee. If very old casks hold highly oxidized spirits one can only conclude that micro-oxidation cannot play a role in traditional barrel-ageing of distilled spirits.

[0118] Contributing to the higher oxygen exposure of a barrel-ageing spirit compared to wine is the increased solubility of oxygen in ethanol. Oxygen solubility increases with increasing amount of ethanol in a non-linear fashion. At alcohol concentrations of wine, oxygen solubility is about the same as in water, whereas at the much higher alcohol concentration of a barrel-ageing spirit it is nearly twice as high (Shchukarev SA, Tolmacheva TA. 1968. Solubility of oxygen in ethanol - water mixtures. J Struct Chem. 9: 16-21). Assuming equal oxygen permeability of the barrel, a distilled spirit is exposed to about twice as much oxygen than a barrel-ageing wine is. This suggests that spirits might be less oxygen- sensitive than wines.

[0119] If spirits are unlike wines and tolerate higher oxygen levels, then ageing could be further accelerated by increasing oxygen levels inside the barrel. For example, a headspace of pure oxygen would have a 5 -fold higher oxygen concentration than air. By continuously supplying the headspace with pure oxygen, barrel oxygenation would no longer be a rate-limiting step in the ageing of distilled spirit. Such a system could vastly accelerate the ageing process and if done in a sealed barrel, eliminating the wasteful loss of alcohol.

[0120] In the USA, under 27 CFR § 5.22, all whiskeys must be aged in either new or used oak barrels. In the case of “Straight” whiskeys, a minimum storage time of two years is required. “Bottled in Bond” whiskeys must be stored in barrels for at least 4 years. Age statements on bottle labels are mandatory unless the youngest whiskey in a blend has been barrel-aged for at least 4 years (27 CFR § 5.40).

[0121] Based on the Scotch Whiskey Regulation of 2009, Scotch whisky needs to be aged for a minimum of 3 years in oak casks of less than 700 liters capacity. Similarly, in the European Union whisky needs to be matured for at least 3 years in wooden casks.

[0122] Container

[0123] In various embodiments, the container comprises stainless steel. In various embodiments, the container is made of plastic. In various embodiments, the container is made of a food-grade plastic. In various embodiments, the food grade plastic is HDPE (high-density polyethylene), LDPE (low-density polyethylene), PP (polypropylene), PET (polyethylene terephthalate), PVC (polyvinyl chloride), polytetrafluoroethylene (PTFE), polystyrene or polycarbonate. In various embodiments, the container comprises an impermeable material. In certain embodiments wherein an impermeable material is desired, the material comprises a suitable thickness to render the material to be an impermeable material. In certain non-limiting examples, PTFE may be used to construct an impermeable container having a thickness at least 5 mil.

[0124] In various embodiments, the container comprises glass. In various embodiments, the container is made of glass. In various embodiments, the container is a bottle. In certain embodiments, the size of the bottle is 50 mL, 100 mL, 200 mL, 375 mL, 500 mL, 700 mL, 720 mL, 750 mL, 900 mL, 1 liter, 1.5 liters, 1.75 liters, 1.8 liters, 3 liters, or 4.5 liters.

[0125] In various embodiments, the container comprises wood. In various embodiments, the container is made of wood. Any suitable wood species may be used. In various embodiments, the wood comprises a hardwood. In various embodiments, the wood comprises a softwood. In various embodiments, the wood comprises wood-like grass. In various embodiments, the hardwood comprises oak, acacia, chestnut, cherry, mulberry, elm, beech, ash, juniper, black locust, apple, maple, or hickory. In certain embodiments, the softwood comprises cedar, juniper, pine, or spruce. In certain embodiments, the wood-like grass comprises bamboo. In particular embodiments, the wood comprises oak.

[0126] In various embodiments, the container comprises a barrel. In various embodiments, the container comprises a cask. In various embodiments, the container comprises an oak cask. In various embodiments, the oak barrel is a standard oak cask. Numerous barrel sizes are used in the art. In various embodiments, the container comprises a volume of about 5 gallons, 10 gallons, 15 gallons, 30 gallons, 53 gallons (e.g., a Bourbon Barrel), 59 gallons (e.g., a Bordeaux Cask), 60 gallons (e.g., a Burgundy Cask), 66 gallons (e.g., a Hogshead), 79 gallons (e.g., a Cognac Cask), 132 gallons (e.g.,T1a Sherry Butt), 145 gallons (e.g., a Port Pipe), 172 gallons (e.g., a Madeira Drum), 200 L, 240 L, 250 L (e.g., a tierce), 256 L, 500 L (e.g., a puncheon), 570 L (e.g., a pipe or tun), 600 L (e.g., a demi-mud), 900 L (e.g., a tun), 1000 L, 2000 L, 5000 L, 8000 L, 10000 L or 230000 L (e.g., the Heidelberg tun).

[0127] In various embodiments, the container comprises an oak barrel. In various embodiments, the oak barrel is a standard oak barrel.

[0128] Container Placement

[0129] The container may be placed on its side or upright. In various embodiments, the container is placed on its side. In various embodiments, the container is placed upright. The container may be relocated one or more times from upright to its side or from its side to upright. In various embodiments, the assembly comprises a support for holding the container in place. Such support may prevent unwanted rolling or shifting of the container. Examples of suitable supports include, but are not limited to, cradles, racks, and stands.

[0130] A container may be placed on its side with its opening hole facing upwards or to its side. In one embodiment the opening hole is situated above the liquid level inside the container. A container may alternatively be placed upright with an opening through its top head. The opening may be a hole or any other suitable opening. In one embodiment, a container is placed upright, and its top head is removed. Such openings may be used to attach a reservoir either directly or indirectly via a conduit.

[0131] Barrel Placement

[0132] The cask may be placed on its side or upright. In various embodiments, the cask is placed on its side. In various embodiments, the cask is placed upright. The cask may be relocated one or more times from upright to its side or from its side to upright. In various embodiments, the assembly comprises a support for holding the container in place. Such support may prevent unwanted rolling or shifting of the container. Examples of suitable supports include, but are not limited to, barrel cradles, racks, and stands.

[0133] A cask may be placed on its side with its bung hole facing upwards or to its side. In one embodiment the bung hole is situated above the liquid level inside the cask.A cask may alternatively be placed upright with an opening through its top head. The opening may be a bung hole or any other suitable opening. In one embodiment, a cask is placed upright, and its top head is removed, as illustrated by Figure 8(B). Such openings may be used to attach a reservoir either directly or indirectly via a conduit.

[0134] Reservoir

[0135] In various embodiments, the container is connected to a reservoir. In various embodiments, the container is connected to at least one reservoir. In various embodiments, the container is connected to at least two reservoirs.

[0136] In various embodiments, the reservoir is an oxygen supply reservoir.

[0137] In various embodiments, the container is placed inside the oxygen supply reservoir.

[0138] In relation to an air gate, the oxygen supply reservoir is ambient air. In this aspect, the assembly of the invention may be referred to as an “open” system or an “oxygen-permeable system.”

[0139] In various embodiments, at least one container is connected to the oxygen supply reservoir. In various embodiments, at least two containers are connected to the same oxygen supply reservoir. In various embodiments, about 2 to about 100,000 containers are connected to the same oxygen supply reservoir. In various embodiments, about 2 to about 10,000 containers are connected to the same oxygen supply reservoir. In various embodiments, about 2 to about 1,000 containers are connected to the same oxygen supply reservoir. In various embodiments, 2 to about 100 containers are connected to the same oxygen supply reservoir. In various embodiments, 2 to about 10 containers are connected to the same oxygen supply reservoir. In various embodiments, one, two, or three containers are connected to the same oxygen supply reservoir. See for example, Figure 4.

[0140] In various embodiments, the oxygen supply reservoir is made of an impermeable material. In various embodiments, the oxygen supply reservoir is surrounded by an impermeable material.

[0141] In various embodiments, the oxygen supply reservoir comprises a metal, plastic, or glass. In various embodiments, the reservoir material comprises a polymeric, non-polymeric, synthetic, or natural material. In various embodiments, the polymeric material comprises acrylic, polyester, silicone, polyurethane, or halogenated plastic. In various embodiments, the polymeric material comprises a thermoplastic, thermoset, conductive polymer, biodegradable plastic, engineered plastic or elastomer. In various embodiments, the polymeric material comprises polyethylene (PE) including low-density polyethylene (LDPE), high-density polyethylene (HDPE), polypropylene (PP), polyvinyl chloride (PVC), polyethylene terephthalate (PET), polyamide (Nylon), polystyrene (PS), polyethylene naphthalene (PEN), polyimide (PI), polyvinylidene chloride (PVDC), ethylene vinyl alcohol (EVOH), methyl methacrylate (PMMA), polybutylene terephthalate (PBT), polyether ether ketone (PEEK), acrylonitrile butadiene styrene (ABS), high impact polystyrene (HIPS), polycarbonate (PC), polycarbonate + acrylonitrile butadiene styrene (PC + ABS), polyethylene + acrylonitrile butadiene styrene (PE + ABS), polyetherimide (PEI), polyimide, poly sulfone, polytetrafluoroethylene (PTFE), polyamide-imide (PAI), polylactic acid (PLA) or latex. In various embodiments, the non-polymeric material comprises a metal or non-metal. In various embodiments, the metal comprises a pure metal or a metal alloy. In various embodiments the metal comprises aluminum, copper, iron, stainless steel, or brass. In various embodiments, the non-metal comprises glass, ceramic, or composite material.The reservoir may be expandable or non-expandable. The reservoir may be stretchable or non-stretchable. The reservoir may be formed by a stretchable or non-stretchable material.

[0142] The oxygen supply reservoir may comprise any suitable enclosure. In various embodiments, the oxygen supply reservoir comprises a cylinder, a bag, a balloon, a cover, a wrap, a sack, or a pack. In certain embodiments, the wrap is an overwrap that forms a bag surrounding the container. In certain embodiments, the bag is an end seal bag. In various embodiments, the cylinder comprises a piston to adjust volume. In various embodiments, the oxygen supply reservoir comprises a bag. In particular embodiments, the oxygen supply reservoir comprises a bag encasing the container. In particular embodiments, the bag is sealed around the container. See for example, Figure 5 and Figure 6.

[0143] In various embodiments, the oxygen supply reservoir comprises a rigid material. In embodiments wherein the oxygen supply is a rigid object surrounding the container, the oxygen supply reservoir may be referred to as a “housing” or “oxygen housing.” In certain embodiments, the reservoir is a stainless-steel housing. In certain embodiments, the reservoir is a stainless-steel tank.

[0144] In one aspect the oxygen supply reservoir is placed on top of the container. In various embodiments, the oxygen supply reservoir is placed on top of the container and connected to the container via a conduit. In various embodiments, the oxygen supply reservoir is placed on top of the container and connected to the container directly.Without being bound by theory, this placement may eliminate vapor condensation in parts of the assembly that is lower than the liquid surface inside the barrel. Without being bound by theory, ethanol is heavier than air, and without any temperature gradient, would remain above the liquid surface area without rising and condensing anywhere else.Examples of such assemblies include, but are not limited to, those illustrated in Figure 7 (A), Figure 7 (B), Figure 8(A), and Figure 8 (B).

[0145] In one aspect, the container is encased within a bag and the bag is attached to a reservoir. In another aspect, the container is encased within a bag and the bag serves as a reservoir. Examples of such a system include, but are not limited to, those illustrated in Figure 3, Figure 5, and Figure 6.

[0146] Oxygen gas mixture

[0147] In various embodiments, the oxygen supply reservoir holds pure oxygen (O2). It is understood that while pure oxygen is intended to mean 100% oxygen, minor impurities may be present. In various embodiments, the oxygen supply reservoir holds a diluted oxygen mixture. The diluted oxygen mixture comprises an inert gas and oxygen gas.

[0148] Any suitable inert gas may be used. In various embodiments, the inert gas is nitrogen (N2). In various embodiments, the inert gas is a noble gas. In various embodiments, the inert gas is helium (He). In various embodiments, the inert gas is neon (Ne). In various embodiments, the inert gas is argon (Ar). In various embodiments, theinert gas is carbon dioxide (CO2). In various embodiments, the inert gas is hydrogen (H2).In various embodiments, the inert gas is nitrous oxide (N2O).

[0149] In various embodiments, the oxygen supply reservoir holds an inert gas - oxygen mixture (v / v) comprising an oxygen content ranging from about 1% to about 100%, ranging from about 10% to about 100% oxygen, ranging from about 21% to about 100% oxygen, ranging from about 50% to about 100%, ranging from about 75% to about 100%. In various embodiments, the oxygen supply reservoir holds a gas comprising an oxygen content greater than air at standard temperature and pressure (STP). Air typically has a content of about 21% oxygen. In various embodiments, the oxygen supply reservoir holds at least about 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85 %, 90%, or 95% oxygen. In various embodiments, the oxygen supply reservoir holds at least about 90%, 91%, 92%, 93%, 94 %, 95%, 96%, 97%. 98%, or 99% oxygen. In various embodiments, the oxygen supply reservoir holds about 25%, 30%, 35%, 40%, 45 %, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85 %, 90%, 95% or 100% of oxygen. In various embodiments, the oxygen supply reservoir holds at least about 90%, 91%, 92%, 93%, 94 %, 95%, 96%, 97%. 98%, 99% or 100% oxygen. In various embodiments, the inert gas - oxygen mixture comprises an oxygen content of about 100%.

