Coopering 2 PDF

● BIOCHEMISTRY
Way through the wood

Barrel biochemistry for brewers and distillers
By Ian Hornsey generally being used for ageing being

towards the mid-range (18 gallons;
kilderkin and 36 gallons; barrel).
“Wooden barrels have been arguably the most significant Casks/barrels are characterised by
shipping container in history. They served Romans, being tapered at each end and consist
of curved wooden slats (staves) along
explorers, pilgrims, pirates, pioneers and samurai their long axis; ‘a bulbous cylinder
through 2,000 years of civilisation.” Diana Twede, with flat ends’. In this respect they
have some structural relationship to
packaging professor and author, 2005. the wooden bucket, except that these
have a closure at one end only, and the
U ntil the advent of plastic, wooden

containers, commonly referred to
as ‘barrels’ in the US and called ‘casks’
solid foodstuffs, they were the result of
the skill of coopers who were masters
of woodworking and metalworking.
component staves are not curved.
The ability to curve wooden slats
would have been learned from early
in the UK (because there the barrel is The UK term ‘cask’ encompasses boat builders, as author Henry Work
a measure), had been a feature of eve- a number of container sizes from related: “The evolution of wooden
ryday life for nearly two millennia. Ca- 4½ gallons (pin) through 54 gallons barrels interweaves constantly with
pable of holding a variety of liquid and (hogshead) to 216 gallons (tun). Those that of wooden boats – those built with
bung hole
stave bilge
head hoop
rivet
cant
head
stave joint
bilge hoop chime

quarter hoop croze
Parts of a cask Ceramic dolia, used to ferment and store wine
48 z Brewer and Distiller International April 2016 www.ibd.org.uk

BIOCHEMISTRY l
to casks filled with firewood pitch and

tallow and were using them offensive-
ly. Previously, in 238 BC, the emperor
Maximinus, wanting to cross a swol-
len river in order to secure Aquileia,
a town in north-east Italy, ordered
his engineers to fashion a ‘floating
bridge’ out of redundant wine casks
in order to achieve his goal. So casks
had multiple uses! The celebrated
Moving wine in Roman times find of casks found at Silchester, the
Roman city of Calleva Atrabatum,
Such wood is not ideal and would be indicated the extent of trade between
avoided these days because it is dif- Britain and mainland Europe during
ficult to bend and fashion. Because the 3rd century AD. Made from silver
wooden artefacts do not usually sur- fir (Abies alba), they probably con-
vive and therefore contribute little to tained Rhenish wine, and had latterly
the archaeological record, it is difficult been used as well linings.
to ascertain exactly when and where Kenneth Kilby notes “That by the
‘Tubs’ from tomb of Hesy-re; coopered above, casks evolved. The ‘favourites’ are the time of the Crusades (starting 1095)
copper below (with lids); ca. 2690 BC Celtic tribes of central and western wooden casks were the standard
timbers and planks”. But as Twede Europe who were skilled in both wood- means of transporting all manner
says: “Wooden barrels are related to craft and metallurgy, but the Vikings of liquids and provisions ... and the
basketry, which is one of the earliest and Romans also have claims. Dates cooper became one of the foremost of
packaging technologies,” adding that for the original Celtic involvement with tradesmen.” By medieval times, the
“The word ‘cooper’ is related to the casks seem to be around 900-800 BC. cask was Europe’s primary storage
word ‘coop’, which originally referred Long before this, open wooden and transport container, and with the
to a basket for chickens.” Others have buckets, clearly made by a cooper, huge variety of products contained
proposed that ‘cooper’ comes from the are documented from the end of the therein, the nature of a cask’s con-
Latin cupa, meaning ‘cask’. Old Kingdom in ancient Egypt. The tents would be known by tradesmen
evidence comes from James Quibell’s by its size, style, and markings. By the
Some early history drawings from the tomb of the ancient 16th century, casks were so important
The robust wooden cask was an effec- Egyptian official Hesy-re (ca. 2690 BC), to trade of all kinds that ships were
tive wine storage replacement for the which show wooden staved buckets as designed specifically to hold them. In
ceramic amphora, which was more part of an extensive row of measuring reality, casks were then a currency of
fragile and suffered from an inherent containers. In Plate XIII he illustrates: sorts, their value being a combination
instability, and the larger, ceramic, “Four tubs, two of wood two of cop-
dolium which was used to ferment per... probably for measuring corn.”
and store wine and was often semi- He remarks upon the graining of the
buried for that purpose. Apart from wooden ‘tubs’, “which is best shown
being more robust, casks could be in the largest tub but one, where five
constructed to greater dimensions and planks are clearly distinguished...it will
their very shape allowed close contact be noted that real cooper’s work is in-
storage; in relation to amphorae, tended – barrels with bevelled staves.
wooden casks could be made much The hoops [made of ebony] at top and
larger without adding significantly to bottom are square in section, those in
their weight and fragility. the middle are rounded.” Later, also
Most authorities would accept that in ancient Egypt, a wall painting in the The Silchester casks
in the Mediterranean region it was tomb of Beni Hassan (1900 BC) shows
around AD 500 that wood replaced raisins (probably) being stored in open
clay as the major construction mate- wooden-staved containers.
rial for wine storage. The main use
for wooden casks today is for ageing From the Roman Empire to the
of alcoholic drinks, mainly wines and Crusades
spirits although beers now figure more By the latter days of the Roman
prominently. For many wines, distilled Empire, the use of casks was clearly
beverages, and beers, wood ageing is widespread, for Pliny the Elder’s
one of the most important (and expen- Naturalis Historiae, in the section
sive!) quality-defining factors. dealing with ‘Wine Vessels and Wine
The 5th century BC Greek historian Cellars’, we find: “In the vicinity of the
Herodotus of Halicarnassus (ca.484- Alps, they put their wines in wooden
425 BC), who travelled widely, related vessels hooped around.” He also
that around 800-900 BC, wine was describes how Julius Caesar found
exported by river from Armenia to himself facing an army of Gauls in
Babylon in casks made of palm wood. south-west France who had set fire Cask identification marks (15th, 16th century)
www.ibd.org.uk Brewer and Distiller International April 2016 z 49

l BIOCHEMISTRY
Cooperages of different ages
Wooden hoops; Northern Europe, 16th century

