Aging Spirit

To round out or smooth the flavour of your liqueur or commercially flavoured drinks, it often pays to artifically age your drinks.

When aging your spirit, it is best done between 58-70% alcohol.

This can be done using : Hexenwolfe explains that glycerine is safe ...

Smoothing Agents

Using a non-sweet aging syrup can mellow out your spirit, without having to store it away for years. Just don't use too much to kill the character of whiskeys.

Try 20g/L of glucose, or 5 mL per litre of glycerine as a starter.

Other Tricks


Other little tricks to help round out/mature your whiskey include adding:
Manuka honey at 1 tablespoon per 1125 mL nicely rounds at the Drambuie type flavours.

Soak raisins and/or prunes in some 70% alcohol for a while, then add to brandy.

Try the "liquid smoke" sold by BBQ shops, to enhance that smokey/peaty flavour (just use it very sparingly !)
Hector advises ...
Maurice writes about some older techniques ... 
....here's something I read in a book called "The Manufacture of Spirit as Conducted in the Distilleries of the UK" by J.A.Nettleton, 1893......

On the maturation of whisky...The raw spirit is placed in a tall cylinder and a currant of air or oxygen under pressure of one or two atmospheres, is forced through the spirit. The operation extending intermittently for ten days. The raw spirit is alleged to acquire a mellowness of three to five years bonding. These process help to rid the whisky of off flavours and helps smooth the taste....

The new whisky is placed in a small vat and alternate currants of hot and cold air are passed through. Both during and after the aeration a little sherry or similar wine is added to the spirit, and so are minute quantities of sulphuric acid or pottasic hydric sulphate. The latter in view of intensifying the action of the wine. The whole of the mineral acid and of the salt is afterwards removed by the addition of a small quantity of powdered and slaked lime, and the whisky then removed from the small sediment which occurs.

Les concurs ...
Following comment by Maurice I discovered reference in Linchines book of world wines reference to the use of sherry to soften taste and add aroma.

Have been using good quality chestnut teal sherry (medium sweet) 75ml to a litre of spirit and the results have been good. The recipe was Country Squire 2000 and SU Mc Gregors concentrate plus a little corn syrup. Its worth a try, does well in blind tastings

Another simple trick is to use corks in your bottles, rather than screw-caps. This helps the spirits breath a little, and help its aging. Jack explains ...
it's been a proven fact (discovered by rum distillers) for years- carbonic acid gasses formed in the mash, then carried over in the distillate, are capable of staying in solution, and causing a noticable sharpness - a period of "breathing" (typically 30 days) can allow this gas to escape.

Caramel for Colour

Regarding using caramel for colour, Wal writes ...
Caramel, a nice name for burnt sugar, is legally added to brandy, scotch whisky, rum but by law not to American whiskey.

How much is used? A site for Georgian brandies gives sugar contents ranging from 0.7%, 1%, 7%, and 12% i.e. from 1 tsp (6 grams) to 20 tsp (120 g). I would be inclined to start with 1 tsp/litre and add extra to taste or color.

The French and English caramel is from the Spanish 'caramelo' which is derived from medieval Latin. The 'mel' part refers to honey (cane honey). Several sites on the subject:
In a cooking site with a recipe for Trinidad Black Cake (Christmas Cake) there is a local method for caramelizing sugar - which is most probably the method used (or was used) for local dark rum:

Caramelizing Sugar
  • 3/4 lb sugar (350 g)
  • 1/2 cup boiling water
Put sugar in a heavy pot. Stir, letting sugar liquefy. Cook over a low heat until dark, stirring constantly, so the sugar does not burn. When almost burnt, remove from heat and stir in hot water gradually. Mix well, let cool.

Lynne cautions ..
In the interests of preserving the flesh of anyone who tries this, I feel compelled to add a safety note: be very careful when you add the water, as it can cause splatter. Molten sugar on human flesh is not a good feel. The longer the stirring spoon handle, the better/safer.

Homemade Caramel For homedistillers a recipe for caramel is to use 2 cups of sugar and 1 cup of water. 
See: http://www.jacquespepin.net/members/recipes/basicbrownsauce.html

I have also successfully browned granular sugar in a frying pan to flavor a vodka which gave it a brandy-like character.

Blending

Jack writes ...
If consistancy (and reproducing your best batches) is becoming a problem- try a fractional blending system, like the Solara system used for sherry, and Jerez brandy in Spain.

The easiest "home method" is like this: set up three bottles of your favorite spirit. One to drink, one to blend, and one to age/store. When the "drinking" bottle gets half full, refill it from the "blend" bottle, which is then refilled from the "aging" bottle. Never let the "drinking" bottle get more than half empty before refilling it. This way, the batches will be linked in their flavor, allowing for consistancy. When the "storing" bottle is empty- you make another batch.

It will take roughly 4 refills of the "drink" bottle before the spirits' flavor profile is markedly different- since you are drinking it as it slowly changes, you won't notice, only someone who tries the batch at the begining, and then again, after the first bottle is emptied would notice a change. "House" spirits you are fond of always having on hand stay more consistant this way- it also works for wine and cider.