[0150] In various embodiments, the oxygen supply reservoir holds ambient air. In various embodiments, the oxygen supply reservoir holds an inert gas - oxygen mixture comprising about 21% oxygen, 78% nitrogen. In certain embodiments, the oxygen supply reservoir holds an inert gas - oxygen mixture comprising about 25% oxygen, 75% nitrogen. In certain embodiments, the oxygen supply reservoir holds an inert gas - oxygen mixture comprising about 40% oxygen, 60% nitrogen. In certain embodiments, the oxygen supply reservoir holds an inert gas - oxygen mixture comprising about 50% oxygen, 50% nitrogen. In certain embodiments, the oxygen supply reservoir holds an inert gas - oxygen mixture comprising about 60% oxygen, 40% nitrogen. In certain embodiments, the oxygen supply reservoir holds an inert gas - oxygen mixture comprising about 75% oxygen, 25% nitrogen. In certain embodiments, the oxygen supply reservoir holds an inert gas - oxygen mixture comprising about 80% oxygen, 20% nitrogen. In certain embodiments, the oxygen supply reservoir holds an inert gas - oxygen mixture comprising about 90% oxygen, 10% nitrogen. In certain embodiments, theoxygen supply reservoir holds an inert gas - oxygen mixture comprising about 95% oxygen, 5% nitrogen.

[0151] Gas Volume

[0152] In various embodiments, the oxygen supply reservoir holds a volume ranging from about 0.1 L to about 10.0 L of oxygen - inert gas mixture for each 1 L of liquid. In various embodiments, the oxygen supply reservoir holds a volume ranging from about 0.1 L to about 1.0 L of oxygen - inert gas mixture for each 1 L of liquid. Certain high volumes of oxygen relative to liquid may allow for some of the unfavorable low boiling volatiles like methanol and acetone to evaporate at the beginning of the maturation process.

[0153] Headspace

[0154] Headspace in a barrel typically refers to the empty space between the surface of the distilled spirit and the top of the barrel. In one aspect of the present disclosure, the assembly or methods of the present disclosure increases headspace. In various embodiments of the present disclosure, the reservoir and the gate increase the headspace of the system.

[0155] Inside a barrel, liquid surface area matters because oxygen uptake by the liquid is a function of temperature, pressure, and surface area. The surface area can be anywhere between 0 in2to the widest horizontal diameter of a barrel.

[0156] In a nonlimiting example, an upright 53-gallon Bourbon barrel, with an internal girth of 24 inches typically may have a liquid surface area up to about 1810 square inches when half full.

[0157] Dimensions of an exemplary 53-gallon Bourbon barrel include Height: 35”, Diameter (belly): 26”, Diameter (head): 22.”

[0158] Surface area of liquid to wood is typically represented by a surface to volume ratio. A typical 53-gallon Bourbon barrel has an inner surface area to volume ratio of about 90 cm2per liter.

[0159] The wood to liquid surface area may be useful for describing the amount of extractives from the wood into the liquid and its relation to various barrel sizes (e.g., a 5 -gallon barrel compared to a 53-gallon barrel).

[0160] Focusing on the headspace is important. One advantage of the present invention is the allowance for a greater initial headspace in a barrel than the initial headspace in a barrel using the traditional ageing process. For example, a completely filled barrel, as used in the present assembly and method, would right away have a headspace and oxygen exposure that it otherwise would only have after many years of ageing (due to liquid volume loss commonly called the angel’s share).

[0161] In various embodiments, a barrel is filled with various volumes of distilled spirit to vary the liquid to gas surface area. The present invention allows for various filllevels of distilled spirit within the container. In various embodiments, the container is filled to a capacity ranging from about 50% to about 100% distilled spirit to total volume capacity of the barrel. In various embodiments, the container is filled to a capacity of about 50%. In various embodiments, the container is filled to a capacity of about 60%. In various embodiments, the container is filled to a capacity of about 70%. In various embodiments, the container is filled to a capacity of about 80%. In various embodiments, the container is filled to a capacity of about 90%. In various embodiments, the container is filled to a capacity of about 100%.

[0162] Pressure

[0163] The oxygen supply reservoir may maintain a positive partial pressure for oxygen or neutral partial pressure for oxygen. In various embodiments, the pressure is a positive pressure. In various embodiments, the pressure is a partial positive pressure. In various embodiments, the oxygen supply reservoir maintains a pressure ranging from about 0.1 to about 10 atm, ranging from about 0.5 to about 2 atm, or of about 1 atm. In various embodiments, the oxygen supply reservoir maintains a pressure of about 1 atm.

[0164] Conduit - Tube, Pipe, Hose

[0165] Connections between a reservoir or an air gate and the container may be a direct connection, or an indirect connection. Such indirect connection may be by means of a conduit. A conduit is a non-limiting example of an indirect connection. In oneexample, a gas reservoir or air gate may be indirectly connected to the container or barrel via a connector or via a tube, hose, or pipe. In another example, a gas reservoir is connected to an air gate through a first conduit and the air gate is connected to a barrel through a second conduit.

[0166] In one aspect, a conduit is used to connect a reservoir or air gate to a container. A conduit is any suitable object capable of providing a channel through which gas, liquid or other fluid passes or is conveyed. Examples of suitable conduits include, but are not limited to, any tube, pipe, or hose. As used herein, the terms tube, pipe, or hose may be used interchangeably. Typically, tubing or a tube may be round, cylindrical, rectangular, square, or oval. Typically, piping or a pipe, is cylindrical or round.

[0167] Conduits may be flexible or rigid. Conduits may comprise a combination of rigid and flexible materials. Conduits may comprise a polymeric, a non-polymeric material, or a combination of polymeric and non-polymeric materials. In nonlimiting examples, a tube, or tubing may be flexible and made of polymeric or non-polymeric material. In nonlimiting examples, a pipe, or piping, may be rigid and made of polymeric or non-polymeric material.

[0168] Conduits may comprise a synthetic material, a non-synthetic material, or a combination of synthetic material, a non-synthetic material.

[0169] In various embodiments, the conduit comprises any suitable non-permeable material.

[0170] In certain embodiments, the conduit is a stainless-steel tube. In certain embodiments, the conduit is a polymeric hose.

[0171] Any suitable length may be used. In various embodiments, the conduit can have a length ranging from about 0.1 inch to about 1000 yards. In various embodiments, the conduit can have a length ranging from about 1 inch to about 1000 inches. In various embodiments, the conduit can have a length ranging from about 1 inch to about 100 inches. In various embodiments, the conduit can have a length ranging from about 1 inch to about 10 inches.

[0172] In various non-limiting examples, A gas reservoir or air gate could be directly connected to the barrel via a connector or via a tubing or pipe. A tubing is flexible made of polymeric or non-polymeric material. A pipe is rigid made of polymeric or non- polymeric material. The connector, tubing or pipe can have any suitable length, for example, anywhere between 0 inches to 1000 yards.

[0173] Air Gate

[0174] One aspect of the invention includes, but is not limited to an air gate. In various embodiments, the air gate comprises an oxygen-permeable film and a means for securing the film. In various embodiments, the air gate comprises an oxygen-permeable film and a holder.

[0175] Figure 9 and Figure 10 illustrate non-limiting examples of an air gate. FIG. 9 (A) is a drawing illustrating an assembled view of an exemplary air gate 200. Fig 9 (B) shows an assembled air gate 200 attached to a barrel 104B. FIG. 9 (C) shows an air gate attached to a demijohn or bottle. FIG. 10 (A) shows a cross-sectional view of an exemplary air gate wherein the air gate comprises an assembly comprising a holder 202, and an oxygen permeable film 201. In this particular example, the film 201 is held in place between two halves of a holder, an upper plate 207 and a lower plate 208. The assembly may be secured together using one or more bolts 205 and nuts 206. In another example, the assembly is held together by rivets. In another example, the assembly is held together by tongue and groove joints. In another example, the assembly is welded together. Alternatively, the assembly may be held together by an adhesive. The holder comprises a size and shape suitable for receiving the film. The upper and lower plates are shaped in a configuration that, when assembled, a cavity is formed around the film allowing air to be distributed along the surface area of the film. The upper plate and lower plate each independently comprise an opening. The upper plate comprises an opening to ambient air 205. The lower plate comprises an opening 206 to the container or barrel. Optionally, the air gate comprises a dust cover 209 over the opening of the upper plate. In one embodiment, the opening of the lower plate comprises a neck 210 for inserting into an opening of a container. In one example, the neck of the lower housing can be placed through a stopper or bung 103. Alternatively, the opening and bung are a single unit. FIG. 10 (B) shows an air gate comprising a film 201 in the form of a pleated sheet.

[0176] Holder

[0177] In certain embodiments, the holder comprises an opening to an oxygen supply. In certain embodiments, the holder comprises an opening to a container. In certain embodiments, the holder comprises a first opening and a second opening, wherein the first opening is an opening to an oxygen supply, and wherein the second opening is an opening to a container.

[0178] The opening to the container may be a direct connection or may comprise an indirect connection. In certain embodiments, the indirect connection comprises a conduit.

[0179] The opening to an oxygen supply may be a direct opening or an indirect opening. In certain embodiments, the indirect connection comprises a conduit.

[0180] In certain embodiments, the holder comprises an opening direct to ambient air. Ambient air may include, by non-limiting example, surrounding air in a building or room such as a rackhouse, or the outdoors. In certain embodiments, the holder comprises an opening through a conduit to the ambient air. In certain embodiments, the holder comprises an opening direct to an oxygen supply reservoir. In certain embodiments, the holder comprises an opening through a conduit to an oxygen supply reservoir.

[0181] In various embodiments, the holder is circular, elliptical, polygonal, n-sided polygonal having n equal to about 3 to 20. In certain embodiments, the housing is circular, oval, triangular, square, rectangular, hexagonal, octagonal. In certain embodiments, the housing is of regular or irregular shape.

[0182] In various embodiments, the holder consists of an inlet portion, an outlet portion and a semi-permeable film located therebetween. The inlet portion is open to the surrounding atmosphere, allowing the surrounding atmosphere to enter the inlet portion, penetrate the semi-permeable film, enter the outlet portion and leave the outlet portion via a conduit connected to a container.

[0183] In various embodiments, the surface area of the opening of the inlet portion to the surrounding atmosphere is smaller than the surface area of the semi-permeable film between the inlet and outlet portion. In various embodiments, the surface area of the opening of the inlet portion to the surrounding atmosphere is the same as the surface areaof the semi-permeable film between the inlet and outlet portion. In various embodiments, the surface area of the opening of the outlet portion to the conduit is smaller than the surface area of the semi-permeable film between the inlet and outlet portion.

[0184] In various embodiments, the holder is attached to a bung. In various embodiments the holder is itself a modified bung.

[0185] In various embodiments, the holder comprises two components. In various embodiments, the holder comprises an upper plate and a lower plate. The upper plate and lower plate may be unsymmetrical, symmetrical or identical.

[0186] The upper and lower plate may be secured by any suitable means. In various embodiments, the plates are secured using one or more screws, bolts or rivets. In various embodiments, the plates are welded together. In various other embodiments, the plates are secured using an adhesive. In various embodiments, the plates are secured using a tongue and groove joint.

[0187] The holder comprises a size and shape suitable for receiving the film. The upper and lower plates are shaped in a configuration that, when assembled, a cavity is formed around the film allowing air to be distributed along the surface area of the film. The upper plate and lower plate each independently comprise an opening. In various embodiments, the upper plate comprises an opening to ambient air. In various embodiments, the lower plate comprises an opening to the container or barrel. Optionally, the air gate comprises a dust cover over the opening of the upper plate. In one embodiment, the lower plate comprises a neck for inserting into an opening of a container. In one example, the neck of the lower housing can be placed through a stopper or bung. Alternatively, the opening and bung are a single unit.

[0188] In various embodiments, the film is pressed or sandwiched between two halves of a holder. The openings of the upper and lower plates may be differing in size, similar in size, or identical in size. In various embodiments, the opening in the upper plate is wider than the opening in the lower plate. In various embodiments, the opening in the upper plate is narrower than the opening in the lower plate. In certain embodiments, the openings are substantially the same size. The holder may be made of any suitable substantially impermeable material as described herein. In various embodiments, theholder is substantially impermeable to water, ethanol, and / or aroma vapors. In various embodiments, the holder is permeable to oxygen and substantially impermeable to water, ethanol, and / or aroma vapors. In various embodiments, the holder comprises a food-grade material. In various embodiments, the holder comprises a metal. In various embodiments, the holder comprises stainless-steel. In various embodiments, the holder comprises aluminum. In various embodiments, the food-grade material is a food-grade plastic. In various embodiments, food— grade plastic is HDPE (high-density polyethylene), LDPE (low-density polyethylene), PP (polypropylene), PET (polyethylene terephthalate), PVC (polyvinyl chloride), polytetrafluoroethylene (PTFE), polystyrene or polycarbonate.

[0189] In one aspect the air gate holder and the container housing comprise identical materials. In another aspect the air gate holder and the container housing comprise different materials.

[0190] Semi-permeable Film

[0191] In one aspect, the film comprises a semi-permeable material. In various embodiments, the film comprises a semi-permeable polymer.