of their size and content and because
of this, casks transcended language 18th century French cooperage
and cultural differences. Traders, pi-
rates and customs officials in the 16th
century would have learned the worth
of a cask size in much the same way
people today learn the worth of a £50
or $50 note!
Because of their value, casks con-
taining wine or spirits were susceptible
to tampering. “Sucking the monkey”
is a term that was applied to the act of Cooperage at T. & R. Theakston, Masham, ca.
drilling two small holes in a cask hold- 16th century German cooperage 1990
ing alcohol and the offender would then
blow through one hole which would (or ‘dry’). The former is for storing North America or in much of conti-
induce the liquid to flow from the other. and transporting liquids, the latter for nental Europe, for example, the climax
After the theft, the holes would be other goods. Some dry cooperage was vegetation could be mixed deciduous
plugged with small pieces of wood. for carrying dry cargo that must not forest and there were plentiful sup-
get wet (e.g. gunpowder) and this is plies of oak species. This meant that
The wood of choice defined as ‘dry-tight’ wines and spirits produced in these ar-
The metal hoops used to hold staves eas could be stored in new casks, but
together were not in common use until Wood and drink in most of Scotland, where the climax
the late 18th century, prior to this time Experience tells us that fresh distilled vegetation is mixed pine/birch forest,
staves were bound by strands of a spirit can be undrinkable because of there was a paucity of mature oak and
flexible wood such as willow, hazel, or its harsh taste and pungency, as well so a constant supply of new wood was
chestnut. With plentiful supplies, oak as the fact that its consumption can not forthcoming, meaning that second-
became the wood of choice in Europe produce harmful side effects. Pro- hand containers became de rigueur.
and North America for wine storage. longed storage in oak casks imparts These had mostly been used for
In addition, the porosity of oak wood colour, a complex aroma, and harmony the maturation of bourbon or for the
permitted evaporation and oxygenation in the mouth. Not only are complex fermentation and shipment of sherry.
of the liquid contents. In the days when wood phenolics extracted into the In Scotland, ex-bourbon (from US) and
beer was fermented and then shipped spirit, but structural molecules, such ex-sherry casks (from Spain) are used
in wooden casks, internal pressure as cellulose and hemicellulose are de- repeatedly (‘re-filling’) until they can
was such that leakage was a major polymerised and the products thereof no longer fulfil their function (i.e. ‘ex-
problem and to counteract this, an in- are also extracted. In all, around 200 hausted’) whence they may be regen-
ner layer of pitch was added to casks. substances can be extracted or trans- erated in the cooperage. Sherry casks
Overall, there are two basic types of formed from oak by ethanol which will have a longer ‘maturation capability’
cooperage; ‘tight’ (or ‘wet’) and ‘slack’ directly participate in the formation of than ex-American bourbon casks,
flavour, aroma, and mouth feel of the and would normally be preferred but
final product. demand for these exceeds supply.
1st stave cut
Since the production of spirits In the case of Scotch whisky, the
3rd stave cut
and wine would have originally been maturation period became so im-
heartwood
seasonal activities, it is assumed that portant that it became incorporated
sapwood
the practice of maturing these drinks into the legal definition of the drink!
2nd would have evolved from the need to To conform to this, one finds that a
stave cut store the final product. Manufactur- considerable proportion of the produc-
ers would soon have found that oak tion costs of Scotch whisky distillers
casks were usually the most suitable are attributable to cooperage oak
containers for doing so. Even so, John investment. Storage in oak casks is an
Conner believes that: “Historically the expensive process in any stored/aged
quarter sawing origins of maturation are obscure, with alcoholic drink.
medullary
the majority of whisky in the 18th and
rays
19th centuries being probably drunk Tree type and basic wood
un-matured.” Bio-geographical crite- chemistry
ria would determine the wherewithal An oak is a tree or shrub in the genus
Stave cuts in timber processing (from Russell, 2003 – by for storage which would vary with tree Quercus. There are around 600 spe-
kind permission) species availability. In many parts of cies of Quercus worldwide, of which

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about 20 are economically important. species, and its wood is denser and grain and few knots. Slow-growing
Just to confuse taxonomy, many more coarse-grained than European specimens produce wood with tighter
Quercus species readily form hybrids. oaks. Other American oak species that grain. Ideally, trees should be around
Historically, the species most used have been used include: Q.bicolor, Q. 100 years old, with a straight unblem-
in cooperage are Q. alba (American macrocarpa, Q. stellata, and Q. lyrata, ished trunk, and around five feet in
white oak), and two European spe- while Q.pyrenaica is an alternative circumference. Only the wood from
cies, Q. robur (pedunculate oak) and Q. European species. The important ground level to the appearance of
petraea (sessile oak). In practice, they Mediterranean species, Q. suber, is the first lateral branches is used and
can often serve the same purposes, only used for cork manufacture. this should be able to yield up to four
but there are differences in wood The best oak wood for casks is casks, depending on size.
extractives; most notably the fact that from slow-growing trees grown in Once staves are cut from the trunk,
American oak wood contains a lower dense groves, which produces an they are left to dry for 3-5 years (sea-
ellagitannin content than the European upright trunk growth with a straight soning), a process that will reduce the
Wood polymers
oak heartwood
major cell-wall components extractives
lignin hemicellulose cellulose phenolics fatty acids other extractibles
guaiacyl & hexoses, hexose: polyphenols simple phenols lactones

syringyl propanes pentoses D-glucose (ellagitannins) alcohols
hydrocarbons
norisoprenoids
inorganic substances
Oak heartwood components
Wood tissue is composed of discreet cells and an intercellular zation of three phenypropanoid monomers; coniferyl, sinapyl and
material that separates the cells, called the ‘middle lamella’, p-coumaryl alcohols.” The latter is only founds in grasses.
and three insoluble polymers comprise the main part of (oak) In oak, lignin is formed by the polymerisation of coniferyl al-
wood: cellulose, hemicellulose and lignin. cohol and sinapyl alcohol, yielding ‘guiaiacyl lignin’ and ‘syringyl
Cellulose, which represents about half of total wood content, alcohol’ respectively. Cell walls contain all three polymers, while
constitutes the wood ‘framework’. It is a linear polymer with a the middle lamella, which cements cells together, consists of a
uniform chain structure, individual glucose-based units being pectic base mainly impregnated with lignin (around 30% of all
bound by β(1-4)-glycosidic linkages. Internal H-bonding between lignin). Oak woods vary in composition, and the heartwood of Q.
chains yields a cell wall framework onto which other molecules alba, for example, is composed of cellulose (49-52%) lignin (31-
can adhere. 33%), hemicellulose (22%), and a fraction which can be extracted
A matrix for the cellulose superstructure is provided by in hot water or ethyl ether (7-11%). The latter contains volatile
hemicelluloses which are branched heteropolymers containing oils, volatile and non-volatile acids, sugars, steroids, tannic com-
a variety of sugars, such as hexoses and pentoses. In oak wood, pounds, pigments, and inorganic compounds.
hemicelluloses comprise some 15-30% cell wall dry weight, and In their native form, the three major wood polymers contrib-
they are largely xylose based (i.e. xylans). ute nothing to beverage flavour, but via a series of reactions,
The third major component, lignin, normally around 15- such as hydrolyses, oxidations, esterifications, acetalisations,
30% in woods, is a highly-branched three-dimensional polymer and polymerisations, their structures are modified to provide the
structure, and, after, cellulose, is the second most abundant required compounds for the visual, taste and flavour characters
polymer in the plant kingdom. Lignin confers mechanical for the stored beverage. Pyrolysis of cellulose and hemicel-
strength to a tree by helping to bond cellulose and hemicellulose lulose during coopering leads to the formation of substituted
together, as well as providing protection through its antioxidant furans and pyrans, the most significant entities being furfural
capabilities. and 5-hydroxymethyl furfural (5-HMF). Phenolics resulting from
HO
A descrip- the breakdown of lignin and which are often present in seasoned
tion of lignin and toasted wood include hydroxybenzoic acids (e.g. gallic,
OH coniferyl alcohol
would be: “An H3CO syringic, and vanillic) and hydroxycinnamic acids (e.g. p-cou-
amorphous, maric and ferulic). Related compounds include hydroxybenzoic
polyphenolic OCH3 aldehydes, such as vanillin, syringaldehyde, coniferaldehyde,
material aris- and sinapaldehyde. There are several other volatile phenols and
HO
ing from an en- most of these compounds can be categorised according to their
zyme-mediated biogenic or chemical origin; for example those based upon the
OH sinapyl alcohol
dehydrogena- guaiacyl (4-hydroxy-3-methoxyphenyl) or syringyl (4-hydroxy-3,
H3CO
tive polymeri- 5-dimethoxyphenyl) nucleus emanate from lignin degradation.