Jack offers the following suggestion ...
I've been doing some more reading on how commercial spirits are produced and I think I may have found something that Nixon/Stone still owners may find usefull. As you may already know, not too many large producers of spirits just distill, age, then bottle. Somewhere in between these stages is where blending takes place. For spirits like rum, instead of just distilling to a high proof then cutting it back with water to make a light style, many distilleries either make (or buy) a 95% "base blending spirit" that has no flavor, they then add certain amounts of a spirit distilled to a lower proof, say, 50-70% alcohol. If they add a lot of the low proof spirit they get a "dark rum", if you only add a little you get a "light rum".

If someone were to run a batch of sugar alcohol through a good reflux still, and get it up to 95% pure, they could set this aside (undiluted), and then using a pot still (or with the collection valve wide open on an NS still), they could run of a 10% mash of grain (for whiskey) or molasses (for rum), and only distill it to about 50%. Then by adding various amounts of 95% spirit you could get a dark, heavy rum/whiskey, or a light version of the same drink (how much water you add is up to you).

From what I have seen this would beat any "flavor essence" on the market, while providing a spirit that is cleaner, and less likely to give a hangover because any where from one-fourth to three-fourths of the final spirit was made from pure ethanol. It would also add yet another way to "tinker around" with the hobby distillers favorite drink-from what I've seen this would be a welcome added step to the production of spirits, because it allows for something that is unique- a "house style" for the hobbyist that can be changed easily.

Charcoal & Wood Flavouring

It is estimated that around 80% of the flavour of bourbon and whisky comes from the oak barrels used to store them in. We can replicate those flavours by soaking our spirits with oak chips or shavings. Start by using one teaspoon of oak per litre of alcohol, and let it soak for a week. Taste test frequently to find the level of flavour intensity that suits you - eg maybe a little more oak, or longer, or different % alcohol, or different levels of oak toasting.

Geoff writes ...
Maybe consider the size and shape of the barrels that are used to age the spirits you are trying to emulate. Calculate the ratio of the inner surface area to the volume of the barrel. Based on some whisky barrels I've seen, I add about 70 square centimetres of oak per litre of 55% spirit. Keep in mind that one "strip" of oak has two surfaces that interact with the spirit. I age spirits in 4 litre glass bottles and add thin strips (<1mm) of oak that I had wrapped in aluminum foil and lightly charred on the stovetop. So if my oak strips are 2 cm wide I cut a total length of 70 cm, but I usually break such a strip into a few pieces before charring and adding them to the jug. Gives nice colours and flavours and generally a smoother drink.

For an excellent article on the composition of Oak, and its affect on maturation, download oak.pdf (690kB) which was from the Cooperage website http://www.worldcooperage.com.

Donald advises ...
Oaking - Several different flavors can come from a single type of oak if alcohol strength is adjusted during maturation. 55%-53% will give vanillins, 40%-50% will give a mix of vanillins and sugars, 40%-49% will give sugars.

What I like to do is start at 55%-53% for first phase (1 to 12 months) then dilute to 40% (3- 12 months). In this manner I am adding sugar from the cells of the wood while I marry the dilution water to the whiskey. This results in rich vanilla oak charater with silky legs that cling to the side of the glass. The procedure works well with all types (chips or BBL) and varieties of Oak.

If you can't buy the commercial toasted/natural oak chips for flavouring and aging, you can try making your own. Make sure you use oak or non-resinous wood - using a soft resinous pine will only give you a retsina. Be ingenious when looking for old oak - locals here use bits of old furnature etc (after shaving off the varnishes etc). Smoked manuka timber is particularly good.

To make your own toasted timber, find a tin with a push on lid of 1-2L. Split your timber into thin enough strips to fit your bottles. Light the pieces, and when well charred, place in the tin. Place the lid on lightly to snuff out the flames. Add more wood as it becomes ready, replacing the lid each time. When cooled, push the lid on tightly to retain the smokey aroma until ready to use.

Another way is to wrap the oak chips/shavings in aluminium foil, and bake them in your oven for a while.

The temperature of the toasting will affect the flavour that develops...


Diagram from http://www.worldcooperage.com

Hexenwolfe writes ..
Jack advises :
Charcoal that can be used to smooth the flavor of bourbons and rums may be made at home like this: use either hickory, oak, or sugar maple wood (buying it from a lumber supplier is easy enough) as these are proven to be nontoxic.

Split the wood into finger- width sticks about 4 to 6 inches long, then pack them into an old coffee can that has no more of that coffee smell or any rust. Pack them in standing upright so there isn't much space between them. Once the can has a solid layer of these sticks crammed in together like sardines standing upright, cover the top of the can with a layer of heavy tinfoil that has a pencil sized hole in the middle of it. Place this arrangement on your propane burner (this is not to be done inside!!), and set the heat on high. After a bit of heating up, some steam, then other various flammable organic gases will evolve off (if the foil swells up, make the hole a bit larger- try not to burn yourself). Once there is no more gas/steam coming out, turn off the heat and let the can sit outside to cool on it's own with a cover to exclude any air from getting in. Once cool, rinse any ash off in some cold water and use however you wish. Do not poke any holes in the coffee can - that will allow air into the mix and turn all of the wood into ashes, instead of turning it into charcoal.

Using a pressure cooker to inject steam could also be attempted to try an make activated carbon, but I haven't tried it.