[0192] In another aspect, the film is permeable to oxygen. In various embodiments, the film is substantially impermeable to liquid or vapor. In various embodiments, the film is substantially impermeable to water and ethanol. In various embodiments, the film is further substantially impermeable to aroma compounds. In various embodiments, the film is permeable to oxygen and is substantially impermeable to liquid or vapor of ethanol and water, and aroma compounds.

[0193] The film may comprise a natural material, a synthetic material, or a combination of natural and synthetic materials. In various embodiments, the film material comprises a semi-permeable polymer. Preferably, the film comprises a food grade material.

[0194] Examples of suitable film material include, but are not limited to, Acrylonitrile -Styrene co-polymer, Acrylonitrile Butadiene Styrene (ABS), Dow Acrylonitrile ABS Films, Polystyrene (PS), Dow Try cite Oriented PS Film, BASF AG Polystyrol 168 N GPPS Film, Rubbers, Polyisoprene, Methyl rubber, Natural rubber,Neoprene, Silicone rubber, Mid Density Polyethylene (MDPE), Low Density Polyethylene. (LDPE), Fluoroplastics, Fluorinated ethylene propylene (FEP), Polytetrafluoroethylene (PTFE), Teflon AF, Amorphous Perfluoropolymers, Cytop, Hyflon AD, Fluorinated Cyclopolymer, Perfluorodioxole-based Polymer, PVC, Poly Propylene (PP), Polycarbonate (PC), Polydimethylsiloxane (PDMS), and Polylactic acid (PLA).

[0195] In various embodiments, the film material comprises a spin-coated, a dip- coated, a vapor deposited, a hot pressed, a stretched, a hot-rolled or a electrostatically deposited polymer.

[0196] In various embodiments, the film material comprises a skived polymer. In various embodiments, the film material comprises a skived sheet.

[0197] In various embodiments, the film comprises PTFE. In various embodiments, the film comprises skived PTFE. In particular embodiments, the film comprises a PTFE skived sheet.

[0198] An air gate film is preferably thin. Permeability of a material is a function of thickness. Total permeability typically decreases with increasing thickness for any compound. Typically, a thicker film is less permeable for liquids, gases, and vapors such as oxygen, ethanol, water, and aroma compounds. Typically, a thicker film is less permeable for oxygen. In one non-limiting example, a PTFE film of about ten times the thickness may be, in contrast, a substantial barrier for oxygen. In one rough estimate, a PTFE film having a thickness of about 100 pm, ten times thicker than a 10 pm PTFE film, may only allow 10% of the oxygen that would be expected to go through the 10 pm PTFE film.

[0199] Without being limited by theory, a material, at a first thickness, may be used as an impermeable material, and at second thickness, be used as a semi-permeable material. For example, in various embodiments, a 5 mil thick portion of PTFE may be used as an impermeable material, and in various other embodiments, a 0.5 mil PTFE sheet may be used as a semi-permeable film.

[0200] A preferred thickness of the film may be determined in terms of the preferred oxygen permeability desired. In one aspect, a user may select various film thicknesses based on how much oxygen permeability the user wishes to use during the ageing process.

[0201] Permeability is based on Fick’s Law in combination with Darcy’s law principles for gases or solutions. (See, Cooksey K et al. 1999. Predicting Permeability & Transmission Rate for Multilayer Materials. , Food Technology. 53: 60-63) (See also www.stevenabbott.co.uk / practical-coatings / permeability.php).

[0202] In various embodiments, the thickness of the air gate film is less than or equal to about 10 mm. The thickness of the film is less than or equal to about 1 mm. The thickness of the film is less than or equal to about 0.1 mm. The thickness of the film is less than or equal to about 0.01 mm. The thickness of the film is less than or equal to about 0.001 mm.

[0203] In various embodiments, the air gate film comprises a thickness ranging from about 1 mm to about 10 mm. In various embodiments, the film comprises a thickness ranging from about 1 mm to about 10 mm. In various embodiments, the film comprises a thickness ranging from about 0.1 mm to about 1 mm, from about 0.01 mm to about 0.1 mm, or from about 0.01 mm to about 0.001 mm.

[0204] In various embodiments, the film comprises a thickness ranging from about 0.5 mil (.0005") to about 125 mil (.125”). In various embodiments, the film comprises a thickness of about 0.5 mil, 0.8 mil, 1.0 mil, 1.5 mil, 2.0 mil, 3.0 mil, or 4.0 mil.

[0205] In one particular example, a thin film comprises a thickness of about 12.7 pm (about 0.0005 inches). In another example, a thin film comprises a thickness of about 25.4 pm (0.001 inches).

[0206] In one embodiment, the film comprises a 0.5 MIL (0.0005 in) skived PTFE sheet. In another embodiment, the film comprises a 1.0 MIL (0.001 in) skived PTFE sheet.

[0207] In various embodiments, the film comprises a surface area greater than or equal to about 1 cm2. In various embodiments, the film comprises an area greater than or equal to about 1 cm2, greater than or equal to about 10 cm2, greater than or equal to about 100 cm2, greater than or equal to about 1,000 cm2, greater than or equal to about 10,000 cm2, greater than or equal to about 20,000 cm2greater than or equal to about 30,000 cm2greater than or equal to about 40,000 cm2, or greater than or equal to about 50,000 2 cm .

[0208] In various embodiments, the film comprises an area ranging from about 1 cm2to about 10 cm2, from about 10 cm2to about 100 cm2, from about 100 cm2to about 1,000 cm2, or from about 1,000 cm2to about 10,000 cm2, or from about 10,000 cm2to about 50,000 cm2.

[0209] In various embodiments, the film comprises an area of about 1 cm2, about 10 cm2, about 20 cm2, about 30 cm2, about 40 cm2, about 50 cm2, about 60 cm2, about 70 cm2, about 80 cm2, about 90 cm2, about 100 cm2, about 200 cm2, about 300 cm2, about 400 cm2, about 500 cm2, about 600 cm2, about 700 cm2, about 800 cm2, about 900 cm2, about 1,000 cm2, about 2,000 cm2, about 3,000 cm2, about 4,000 cm2, about 5,000 cm2, about 6,000 cm2, about 7,000 cm2, about 8,000 cm2, about 9,000 cm2, or about 10,000 2 cm .

[0210] The film may be any suitable shape. In some embodiments the film is circular. In some embodiments the film is rectangular. In some embodiments the film is a square. In some embodiments the film is an w-sided polygon. In some embodiments, the polygon is regular. In some embodiments, the polygon is irregular.

[0211] The film may comprise a pure material or a tensiled material. Typically, a tensiled material comprises incorporated reinforcing fillers such as glass fibers or carbon fibers into material resin during the manufacturing stage. Reinforcing fillers may enhance a material’s tensile strength and overall mechanical properties.

[0212] In one embodiment, the film comprises a substantially pure material. In various embodiments, the film comprises a substantially pure semi-permeable material. In various embodiments, the substantially pure semi-permeable material comprises asubstantially pure semi-permeable polymer. In various embodiments, the substantially pure semi-permeable material comprises a substantially pure PTFE polymer.

[0213] In another embodiment, the film comprises a tensiled material. In various embodiments, the tensiled material comprises a filler. Fillers include, but are not limited to, glass fiber, carbon powder, carbon fiber, graphite, bronze powder, or molybdenum disulfide powder. In various embodiments, the film comprises a tensile strength ranging from about lOMpa to about 40Mpa.

[0214] The film may be amorphous, crystalline, or semi-crystalline. Typically, a fully amorphous film would be more permeable than a fully crystalline film. Typically, a semicrystalline polymer allowing molecules to permeate the film at the non-crystalline phases of the film. PTFE is a non-limiting example of a semi-crystalline polymer. In certain embodiments, the film is a semi-crystalline polymer. In certain embodiments, the film is a semi-crystalline PTFE.

[0215] The film may be any suitable shape. In certain embodiments, the film is circular, elliptical, polygonal, w-sided polygonal having n equal to about 3 to 20. In certain embodiments, the housing is circular, oval, triangular, square, rectangular, hexagonal, octagonal. The film may be of regular or irregular shape. In certain embodiments, the film is a regular polygon or an irregular polygon.

[0216] In one aspect, the film comprises a sheet. The sheet may be flat, pleated, fluted, folded, creased, or crimped. Pleats may be pressed or rounded.

[0217] In certain embodiments, the semi-permeable film between the inlet and outlet portion of the housing is pleated to increase its surface area. In one non-limiting example, the film comprises a pleated 12-inch-wide film.

[0218] The film comprises a substantially non-porous material sheet. Typically, a non-porous material does not have any openings, holes, cavities, channels or voids that would allow liquids, solids or vapor to freely pass through. In one embodiment, the film comprises a porosity of about 0%. In various embodiments, the film comprises a porosity of at most about 1%. In various embodiments, the film comprises a porosity of less than 1%. In various embodiments, the film comprises a porosity of at most 0.1%.

[0219] In one aspect, the oxygen permeability coefficient of the film is at least about 1 (mL mm) / (m2atm day), preferably more than 10 (mL mm) / (m2atm day) and more preferably at least about 100 (mL mm) / (m2atm day). In various embodiments, the film comprises an oxygen permeability coefficient of at least about 10 (mL mm) / (m2atm day), at least about 20 (mL mm) / (m2atm day), at least about 30 (mL mm) / (m2atm day), at least about 40 (mL mm) / (m2atm day), at least about 50 (mL mm) / (m2atm day), at least about 100 (mL mm) / (m2atm day), at least about 200 (mL mm) / (m2atm day), at least about 300 (mL mm) / (m2atm day), at least about 400 (mL mm) / (m2atm day), at least about 500 (mL mm) / (m2atm day), at least about 1,000 (mL mm) / (m2atm day), at least about 2,000 (mL mm) / (m2atm day), at least about 10,000 (mL mm) / (m2atm day), or at least about 20,000 (mL mm) / (m2atm day).

[0220] In various embodiments, the film comprises an oxygen permeability coefficient ranging from about 100 to about 1,000 (mL mm) / (m2atm day). In various embodiments, the film comprises an oxygen permeability coefficient ranging from about 100 to about 1,000 (mL mm) / (m2atm day). In various embodiments, the film comprises an oxygen permeability coefficient ranging from about 200 to about 400 (mL mm) / (m2atm day). In various embodiments, the film comprises an oxygen permeability coefficient ranging from about 222 to about 387 (mL mm) / (m2atm day).

[0221] An example of an oxygen permeable film is PTFE (Teflon), having a permeability coefficient for oxygen of 222 to 387 cm3mm / m2atm day (Keller PE, Kouzes R. 2017. Water Vapor Permeation in Plastics. Pacific Northwest National Laboratory PNNL-26070. Prepared for the U.S. Department of Homeland Security, Domestic Nuclear Detection Office under U.S. Department of Energy Contract DE- AC05-76RL01830). As an example, the oxygen transmission rate of a PTFE film having a permeability coefficient for oxygen of 222 cm3mm / m2atm day, a thickness of 12.7 um (0.5 MIL) and a surface area of 62 cm2would be similar to the oxygen transmission rate of a standard 53-gallon oak barrel at the same oxygen partial pressure differential. Consequently, the same PTFE film with a surface area of 620 cm2would increase the oxygen transmission rate 10-fold compared to a standard oak barrel.

[0222] A skived PTFE sheet typically has a water vapor permeability coefficient of about 0.0045-0.30 (g mm) / (m2day). In one aspect, the permeability coefficient for watervapor of a PTFE film is at most about 10 (g mm) / (m2day), preferably at most about 1 (g mm) / (m2day) and more preferably at most about 0.3 (g mm) / (m2day).

[0223] In various embodiments, the film comprises a water vapor permeability coefficient of at most about 10 (g mm) / (m2day). In various embodiments, the film comprises a water vapor permeability coefficient of at most about 5 (g mm) / (m2day), 4 (g mm) / (m2day), 3 (g mm) / (m2day), 2 (g mm) / (m2day), or 1 (g mm) / (m2day). In various embodiments, the film comprises a water vapor permeability coefficient of at most about 0.5 (g mm) / (m2day), 0.4 (g mm) / (m2day), 0.3 (g mm) / (m2day), 0.2 (g mm) / (m2day), or 0.1 (g mm) / (m2day). In various embodiments, the film comprises a water vapor permeability coefficient of at most about 0.05 (g mm) / (m2day), 0.04 (g mm) / (m2day), 0.03 (g mm) / (m2day), 0.02 (g mm) / (m2day), or 0.01 (g mm) / (m2day). In various embodiments, the film comprises a water vapor permeability coefficient of at most about 0.005 (g mm) / (m2day), 0.004 (g mm) / (m2day), 0.003 (g mm) / (m2day), 0.002 (g mm) / (m2day), or 0.001 (g mm) / (m2day).

[0224] In one aspect, the permeability coefficient for ethanol vapor is at most about 10 (g mm) / (m2day), preferably at most about 1 (g mm) / (m2day) and more preferably at most about 0.3 (g mm) / (m2day). (See, Keller PE, Kouzes R. 2017. Water Vapor Permeation in Plastics. Pacific Northwest National Laboratory PNNL-26070. Prepared for the U.S. Department of Homeland Security, Domestic Nuclear Detection Office under U.S. Department of Energy Contract DE-AC05-76RL01830).