l BIOCHEMISTRY
Tannins ellagitannins have been characterised in oak wood; castalagin;

vescalagin; grandinin, and roburins A-E, and most can be extracted
by aqueous alcoholic solutions (and other organic solvents). The
Classification two most abundant are the stereoisomers vescalagin and casta-
Non-hydrolysable tannins were called ‘condensed tannins’, and lagin, which comprise 40-60% of all ellagitannins. and the others
consisted of oligomeric and polymeric proanthocyanidins. To com- are either dimers of these two or differ by presence of a pentose
plicate matters, some ellagitannins are not totally hydrolysable substituent.
because they possess additional bonds (due to the C-C coupling In the European oaks, Quercus robur and Q. petraea, ellagitan-
of their catechin units to glycosidic moieties). Such tannins were nins can comprise up to 10% dry weight of heartwood. In addition,
originally called ‘non-classified tannins’, but this changed to ‘com- flavanols, including dihydroflavonols, often occur in association with
plex tannins’. Over the years there have always been nomenclatu- ellagitannins to give flavano-ellagitannin derivatives such as acutis-
ral problems over the disparity in ‘tannin’ molecule size, with both simin A and acutissimin B. These compounds can occur in whisky,
large and small molecules exhibiting ‘tannin properties’. as can the related gallagyl-glucosides peduncalagin and punica-
lagin. The level of these latter compounds in a product depends
tannins upon oak species and wood seasoning and toasting.
hydrolysable tannins complex tannins condensed tannins
gallotannins
ellagitannins
Recent advances in tannin chemistry have seen a reassess-

ment of classification and this has meant that tannins and ‘related
polyphenols’ can now be placed in two categories: Type A, with
“constant structures” and Type B, “of variable composition”. This
distinction can be used alongside the previously mentioned stand-
ard classification of ‘hydrolysable’ and ‘condensed’ tannins.
From the point of view of this article, it is hydrolysable tannins
that provide the major compounds in oak heartwood, which con-
tains high concentrations of these phenolic extractives, principally
the ellagitannins. With more than 500 natural products identified
so far from the plant kingdom, these are by far the largest group of
known tannins. Gallotannins are the simplest hydrolysable tannins,
containing a polyphenolic and a polyol residue, mostly derived from
D-glucose. The hydroxy functions of the polyol residues may be
partly, or fully, substituted with galloyl units. Gallotannins are eas-
ily degraded by many microbes, while ellagitannins are relatively The eight oak heartwood ellagitannins
resistant because of the more complex structure conferred by the The amount of vescalagin and castalagin that is extractable by
further C-C coupling. The presence of gallotannins in oak heart- organic solvents declines as the heartwood ages, due to a decrease
wood has not been unequivocally determined. in solubility caused by tannin polymerisation. Hydrolysis of casta-
Ellagitannins are derived from lagin gives ellagic acid and castalin and that of vescalagin gives
HO
biosynthetic stepwise oxidation ellagic acid and vescalin. Despite the high solubility of hydrolys-
of gallotannins and subsequent O able ellagitannins in ethanol-water solutions, they are not found in
oligomerisation processes, and HO
spirits or wines that have been matured in oak casks. Admittedly,
OH
can be classified according to their OH ellagitannins are rapidly denatured when wood is heated during
biogenic oxidation stages. They are HO toasting but since they are not present in spirits aged in non-
esters of hexahydroxydiphenic acid HO
OH toasted casks, this cannot totally explain ellagitannin absence in the
(HHDP) and a polyol, usually glu- final product. It has long been known that the relationship between
cose or quinic acid. HHDP is the O
known wood-derived compounds and distilled alcohol is not always
product of the first-stage biogenic OH straightforward, for some, such as vanillin, are often found in new-
oxidation of galloyl groups. Ellagi- make spirit, albeit at low levels. In malt whisky production, this is
tannins have enormous structural Hexahydroxydiphenic acid (HHDP) likely to be attributable to barley lignins emanating from the wash.
variability because of the different linkages of HHDP residues with Using the ratio of vescalagin to castalagin, it has been shown
the glucose moiety and their strong tendency to form dimeric and that the composition of ellagitannins varies with heartwood and that
oligomeric derivatives. this is independent of the decline in the concentration of extract-
able ellagitannins with increasing heartwood age. Wood density
Ellagitannins in oak wood is another important factor, as is flexibility which is governed by
When exposed to acids or bases, ester bonds are hydrolysed and way in which the long wood (‘medullary’) cells are arranged. The
HHDP spontaneously rearranges into water insoluble ellagic acid conversion of sapwood into heartwood is critical since it determines
(EA). Ellagitannins are thought to derive from a common gallotan- the number of blockages (‘tyloses’) formed in medullary cells and
nin biosynthetic precursor, penta-O-galloyl-β-D-glucose. Eight these reduce the likelihood of leakage.

BIOCHEMISTRY l
likelihood of cask leakage and extract

more tannin from the wood. Cutting
the trunk for stave production is a real
skill and follows a set pattern. Sea-
soning results in wood dehydration,
until it becomes aligned with ambient
humidity. During the process, there is
a reduction of hydrolysable polyphe-
nols, such as ellagitannins, which are
polymerised and precipitated – thus
decreasing astringency. Most of this
occurs on the wood surface, but is also
known in inner wood. A combination
of the effects of rainfall, temperature
variation, and UV radiation contribute
to these chemical changes.
Brown-Forman.com
Toasting the wood
Later, during coopering, it is toasting
(or charring, at higher temperatures)
where the most significant changes
take place, the most important being Tannins are polyphenolic secondary species differences as well as those
the decrease in ellagitannins and the metabolites of higher plants, some- due to geography, etc. American oak
concomitant increase in ellagic acid. times called ‘plant polyphenols’ and, has a lower ellagitannin content than
In addition, the three main polymers because of their enormous structural its French (European) counterparts,
pyrolyse to yield volatile extractables, diversity, have enjoyed several dispa- and higher levels of β-methyl-γ-
such as guaiacol, 4-methylguaiacol, rate ‘definitions’ over the years. For octalactone particularly the cis isomer.
trans-oak lactone, cis-oak lactone, and example, one (not so ancient!) organic These cis- and trans-lactones are of
vanillin which are formed mainly from chemistry text defines tannins as: “C- great importance in Scotch whisky
the degradation of lignin. Over 100 and O-glycosidic derivatives of gallic ageing and are known as the ‘whisky
volatile phenolics have been identified acid (3,4,5-trihydroxybenzoic acid)”, lactones’. They are formed during
from oak wood, with the oak lactones which is far too specific because not all charring of bourbon casks or toasting
being most important. Heat will also tannins necessarily contain a galloyl of wine casks alongside coloured com-
destroy undesirable resinous com- unit or derivative (i.e. condensed tan- pounds, which give the finished whisky
pounds in wood (e.g. ‘sawdust’ aroma, nins which are built up from flavanoid a ‘mature colour’.
mainly due to trans-2-nonenal). precursors. The name ‘tannin’ was Certain types of molecule, exhibit
When considering seasoning and originally given to any plant extract great variation between these two oak
toasting oak, it is important to realise that exhibited astringency, without any types and can be used as markers for
that many of the numerous flavour regard for its chemical structure. oak wood origin. Most notable in this
compounds are produced at different Features that distinguish tannins respect are norisoprenoids, several of
temperatures, and that oak species from other types of plant polyphenol which have been found in significant
toast differently. Seasoning and toast- are the ability of the former to bind amounts in American oak, but are
ing ensure the structural integrity of to proteins, basic compounds, large absent/present in trace amounts in
the finished cask. The former prevents molecular compounds, pigments, and European oak. Conversely, 4-oxo-7,8-
shrinkage, while toasting is aimed at metallic ions. Many tannins also have dihydro-β-ionol was a major noriso-
stabilising the curve of the wood. It is important biological characteristics, prenoid in European oak, but absent
the wood ultra-structure of certain oak including anti-oxidant, antimicrobial, in Q. alba. Over thirty norisoprenoids
species that marks them out as ideal and anti-tumour activity. The proper- have been identified from oak, the first
for tight cooperage. For details of cask ties of tannins, which are moderately being β-ionone.
manufacture see Conner et al., (2003) size molecules, are based on the fact In bourbon manufacture, casks
and Work, (2014). that they have two or three phenolic tend to be re-used many times, re-
hydroxyl groups on a phenyl ring. Ac- sulting in a diminution of the overall
From sapwood to heartwood cording to the polyphenol groups in quality of substances leached from
Large quantities of tannins and related their molecules, tannins were once the wood and the depth at which
polyphenols are laid down in oak dur- classified into two groups: pyrogallol- leaching occurs increases. In some
ing the transformation of sapwood type and catechol (catechin)-type. experiments with cask staves pre-
into heartwood. These compounds Subsequently, these two groups were pared from Q. alba, it was found that
provide protection for the plant against renamed to ‘hydrolysable tannins’ and repeated exposure to whisky led to
invasive micro-organisms; such resist- ‘condensed tannins’ respectively. less leaching. New charred (unused)
ance being conferred by the ability of bourbon staves had more extractable
tannins to complex with proteins and Whisky lignin hydrolysis products, whisky
polysaccharides. In addition to species Regarding the chemical nature of lactones and coloured substances
differences, the content of oak extrac- oak woods, most attention has been than either used Bourbon or first fill
tives varies with factors such as geo- paid to trees grown in France and Scotch staves, and ‘exhausted’ Scotch
graphical origin and forestry practice. North America, where there are clear staves had the least. It has been