Jack also writes :
I see people trying to duplicate Jack Daniel's Tennessee Whiskey (It is NOT a bourbon - the charcoal filtering procedure was legally recognized as producing a separate type of whiskey after World War II) on some of the e-groups; the essential step is to filter the unaged spirit through charcoal (not activated carbon) that has been made out of sugar maple wood (see How to Make Charcoal at Home by Dan Gill).

The residual sugars in the charcoal give a slight sweetness to the finished spirit, and the limited absorbing ability of the charcoal only makes the stuff smoother, but doesn't strip all the flavor out. I have tasted homemade whiskey and rum made and filtered in this method, even at "barrel strength" (75%) they were very smooth - no ice was even needed.

For a "Wild Turkey" style flavour, Wal advises ...
No recipe, but here are some quotes that might give a lead:
1) Aging technique. "Wild Turkey is distilled and put into new barrels at a much lower proof than most Bourbons - a costly method that results in less of the flavor being cooked out. The barrels are made of the finest new oak with the heaviest char available, imparting a smoother flavor and a deep amber color."
2) Taste. "best flavors of our premium bourbon, but with real honey to give it sweetness...." "real honey" "obvious notes of vanilla and citrus" (this could come from the heavily charred American oak barrels). "Wild Turkey Liqueur is a sweetened cordial with honey" - 30%abv.
3) Wild Turkey Liqueur was introduced in 1976 - htp://www.wildturkeybourbon.com/nest/history.pdf (possibly it was introduced to compete with honey based Scottish whisky liqueurs).

It appears to me that a starting point would be to age your raw whiskey distillate in heavily charred American oak chips, and then add a pure honey to say 25% sweetness (start with a 250 ml cup/l). Some orange peel might have been added to imitate Southern Comfort(?) The vanilla would probably come from the American oak which has that characteristic.

The "Household Cyclopedia" recommends ...
The flavor of malt spirits is highly improved by putting 3 1/2 oz. (100 g) of finely-powdered charcoal, and 4 1/2 oz. (125 g) of ground rice into a quart (1 L) of spirits, and letting it stand during 15 days, frequently stirring it; then let the liquor be strained, and it will be found of nearly the same flavor as brandy.

You can also use virgin wood shavings - the greater surface area will work faster. Taste regularly to ensure that it doesn't get too wooded, then filter out when ready.

Wood-essence can be made by soaking the shavings or toasted wood in 70% alcohol for a couple of weeks, then strain them off. Another suggestion is to pressure-cook the shavings with neutral spirit for 10 minutes at medium pressure, but this sounds risky!).

Brian writes ...
Oak chips in Australian home brew shops anyway are usually Quercus Alba (American White Oak) and are applied as per the label. I prefer to use a natural essence as not only is it more accurate, but is actually "less harsh". To make this infusion yourself, take equal proportions (by volume) of chips and neutral spirit at about 70% and soak for approximately one month, agitating as often as possible or percolate using a pump, then separate the two and apply solution (tincture) at a rate of about 10/15 ml per litre, or to taste of spirit at 40%. Or if you want to be really upmarket, take the tincture and simmer it very slowly until the volume is 75% less than original and you should have a fairly concentrated essence. In processing, remember it's frightfully volatile!!!

Jeanette suggests to use the toasted oak by ...
I am writing to tell you of my way of aging bourbon ( or whisky for that matter ) We are doing this one bottle at a time.
  1. Line up bottles to be used, add your undiluted spirit, and put in appropriate amount of flavouring. Personally, if it says 10ml per litre, I add 15ml.
  2. In a stainless steel saucepan, put in amount of water needed to top up one bottle only. Add one tablespoon of toasted oak chips.
  3. Bring to boil, then immediatly turn heat down and simmer. We don't want to boil off all the aromatics of the oak. At this stage add a large teaspoon of glucose and stir in well.
  4. Simmer for about 5 minutes, bring to boil again, then take off heat and let cool. The mixture should be a lovely brown colour.
  5. Strain and add cooled mixture to your bottle of spirit and it is ready to drink. Or don't strain, and keep the flavour coming for an even smoother, flavourful drop in the future.
Compare the aroma of your liquor to the conventional, and long way of aging.

From Cheryl (Victoria, Canada)...(posted on Distillers newsgroup)
The way I make my whiskey is a cup of virgin (untoasted, french oak) oak to 1 gallon of vodka, and it sits for a month and gets filtered and is ready to drink. I have made a scotch tasting whiskey using the same method, only with toasted oak.
to which Ray Toms added ..
I find that you can overdo the toasted oak but not the plain oak. I restrict my toasted oak to one teaspoon for short term oak aging and double it to two teaspoons for long term (in excess of 12 months) aging whereas I use 3 teaspoons of plain oak for short term aging and 6 teaspoons for long term aging. Excessive use of toasted oak can leave a burnt flavour in the whisky.

See below about using casks

Where to source the wood chips ? Donald suggests ...
Whiskey barrel chips can be obtained by routing the inside a used whiskey barrel. Good results also come from wine barrels (sherry & port if possible). There used to be companies (20 years ago) that would convert whiskey barrels to wine barrels by shaving the charred wood layers out to toasted wood. They would just give the chips away. FYI - red oak has good flavor too, it just needs to be used in chip forms because red oak barrels leak.