[0225] In various embodiments, the film comprises an ethanol vapor permeability coefficient of at most about 10 (g mm) / (m2day). In various embodiments, the film comprises an ethanol vapor permeability coefficient of at most about 5 (g mm) / (m2day), 4 (g mm) / (m2day), 3 (g mm) / (m2day), 2 (g mm) / (m2day), or 1 (g mm) / (m2day). In various embodiments, the film comprises an ethanol vapor permeability coefficient of at most about 0.5 (g mm) / (m2day), 0.4 (g mm) / (m2day), 0.3 (g mm) / (m2day), 0.2 (g mm) / (m2day), or 0.1 (g mm) / (m2day). In various embodiments, the film comprises an ethanol vapor permeability coefficient of at most about 0.05 (g mm) / (m2day), 0.04 (g mm) / (m2day), 0.03 (g mm) / (m2day), 0.02 (g mm) / (m2day), or 0.01 (g mm) / (m2day). In various embodiments, the film comprises an ethanol vapor permeability coefficient ofat most about 0.005 (g mm) / (m2day), 0.004 (g mm) / (m2day), 0.003 (g mm) / (m2day), 0.002 (g mm) / (m2day), or 0.001 (g mm) / (m2day).

[0226] In one example, a container is partially filled with a distillate, leaving a gas space above the distillate, the so-called headspace. An opening above the liquid surface area of the distillate connects the headspace with the surrounding atmosphere. The opening is closed via a semi-permeable film which is oxygen permeable but not permeable to ethanol vapor. The semi-permeable film closes the opening. The semi- permeable film can be directly attached to the opening or be part of an apparatus which is attached to the opening. The apparatus is designed to allow oxygen to enter the headspace from the surrounding atmosphere through the film. If the film is attached directly to the container, the surface area of the film can be smaller than the surface area of the hole of the container or it can be equal to the surface area of the hole. If the film is part of an apparatus which is attached to the hole of the container, the surface area of the film can be smaller, equal or larger than the surface area of the hole.

[0227] Total oxygen transmission through the film can be smaller, equal or larger than the oxygen transmission through the entire surface area of the oak barrel.

[0228] Seal

[0229] In various embodiments, the assembly or its component parts are sealed. In various embodiments, the assembly, as a whole, is sealed. In various embodiments, individual components alone or in combination are sealed.

[0230] In various embodiments, the assembly comprises a seal. In various embodiments, the assembly comprises at least one seal. In various embodiments, the assembly comprises at least two seals.

[0231] The seal may be a one-way or a two-way seal. The seal may be impermeable in one direction, either in or out. The seal may be impermeable in both directions, in and out.

[0232] In various embodiments, the seal comprises an impermeable material. Any suitable impermeable material may be used.

[0233] In various embodiments, the impermeable material comprises a metal, plastic, or glass. In various embodiments, the polymeric material comprises acrylic, polyester, silicone, polyurethane, or halogenated plastic. In various embodiments, the polymeric material comprises a thermoplastic, thermoset, conductive polymer, biodegradable plastic, engineered plastic or elastomer. In various embodiments, the impermeable material comprises a polymeric, non-polymeric, synthetic, or natural material. Examples of suitable impermeable materials include but are not limited to, polyethylene (PE) including low-density polyethylene (LDPE), high-density polyethylene (HDPE), polypropylene (PP), polyvinyl chloride (PVC), polyethylene terephthalate (PET), polyamide (Nylon), polystyrene (PS), polyethylene naphthalene (PEN), polyimide (PI), polyvinylidene chloride (PVDC), ethylene vinyl alcohol (EVOH), methyl methacrylate (PMMA), polybutylene terephthalate (PBT), polyether ether ketone (PEEK), acrylonitrile butadiene styrene (ABS), high impact polystyrene (HIPS), polycarbonate (PC), polycarbonate + acrylonitrile butadiene styrene (PC + ABS), polyethylene + acrylonitrile butadiene styrene (PE + ABS), poly etherimide (PEI), polyimide, poly sulfone, polytetrafluoroethylene (PTFE), polyamide-imide (PAI), polylactic acid (PLA), or latex. In various embodiments, the non-polymeric materials comprise a metal or non-metal. In various embodiments, the metal comprises a pure metal or a metal alloy. In various embodiments, the metal comprises aluminum, stainless steel, brass, or copper. In various embodiments, the non-metal comprises glass, ceramic, or composite material. The impermeable material may be expandable or non-expandable. The impermeable material may comprise a stretchable or a non-stretchable material.

[0234] In various embodiments, the impermeable material is a PET / Aluminum / Nylon / polypropylene composite. In certain embodiments, the impermeable material provides a substantially complete oxygen / alcohol barrier. In various embodiments, the impermeable material is substantially inert. In certain embodiments, the impermeable material comprises a food grade material. In various embodiments, the impermeable material comprises a food grade material on the inside (i.e., the side proximal or close to the cask). A composite may comprise two or more layers of polymer and metal foils.

[0235] In various embodiments, the non-permeable or impermeable material is a material that allows about 0% to about 10% of a substance to pass through the material in a year. In various embodiments, the impermeable material is a material that allows about 0% to about 1% of a substance to pass through the material in a year.

[0236] In various embodiments, the impermeable material is a material that allows less than about 1% of a substance to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.5% of a substance to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.1% of a substance to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.01% of a substance to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.001% of a substance to pass through the material.

[0237] In various embodiments, the impermeable material is a material that allows less than about 1% of oxygen to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.5% of oxygen to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.1% of oxygen to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.01% of oxygen to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.001% of oxygen to pass through the material.

[0238] In various embodiments, the impermeable material is a material that allows less than about 1% of ethanol to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.5% of ethanol to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.1% of ethanol to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.01% of ethanol to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.001% of ethanol to pass through the material.

[0239] In various embodiments, the impermeable material is a material that allows less than about 1% of water to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.5% of water to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.1% of water to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.01% of water to pass through the material. In various embodiments, the impermeable material is a material that allows less than about 0.001% of water to pass through the material.

[0240] In various embodiments, the impermeable material is a material that has a permeability coefficient for ethanol vapor of at most about 10 (g mm) / (m2day). In various embodiments, the impermeable material is a material that has a permeability coefficient for ethanol vapor of at most about 1 (g mm) / (m2day). In various embodiments, the impermeable material is a material that has a permeability coefficient for ethanol vapor of at most about 0.5 (g mm) / (m2day), at most about 0.3 (g mm) / (m2day), or at most about 0.1 (g mm) / (m2day).

[0241] In various embodiments, the impermeable material is a material that has a permeability coefficient for water vapor of at most about 10 (g mm) / (m2day). In various embodiments, the impermeable material is a material that has a permeability coefficient for water vapor of at most about 1 (g mm) / (m2day). In various embodiments, the impermeable material is a material that has a permeability coefficient for water vapor of at most about 0.5 (g mm) / (m2day), at most about 0.3 (g mm) / (m2day), or at most about 0.1 (g mm) / (m2day).

[0242] In particular embodiments, the container is sealed from the outside to prevent the liquid from evaporating through the walls of the container. A seal on the outside of the container allows the liquid to remain in contact with the container. For example, with a seal on the outside of an oak barrel, a distilled spirit may interact with the inside of an oak barrel while not traversing oak of the barrel and then evaporating to the air outside of the barrel. In various embodiments, the container is sealed from the outside to prevent oxygen from escaping from the barrel. In various embodiments, the container is sealed from the outside to prevent alcohol from escaping the barrel.

[0243] In various embodiments, the seal is substantially non-permeable to alcohol and substantially non-permeable to oxygen. Although less than ideal, it is acceptable if the reservoir is refilled during ageing. Losing alcohol may still be acceptable as long as the amount is small. The typical angel's share is about 2% a year. Losing 0.02 or even 0.2% of alcohol a year could still be acceptable.

[0244] In various embodiments, the seal is substantially impermeable to alcohol. In various embodiments, the seal is substantially impermeable to ethanol. In various embodiments, the seal is a foil substantially impermeable to ethanol. In various embodiments, the seal is substantially impermeable to water. In various embodiments, the seal is a foil substantially impermeable to water.

[0245] In various embodiments, the seal is a foil. In various embodiments, the seal is a bag. Optionally, the bag is placed around the container. Optionally, the seal is placed over an opening in the container. In various embodiments, a container such as a barrel is placed inside a seal bag.

[0246] In various embodiments, the seal is applied to the outside of the barrel with a brush or sprayed. In various embodiments, the seal is applied to the outside of the barrel by wrapping a material around the container.

[0247] The seal may also be a foil made of the same materials as listed for the reservoir. The seal may also be a foil made of the same flexible materials as listed for the reservoir. In various embodiments, the seal comprises a foil. In certain embodiments, the foil is a multilayered polymeric material. In certain embodiments, the foil is a multilayered polymeric material substantially impermeable to oxygen and distilled spirit.

[0248] In various embodiments, the seal comprises a food grade material.

[0249] In various embodiments, the seal is a natural product, a modified natural product, a synthetic product, a semisynthetic product, or any combination thereof. In various embodiments, the seal is a natural product. In various embodiments, the seal is a modified natural product. In various embodiments, the seal is a synthetic product. In various embodiments, the seal is a semisynthetic product. In various embodiments, theseal is any combination of a natural product, a modified natural product, a synthetic product, a semisynthetic product.

[0250] In various embodiments, the seal comprises a foil. In various embodiments, the seal comprises a flexible foil. In various embodiments, the seal comprises a multilayered material. In various embodiments, the seal comprises a heat sealable material. In various embodiments, the seal comprises a material that can be glued to itself or another component of an assembly.

[0251] In various embodiments, the seal comprises MARVELSEAL MS-360 comprising an O2 transmission rate (MOCON) of 0.0006 cc / 100 in2 / 24 h, water vapor transmission rate (ASTM F 1249) of 0.0005 gm / 100 in2 / 24 h and a thickness (TAPPI 411) of 5.2 mil (nominal).

[0252] In various embodiments, the seal comprises PAKDRY7500 (Impak Corp.) comprising an O2 transmission rate of less than 0.0005 cc / 100 in2 / 24 h, water vapor transmission rate (ASTM F 1249) of less than 0.0006 gm / 100 in2 / 24 h and a thickness of 7.5 mil (minimum). Alternatively, the seal comprises MIL-PRF-13 L

[0253] In various embodiments, the seal comprises a natural product. In various embodiments, the seal comprises a natural product comprising a wax or wax -like material. In various embodiments, the wax is a natural wax. In various embodiments, the wax is a synthetic wax. In various embodiments, the wax is a bees-wax, a paraffin wax or a combination of bees-wax and paraffin wax. In certain embodiments, paraffin wax is used to seal the barrel. In various embodiments, the seal comprises a natural product comprising a shellac or shellac-like material. In various embodiments, the shellac is a natural resin-based shellac. In various embodiments, the seal comprises a natural product comprising rubber. In various embodiments, the natural rubber comprises a natural latex or isoprene (latex). In various embodiments, the synthetic material is a synthetic rubber. In various embodiments, the synthetic material comprises an isoprene product. In various embodiments, the synthetic rubber is a synthetic latex.

[0254] In various embodiments, the seal comprises a synthetic product. In various embodiments, the seal comprises a synthetic product comprising a polymer. In various embodiments, the synthetic product comprises a plastic. In certain embodiments, theplastic comprises polyethylene (PE) including low-density polyethylene (LDPE), high- density polyethylene (HDPE), polypropylene (PP), polyvinyl chloride (PVC), polyethylene terephthalate (PET), polyamide (Nylon), polystyrene (PS), polyethylene naphthalene (PEN), polyimide (PI), polyvinylidene chloride (PVDC), ethylene vinyl alcohol (EVOH), ethylene vinyl alcohol (EVOH), methyl methacrylate (PMMA), polybutylene terephthalate (PBT), polyether ether ketone (PEEK), acrylonitrile butadiene styrene (ABS), high impact polystyrene (HIPS), polycarbonate (PC), polycarbonate + acrylonitrile butadiene styrene (PC + ABS), polyethylene + acrylonitrile butadiene styrene (PE + ABS), polyetherimide (PEI), polyimide, poly sulfone, polytetrafluoroethylene (PTFE), polyamide-imide (PAI), polylactic acid (PLA), AB S / Poly carbonate Polyethylene, PF A, PFE, or latex.

[0255] In various embodiments, the seal comprises a synthetic product comprising synthetic rubber. Synthetic rubber is typically an artificial elastomer. Advantages of synthetic rubber include resistance to oxidizing agents. A common synthetic rubber is styrene-butadiene rubber (SBR) derived from the copolymerization of styrene and 1,3- butadiene. Additional synthetic rubbers include, but are not limited to, silicone rubber, polyisoprene, polyisobutylene, neoprene, and nitrile. Nitrile rubber is typically made from cyanobutadiene or 2-propenenitrile and butadiene.

[0256] In various embodiments, the synthetic rubber is PlastiDip® or HCFeccs®. In various embodiments, the synthetic product comprises an acrylic-based polymer.Examples of an acrylic-based polymer include, but are not limited to, HCFeccs® F-688 / F-688 s (Performix brand).

[0257] In various embodiments, the seal comprises a dip coating. In various embodiments, the dip coating is PlastiDip® or HCFeccs®. Typically, a dip coating involves immersing a substrate in a precursor solution and then lifting it vertically from the solution at a certain velocity. A certain wet coating thickness is dragged from the liquid upward along with the moving substrate. In various embodiments, the dip coating is applied by inserting and removing the container from a bath of coating. In various embodiments, the dip coating may be sprayed onto the container. In various embodiments, the dip coating may produce a coating on the container.