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and heavy), an increase in concentra-

tion of nine monophenols (vanillin,
acetovallinone, syringaldehyde, aceto-
syringone, guaiacol, 4-ethylguaiacol,
eugenol, thymol, and salicylalde-
Wood-ageing beer at Epic Brewing, Denver, CO
hyde) was observed. Wood origin and
suggested that the concentrations of beers because of the decreasing level degree of toasting influenced both
lignin-derived guaiacyl and syringyl of ethanol contained in these drinks. monophenol concentrations and their
compounds could be used as an indi- For convenience, most experi- sensory effects. Medium toasted
cator of cask exhaustion. ments on beer seem to have been chips promoted eugenol, thymol, and
carried out by using oak chips. During salicylaldehyde levels in beer, while
Beer brewing, malt and hops are the pri- the other six monophenols were most
Most research into wood ageing marily responsible for imparting aro- associated with heavy wood toasting.
relates to spirits and wines, with matics to beer. Phenolic compounds Beer flavour was greatly influenced
relatively little published on beer. such as ferulic acid, gallic acid, vanillic by wood, with notes such as ‘va-
With the never-ending search for new acid, quercetin and vanillin are known nilla’, ‘woody’, ‘smoky’, ‘creamy’, and
products, especially by craft brew- beer phenolics and contribute to fla- ‘burned’ being to the fore.
ers, beer wood-ageing is now a fertile vour, colour and body as well as haze Further work with model solu-
field of study and there is an increased and astringency. tions showed that process parameters
consumer interest in such beer. In a Brazilian study, a young influenced the availability of the nine
Superficially, one might propose that, Pilsner-style beer was subjected to a monophenols mentioned above. They
using the same wood and conditions, 3-month maturation period (at 0°C) all increased quasilinearly in intensity
a different rate and type of in the presence of French oak cubes with increasing amounts of oak chips
uptake in wood extrac- with different toasting regimes. and their extraction was enhanced
tives might occur Oak barrels were also used. Beer by low pH (3.5) and higher ethanol
in spirits, sample strength varied between content (→8-10%v/v). Elevated storage
wines and 4.34 - 5.19% v/v and samples were temperature (20°C) also enhanced
analysed monthly. Results indicated extractability, but, conversely, pres-
that there were some interactions ence of yeast and oxygen decreased
between wood and beer but they extraction of some phenolics. Vanillin,
were “smaller than expected,” and acetovanillone, syringaldehyde, and
this was attributed to the low level of acetosyringone are particularly unsta-
alcohol in the beer, low maturation ble when oxygen is present.
temperature and short maturation
period. The lager stored with the Other wood for cooperage
most heavily toasted cubes had the In a comparison of East European (Ro-
highest concentration of low-molec- mania, Ukraine, Moldova) Q. robur and
ular weight phenolics, followed by Q. petraea wood with that from French-
beer matured in an oak barrel. It was grown samples, and with American
agreed that neither oak cubes nor Q. alba, discrete chemical differences
wooden casks affected the quality of in their extractives were revealed. As
the beer. judged by their ellagitannin and whisky
In experiments carried out at KU lactone levels, the greatest disparity
Leuven over a period of 60 days with was between American- and French-
an 8.3% ABV ‘neutral blonde beer’ grown wood, whereas East European
suffused with oak chips (identical samples were somewhat intermedi-
dimensions) of Q. robur and Q. alba, ate between these extremes. Eastern
Oak wood toasted to different degrees (medium European wood could be characterised

BIOCHEMISTRY l
by high levels of eugenol, 2-phenyle- acacia, cherry and mulberry (in

thanol and aromatic aldehydes. that order). Over 50 different
Oak wood is still the main mate- volatiles were identified from
rial used in cooperage, certainly these woods, with each spe-
for products such as vinegar, cies showing a characteristic
cider, and some spirits such as profile. Oak proved to be
brandy, although only oak and the richest in volatiles, with
chestnut (Castanea sativa) chestnut running second;
are at present approved by mulberry had the lowest
the International Organisa- levels of volatiles.
tion of Vine and Wine (OIV) for
winemaking. Some produc- Accelerated ageing
ers prefer their drink to be For drinks that must be ma-
non-oak matured, and this is tured for extended periods, such
not always on financial grounds. as brandy, where some 200 phe-
A compromise would be to use oak nolics may be extracted from wood,
casks with non-oak staves incorpo- any means of hastening the process
rated. has to be considered. Whatever the
When assessing other woods for method, there should be no deleteri-
ageing suitability, it is the phenolic ous effect on those phenolics neces-
fraction that is the most important sin- Chestnut sary for taste, aroma, etc. Several
gle parameter. Among woods that have physical methods have been used to
been studied extensively for possible tion of castalagin or vesacalagin with a accelerate wine ageing processes,
cooperage use are chestnut (Castanea gallic acid residue. including γ-irradiation, ultrasonics,
sativa), , cherry (Prunus avium) acacia Chestnut and oak are both in the UV visible light, as well as electric
(Robinia pseudoacacia), ash (Fraxinus same flowering plant family, Fagace- fields (EFs), including pulsed AC
excelsior; F. americana), and to a lesser ae, as is beech (Fagus),and both are electric field (PEF) and static electric
extent, mulberry (Morus alba; M. nigra). characterised by having high levels of field (SEF).
Before toasting, each wood exhibits ellagitannins after seasoning, espe- In general, these methods are
a different and specific polyphenolic cially vescalagin and castalagin. After efficient, non-thermal, and inexpen-
profile, with both qualitative and quan- light toasting of seasoned chestnut, sive. For example, it has been shown
titative differences. Toasting changes concentrations decreased by 70%, that treatment with 20 kHz ultrasonic
these profiles according to the level and this was increased to a 95% loss waves aged rice wine much more
of heat applied and wood thus treated after an intense toasting. Levels of quickly than standard methods, and
will assume its own set of phenolic ellagitannins in seasoned and lightly that γ-irradiation rapidly produced
markers. toasted oak followed the same pat- very high quality rice wine. Treatment
In toasted cherry wood, for exam- tern, but detected levels were lower of a young red wine with PEF gave an
ple, methyl syringate, benzoic acid, than chestnut; even an elimination of increase in the concentration of most
methyl vanillate, p-hydroxybenzoic ellagitannins from heartwood surface phenolics.
acid, 3,4,5-trimethylphenol, and p- layers being observed after heavy When EF treatments were ap-
coumaric acid, the flavonoids narin- toasting. Since it is only stave wood plied to brandy ageing, promising
genin, aromadendrin, isosakuranetin that has to be toasted, higher levels results were obtained. Most beneficial
and taxifolin can be used as markers. of ellagitannins will be available for substances, such as tannins, total
Cherry wood also contains many con- extraction from cask head wood. phenols, volatile phenols, and, esters
densed tannins of the procyanidin type Gallotannins are present in chestnut were increased, while some harmful
which can be useful markers. In acacia wood and were found at their highest ones (acetaldehyde, acetal, and higher
heartwood, where there are relatively levels in seasoned wood. They also alcohols) were decreased. Most of this
low levels of condensed tannins and showed a 70% decrease after a light sort of work is carried out on small
no hydrolysable tannins, one finds high heat treatment and a 95% reduction casks (i.e.2L or 5L), but scientists
levels of the flavonoids robinetin and at higher temperature. Such facts believe that similar effects should
dihydrorobinetin, which are found in no allow us to distinguish chemically exist when EF treatments are applied
other cooperage woods. The latter is a between these two woods. to production size casks (i.e. 225L or
marker for ‘upmarket’ vinegars aged When oak, chestnut, acacia, above).
in acacia. cherry and mulberry woods were
exposed to a 50:50 ethanol-water References
Chestnut wood solution (‘model spirit’) and a 12% Kilby, K. The Cooper and His Trade. J. Baker,
Chestnut wood, which is especially ABV ‘model wine’ solution, there was London. 1971.
rich in gallic acid and ellagitannins, considerable variation in polyphe- Russell, I. (ed.) Whisky, Technology, Pro-
has been used enologically around nol extractability. The model spirit duction and Marketing, Academic Press,
London. 2003.
the Mediterranean for years. It is now extracts of chestnut and mulberry ex-
Twede, D. The cask age: the technology and
known that chestnut heartwood has a hibited the highest total polyphenols, history of wooden barrels. Packaging and
polyphenolic profile very similar to that followed by cherry, acacia and, finally, Technology Science. 18(5): 253-264. 2005.
of oak. A difference, however, revolves oak, whereas the model wine solution Work, H.H., Wood, Whiskey and Wine: A
around 1-O-galloyl castalagin, which extracted most polyphenolic mate- History of Barrels, Reaktion Books, London.
seems to originate from the esterifica- rial from oak – followed by chestnut 2014.