Wal writes ...
its worthwhile to extract notes from University of Nevada, Tourism course 'FAB 362 Distilled Spirits and Liqueurs': (of which I have a local copy : http://homedistiller.org/detail/362Index.htm because their link is no longer working)

The changes in the spirit during wood aging are caused by 3 types of reactions occuring simultaneously and continuously in the barrel.
1)complex wood constituents are extracted by the liquid
2)there is oxidation of components originally present in the liquid as well as of material extracted from the wood
3)there are reactions between various organic substances present in the liquid, leading to the formation of more and new congeners

As with wine, the type of wood is very important and most of the major spirits have strict requirements. Bourbon whiskey regulations require that the barrels be new, and that the insides be charred. This is done by setting the inside of the barrel on fire until a layer of char is developed. Most other whiskies and other spirits do not have to be aged in new, unused wood, nor do the barrels have to be charred. Charring improves and softens the taste of the spirit and provides both body and color.

The manufacturer will decide what specific type of spirit to make and there is a close relationship between distilling and aging strategies.
Anything distilled over 95%abv is legally termed "neutral" spirits.
Bourbon cannot be distilled over 80%abv
Cognac cannot be distilled over 72%abv
Rum is distilled at 85-96%abv
Scotch malt whiskey is distilled at 70-71%abv
Canadian whisky is distilled at 70-90%abv

The congeners, those secondary products produced during alcoholic fermentation, consist of acids, esters, aldehydes, fusel oils, extracts of mineral salts and solids in minute quantities. Collectively, they do not amount to much from a percentage standpoint, but they are determining factors as regards product character.

Esters are volatile substances which give aroma to the spirits Aldehydes are produced from alcohol/air reactions and contribute to the character of the spirit.
Fusel oils are higher alcohols and form complex mixtures. Not all these compounds are desirable, and even those which are, should be present in specific amounts.

Cognac/Brandy
The use of copper stills is important because the contact between copper and liquid traps fatty acids and sulphur elements. Cognac regulations permit French oak only. The barrels are not charred. Freshly distilled cognac is placed in new barrels perhaps for 16-18 months. Barrels are considered new the first 3 times they are used. The first of the 3 will be for only a few months since the wood will impart excessive tannin to the spirit. The second use may be for up to 2 years and the third even longer. The barrels are kept filled unlike bourbon and malt scotch whisky. Blending is a key factor. Both caramel and sugar syrup are legal and regulated additives. An unregulated practice is the use of oak chips soaked in old cognac and left in cask for months or years. The purists regard that the character from this is rather hard and tannic.

Bourbon whiskey
Charred barrel aging is said to impart the characteristic vanilla and caramel flavor of Bourbon. There are 4 grades of char and each distiller has their preference. Charring produces a layer of partially caramelised sugars below the char. Charring imparts color to the spirit and whiskey stored in new, charred white oak develops the distinctive red-amber color. Additives are not permitted. The used barrels are sold to distilleries in Ireland and Scotland.

Scotch malt whisky and Irish whiskey
Most malt whisky is matured in Bourbon barrels, only 4% is in sherry barrels. One difference between American oak and Spanish oak is that the American species is harder and consequently matures whisky more slowly. Spanish oak contains more resin which effects the flavor. Sherry and bourbon leach out the stronger tannins and oak extracts, creating a lighter product.

Rum
Maturing is done is used in previously used barrels which may or may not have been charred. Puerto Rican law requires a minimum of 1 year in wood. Fuller and more distinctive rums result from increased wood aging of a minimum of 3 years. Caramel is used to adjust the color. The typical dark color of Jamaican rums is due to the caramel added. The coloring is produced by heating sugar solutuins to about 82C (180F) to evaporate the water and caramelize the sugars.

Wal then asks ...
Could the homedistiller make a convenient oak essence? In France flavoring/maturation shortcuts are practiced that homedistillers can copy. In France, four additives are allowed for cognac and armagnac. See: http://home.tiscali.no/boruud/the1.htm
  1. Water
    To cut excessive alcohol. But vintage cognacs/armagnacs achieve their 40%abv by slow evaporation (3% a year), so dilution has an effect on flavor and for traditionalists reduction is a bad word. For homedistillers a lower %abv distillation will contain more flavor compounds.
  2. Boise (e is accented)
    A boise essence is made by boiling chips in water and then removing the chips and slowly reducing the remaining liquid. What one is left with is a dark brown liquid that is replete with wood flavor and tannin. Another source mentions infusing shavings in cognac. Charred French oak chips are also available which act like charred white Ameican oak chips - more caramelised sugars and vanillin i.e. softer flavors.
  3. Sugar Syrup
    Used to add sweetness. Normally added if a cognac/armagnac is too tannic, or to remove any rough edges. It is viscous, and can either be dark or light. Legally 2% can be sugar syrup. 1 tsp/1 litre(quart) is a good starting point.
  4. Caramel
    A liquid from burnt sugar. It is dark in color and slightly bitter in taste. It is used to adjust color and establish consistency or give the spirit the impression of being older and therefore smoother.
Ideas for discussion:

American whiskey can gets flavors only from the charring of American white oak staves. American white oak contains less tannins and more vanillin than French oak. Filtering through maple charcoal is also practiced, and this has an effect on flavor due to caramelised sugars in the maple charcoal. A Bourbon essence could possibly be made by soaking charred American oak chips in Bourbon.