[0258] In various embodiments, the seal may be a thick or thin coating. In various embodiments, the coating may produce a thin seal on the container. In various embodiments, the seal comprises a thickness within a nanometer, micrometer, or millimeter range. In various embodiments, the seal comprises a thickness within the millimeter range. In various embodiments, the seal comprises a thickness of at least about 0.1 mm. In various embodiments, the seal comprises a thickness of at least about 0.2 mm. In various embodiments, the seal comprises a thickness of at least about 0.5 mm. In various embodiments, the seal comprises a thickness of at least about 1 mm. In various embodiments, the seal comprises a thickness of at least about 10 mm. In various embodiments, the seal comprises a thickness of at least about 100 mm.

[0259] The seal thickness may be within the nanometer (nm) or micrometer (pm) range. In various embodiments, the seal comprises a thickness ranging from about 1 nm to about 1 pm, ranging from about 5 nm to about 500 nm, or ranging from about 10 nm to about 100 nm. In various embodiments, the seal comprises a thickness of about 25 nm. In various embodiments, the seal comprises a thickness ranging from about 1 nm to about 1 mm, between 25 nm and 50 pm.

[0260] In various embodiments, the seal comprises a thickness ranging from about 1 pm to about 1 mm. In various embodiments, the film comprises a thickness ranging from about 5 pm to about 500 pm, ranging from about 10 pm to about 100 pm.

[0261] In various embodiments, the seal comprises a thickness ranging from about 1 mm to about 100 mm. In various embodiments, the seal comprises a thickness ranging from about 1 mm to about 10 mm. In various embodiments, the seal comprises a thickness ranging from about 5 mm to about 500 mm, ranging from about 10 mm to about 100 mm.

[0262] In various embodiments, the seal comprises a thickness of at least about 10 pm, 25 pm, 50 pm, 75 pm, or 100 pm. In various embodiments, the seal comprises a thickness of at least about 10 nm, 25 nm, 50 nm, 75 nm, or 100 nm. In various embodiments, the seal comprises a thickness of at least about 10 mm, 25 mm, 50 mm, 75 mm, or 100 mm.

[0263] In various embodiments, the seal comprises a thickness of about 5 nm, 10 nm, 15 nm, 20 nm, 25 nm, 30 nm, 35 nm, 40 nm, 45 nm, 50 nm, 55 nm, 60 nm, 65 nm, 70 nm, 75 nm, 80 nm, 85 nm, 90 nm, 95 nm, or 100 nm. In various embodiments, the film comprises a thickness of about 100 nm, 200 nm, 300 nm, 400 nm, 500 nm, 600 nm, 700 nm, 800 nm, 900 nm, or 1000 nm.

[0264] In various embodiments, the seal comprises a thickness of about 5 pm, 10 pm, 15 pm, 20 pm, 25 pm, 30 pm, 35 pm, 40 pm, 45 pm, 50 pm, 55 pm, 60 pm, 65 pm, 70 pm, 75 pm, 80 pm, 85 pm, 90 pm, 95 pm, or 100 pm. In various embodiments, the film comprises a thickness of about 100 pm, 200 pm, 300 pm, 400 pm, 500 pm, 600 pm, 700 pm, 800 pm, 900 pm, or 1000 pm.

[0265] In various embodiments, the seal comprises a thickness of about 5 mm, 10 mm, 15 mm, 20 mm, 25 mm, 30 mm, 35 mm, 40 mm, 45 mm, 50 mm, 55 mm, 60 mm, 65 mm, 70 mm, 75 mm, 80 mm, 85 mm, 90 mm, 95 mm, or 100 mm. In various embodiments, the film comprises a thickness of about 100 mm, 200 mm, 300 mm, 400 mm, 500 mm, 600 mm, 700 mm 800 mm, 900 mm, or 1000 mm. In various embodiments, the film comprises a thickness of about 1 mm, 2 mm, 3 mm, 4 mm, 5 mm, 6 mm, 7 mm, 8 mm, 9 mm, or 10 mm.

[0266] In various embodiments, the seal comprises a thickness of about 1 mil to about 10 mil. In certain embodiments, the bag has a thickness of about 1.0, 1.5, 2.0, 2.5, 3.0, 3.5, 4.0, 4.5, 5.0, 5.5, 6.0, 6.5, 7.0, 7.5, 8.0, 8.5, 9.0, 9.5, or 10 mil.

[0267] In various embodiments, the seal comprises a thickness ranging from about 0.1 mm to about 10 mm. In various embodiments, the seal comprises a thickness ranging from about 0.5 mm to about 5 mm. In various embodiments, the seal comprises a thickness ranging from about 1 mm to about 5 mm.

[0268] In various embodiments, the seal comprises a thickness of about 0.1 mm. In various embodiments, the seal comprises a thickness of about 0.5 mm. In various embodiments, the seal comprises a thickness of about 1 mm. In various embodiments, the seal comprises a thickness of about 2 mm. In various embodiments, the seal comprises a thickness of about 3 mm. In various embodiments, the seal comprises a thickness of about 4 mm. In various embodiments, the seal comprises a thickness of about 5 mm. In variousembodiments, the seal comprises a thickness of about 6 mm. In various embodiments, the seal comprises a thickness of about 7 mm. In various embodiments, the seal comprises a thickness of about 8 mm. In various embodiments, the film comprises a thickness of about 9 mm. In various embodiments, the film comprises a thickness of about 10 mm.

[0269] In various embodiments, the seal comprises a support. In various embodiments, the seal is a foil. Typically, a foil may support itself. Typically, a seal may be a homogenous thin thermoplastic material or mix of materials. Typically, a foil may be two or more films laminated together. As a non-limiting example, Mylar (©DuPont) may be a film or may be a component of a metalized foil as used in helium balloons. In certain embodiments, the film comprises Mylar. Several types of Mylar are commercially available, in a variety of thicknesses. (See for example, www.tekra.com / products / films / polyester-films / polyester-pet / mylar).

[0270] In various embodiments, the seal comprises a polyester film. In various embodiments, the seal comprises a metallized film. In various embodiments, the seal comprises a metalized polyester film. In various embodiments, metalized polyester film comprises aluminum.

[0271] In various embodiments, the seal comprises an acetate. In various embodiments, the seal comprises an acetate foil or acetate film. In various embodiments, the acetate is cellulose diacetate.

[0272] In various embodiments, the seal comprises a high tensile strength, high chemical stability, and high dimensional stability.

[0273] In certain embodiments, the seal is a barrier bag. In certain embodiments, the seal is a Mylar foil bag or Versify (©DOW Chemical) Series material. In certain embodiments, the seal is Mylar foil bag or Versify bag.

[0274] In certain embodiments, the bag has a thickness of about 1 mil to about 10 mil. In certain embodiments, the bag has a thickness of about 1.0, 1.5, 2.0, 2.5, 3.0, 3.5, 4.0, 4.5, 5.0, 5.5, 6.0, 6.5, 7.0, 7.5, 8.0, 8.5, 9.0, 9.5, or 10 mil.

[0275] Suitable bags are typically large enough to enclose one or more barrels. As a non-limiting example, a bag may have dimensions of about 36” in height and 24” in outer diameter. A 53-gallon barrel may fit inside a 38” x 42” Mylar foil bag. See for example, IMPAK 38MFS42, 4.3 mil, 38” x 42” Mylar Foil Bag / Box Liner.

[0276] In various embodiments, the seal comprises a polyester foil comprises a stretched polyethylene terephthalate (PET). In various embodiments, the polyester foil comprises biaxially oriented polyethylene terephthalate (BoPET; Mylar, DuraLar (Grafix Plastics)), or propyl ene / ethylene elastomer such as Versify.

[0277] In certain embodiments, the seal comprises a polymer foil is opaque. In certain embodiments, the polymer foil comprises a metal coating. In certain embodiments, the polymer foil comprises an aluminum coating. In certain embodiments, the polymer foil comprises a metalized polymer. In certain embodiments, the metalized polymer comprises aluminum.

[0278] Examples of foil material that is particularly well suited for the present application include, but are not limited to, PAKVF4PC, PAKVF4MCP, PAKVF4PCA and PAKSAFE320 (IMPAK Corporation). They are, respectively, Biaxially Oriented Nylon) / .5mil ALUMINUM FOIL / 4.4 mil CAST POLYPROPYLENE; 48GaPET / . 9 mil PE / . 0003 FOIL / 2.4mil Cast Polypropylene; 48gaPET / .00035 Aluminum Foil / 60 ga Biaxially Oriented Nylon [BON] / 2.75 mil high temperature cast polypropylene; 60 Gauge biaxially oriented NYLON / 0.00035” FOIL / 60-Gauge biaxially oriented NYLON / Proprietary Adhesive / 3.5 mil Ultra High Temperature Grade Cast Polypropylene.

[0279] As a non-limiting example, PAKDRY7500 (IMPAK Corp.) is a 7.5 mil thick (minimum) high moisture and gas (oxygen, carbon dioxide et al) barrier foil with a dual layer of both 48-gauge polyester and 60-gauge biaxially oriented nylon providing very high tensile strength and resistance to puncture, making this product suitable for vacuum packaging applications and for very large bags including cargo container liners. As an FDA approved substrate for food contact the 6.0 mil metallocene P.E. sealant layer has made PAKDRY7500 the product of choice for bulk food, fine pharmaceutical powders, and medical device engineering specifications.

[0280] In various embodiments, the seal comprises a thermoplastic polymer. In various embodiments, the seal comprises Polyethylene terephthalate [polyethylene terephthalate); PET],

[0281] In various embodiments, the seal comprises a natural product. In various embodiments, the natural product is rubber. In certain embodiments, the natural product is latex.

[0282] In certain embodiments, the seal comprises a synthetic product. In various embodiments, the synthetic product is latex, polychloroprene, or a nylon fabric.

[0283] In various embodiments, the seal comprises glass. Suitable glass includes, but is not limited to, borosilicate glass, and Pyrex. In various embodiments, the reservoir is a glass reservoir. In various embodiments, the reservoir is made of borosilicate glass or Pyrex.

[0284] In various embodiments, the seal foil can be a monolayer foil or a multilayer foil. In a non-limiting example, the foil comprises a first layer that is an inner foil layer which serves as a heat-seal layer, a second layer that is a first outer foil layer and which serves as an impermeable barrier layer. In certain embodiments, the foil further comprises a third layer which is a second outer foil layer. The outermost layer may serve as an abuse layer.

[0285] As used herein, the term “heat-seal,” and the phrase “heat-sealing” refer to any seal of a first discrete region of a foil surface to a second discrete region of a foil surface, wherein the heat seal is formed by heating the discrete regions to at least their respective seal initiation temperatures. Suitable polymers for use in heat seal layers are homogeneous ethylene / alpha-olefin copolymer, ethylene / vinyl acetate copolymer, and ionomer resin.

[0286] In various embodiments, the foil comprises a means of creating a seal or impermeable closure. In various embodiments, the foil comprises a self-sealing valve. In various embodiments, the foil comprises an adhesive. In various embodiments, the foil comprises a heat-seal.

[0287] Alternatively, seals may be closed using any suitable sealing clip, adhesive tape, a zipper, zipper tape, sealing tape, or impulse sealer, glue, or an adhesive. Suitable zipper seals include but are not limited to ZipSeal™ (Impak) and Ziploc™ (J&J). Open Zipper End (OZE) ZipSeal™ Bags are closed on 3 sides and open at the zipper end. In various embodiments, the reservoir is sealed using an adhesive or glue.

[0288] Duration

[0289] In one aspect, the present disclosure provides a method for decreasing the time required to age a distilled spirit. In various embodiments, the distilled spirit is aged for 50 years or less. In various embodiments, the distilled spirit is aged for 20 years or less. In various embodiments, the distilled spirit is aged for 15 years or less. In various embodiments, the distilled spirit is aged for 10 years or less. In various embodiments, the distilled spirit is aged for 5 years or less. In various embodiments, the distilled spirit is aged for 3 years or less. In various embodiments, the distilled spirit is aged for 2 years or less. In various embodiments, the distilled spirit is aged for 1 year or less. In various embodiments, the distilled spirit is aged for less than about 10 years. In one embodiment, the distilled spirit is aged for less than about 9 years. In various embodiments, the distilled spirit is aged for less than about 8 years. In various embodiments, the distilled spirit is aged for less than about 7 years. In various embodiments, the distilled spirit is aged for less than about 6 years. In various embodiments, the distilled spirit is aged for less than about 5 years. In various embodiments, the distilled spirit is aged for less than about 4 years. In various embodiments, the distilled spirit is aged for less than about 3 years. In various embodiments, the distilled spirit is aged for less than about 2 years. In various embodiments, the distilled spirit is aged for less than about 1 year.

[0290] In various embodiments, the distilled spirit is aged for less than about 12 months. In one embodiment, the distilled spirit is aged for less than about 11 months. In one embodiment, the distilled spirit is aged for less than about 10 months. In one embodiment, the distilled spirit is aged for less than about 9 months. In one embodiment, the distilled spirit is aged for less than about 8 months. In one embodiment, the distilled spirit is aged for less than about 7 months. In one embodiment, the distilled spirit is aged for less than about 6 months. In one embodiment, the distilled spirit is aged for less than about 5 months. In one embodiment, the distilled spirit is aged for less than about 4 months. In one embodiment, thedistilled spirit is aged for less than about 3 months. In one embodiment, the distilled spirit is aged for less than about 2 months. In one embodiment, the distilled spirit is aged for less than about 1 month.