● DISTILLING
The Cask
An amazing element in the
wonderful process of making whisky
©istock.com/ksmith0808
By Billy Mitchell
Much has been researched

and written to explain in
great technical and sci-
entific detail the various
processes used in the pro-
duction of whisky – many
articles have been written
on raw materials, malting,
mashing, yeast, fermenta-
tion and distillation of many
new make whiskies.
W ith this article I hope to provide

some generic insight to another
©istock.com/EdStock
key element in the process of mak-

ing whisky – the cask. This is not a
detailed scientific explanation of cask
construction, wood treatment or even
the maturation process itself. I would
A cooper works on a cask at the Speyside Cooperage
say this is an introduction into yet an-
other amazing element of the wonder- by heating were borrowed from the show that ancient coopers’ tools dating
ful world of whisky. boat builders of yester year who used back to 100 years BC have been found
this technique to bend planks of wood and recorded.
Cask – the history for the hulls of ships. The barrel or cask has proven to be
The use of watertight, barrel shaped Historically the barrel was used the most convenient method of storage
wooden containers that could be rolled to hold water, wine and other liquids and shipping for almost 2000 years
and stacked has been recorded in his- such as vinegar, oil and water, but also – apart from storage and transport
tory dating back to around 300 – 400 became the method of choice for stor- of many of the materials previously
years BC. These containers proved to age and transportation for solids such noted they were ideal for carrying all
be very strong and could withstand as metals, nails and gun powder. It types of bulk goods. The wooden cask
the stresses of the basic methods of could also be used for the preservation proved much easier to manhandle
transport at that time. It is likely the of foods such as fish and other sweet, and was significantly sturdier than the
techniques of bending wood into shape slated or pickled food. Historic records cheaper bags and crates – on a weight
22 ❚ Brewer and Distiller International May 2015 www.ibd.org.uk

DISTILLING ●
The various sizes and shapes of the most commonly used oak casks
for weight basis they could be read- By definition Scotch whisky, “has
ily moved. However, much the same been matured only in oak casks of a
as the whisky and other industries capacity not exceeding 700 litres”. All
introduced more modern production of the casks in Table 1 have been used
processes, the wooden cask lost its to mature Scotch whisky. They range in
The wooden cask and its parts
place as method of choice for storage capacity from the American Standard
and transportation and was eventually Barrel holding ~ 200 litres to the larg-
replaced by pallet based and contai- est, the Puncheon holding around 560
nerisation systems introduced during litres. The American Standard Barrel
the 20th century. has the greatest internal surface area
With the movement of casks across to liquid volume ratio and is often rec- A section through a head
the globe to support all types of trad- ognised as the industry standard for
ing activity it should be of no surprise maturing both malt and grain whisky.
A schematic showing all the elements which combine to
to learn that the early distillers, either The oak tree is the starting point form a cask
illicit or eventually legal, came across for all casks used to mature Scotch
the opportunity to store their product whisky. There is yet another very large of immature wood to dry and season
in these wooden containers. During industry supporting the sustainability prior to raising into casks. This storage
the years of illicit whisky production in of the European and American oak acts as a buffering capacity between
Scotland the transport of the distilled forests – I will not get into any real the availability of new wood from the
liquid was limited as concealment of discussion in this article but need- saw mills and seasoned wood entering
the distillate was required. Transpor- less to say production volumes can cask production.
tation was mostly carried out using and do fluctuate. Once the mature oak Oak is used to mature Scotch
disused wine, sherry and port casks trees have been cut down, logged and whisky due to its physical and chemi-
originally from Southern Europe. The processed through the saw mill into cal properties. Oak wood has physical
transport of whisky in wine, port and useable materials the wood can then strength due to its natural develop-
sherry casks brought about differences be turned into casks. The fluctuation in ment during growth which allows the
in the whisky which is still recognised new wood supply can have an impact wood to be bent by heating without
in the maturation processes of today. on the availability of wood entering the splitting. This gives strength when
I suspect very little was known or coopering businesses although this formed into a cask. Oak has a tight
understood about the importance of can be mitigated to some extent by grain which prevents leakage of
wood at that time other than it had an the requirement to hold large stocks product - it is also porous and allows
effect on the liquid. Eventually as the
Whisky Industry grew it became very Size and Shape
aware of the importance of maturation
in wood to soften otherwise a very im-
mature product. The role of wood was
finally recognised!
There has been much research
into this very important facet of whisky Type BUTT HOGSHEAD American PUNCHEON DUMPY
production and I recommend and direct Standard PUNCHEON
your attention to the respective chapters Barrel (A.S.B)
by John Conner, Ken Reid and Frances
Approx. Capacity
Jack in the first edition and by John 500 254 191 558 463
(litres)
Conner in the second edition of Whisky,
Technology, Production and Market- Height (m) 1.27 0.86 0.88 1.13 0.99
ing edited by Inge Russell and Graham
Max. Diameter (m) 0.90 0.72 0.63 0.96 0.95
Stewart, for more detailed reading.
Internal surface
3.55 2.25 1.90 3.78 3.34
The cask – a maturation container area (m2)
for Scotch whisky
Surface/Volume
There are several types of cask gener- 71 88.5 100 67.5 72
Ratio (cm2/l)
ally differentiated by the volume of
liquid they hold and their shape. Table 1 – Cask specifications
www.ibd.org.uk Brewer and Distiller International May 2015 ❚ 23