Rum is aged generally in used Bourbon barrels. Reusing the chips from making a Bourbon essence and soaking in aged rum (in effect diluting the wood character) would emulate a used Bourbon barrel.

Scotch and Irish whiskies are aged by reusing Bourbon or Spanish sherry barrels. Irish whisky is usually triple distilled (90%abv) as opposed to the double distilled peated malt Scotch whisky. So the amount of distilled congeners is different in the two styles. An essence could be made by soaking in aged whisky for a second time, American oak chips that were soaked previously in Bourbon, or European oak chips previously soaked in Spanish dry oloroso sherry.

The use of sugar and caramel is practiced in all the above liquors except Bourbon and Tennessee whiskies, and a starting quantity to achieve smoothness would be 1 tsp/litre. The amount of caramel (burnt sugar) used would depend on the style required.

Casks

Some wine-making shops sell little oak casks. These really do work well. Leave your finished liqueur in these for a while, and they mellow out even more.

See http://www.ibrew.com.au for a selection of the small casks available in Australia.

If you leave the bung-hole of the cask (once filled) open for several days, it is said to improve the flavour. Donald disputes this ...
... that taking the bung out of a barrel might help the whiskey age with a quicker maturation. It will not! This will only cause the alcohol to evaporate will not add improvement to the whiskey. This does bring up an important point of evaporation and the "angels share" the part of the alcohol that evaporated though the wood and is therefore "lost to the angels".

The truth is, we don't need any drunken angels! More to the point, the process of evaporation is distinct from the process of oxidation. Although they are often confused and used interchangeably. The whiskey flavour can be achieved with out any evaporation at all, because the flavour component comes from oxidation process alone. The alcohol solubilizes the lignins of the oak which then oxidize into vanillins. Usuing oak chips with an air tight container (stainless steel or glass) with a 1/3 to 1/4 air space at the top, so 100% evaporation is recaptured with 100% oxidation. This also eliminates the risk of a sour barrel, just like a screw cap prevents rotten cork spoilage (3%-4% average).

To price out full sized barrels for yourself, see

Kristofer D offers the following advice :

I have decided the best way to age alcohol is in a charred barrel. Sometimes prechared barrels can be found, but they are hard to find. I have charred my own barrels that were bought at homebrew stores. I also add about a cup or two of charcoal that has been made from hard wood. A five gallon barrel works best. Any smaller is too small, and any larger takes to long to age. When ageing in a barrel about a quart of alcohol is lost every month. To make up for this you must add to the barrel once a month. I stop the process when half of the original amount has evaporated. In a five gallon barrel that takes about eight months. After this period the alcohol should of mellowed greatly and also become a golden brown color from the charcoal. I have found the best why to char a barrel is by putting a small layer of hot coals in the barrel, and then using an air compressor to blow oxygen into the barrel. By rolling the barrel slowly a complete charing is possible. It takes about an hour. You should feel the hoops on the barrel get hot. Usually hot enough to boil a drop of water. If time is taken to age alcohol in this manner I guarantee it will be the best ever. I have done this with apples, peaches, choke cheeres, and malted barley all grain. Each one came out superb, and the charicteristics of the fruit wasn't even lost.

Mike P writes :
... Then I bought an oak keg and tried aging the stuff, well after six months it just wasn't ready and I was getting err... impatient. So I surmised that the surface area of the keg was too low compared to the amount of contents to produce much of a surface contact for the liquor. I added lots of charred oak chips!! Bout 4 qts to my little 4 gallon keg! My mom was beginning to wonder when she came home one night and I had the oven mitts on and was peering into the oven at a cookie sheet full of smoking oak chips!! However the increased surface area did just the trick! The now golden liquor was a great tasting and visually appealing product.

An old codger from down the road told me if I added a few (6-10) black peppercorns to my aging process I would get a new appreciation! I did and it worked very well, there was no taste whatso ever from the peppercorns but you got that warm feeling inside right away after drinking it! It was a nice touch. I have used it often since then with very pleasing results, careful though and don't fall into the same trap I did, if 10 was good, then 20 must be better and a 100 would be better yet!!! Ohhhhhh... the heartburn!!! :-)

How do casks work to mature the spirit ? Its a matter of the wood letting in a little oxygen, and letting out different proportions of the alcohols and cogeners present, as well as reacting with some of the ligins & other substance of the wood. An email from Jim Busch, to the HBD, offers:
As for the issue of casks and diffusion of ethanol/fusels:

In whiskey maturation one of the key reactions involves diffusion of products from within the cask, through the cask wall. Basically its called a subtractive reaction in this case. The key parameters that pass through the cask are water and ethanol. The lower the molecular weight of the compound the easier it is to evaporate through the cask. This means that it is much easier to reduce the concentration of ethanol in a cask than it is to reduce fusel alcohols, as the latter are longer carbon chained alcohols. This route is also the main factor in DMS reduction in whiskeys. Hasuo and Yoshizawa, '86, found that the rate of evaporation of a model whiskey ranged from 32% of the total present in the spirit for acetylaldehyde to 5% for isoamyl alcohols to 1% for ethyl hexanoate and acetic acid. So the permeability per compound is quite different. The texts seem to indicate that in whiskey maturation there is a net concentration of fusel alcohols and esters of fatty acids. Similar results apply to cognac production where Ive seen a reference that indicates a typical loss of 3% per year in both water and ethanol and a concentration of fusel alcohols.