[0291] Additional components

[0292] Optionally, the assembly of the present disclosure additionally comprises one or more of the following: Oxygen sensor, Methanol sensor, Acetone sensor, Ethyl acetate sensor, Volatile Organic Compound (VOC) sensor, Port to take gas samples for analysis (e.g., GC / MS), Air / gas Regulator, and / or Airtight connections.

[0293] Methods

[0294] The present disclosure also provides methods of ageing a distilled spirit.

[0295] In one aspect, the method of ageing a spirit, comprises the steps of: (a) providing a substantially increased amount of oxygen for the spirit, and (b) preventing evaporation loss from the spirit. In various embodiments, the step of substantially increasing the amount of oxygen comprises increasing headspace in a container. In various embodiments, the step of substantially increasing the amount of oxygen comprises providing a container with a semi-permeable material, wherein the material is permeable to oxygen and substantially impermeable to vapor. In various embodiments, the step of substantially increasing the amount of oxygen comprises the step of attaching an oxygen supply reservoir to a container.

[0296] In one aspect, the method for ageing a spirit comprises the step of attaching an air gate to a container, wherein the container holds the distilled spirit, and wherein the air gate comprises a semi-permeable film, and wherein the semi-permeable film is permeable to oxygen and substantially impermeable to vapor.

[0297] In one aspect, the method for ageing an alcoholic beverage comprises the steps of: a. providing a container; b. providing a reservoir; c. adding a distilled spirit to the container; d. adding oxygen gas or an oxygen-inert gas mixture to the reservoir; and e. connecting the reservoir to the container.

[0298] Another aspect of the present disclosure provides a method of oxygenating a distillate spirit by having the surface of the distillate spirit be in direct contact with oxygen, or an oxygen - inert gas mixture or air such that the oxygen concentration in the gas phase is higher than the oxygen concentration in the distillate spirit.

[0299] In various embodiments, the method for oxygenating a spirit comprising the steps of: a. providing a container; b. providing a reservoir; c. adding a distilled spirit to the container; d. adding oxygen gas or an oxygen-inert gas mixture to the reservoir; and e. connecting the reservoir to the container.

[0300] An exemplary method is shown by the flowchart shown in Figure 9. In such a method, an unsealed container is first sealed with an impermeable material to form a sealed container. Secondly, liquid such as a distilled spirit is added to fill the container forming a filled sealed container. Thirdly, an oxygen reservoir is attached to the filled sealed container to form a filled sealed container with an attached oxygen reservoir. A reservoir is filled with oxygen to form an oxygen reservoir.

[0301] The methods of the present invention may use any suitable sequence of steps. In one non-limiting example, the method comprised a sequence of first filling the reservoir with oxygen followed by connecting the reservoir to the container. In anothernon-limiting example, the method comprises first connecting the reservoir to the container, followed by filling it with oxygen.

[0302] In one non-limiting example, a standard barrel is transported from the cooperage to the distillery, filled with a distilled spirit at the distillery, transported to the warehouse (rick house), wrapped in an impermeable foil, placed in its storage location, and attached to the oxygen reservoir.

[0303] Kits

[0304] One aspect of the present disclosure provides a kit comprising a selection of component parts of the assembly for ageing an alcoholic beverage. In certain embodiments, the kit additionally comprises a set of instructions for assembling and / or using the assembly.

[0305] Analysis

[0306] A spirit’s composition, and effects of the invention, may be analyzed using instruments and techniques including, but not limited to, ultraviolet-visible spectroscopy (UV / VIS), Raman spectroscopy, X-ray fluorescence (XRF), liquid chromatography coupled with mass spectroscopy (LCMS), inductively coupled plasma mass spectroscopy (ICPMS), electronic nose (E-nose), chromatography (GC) coupled with flame ionization detector (FID), gas chromatography coupled with mass spectrometry (GC-MS) or infrared (IR) spectroscopy, or nuclear magnetic resonance (NMR). The results indicate that ageing markers such as ethyl acetate, ethyl formate, ethyl caproate, ethyl caprylate, ethyl caprate, ethyl laurate, isoamyl acetate, phenethyl acetate and higher alcohol esters increase in concentration and that higher alcohols such as n-propanol, n-butanol, isobutanol, isoamyl alcohol, phenethyl alcohol, etc. decrease in concentration. GC-MS analysis indicates that the sulfur compounds, after ageing as described herein, exhibit partial to complete reduction in their response without any additional peaks. No additional peaks in GC-MS analysis indicate that the sulfur compounds are not transformed to other chemical form during the treatment but are completely oxidized into oxides.

[0307] Assemblies

[0308] Referring to the figures, FIG. 1 A. shows one aspect of the invention wherein an oxygen supply reservoir 101 is connected to a container 104 containing a distilled spirit 108 though a conduit 102 such as plastic tubing. In this particular example, the oxygen supply reservoir is used to increase the headspace 109 from the container. Figure IB shows another aspect of the invention wherein the container is an oak barrel 104B. In this particular example, the barrel is attached to an oxygen supply reservoir 101 through a conduit 102. One end of the conduit is attached to the oxygen supply reservoir, and the opposite end of the conduit is attached to the barrel through a bung 103.

[0309] FIG. 2. shows a container 104 attached to a reservoir 101. In this particular example, inside the container is a distilled spirit 108 to be aged filling a portion of the container’s volume, with headspace 109 filling the remaining space within the container. The container is attached to one end of a first length of tubing as a conduit 102 through a bung plug 103. The tubing is used as a means to connect the container to an oxygen supply reservoir. The other end of the tubing is attached to a valve 111 that is connected to an oxygen supply reservoir. The valve is also connected to a second length of tubing that in turn is connected to an air regulator 110 on a pressurized oxygen tank 105. The pressurized oxygen tank is used as a means for replenishing the supply of oxygen 106 in the reservoir and headspace. An impermeable coating 107 surrounds the container.

[0310] FIG. 3 (A) shows one aspect of an assembly of the invention wherein a barrel 104B is placed on its side within a reservoir bag 101B and supported by a barrel cradle 114. In this particular example, the barrel is placed inside an oxygen supply reservoir bag comprising a material impermeable to water and ethanol. The barrel’s bung hole 115 is left open, either without a bung, or with an open bung cover 113. The reservoir bag comprises a closure 112 that is attached to a conduit 102 to a pressurized oxygen tank 105. The oxygen tank is used to inflate the oxygen reservoir bag. Then the closure is sealed. The oxygen tank and conduit may be removed from the bag or may be reattached or kept in place to refill the reservoir if desired. Fig. 3 (B) shows an analogous assembly with a barrel placed upright.

[0311] FIG. 4 shows one aspect of the invention wherein a single oxygen supply reservoir 101 supplies oxygen to a plurality of containers 104 filled with distilled spirit 108 and headspace 109. The containers may be placed in line, in an array, sequential, ornonsequential such as in a branched configuration. In this particular example, an oxygen supply reservoir 101 is attached to a series of three containers 104 containing distilled spirit 108. Valves 111 are attached to the reservoir and containers allowing them to be attached to conduits 102 for connecting to an oxygen tank 105 via an air regulator 110 attached to the tank. By manipulating the valves and regulator, a user can adjust the amount of oxygen 106 and contents of the headspace 109 in the system. A coating 107 may be applied to the surface of the containers.

[0312] FIG. 5 shows one aspect of the invention wherein an oxygen supply reservoir surrounds several containers holding distilled spirit. A plurality of barrels 104B are enclosed in a single oxygen reservoir bag 101B. In this particular example, three barrels are each placed on a barrel cradle 114 and then surrounded by a large bag 101B, comprising a material impermeable to oxygen, water and ethanol, to be used as an oxygen supply reservoir. The barrels bung holes 115 are left open, either without a bung, or with an open bung cover 113. The reservoir bag comprises a closure 112 that is attached to a conduit 102 to a pressurized oxygen tank 105. The oxygen tank is used to inflate the oxygen reservoir bag. Then the closure is sealed.

[0313] FIG. 6 shows one aspect of the invention wherein an oxygen supply reservoir 101 is placed on top of or above a container 104 or barrel 104B holding distilled spirit 108 to function as a means for increasing headspace 106. In one particular example, Fig. 6A shows a reservoir supported by a cradle 114 on top of a container holding a particular volume of distilled spirit. The total headspace includes the volume of headspace 109 comprising oxygen 106 in the container and the extended headspace from the reservoir. Fig. 6B shows a reservoir supported by a cradle 114 on top of a barrel 104B holding a particular volume of distilled spirit. In one particular example, a coating 107 is applied to the surface of the container 104 or barrel 104B. The oxygen supply reservoirs are connected to the containers using a conduit 102 and a stopper or bung.

[0314] FIG. 7 shows one aspect of the invention wherein an oxygen supply reservoir 101 comprises an impermeable bag 101B attached above a barrel that is either upright or on its side resting on a barrel cradle 114. Fig. 7A shows a barrel connected to a reservoir comprising an impermeable bag via a conduit 102 through a bung 103. Fig. 7B shows an impermeable bag covering an open top of a barrel. In this particular example, the top headof the barrel is removed. The reservoir 101B is connected to the barrel’s head hoop using a reservoir bag closure 112. The reservoir is filled with a volume of oxygen gas 106.

[0315] FIG. 8 is a flowchart illustrating an exemplary method of the present invention. In one particular example, a seal is added to an unsealed container to form a sealed container. Liquid, such as a distilled spirit, is added to the sealed container to form a filled sealed container. A reservoir is filled with oxygen to be an oxygen reservoir. An oxygen reservoir is attached to a sealed container to form an assembly comprising a sealed container and an oxygen supply reservoir.EXAMPLES

[0316] Exemplary methods and materials are described below, although methods and materials similar or equivalent to those described herein can also be used in the practice of the present invention and will be apparent to those of skill in the art. The materials, methods, and examples are illustrative only and not intended to be limiting.

[0317] Accordingly, the following examples merely illustrate the principles of the present disclosure. It will be appreciated that those skilled in the art will be able to devise various arrangements which, although not explicitly described or shown herein, embody the principles of the invention and are included within its spirit and scope. Furthermore, all examples and conditional language recited herein are principally intended to aid the reader in understanding the principles of the invention and the concepts contributed by the inventor to furthering the art, and are to be construed as being without limitation to such specifically recited examples and conditions. Moreover, all statements herein reciting principles, aspects, and embodiments of the invention as well as specific examples thereof, are intended to encompass both structural and functional equivalents thereof. Additionally, it is intended that such equivalents include both currently known equivalents and equivalents developed in the future, i.e., any elements developed that perform the same function, regardless of structure. The scope of the present invention, therefore, is not intended to be limited to the exemplary embodiments shown and described herein.

[0318] Example 1

[0319] Controlled Ageing Experiment with Oak Chips Under Pure Oxygen at Elevated Temperature

[0320] Whiskey distillate (2044 mL at 62.5% ABV) was added to a 5 L demijohn. Oak chips (24.5 g toasted at 425 deg F for 40 minutes) were added to the distillate followed by flushing the headspace of the demijohn with pure oxygen gas. A Mylar balloon of equal size to the demijohn was inflated with pure oxygen gas before attaching it to the demijohn airtight via a silicon stopper. The demijohn was then kept at room temperature, exposing the whiskey distillate to oak chips under pure oxygen. Within one month, the flavor and aroma profile improved significantly, with fruity, sweet andcomplex notes developing without any oaky / woody notes remaining from the initial stage of oak chip ageing. After 4 months at room temperature, the demijohn was placed on a heating plate, increasing the temperature of the whiskey distillate to 33 degrees Celsius. This was maintained for another 8 months. The distillate continued to improve throughout, with increased complexity developing as the ageing process advanced. There was no evaporation loss throughout the ageing process as the system was perfectly closed. At intervals, the mylar balloon was reinflated with pure oxygen to ensure that the distillate was kept under a pure oxygen atmosphere. The color of the distillate intensified throughout as measured spectrophotometrically at 520 nm (1 cm path cuvette, ambient temperature and atmosphere, Spectronic 21 Milton Roy Company), reaching 0.305 (5 months), 0.335 (6 months), 0.338 (8 months) and 0.360 (13 months).

[0321] Example 2

[0322] Controlled Ageing Experiment in a Sealed Oak Cask Under Oxygen

[0323] Whiskey distillate (15.3 kg at 62.5% ABV) was added to an oak cask previously used for ageing Bourbon (5 gallon), leaving a headspace of about 8 cm as measured at the bung hole (bottom of oak stave to top of distillate). The bung hole was kept open and the cask was generously wrapped and sealed into a foil impermeable to oxygen and ethanol (IMPAK Corporation, PAKVF4PCA Mylar Foil Moisture Barrier Drum Liner, 48ga PET / 0.00035 Aluminum Foil / 60 ga Biaxially Oriented Nylon / 2.75 mils high temperature cast polypropylene). After sealing, the bag was inflated with pure oxygen by connecting it to an oxygen tank via a silicone tube and a syringe needle. With this volume, the bag held enough pure oxygen for maturing the barrel-ageing spirit for more than 10 years based on the estimated oxygen permeability of an oak barrel. The whiskey was aged for 7 months during which the color of the distillate changed from colorless to amber, and the sharp and raw odor typical for fresh whiskey distillate changed to a rounded, soft and mellow aroma.