● DISTILLING
the maturing whisky. tion. Initially these casks were broken

There are two main sources of down in “shook” bundles for transport
cask for the Scotch whisky businesses. across the Atlantic before being rebuilt
The majority of casks are sourced as in cooperages in Scotland – although
ex-bourbon wood from the bourbon these practises still remain in some
industry in the United States. They are cases, ASB’s are now more commonly
all produced from American White Oak transported as casks by container to
(Quercus Alba) and these are the most Scotland.
commonly used cask in the Scotch Similarly in Europe, sherry, port
whisky industry. The other source of and wine casks are generally only
casks is from the European sherry, used once in the maturation cycle for
port and wine businesses – these these products and again they then
casks can also be produced from become available for Scotch whisky
American White Oak but are more maturation. Changes in scale of these
commonly made from Quercus Robus European businesses also impacts on
and Quercus Petraea, both European the availability of this wood. Importa-
species of oak. tion of sherry from Spain to the United
By definition all bourbon must Kingdom started in the mid-1800s –
be aged in new, charred oak bar- the casks used to transport the sherry
rels known collectively as American were made from Spanish oak – these
An example of the automated equipment for the mechanical
Standard Barrels (ASB’s). The scale of are still used by many distilleries even
tightening of cask hoops – cask hardening.
this industry, either through expansion although they are substantially more
permeation of air (oxygen) in and out or contraction, has a corresponding expensive than the American bourbon
of the cask. The oak is also different to knock on effect on their sourcing for cask.
other wood species like pine or rubber Scotch whisky maturation. American Some distilleries in Scotland also
trees which contain resin materi- Standard Barrels are a fairly new ad- use specialist oak casks for finish-
als that could eventually pass strong dition to the Scotch whisky industry ing product – these are generally
flavours into the maturing liquids. becoming readily available from the sourced from specific oak species
Chemical transformations can be pro- end of the Second World War. A new to deliver alternative flavours to the
duced on the internal surfaces of the law was formulated at that time by the final product. American oak is seen
oak casks by the use of various heat Cooper’s Union in the United States as perfect for whisky cask construc-
treatments after the cask has been that stipulated that bourbon must be tion – the trees are fast growing with
raised. These treatments can include matured in new oak barrels – this was tall straight trunks, giving quality wood
various degrees of toasting and char- done to boost the coopering industry with high levels of flavour compounds.
ring of the internal surfaces – each dif- after its collapse during Prohibition. It is said that approximately 90% of
ferent heat treatment has the potential This resulted in a massive increase in all the world’s whisk(e)y is matured in
to deliver different flavour profiles in numbers for Scotch whisky matura- American oak ex-bourbon casks. The
Three casks sit in the firing chamber at various stages of the charring and heat treatment process as part of cask rejuvenation.

DISTILLING ●
ing maturation, this well known filter

Cask too strong aid is capable of removing odours,
Ideal maturation particularly sulphur compounds, from
the maturing liquid which were formed
during the fermentation or distillation
processes.
Taste
Additive Activity
Lighter char levels tend to show fruit
esters and spice notes while the heavi-
er char gives rise to extraction of oak
flavours into the spirit more quickly.
Cask too weak
During the process of caramelisation,
wood sugars are transformed into
Time
many new aromatic compounds – the
Distillery character Un-matured whisky (subtractive activity)
“toasty” compounds in the wood will
Cast maturation (additive activity) be extracted into the liquid during
maturation contributing to the colour
Figure 1 shows an overview of the maturation process
and flavour of the product.
key flavours associated with American undergone some form of rejuvenation Figure 1 gives a very simple
oak include vanilla, honey, nuts, fudge prior to their ongoing use in whisky overview of the maturation process
and ginger spice – this is not a fully maturation. Charring an oak cask in- over time. It can be seen the distillery
inclusive list. volves a number of complex reactions character changes very little over
Spanish or French are the two which take place over a very short time and this is driven by raw mate-
predominant sources of European oak, timeline. Whisky casks are charred rial selection, mashing and fermenta-
although there is now wood available to create flavour, colour and different tion conditions and the total distilla-
from the Eastern European countries – aromas - a char layer acts as a filter tion process. The subtractive activity
these were either made for the sherry and to break down the oak cell walls is driven by the condition of the char
or wine industries in their respective so the spirit can extract flavour from layer on the internal surfaces of the
countries. They are generally much the oak. cask and the quality of the original
slower growing species when com- Charring a cask requires the total new make whisky. The additive activity
pared with American white oak. The interior of the cask shell to catch fire is driven by the many chemical reac-
key flavours associated with theses for a pre-determined length of time. tions within the wood / liquid interface
oaks include sherry, dried fruits, wood, This will either take place when the and can be variable depending on the
caramel, orange and various spices – cask is first raised or during a reju- condition of the cask.
again this is not a fully inclusive list. venation process where an exhausted If the maturing liquid is left too
cask has had the original charred long in an active cask it may eventually
Maturation – a brief overview. layer removed leaving a new fresh be described as woody while converse-
Many of the flavours and characteris- oak surface area available for a new ly if matured in an unreactive cask
tics of whisky are picked up from the charring process. Ideally the charring for a short period of time it may be
oak casks in which it is matured – by process should take place with both described as immature. What seems a
law this must be for a minimum of ends removed to ensure consistent very simple process from an external,
three years in Scotland. and efficient firing. The inside of each non-blender perspective is in fact a
Research has shown that changes cask catches fire and in that short very complicated algorithm with many
in raw materials, pre-distillation and period of time a char layer is created complicated, interactive and interde-
distillation processes can alter the on the internal shell of the cask. As the pendent reactions. This is where the
quality and character of the new make heat from this process gradually pen- experiences, skills and understanding
whisky distillate – this is also appli- etrates into the oak the chemistry is of each of the Master Blenders from
cable to the maturation process where significantly modified in these interior the Scotch producers comes into play
wood type, wood treatment by toasting wood layers – sugars are caramelised – they will fully understand the many
or charring and length of time in cask giving both flavour and colour and variables in the production processes
can have a significant impact on the vanillin and other flavour characters through maturation and will ensure
flavour and character of the matured are created. Each whisky producer that stocks are laid down to ensure
liquid. will have their own standard of char final product quality is achieved on an
There are three main contributors which supports the quality required for annual basis.
to the total maturation phase – these their own product portfolio – once the Key to the whole process will be
are the actual distillery character of desired level of char has been reached the provision of a wood policy, most
the new make whisky, the subtractive the casks are normally sprayed with likely to be specific for each whisky
activity of maturation and the added water to halt the charring process. business, which, when applied, will
activity. ensure that all the variables previously
All casks used in the Scotch whisky Subtractive Activity noted are addressed to ensure that
industry have either been toasted or The process of charring produces product quality is not compromised.
charred prior to use in their origi- carbon on the internal surface of These Master Blenders will also use
nal roles as maturation vessels for the oak staves. While this does not their skills and expertise in both wood
bourbon, sherry, port or wine or have directly contribute to the flavour dur- and liquid quality to continually create

● DISTILLING
whisky maturation process. Generally ditional filling stores and warehouses

coopers working in these larger types at distillery sites and the coopering
of cooperages were known as PBR industry has followed a similar model
(paid by results) coopers and their sal- – centralised coopering operations
ary was directly related to the output are the norm with little or no cooper-
and performance of their own work. ing presence on the majority of the
There were many payment schemes distillery sites. The physical demand
where coopers were paid by either on the service or PBR coopers led
minute values (time allotted for each the industry to seek out mechanical
repair type) or by the scale of the tasks solutions and aids to minimise many
required on each cask and even by the of the physical, labour intensive tasks
number of staves replace or repaired. required to breakdown, repair and
Needless to say these roles, either as a re-build casks. There now remains a
service cooper or PBR cooper required much smaller coopering footprint in
great skill, energy, stamina and overall Scotland where mechanical, semi-
physical strength in what was and mechanical, and traditional manual
remains a very demanding job. operations are undertaken to repair,
A selection of coopers tools including plucker (or down-
Much has changed over the years rejuvenate and re-build casks for the
right), croze board, topper, heading knife, driver, cooper’s
hammer, crumb knife, punch and adze. where centralised cask filling and whisky industry.
maturation warehouse operations have In the early 1970s there were
new products for the ever changing more or less replaced the small tra- some 1151 coopers and apprentices
demands of the market place.
The cooper – a master craftsman.