The chemistry of spirit maturation in casks is quite involved and interesting. The key reactions are extractions from the cask, chemical reactions and oxidative reactions inside the vessal (which continue as the flavanols, tannins, hemicelloses and lignins leach) and concentration reactions.

Arthur Bell, at http://claymore.wisemagic.com (dead link ?) says ..
Over the decades OAK wood has proven itself supreme for ageing potable liquors, became it is semi permeable and allows the diffusion of alcohol and water through the thickness of the barrel STAVE promoting minimal evaporation on the wood surface to the extent of 2% per annum in Scotland. This is the slow process of maturation so essential to product quality. By tradition Scotch whisky is not matured in a NEW cask as with Brandies (Cognac and Spanish) and Bourbon, which historically have benefited from the new oak extracts. The associated CARAMEL bitterness of the new oak due to excess TANNINS, LIGNIS, PHENOLS and RESINS are rarely present and are not appreciated by the connoisseur of aged malt whisky.

Within the Scotch whisky COOPERAGE two distinctive types of white oak are employed to fashion barrens from America or from Spain. The AMERICAN oak (Quercus ALBA) contains less than half of the total wood extract found in the EUROPEAN oak (Quercus ROBUR). The Bourbon Whiskey industry uses solely American oak suitably charred to promote the carmelisation of the wood sugars, so essential to bourbon character. This pre-treatment of the American barrels with fire and spirit has become acceptable to the Scotch distiller. The alternative and much sought after source of pre used cask is JEREZ Spain which offers both American and European oak casks having previously contained SHERRY wines.

It will be appreciated, as with all things in life, the expected enhancement of spirit quality within the cask does not always materialize and those SULLIED barrels are discarded, no matter how slight the imperfection. A similarity exist between CORKS in wine or whisky and wood for casks, that the SOURISH MUSTY - DANK flavours of bad wood spoils the barrel content.

Charlie Maclean, writing "The Language of Whisky Tasting" at the Scotch Malt Whisky Society offers ..
...we were delighted to be able to help Colin Brown, a Manufacturing Scientist undertaking an Investigation by Analytical Chemistry of Compounds Affecting Flavour in Single Malt Whiskies, for Napier University, Edinburgh, with the support of United Distillers.

He writes: "Single malt whiskies are chemically complex and are known to contain several hundreds of individual components (congeners) including a variety of alcohols, aldehydes, acids, esters and phenols, as well as carbonyl-, sulphur- and nitrogen-containing compounds. Many of these contribute to the flavour of a whisky and the relative concentrations of each are dependent upon variations in raw materials and production methods. Consequently, each single malt whisky is discernable from any other, including those produced at a neighbouring distillery."

The investigation, which is continuing, began by identifying the relative concentrations of compounds known to be extracted from the cask during maturation ('cask-extractive congeners') and a group of those which arise from the raw materials and during production ('volatile phenolic congeners'). It went on to make a correlation between these and the perceived flavour of the finished product.

Four samples of whisky were considered, affording a regional spread. They were: Caol Ila (Islay), Scapa (Orkney), Rosebank (Lowland) and Balvenie (Speyside). "Cask-extractive congeners are of great importance to the overall flavour as well as the aroma and colour of the finished beverage.

Whisky casks are traditionally treated to thermally degrade the internal surface of the cask, by firing and charring, for three major reasons:
  • to generate a layer of active carbon which removes undesirable flavour substances;
  • to effect the release and dissolution of flavour compounds such as vanillin during maturation;
  • to yeild colour and phenolic substances which result in new flavour compounds by oxidative interactive reactions.
The results revealed that all four samples contained similar levels of the compound furfural, which is associated with a general 'whisky flavour'. The unmistakably woody flavour in the Scapa sample is attributable to syringealdehyde, which is also present in Caol Ila, although the dominating flavours of the Islay whisky are discussed later. The Balvenie chromatogram reveals a high level of ellagic acid, a compound known for its pungent odour and flavour. The number and relatively large abundance of lignin degradation products in the Caol Ila sample would suggest that a heavily charred oak cask was used for the maturation process. The presence of 5-hydroxymethyl furfural in Caol Ila would allow the taster to expect a slightly reddish tint to the whisky.

"Volatile phenolic congeners' primary source is from the peated malt used in whisky production. So it was not surprising to discover that the Caol Ila sample had a large number present and in concentrations greatly in excess of the other whiskies under investigation. "The presence of phenol at 2.1 parts per million (ppm), was almost five times that for Rosebank, 20 times that for Balvenie and 200 times greater than that found in Scapa. Phenol has a medicinal taste and therefore would be expected to be present in an Islay whisky. Guaiacol, known for its smoky and phenolic flavour, was detected in concentrations of 1.2 ppm in Caol Ila, but was barely detectable in the others. Further investigation showed that the levels of compounds responsible for 'tarry' and 'disinfectant' flavours (m-, p- and o-cresol) were evident in the Islay sample but rela tively low in Rosebank, very low in Balvenie and not detectable in Scapa. However, similar concentrations of the compound eugenol (perceived as having a flavour not dissimilar to that of cloves) were determined in both Scapa and Caol Ila. All of the whiskies investigated contained varying concentrations of 4-ethyl phenol and 2,5-xylenol, which co-eluted and could not be determined separately. Both of these substances have a powerful 'whisky' flavour."