[0324] Example 3

[0325] Controlled Ageing Experiment in an Oak Cask

[0326] Whiskey distillate (16.2 kg at 62.5% ABV) was added to an oak cask previously used for ageing Bourbon (5 gallon), leaving a headspace of about 8 cm depthas measured at the bung hole (bottom of oak stave to top of distillate). The bung hole was closed with a silicone bung. The whiskey was aged for 7 months during which the color of the distillate changed from colorless to amber. The sharp and raw odor typical for fresh whiskey distillate partially changed to a rounded, soft and mellow aroma, but was still noticeable. Dominating oaky / woody notes were noted, typical for a young or over-oaked whiskey.

[0327] Example 4

[0328] Controlled Ageing Experiment in an Oak Cask Inside a Sealed Bag

[0329] Whiskey distillate (15.6 kg at 62.5% ABV) was added to an oak cask previously used for ageing Bourbon (5 gallon), leaving a headspace of about 8 cm as measured at the bung hole (bottom of oak stave to top of distillate). The bung hole was closed with a silicone bung and the cask was wrapped and sealed into a foil impermeable to oxygen and ethanol (IMPAK Corporation, PAKVF4PCA Mylar Foil Moisture Barrier Drum Liner, 48ga PET / 0.00035 Aluminum Foil / 60 ga Biaxially Oriented Nylon / 2.75 mils high temperature cast polypropylene). After sealing, air from the inside of the bag was evacuated by connecting it to a vacuum via a silicone tube and a syringe needle. The whiskey was aged for 7 months during which color of the distillate changed from colorless to amber. The sharp and raw odor typical for fresh whiskey distillate partially changed to a rounded, soft and mellow aroma, but was still noticeable. Dominating oaky / woody notes were noted, typical for a young or over-oaked whiskey.

[0330]

[0331] Example s

[0332] Controlled Ageing Experiment in a Sealed Oak Cask Attached to an Oxygen Reservoir

[0333] Whiskey distillate (15.6 kg at 62.5% ABV) was added to an oak cask previously used for ageing Bourbon (5 gallon), leaving a headspace of about 8 cm as measured at the bung hole (bottom of oak stave to top of distillate). The bung hole was closed with a silicone bung and the cask was wrapped and sealed into a foil impermeable to oxygen and ethanol (IMPAK Corporation, PAKVF4PCA Mylar Foil Moisture Barrier Drum Liner, 48ga PET / 0.00035 Aluminum Foil / 60 ga Biaxially Oriented Nylon / 2.75mils high temperature cast polypropylene). A separate oxygen reservoir was created using the same impermeable material, having an oval base of 13 cm by 17 cm and a length of 26 cm. With this volume, the reservoir held enough pure oxygen for maturing the barrelageing spirit for more than 10 years based on the estimated oxygen permeability of an oak barrel. A stainless-steel valve was attached to one side of the reservoir. The reservoir was filled with pure oxygen and attached via the silicone bung to the sealed barrel. The whiskey was aged for 7 months during which the color of the distillate changed from colorless to amber, and the sharp and raw odor typical for fresh whiskey distillate changed to a rounded, soft and mellow aroma.

[0334] Example 6

[0335] Controlled Ageing Experiment with Oak Chips Under Ambient Air

[0336] Whiskey distillate (2645 mL at 62.5% ABV) was added to a 5 L demijohn.Oak chips (31.7 g toasted at 425 deg F for 40 minutes) were added to the distillate. The opening of the demijohn was closed with filter paper, allowing the distillate to be in contact with ambient air. The demijohn was then kept at room temperature, exposing the whiskey distillate to oak chips under ambient air. Over the course of several months, the initial sharp and raw odor typical for fresh whiskey distillate changed to a rounded, soft and mellow aroma. Evaporation losses were linear with 3.3% weight loss after 131 days. Within the first day of ageing, the color of the distillate changed from colorless to red, yellow and brown hues typical for an aged whiskey. After about 8 days, it became lighter before darkening again from day 29 onwards. This might be the result of an initial extraction of oak phenols followed by their oxidation. Color changes were measured spectrophotometrically at 520 nm (1 cm path cuvette, ambient temperature and atmosphere, Spectronic 21 Milton Roy Company). The observed absorbance corrected for evaporation losses was 0.165 (day 1), 0.168 (day 8), 0.136 (day 15), 0.129 (day 23), 0.131 (day 29), 0.154 (day 59), 0.197 (day 131), 0.228 (day 224).

[0337] Example 7

[0338] Controlled Ageing Experiment Without Oak Chips under Oxygen

[0339] A 500 ml round bottom flask was partially filled with a commercial American Single Malt Whiskey (45 % abv) with the fill level reaching the widest circumference ofthe flask. The flask was flushed with pure oxygen for 30 seconds before sealing it with a silicon stopper. After 8 months at room temperature, a sample was taken for analysis and sensory evaluation. Color changes were measured spectrophotometrically at 520 nm (1 cm path cuvette, ambient temperature and atmosphere, Spectronic 21 Milton Roy Company). The observed absorbance for the distillate kept under oxygen was 0.218, compared to 0.198 for the untreated commercial product. This change in absorbance was likely due to the oxidation of phenolic compounds, leading to higher absorbing chromophores. Sensory evaluation did not detect any harsh, off-notes from overoxidation. Flavor and aromas were similar to the commercial product.

[0340] Example 8

[0341] Controlled Ageing Experiment with Oak Chips under Pure Oxygen at Room Temperature

[0342] Whiskey distillate (2653 mL at 62.5% ABV) and oak chips (31.8 g toasted at 425 deg F for 40 minutes) were added to a 5 L demijohn. The demijohn was flushed with pure oxygen for 30 seconds and closed with a silicone stopper. An oxygen reservoir having an oval base of 11 cm by 13 cm and a length of 24 cm made of foil impermeable to oxygen and ethanol (IMPAK Corporation, PAKVF4PCA Mylar Foil Moisture Barrier Drum Liner, 48ga PET / 0.00035 Aluminum Foil / 60 ga Biaxially Oriented Nylon / 2.75 mils high temperature cast polypropylene) with a built-in stainless-steel valve was filled with pure oxygen before closing the valve. The reservoir was then attached to the demijohn via a silicone stopper and the valve opened allowing for a continuous oxygen supply of the distillate. The reservoir dimension was chosen to provide access oxygen for the distillate during the entire maturation process based on the known oxygen permeability of an oak cask. The whiskey was aged for 8 months during which the sharp and raw odor typical for fresh whiskey distillate changed to a rounded, soft and mellow aroma. There was no evaporation loss throughout the ageing process as the system was perfectly closed. Within the first day of ageing, the color of the distillate changed from colorless to red, yellow and brown hues typical for an aged whiskey. After about 8 days, it became lighter before darkening from day 31 onwards. Color changed were measured spectrophotometrically at 520 nm (1 cm cuvette, room temperature, (1 cm path cuvette, ambient temperature and atmosphere, Spectronic 21 Milton Roy Company), reaching0.192 (day 1), 0.155 (day 8), 0.115 (day 15), 0.110 (day 24), 0.110 (day 31), 0.118 (day 39), 0.122 (day 45), 0.142 (day 75), 0.171 (day 147), 0.190 (day 241).

[0343] Example 9

[0344] Controlled Ageing Experiment in an Oak Cask Connected to an Oxygen Reservoir

[0345] Whiskey distillate (8 gallon at 62.5% ABV) is added to an oak cask (10 gallon). The cask is wrapped and sealed into a foil impermeable to oxygen and ethanol and connected to a 3 L oxygen reservoir. With this volume, the reservoir holds enough pure oxygen for maturing the barrel-ageing spirit for an estimated 10 years. The reservoir is connected to the barrel via a Tygon tube attached to a silicon stopper closing the bung hole of the barrel. The whiskey is aged for 10 months during which it develops the fruity and complex notes of a well-aged whiskey. As the barrel is completely sealed, no loss due to evaporation (angel’s share) was observed.

[0346] Example 10

[0347] Controlled Ageing Experiment in an Oak Cask Connected to an Air Gate

[0348] Whiskey distillate (8 gallon at 62.5% ABV) is added to an oak cask (10 gallon) previously used for ageing Bourbon, leaving a headspace of about 20%. The bung hole is closed with a silicone bung and an air gate is attached to the silicone bung allowing air to enter the headspace of the cask. The whiskey is aged for 7 months during which the color of the distillate changed from colorless to amber and the sharp and raw odor typical for fresh whiskey distillate changes to a rounded, soft and mellow aroma.

[0349] Example 11

[0350] Ethanol Permeability of PTFE Film at Ambient Temperature

[0351] A 500 mL mason jar was filled with 267 g ethanol (95% abv). A circular opening was cut into the lid of the mason jar to which a 2” Tri Clamp Filter Plate was attached with silicone sealant. The opening of the Filter Plate was covered with 1 / 2 MIL skived PTFE film (CS Hyde Company). A 2” silicone gasket was placed on top followed by a second 2” Tri Clamp Filter Plate to complete the assembly. It was clamped together with a 2” Tri Clamp allowing air to enter the mason jar via the top opening through thePTFE film. The mason jar was kept at room temperature and weight periodically over a 82 day period. No evaporation losses were detected. In contrast, when using PTFE expanded porous membrane (Porex Virtek® MD22, 0.1 mm thickness, pore size range 0.1 - 5 um), 44% of alcohol was lost over a period of 13 days.

[0352] PTFE film is recognized for its relatively low permeability to water vapor ( Keller PE, Kouzes R. 2017. Water Vapor Permeation in Plastics. Pacific Northwest National Laboratory PNNL-26070. Prepared for the U.S. Department of Homeland Security, Domestic Nuclear Detection Office under U.S. Department of Energy Contract DE-AC05-76RL01830)), attributed to its non-polar nature (en.wikipedia.org / wiki / Polytetrafluoroethylene) and high crystallinity (Grytsenko K., et al. 2023. Optical and mechanical properties of thin PTFE Films, deposited from a gas phase. Macromol Mater Eng 308: 2200617). Given that ethanol has a larger molecular diameter than water (4.4 A and 2.8 A, respectively. Graziano G. 2004. Chem Phys Let, 396(4-6):226-231) at similar polarity (1.69 D and 1.8546 D, respectively. CRC Handbook of Chemistry and Physics, 2024, 105th edition), PTFE film is expected to be an effective barrier to ethanol vapor, much like it is to water vapor. This expectation was confirmed by the experiment.

[0353] Example 12

[0354] Air Gate Evaporation Test

[0355] Two 50 ml round bottom flasks were filled with 21 g ethanol 95% abv (Flask #1) and 26 g ethanol 95% abv (Flask #2). Flask #1 was closed with a silicone stopper having a 1 / 4 “ opening. Flask #2 was closed with an air gate attached to a silicone stopper via a 1 / 4” opening. Both flasks were placed in a dehydrator which was set at 40 deg Celsius under continuous ventilation to accelerate evaporation. Evaporation losses were recorded over a 10-day period. At the end of day 10, 100% of ethanol had evaporated from Flask #1, whereas the evaporation loss of Flask #2 was 8%.

[0356] Example 13

[0357] Air Permeability of Skived Teflon

[0358] At room temperature, a 0.5 MIL skived PTFE film (CS Hyde Company) was placed over the opening of a 500 ml wide-mouth mason jar. The band (ring) of the masonjar was loosely placed on top holding the film in place while allowing air to freely circulate in and out of the jar. The assembled jar was placed in a freezer at -18 degree Celsius. After one hour, the band was tightened holding the film firmly in place. It was then removed from the freezer and placed at room temperature (21 degree Celsius) to allow the air inside the mason jar to expand as the temperature increased. After 6 minutes at room temperature the PTFE film showed a slight bulge, evidence that the gas volume inside the mason jar was expanding while the air was gradually warming up to room temperature. After 40 minutes, the PTFE film was again flat, evidence that the increased volume had dissipated through the film.

[0359] The experiment was repeated using polyvinyl chloride film (Stretch-tite®). As the mason jar warmed to room temperature, the film expanded rapidly, forming a large bulge that persisted for over 13 days. This suggests that the polyvinyl chloride film has significantly lower air permeability than the PTFE film. Literature data of oxygen permeability of food grade PVC confirm this finding (Bastarrachea LJ et al. 2011. Engineering Properties of Polymeric-Based Antimicrobial Films for Food Packaging: A Review. Food Eng Rev, 3(2): 79-93).

[0360] Example 14

[0361] Air Gate Design

[0362] An air gate was assembled comprising a circular holder having a diameter of 11 cm with a 1 cm rim, holding in place a zig-zag folded PTFE film with a surface area of 635 cm2. The base of the air gate is securely attached to a silicone stopper, which is fitted into a barrel's bung hole. An opening at the top and bottom of the air gate allows for the free flow of air (oxygen) in and out of the barrel while blocking alcohol vapor from passing through. This assembly essentially creates an infinite headspace for the barrel.

Claims

CLAIMSWhat is claimed is:

1. A method for ageing a spirit, comprising the steps of:(a) providing a substantially increased amount of oxygen for the spirit, and(b) preventing evaporation loss from the spirit.