“Cooper” is the name given to the
tradesman who makes or repairs
casks or wooden barrels – the cooper
would generally work in a cooperage.
The whisky industry has changed
markedly over the years with industry
consolidation, distillery closures and
distillery and central warehouse devel-
opments, varying levels of production
and modern technology replacing some
of the more traditional processes – a
similar picture can be painted of the
coopering industry. When I started my
career in the whisky industry in 1970
almost every distillery would have at
least one cooper working on site – in
fact most distilleries had a cooperage,
the size being dependent on the scale of
distillation, cask filling and warehouse
activities – Her Majesty’s Revenue &
Customs officers also had a significant
presence on the distillery and matura-
tion warehouse sites at that time. The
primary role of the distillery coopers at
that time was to repair leaking casks
during maturation and also to ensure
that casks were fit for filling prior to
maturation to ensure any loss of rev-
enue was minimised – generally their
role was that of a service cooper.
At that time there were also a sig-
nificant number of larger, more cen-
tralised cooperages where casks were
raised from shook bundles purchased
in the US or Europe and where Ameri-
can Standard barrels were enlarged
into hogsheads by the inclusion of
additional staves and enlarged head-
ing wood. They would also be used to
repair and rejuvenate both old and new These photographs give a view of the differences in scale between a large centralised cooper-
stocks of wood prior to entering the age and filling operation (top) and a small distillery operation

DISTILLING ●
employed in Scotland compared to the

211 employed at the end of 2013. This
represents a huge change in coopering
operations in Scotland and could have
impacted on the provision of casks for
the whisky industry. Thankfully this did
not happen and the apprentice popula-
tion has now risen to around 17.0 %
of the total cooper population in 2013
compared to some 13.0 % in the 1970s.
Historically an apprentice cooper
was required to serve some nine years
learning his trade before becoming a
fully qualified cooper – this has subse-
quently been reduced to seven then five
and now finally four years over time. An
apprentice will now likely spend three
three years in a traditional apprentice
workshop with a final year four in the
mechanical processes where these are
employed. It should be noted it takes
considerable skill to raise a cask from
anywhere between 30 and 35 oak staves
of different width, mild steel hoop iron An apprentice hard at work in the workshop A palletised cask warehouse
and end wood produced from other oak learning the arts, crafts and skills of the cooper.
staves - this is even more so when you
consider that there are neither nails or actual fact the volume of new make
glue, nor any other fixings or fastenings filled currently is higher than that
used in this process. disgorged due to the growth in the
The coopering industry has always industry.
been and will always be dependent on If these assumptions mirrored
the scale and volatility of whisky op- reality there will be anywhere be-
erations and will expand and contract tween 1.9 million and 4.8 million casks
in a similar fashion – this is inevitable disgorged in a given year with a higher
but the cooper will always play a huge number being filled. If we assume
role in the quality of the final bottled there are, on average around 80 casks
product. per lorry load there will be anywhere
between 23,750 and 60,000 lorry move-
Casks – the logistics piece ments per year with a similar number
Alan Gray reported in his 2014 annual associated with new make fillings. The
review of the whisky industry there truth is actually somewhat different to
were some 3.7 billion litres of alcohol the above assumptions as the range of
in maturation warehouses in Scotland product in market ranges from product
– this would equate to about 5.8 billion at three years of age to many single
litres of bulk whisky at 63.5 % alcohol malts anywhere between 16 and 28
by volume. years of age.
If all this volume was matured I have used these assumptions to
in American Standard Barrels there demonstrate the huge logistics opera-
would be some 29 million casks in tion employed to support the industry A racked cask warehouse
bond – conversely if this volume was in Scotland. Using these extremes
matured in large wood (butts), there and assumptions gives those outside the overall impact of transport and
would be some 11.6 million casks in the industry an overview of the scale haulage costs.
bond. Obviously these figures are at of operations behind the disgorge of This simplified overview of the
the extremes and the reality is the mature product and the new make cask, the cooper, maturation and
actual number will fall somewhere whisky supply chains. In reality much the logistics piece gives yet another
between the two, with significantly of both new make and mature product great insight into the many varied and
more of the smaller casks in bond so is tankered between production, filling skilled roles across yet another part of
the actual number will trend towards stores, maturation warehouses and the whisky production process – this
the higher figure. bottling and blending operations to adds to the other skills and roles in
If we assume the average age of simplify logistics and minimise haul- the malting and malt and grain whisky
bottled Scotch is, say, six years then age costs. Obviously consolidation and production processes and should
a sixth of the maturing stock will be centralisation of whisky filling, cooper- demonstrate the real opportunities
disgorged on an annual basis and the ing activities, maturation warehouses available to those still looking for
same volume of new make will be and mature whisky disgorge opera- challenging roles in what is currently a
filled to maintain a stock balance - in tions also goes some way to mitigate vibrant industry.

● DISTILLATION
Is the oak industry under threat

from rapid maturation techniques?
Moving things along
iStock.com/liveslow
A look at rapid whisky maturation methods
By Roger Putman fortune, perhaps we should consider

what occurs during maturation and
judge whether the science behind these
It is an oft-quoted old saying, particularly amongst the accelerations is likely to have any com-
brandy fraternity, that: “You make brown spirits for your mercial effect. During the preparation of
this article, I was told of magic and black
sons and daughters and drink the ones your father made.” arts by a number of Scots. Many text
This would suggest that it takes time to mature a spirit into books gloss over ten long years in a dark
cellar by the Hebridean Sea by saying
something of which a father might be proud. According to that the raw spirit fresh off the still is
California-based whisky writer, Bozkurt Karasu, Americans diluted to around 64%ABV in casks pre-
lack one important virtue – and that is patience. viously used in the US bourbon industry,
the angels take their share and hey
presto, a few years later the magic hap-
H ence there has been a lot of inter-

est lately, particularly in the USA
with its 1000 craft distillers, in produc-
wood and if they don’t get that, they are
being cheated. All whisky sold in the EU
must be matured in wooden casks for
pens after the black arts have weaved
their spells and the blender is presented
with something to play with!
ing an acceptable spirit in weeks or at least three years, with the definition
months rather than waiting for years of Scotch whisky requiring maturation Wood and brown spirits
and suffering concurrent losses of in oak. One can experiment with differ- Brown spirits are matured in wood and
volume and alcohol, high stock valu- ent techniques, but whether the final include whiskey, brandies (cognac,
ations, on-going warehouse storage product complies with the definition of armagnac, pisco, aguardiente and
costs and having the Excise breathing whisky in the market concerned (and other grape products) as well as some
down your neck all the time. can therefore be described as whisky) is rums, cachaças and tequilas. I note
On the more cautious side, Rose- a different matter. Such products would that the innovative souls at Watershed
mary Gallagher at the Scotch Whisky have to be described as something else in Columbus, Ohio, first produced a
Association observed that “Traditional – they should not benefit from being barrel-matured gin back in 2012. They
production practices have built up the described as whisky.” were surprised when the sale of a
reputation of whisky as a category. Con- Before we take a look at the various few bottles was announced and 750
sumers expect whisky to be matured in methods supposed to save distillers a folk turned up to buy some. Hernö in
36 z Brewer and Distiller International November 2016 www.ibd.org.uk