Mr Brown concludes: "Many other compounds were determined analytically during this investigation, however their individual impact on flavour is considered less important than their contribution to the overall flavour of each whisky. These analyses are intended to give an insight into the complex chemistry of single malt whiskies and the impact which each of the many hundreds of compounds has on the characteristics of the finished product."

Charlie Maclean

Another article, "Whisky Dectectives" at the Scotch Malt Whisky Society describes how different techniques for drying the wood affects how well the spirits mature.

Yue Hung has forwarded some information from an article "The Production and Aging Of Wine in Small Oak Cooperage" published in the May 1969 edition of "Wine & Vines¨ ...
Mechanism of Aging

The mechanisms and processes which occur during the aging of wine in the barrel can be grouped roughly into three closely inter-related categories. viz. physical, physico-chemical, and biochemical.

Physical. The most important physical aspect of cooperage in the aging of wine is its size, because the surface-to-volume ratio affects the rapidity with which certain processes take place and the degree to which they influence the character of the wine. Since all of the aging mechanisms are influenced to a different degree by variations in barrel size, it follows that there must be one single optimum size, one ideal surface-to- volume ratio which establishes the best balance of the wine and which most perfectly favors and develops the character of the wine during aging. We are, fortunately, the beneficiaries of centuries of experience in this area, and we can state with some certainty that, in the great wine regions of France, at least, the barrel size of 225 to 230 liters (about 60 U.S. gallons or 50 Imperial gallons) has proven to be the most perfect. We have little reson to double that this size, or a size reasonably close to it, will produce the same good results in other areas. Indeed many of the best wines of California and Australia (to give two examples ) have been produced and/or aged in this size cooperage. Similarly, the optimum barrel size for Cognacs and fine brandies has been established to be 300 liters (about U.S.gallons or 66 Imperial gallons) It should be emphasized that half-quarter-eighth- etc.. size barrel are made for the purpose of storing odd amounts of wine or for breaking down a full barrel when topping.(Not that wine cant be successfully aged in these small sizes, its simply that the results are not quite so satisfactory, and that much greater care must be taken, through more frequent organoleptic examination, to avoid an imbalance in the finished product)

The most obvious physical process which occurs during aging is the slow imbibition some of the liquid by the wood and the subsequent evaporation into the surrounding atmosphere .There are five prince influences in this process : relative humidity, temperature, air movements in the area where the barrels are kept, the physical characteristics of the wood, and finally, the frequency of topping. This last is important because, where the topping is less frequent there is more opportunity for an area of wood to become dry and thus slightly more porous due to shrinkage of the wood tissue The important of the first three items first emphasized by Pasteur,has been forcefully demonstrated by Riberean-gayon(3) whose experiments with 60 gallon oak barrels gave the following results: in good oak barrels which are cold and humid, the evaporation lose can be kept to 1 or 2 per cent; in ordinary wineryies it is 4 or 5 percent;and in poorly designed wineries which are too warm,too dry,and/ or too much expose to air currents, the loss can be as high as 9 per cent. The evaporation loss is also greatly influence by the type and thickness of the wood..

Ian Wisniewski (whisky and spirits writer, and author of Classic Malt Whisky (Prion Books)) wrote about Oak at Whisky World (big thanks to Whisky World for letting me copy these extracts !)

Jack Daniels Whisky

See Jacks instructions on the Preparing Grain Mashes page for the grain bill, and his comments in Aging re passing it through maple charcoal.

Johnnie Walker Whisky

Les suggests ...
My best results came from Top Shelf Classic Reserve Scotch Whisky.. Top Shelf Classic Whisky(green label) and Country Squire Whisky 2000. The Classic Reserve is excellent but requires ageing and is somewhat cloudy to begin with.Try not to consume before six months.I also tart it up with some other ingredients. For ease of use, economy and consistent results the TopShelf Greenlabel Classic is a winner. My formula for this essence is as follows......
  • 1 sachet 40gms Classic Greenlabel Whisky.
  • 2.5 litres 44% alcohol .
  • 100 mls Glycerine
  • 2 teaspoons Eazimix spirit finisher
  • 6 teaspoons Virgin American Oak shavings
  • 150 mls medium dry sherry (good quality)
Leave in 3 litre glass for at least 4 months then fiter off. To test place 1 nip in a wine glass and the same amount of Red Label Johnnie W. in another and compare.I think you will be surprised at how well your product holds up. You can vary the ingredients to your taste. Regards Les

Bourbon

Bill recommends the following for a Bourbon made from essences ... Brian adds ..
don't forget most of that classic bourbon taste is vanillin, so you may need to add some quercus alba [american white oak], liquid oak or some toasted quercus alba chips to truly get that wood/vanillin effect

Mecakyrios writes ...
Sometimes I like to throw in a handful of oak chips in about 2 weeks before I distill. I then transfer the wash and the chips into the still and go to town. I have found that the oak absorbs (or at least makes me believe) some of the fusels that we try to cut. The chips also quickens the distillation times. The oak also adds some interesting flavor when using it this way.

Smudge describes his technique ...
I recently went right back to my roots and purchased a Spirits Unlimited 5 litre Simple Still. This time it's not for distilling washes, but for making flavourings.