2. The method of claim 1, wherein the step of substantially increased amount of oxygen comprises increasing headspace in a container.

3. The method of claim 1, wherein the step of substantially increased amount of oxygen comprises providing a container with a semi-permeable material, wherein the material is permeable to oxygen and substantially impermeable to vapor.

4. The method of claim 1, wherein the step of substantially increased amount of oxygen comprises providing an oxygen supply reservoir.

5. A method for ageing a spirit, comprising the steps of:(a) providing a container;(b) providing a reservoir;(c) adding a distilled spirit to the container;(d) adding oxygen gas or an oxygen-inert gas mixture to the reservoir; and(e) connecting the reservoir to the container.

6. The method of claim 5, wherein the container comprises wood.

7. The method of claim 6, wherein the wood comprises oak.

8. The method of claim 5, wherein the container comprises a barrel.

9. The method of claim 5, wherein the container comprises a bottle.

10. The method of claim 5, wherein the container is enclosed by the oxygen supply reservoir.

11. The method of claim 5, wherein the container is attached to the oxygen supply reservoir through an opening in the container.

12. The method of claim 5, wherein the container is attached to the oxygen supply reservoir using a conduit, wherein the conduit is attached between the container and the oxygen supply reservoir.

13. The method of claim 12, wherein the conduit is a tube or a pipe.

14. The method of claim 12, wherein the conduit comprises an impermeable material.

15. The method of claim 10, wherein the container is placed inside the oxygen supply reservoir.

16. The method of claim 5, wherein at least one container is connected to the same oxygen supply reservoir.

17. The method of claim 5, wherein at least two containers are connected to the same oxygen supply reservoir.

18. The method of claim 5, wherein the oxygen supply reservoir holds an inert gas - oxygen mixture.

19. The method of claim 5, wherein the oxygen supply reservoir holds an inert gas - oxygen mixture comprising an oxygen content ranging from about 1% to about 100%, ranging from about 10% to about 100% oxygen, ranging from about 21% to about 100% oxygen, ranging from about 50% to about 100%, ranging from about 75% to about 100%.

20. The method of claim 5, wherein the oxygen supply reservoir holds substantially pure oxygen gas21. The assembly of claim 5, wherein the oxygen supply reservoir holds a volume ranging from about 0.1 L to about 10.0 L of oxygen - inert gas mixture for each 1 L of liquid.

22. The method of claim 5, wherein the oxygen supply reservoir maintains a pressure ranging from about 0.1 to about 100 atm, ranging from about 0.1 to about 10 atm, ranging from about 0.5 to about 2 atm, or of about 1 atm.

23. The assembly of claim 5, wherein the oxygen supply reservoir maintains a pressure of about 1 atm.

24. The method of claim 5, wherein the oxygen supply reservoir comprises a pressure ranging from about 0.1 to about 10 atm, ranging from about 0.5 to about 2 atm, or of about 1 atm.

25. The method of claim 5, wherein the oxygen supply reservoir comprises a pressure of about 1 atm.

26. The method of claim 5, wherein the container comprises a seal, wherein the container is sealed from the outside to prevent liquid, vapor or gas from permeating through the walls of the container.

27. The method of claim 26, wherein the container comprises a seal, wherein the container is sealed from the outside to prevent oxygen escaping from the container.

28. The method of claim 26, wherein the seal comprises a foil.

29. The method of claim 26, wherein the seal is substantially impermeable to alcohol, water or aroma compounds.

30. The method of claim 26, wherein the seal is applied to the outside of the barrel with a brush or sprayed.

31. The method of claim 26, wherein the seal is a natural or synthetic product.

32. A method for ageing a spirit comprising the step of:(a) attaching an air gate to a container, wherein the container holds the distilled spirit, wherein the air gate comprises a semi-permeable film, and wherein the semi-permeable film is permeable to oxygen and substantially impermeable to vapor.

33. The method of claim 32 wherein the container comprises wood.

34. The method of claim 33, wherein the wood comprises oak.

35. The method of claim 32, wherein the container comprises a barrel.

36. The method of claim 32, wherein the container comprises a bottle37. The method of claim 32, wherein the container comprises a seal, wherein the container is sealed from the outside to prevent liquid, vapor or gas from permeating through the walls of the container.

38. The method of claim 37, wherein the seal comprises a foil.

39. The method of claim 37, wherein the seal is substantially impermeable to alcohol, water or aroma compounds.

40. An assembly for ageing a spirit comprising:(a) a container holding the spirit; and(b) an oxygen supply reservoir.

41. The assembly of claim 40 wherein the container comprises wood.

42. The assembly of claim 41, wherein the wood comprises oak.

43. The assembly of claim 40, wherein the container comprises a barrel.

44. The assembly of claim 40, wherein the container comprises a bottle45. The assembly of claim 40, wherein the container is enclosed by the oxygen supply reservoir.

46. The assembly of claim 40, wherein the container is attached to the oxygen supply reservoir through an opening in the container.

47. The assembly of claim 40, further comprising a conduit attached between the container and the oxygen supply reservoir.

48. The assembly of claim 47, wherein the conduit is a tube or a pipe.

49. The assembly of claim 47, wherein the conduit comprises an impermeable material.

50. The assembly of claim 40, wherein the container is placed inside the oxygen supply reservoir.

51. The assembly of claim 40, wherein at least one container is connected to the same oxygen supply reservoir.

52. The assembly of claim 40, wherein at least two containers are connected to the same oxygen supply reservoir.

53. The assembly of claim 40, wherein the oxygen supply reservoir holds an inert gas - oxygen mixture.

54. The assembly of claim 40, wherein the oxygen supply reservoir holds an inert gas - oxygen mixture comprising an oxygen content ranging from about 1% to about 100%, ranging from about 10% to about 100% oxygen, ranging from about 21% to about 100% oxygen, ranging from about 50% to about 100%, ranging from about 75% to about 100%.

55. The assembly of claim 40, wherein the oxygen supply reservoir holds substantially pure oxygen gas56. The assembly of claim 40, wherein the oxygen supply reservoir holds a volume ranging from about 0.1 L to about 10.0 L of oxygen - inert gas mixture for each 1 L of liquid.

57. The assembly of claim 40, wherein the oxygen supply reservoir maintains a pressure ranging from about 0.1 to about 100 atm, ranging from about 0.1 to about 10 atm, ranging from about 0.5 to about 2 atm, or of about 1 atm.

58. The assembly of claim 40, wherein the oxygen supply reservoir maintains a pressure of about 1 atm.

59. The assembly of claim 40, wherein the oxygen supply reservoir comprises a pressure ranging from about 0.1 to about 10 atm, ranging from about 0.5 to about 2 atm, or of about 1 atm.

60. The assembly of claim 40, wherein the oxygen supply reservoir comprises a pressure of about 1 atm.

61. The assembly of claim 40, wherein the container comprises a seal, wherein the container is sealed from the outside to prevent liquid, vapor or gas from permeating through the walls of the container.

62. The assembly of claim 61, wherein the container comprises a seal, wherein the container is sealed from the outside to prevent oxygen escaping from the container.

63. The assembly of claim 61, wherein the seal comprises a foil.

64. The assembly of claim 61, wherein the seal is substantially impermeable to alcohol, water or aroma compounds.

65. The assembly of claim 61, wherein the seal is applied to the outside of the barrel with a brush or sprayed.

66. The assembly of claim 61, wherein the seal is a natural or synthetic product.

67. An assembly for ageing a spirit comprising:(a) a container holding the spirit; and(b) a film, wherein the film is permeable to oxygen.

68. The assembly of claim 67, wherein the film is substantially impermeable to vapor.

69. The assembly of claim 67, wherein the film is attached to the container in or over an opening of the container.

70. The assembly of claim 67, wherein the film substantially surrounds the exterior of the container.

71. The assembly of claim 67, wherein the film is attached to the container using a holder.

72. The assembly of claim 71, wherein the holder is attached to the container in or over an opening of the container.

73. The assembly of claim 71, wherein the holder is attached to the container by a conduit.

74. The assembly of claim 67, wherein the container comprises a barrel.

75. The assembly of claim 67, wherein the container comprises a bottle.

76. An assembly for ageing a spirit comprising:(a) a container holding the spirit; and(b) an air gate,wherein the air gate comprises a film and a holder; wherein the film is a semi-permeable film; wherein the holder supports the film; and wherein the holder is attached to an opening of the container.

77. The assembly of claim 76 wherein the container comprises wood.

78. The assembly of claim 77, wherein the wood comprises oak.

79. The assembly of claim 76, wherein the container comprises a barrel.

80. The assembly of claim 76, wherein the container comprises a bottle.

81. The assembly of claim 76, wherein the film is permeable to oxygen.

82. The assembly of claim 76, wherein the film is substantially impermeable to vapor.

83. The assembly of claim 76, wherein the film is further substantially impermeable to aroma compounds.

84. The assembly of claim 76, wherein the air gate is connected to a supply of oxygen.

85. The assembly of claim 76, wherein the air gate allows for the flow of oxygen from outside the container to inside the container.

86. The assembly of claim 76, wherein the air gate does not allow for the flow of ethanol vapor from inside the container to outside the container.

87. The assembly of claim 76, wherein the flow of oxygen permeates through an oxygen permeable film.

88. The assembly of claim 76, wherein the film is permeable to oxygen and substantially impermeable to ethanol.

89. The assembly of claim 76, wherein the holder of the gate is made of ethanol impermeable material.

90. The assembly of claim 76, wherein the film has an oxygen permeability coefficient of at least about 20 cm3mm / m2d atm.

91. The assembly of claim 76, wherein the film has an oxygen permeability coefficient of at least about 200 cm3mm / m2d atm.

92. The assembly of claim 76, wherein the film has an oxygen permeability coefficient of at least about 2000 cm3mm / m2d atm.

93. The assembly of claim 76, wherein the film has an oxygen permeability coefficient of at least about 20000 cm3mm / m2d atm.

94. The assembly of claim 76, wherein the film has an ethanol permeability coefficient of at most about 3 g mm / m2d.

95. The assembly of claim 76, wherein the film has an ethanol permeability of at most about 0.3 g mm / m2d.

96. The assembly of claim 76, wherein the film has an ethanol permeability of at most about 0.03 g mm / m2d.

97. The assembly of claim 76, wherein the film has an ethanol permeability of at most about 0.003 g mm / m2d.

98. The assembly of claim 76, wherein the film has a water permeability of at most about 3 g mm / m2d.

99. The assembly of claim 76, wherein the film has a water permeability of at most about 0.3 g mm / m2d.

100. The assembly of claim 76, wherein the film has a water permeability of at most about 0.03 g mm / m2d.

101. The assembly of claim 76, wherein the film has a water permeability of at most about 0.003 g mm / m2d.

102. An apparatus for ageing a spirit comprising:(a) a film;(b) a holder; wherein the film is a semi-permeable film; wherein the holder supports the film; and wherein the holder is attached to an opening of the container.

103. The assembly of claim 102, wherein the container comprises wood.

104. The assembly of claim 103, wherein the wood comprises oak.

105. The apparatus of claim 102, wherein the container comprises a barrel.

106. The assembly of claim 102, wherein the container comprises a bottle.

107. The apparatus of claim 102, wherein the film is permeable to oxygen.

108. The apparatus of claim 102, wherein the film is substantially impermeable to vapor.

109. The apparatus of claim 102, wherein the film is further substantially impermeable to aroma compounds.

110. The apparatus of claim 102, wherein the air gate is connected to a supply of oxygen.

111. The apparatus of claim 102, wherein the air gate allows for the flow of oxygen from outside the container to inside the container.

112. The apparatus of claim 102, wherein the air gate does not allow for the flow of ethanol vapor from inside the container to outside the container.

113. The apparatus of claim 102, wherein the flow of oxygen permeates through an oxygen permeable film.

114. The apparatus of claim 102, wherein the film is permeable to oxygen and substantially impermeable to ethanol.

115. The apparatus of claim 102, wherein the holder of the gate is made of ethanol impermeable material.

116. The apparatus of claim 102, wherein the film has an oxygen permeability coefficient of at least about 20 cm3mm / m2d atm.

117. The apparatus of claim 102, wherein the film has an oxygen permeability coefficient of at least about 200 cm3mm / m2d atm.

118. The apparatus of claim 102, wherein the film has an oxygen permeability coefficient of at least about 2000 cm3mm / m2d atm.

119. The apparatus of claim 102, wherein the film has an oxygen permeability coefficient of at least about 20000 cm3mm / m2d atm.

120. The apparatus of claim 102, wherein the film has an ethanol permeability coefficient of at most about 3 g mm / m2d.

121. The apparatus of claim 102, wherein the film has an ethanol permeability of at most about 0.3 g mm / m2d.

122. The apparatus of claim 102, wherein the film has an ethanol permeability of at most about 0.03 g mm / m2d.

123. The apparatus of claim 102, wherein the film has an ethanol permeability of at most about 0.003 g mm / m2d.

124. The apparatus of claim 102, wherein the film has a water permeability of at most about 3 g mm / m2d.

125. The apparatus of claim 102, wherein the film has a water permeability of at most about 0.3 g mm / m2d.

126. The apparatus of claim 102, wherein the film has a water permeability of at most about 0.03 g mm / m2d.

127. The apparatus of claim 102, wherein the film has a water permeability of at most about 0.003 g mm / m2d.

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