The process is fairly simple – get whatever you want as flavouring, soak it in alcohol, and distil it.
For the sake of consistency, I use 500mls of base material (corn, rye, barley etc) and 2.5 litres of 40% alcohol. It sits for a week, and then I add water to make 4.5 litres and distil it.
OK, for the purists out there, I admit it's not the real thing, but its getting close. And it's better than anything I have ever tasted that wasn't from a bottle shop.
I did some research on bourbon to work out where its characteristic flavours come from:
It is primarily made from corn, but rye is used to give it body. Much of the flavour, however, is obtained from the barrel. Unlike whisky, bourbon is aged in virgin oak. Bourbon barrels are charred with an intense flame, which caramelises the sap producing the characteristic vanilla/caramel flavour.
I set about combining corn, rye, oak, vanilla, caramel and smoke. Here's what I came up with:
I distilled separate batches of corn and rye as detailed above and watered each back to 40%.
I have some 60% alcohol that has been in a 15litre barrel with 2kg of toasted oak staves. It is black as night and has the warm smell of dark rum. I distilled some of it (1.6litres at 60% watered back to 4.5litres volume) to produce a clear liquid with an oak flavour.
I distilled 50ml of liquid smoke (purchased from the supermarket) in the same alcohol/water proportion as above.
I added 50ml of concentrated vanilla extract (the expensive stuff) with 40% alcohol to make a total volume of 500mls.
I caramelised 1 cup of sugar (on the stove) to a rich red/brown colour and diluted it back with 60% alcohol to a volume of 500mls.
I diluted a bottle of Spirits Unlimited Bourbon to 500mls with 40% alcohol. Don't substitute the Premium Bourbon, as it doesn't have the same perfume taste.
I combined the ingredients in the following ratio:
Corn 600 mls
Rye 300 mls
Oak 150 mls
Caramel 80 mls
Vanilla 60 mls
Smoke 30 mls
S/U Bourbon 30 mls

The result is quite pale, but it lets you barrel age it without it getting to dark. It can also be darkened with some concentrated (un- distilled) oaked alcohol.
It involves some effort but the cost of the flavouring is low at about AUD$1 per litre of spirits.

Rum

Ed of http://www.MinistryOfRum.com writes ..
I am familiar with a commercial distiller that pumps clean air into the fermenting molasses wash to strip some of the H2S formed during fermentation. After distillation, more clean air is bubbled through the raw spirit to aerate it more..... This would apply more to fermenting molasses which has a higher sulfur content than the sugar most people are fermenting. A small aquarium pump would do the job on for a small distiller.

Sherry is commonly used as an additive in the rum industry although most distillers won't admit it. For best results, blend the sherry and then dilute the spirit to drinking strength before aging.

In the US, only new barrels are used for aging whisky and they can only be used once. A lot of these once-used barrels end up in the Caribbean at the rum distilleries, aging rum. The rest end up at hardware stores and are sold as planters.

A lecture on "Processing of Jamaican sugar cane" by Robert Lancashire yields ..
How do you get rum from sugar cane?

The Jamaican Excise Duty Law, No 73 of 1941 defined rum as "spirits distilled solely from sugar cane juice, sugar cane molasses, or the refuse of the sugar cane, at a strength not exceeding 150% proof spirit".

Rum is produced from sugar cane by fermentation by yeast. The resultant "wash" has approximately 6% alcohol which after distillation produces rum as a clear, colourless liquid with about 80% alcohol and a sharp taste. White rum is essentially this product diluted to 40% alcohol. Gold rum requires aging in small (40 gallon) oak barrels. The process of aging is very complex, involving evaporation of some of the pungent volatile components, reaction of the rum with the oak wood and perhaps even the absorption of oxygen through the barrel to convert some of the alcohol to aromatic esters.

The total level of flavour components rarely exceeds 1% of the total weight (and is normally much lower) in a base of ethanol. This high concentration of ethanol presents particular problems in both sensory and analytical studies. Furthermore, the advent of gas chromatography has shown that most of the components found in potable spirits are the same and that the nuances of flavour are essentially attributable to small differences in the relative proportions of these components.

Note however that expert tasters have been known to name the district and frequently the actual estate from which the rum originated, just by the sense of taste and flavour.

In Jamaica, gold rum is generally bottled at proof strength (Imperial) which is 57 Volume % alcohol. (By comparison, 100 US proof is 50 Volume % alcohol).

Chemical composition of Rum and comparison to American Bourbon Whiskey

The following figures were found for a light-bodied rum that had been aged in charred oak barrels (previously used for aging bourbon).

Composition of Rum and American Bourbon Whiskey
  Jamaican Rum American Bourbon
Age (years) 0 3 0 3
Constituents Concentration g/100L Concentration g/100L
% alcohol 80.1 78.2 77.5 75.5
total solids (extract) 0 87.6 0 136
fixed acids 0.9 8.8 0 12
volatile acids 1.1 20.9 3.2 50
Total acids 2.0 (pH=4.9) 29.7 (pH=4.5) (3.2) (62)
esters (for years, erroneously called ethers) 9.7 37.5 9.6 42.0
aldehydes 1.9 4.7 0.6 5.6
fusel oils (higher alcohols) 48 66 250 298
furfural n/d 1.6 0.12 1.42
tannins n/d 33.0 0 62

n/d= not detected


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