DISTILLATION l
Brown spirits of course start off

from the still entirely colourless. The
brown comes from the oak cask, its
charring and toasting and the col-
our of any previous incumbent be it
bourbon or sherry. Although still a
niche category, brand owners see an
Char 1 Char 2
angle in acquiring finishing casks that
earlier held port, Madeira or wines
like Sauternes, Tokaji or even Grand
Cru champagne or Chateau Margaux.
France’s Brenne farm distillery near
Cognac makes a single malt and does
things the other way around, starting
Char 3 Char 4 (Alligator char) in new Limousin oak then finishing in
newly disgorged cognac casks.
Charring the casks at the Independent Stave Company and the various levels of char available,
from Char 1 to Char 4 which is the classic Alligator Unaged spirits in the past
Sweden has gone further and used a from Longmorn and Glen Garioch with During the nineteenth century, much
juniper cask for its spell of maturation. whisky from the Hanyu distillery in whisky was bottled soon after distilla-
In the UK, Chris Hayman reports that Japan to produce an offering called tion. But like brewing, whisky-making
for his wood-aged 1850 Reserve he Glover. Perhaps on the more bizarre tended to be seasonal in nature and
had to alter the gin recipe to take ac- but still eye-catching end of innovation the oak barrel would have been the
count of the woody flavours interacting is from independent bottler Caden- most readily available container for
with the botanicals. head’s Stupid Cask range with Fishky storage. Discerning producers and
I do hope we are not about to see which supposedly put Bruichladdich customers must have picked up on
a botanical-infused whiskey but the in a herring cask; pundits Whisky Cast the changed character of the spirit.
whole market is highly competitive and were not complimentary, suggesting The current minimum storage period
innovation to get that edge in the market that: “The nose hides the secrets of embedded in the Scotch Whisky Regu-
is intense. Developing a USP has never the whisky well and the finish is salty, lations is a little known result of Lloyd
been more critical. Once upon a time the greasy and nasty with no redeeming George’s efforts to bolster munitions
sector was driven only by %ABV, pack- qualities.” Westland Distillery also production during the Great War when
age design, age or cask finish. Scottish put out a press release on April Fools drink was apparently causing more
products no longer feature as regularly Day with Inferno, finished in a Tabasco problems than the whole fleet of Ger-
in Jim Murry’s Whisky Bible top five as cask. Roundstone Rye probably had man submarines.
they used to. While at the classic end of more luck with a maple syrup cask. Total prohibition was not an option
the market, a 12yo whisky might now be but a number of measures to curb
more common than a declared 8yo but Vibrant sector immoderate consumption were intro-
there is more and more Scotch on sale So the sector is indeed vibrant and as duced. UK brewers are familiar with
with no age statement. In Ireland, Cooley Bill Owens at the American Distilling the restriction of pub opening hours,
is selling a poteen straight off the still; Institute points out, if you listen care- making the buying of rounds illegal
I trust that it is more potable than the fully to the supply chain for American – and the nationalisation of pubs and
product which surreptitiously appeared whiskey, there is a distinct sucking breweries around the munitions plants
at times in Bass’ Belfast Brewery! sound as demand threatens to outstrip at Enfield in London and Gretna on the
Hybrids are everywhere; Pernod- the ability of the industry to supply. Scottish border – but the Immature
Ricard has Zaconey, a blend of Irish and The market is huge, with Bill’s 1000 or Spirits (Restriction) Act of 1915 banned
US whiskies with berry extracts; Eng- so US craft distillers representing just the sale of any spirit less than two
land’s Lakes Distillery produced a blend 1.5% of American spirits sales (over years old. This was increased to three
of whisky from all parts of the United there craft beer is 12.2% of the market). a year later.
Kingdom called ‘The One’ to sell before We have already seen %ABV reduc- The Act certainly reduced spirit
its own whisky comes of age. Moss- tions and a shortening of the period availability and took immature prod-
wood finished a 7yo Tennessee whiskey in cask so small wonder that brand ucts off the market believing that they
in a cask which had been seasoned with owners are interested in any permitted caused more drunkenness than older
espresso coffee. High West Whiskey’s accelerations as long as they do not and obviously more expensive brands.
Campfire combines American rye with damage brand credentials. No doubt Today the arms factories are long
peated imported Scotch. Similarly Jim much work is going on behind closed gone, but the three-year rule still ap-
Beam Kentucky Dram blends Kentucky doors to avoid accusations of penny- plies for Scotch whisky along with the
Straight Bourbon with an Ardmore pinching corner-cutting but enquiries to restrictions on raw materials, upper
peated malt to ‘marry smoke and va- PR departments are greeted with sharp distillation strength and a minimum
nilla’. Diageo’s Whiskey Union recently intakes of breath and quiet tutting alcoholic strength of 40%ABV in bottle.
launched Huxley Rare Genus Whiskey, sounds for your even suggesting that Immature spirits disappeared from the
comprising Scotch, Canadian and such shenanigans are going on! Heriot market for a century.
American casks while its Boxing Hares Watt University in Edinburgh has also The benefits of aging in oak have
infuses hop flavours. conducted some research but under a long been appreciated, rather than
Adelphi has mixed single malts client non-disclosure agreement. understood. Even today we have only
www.ibd.org.uk Brewer and Distiller International November 2016 z 37

l DISTILLATION
Ian Palmer from Scotland’s newest whisky distillery Inchdairnie says he has looked at lots
of rapid maturation options, not that he wanted to use them but just to understand them.
He tried adding wood into the barrels but this just tasted of sawn wood where the young
spirit flavours are masked as opposed to maturing them out. He added “I am looking for
complexity, mouth feel, long finish and sweetness. Many of these ideas, for a sophisticated
palette, can be just one dimensional which leads to disappointment. Time is only a problem
when you do not have enough of it.”
teraction and masking of low flavour heated elements provides a similar if

threshold, less desirable characters. less pyrotechnic effect.
The tight grain of American oak slows Sherry casks remain popular
chemical interactions so the internal although they are no longer procured
surface of the staves (not usually the from Bristol bottlers as since 1981,
ends) are charred or toasted to create sherry must now be packaged in
both a carbon layer and to damage the Spain. Users should note that only
wood so that lignin derivatives can be about 90% of sherry casks are derived
leached out by the spirit. The staves of from European oak with lighter sher-
elucidated parts of it and the discipline uncharred casks have also been dam- ries demanding wood from America –
of wood management has emerged aged by heat applied during the curving buyers need to ask the right questions.
utilising our current knowledge of a of the staves to make the barrel shape.
highly complex and lengthy process. For charring, a gas flame is Making the casks last longer
Oak wood is a potent source of vanilla deemed more controllable than the The level of charring, initially carried out
and coconut like flavours. traditional fire of oak chippings, with to help mature the bourbon, is still active
The continuing popularity of vanilla the intensity of flame and duration when the cask is used for Scotch. It will
ice cream is testament to how this spice dictating different levels of charring. remain active for up to five fillings over
is inculcated into our flavour preferences Heavy charring can leave a smokiness perhaps 40 or 50 years but each suc-
from an early age. Yet it is not all about and acrid taste which is not always de- cessive use exhibits a drop in activity, so
adding flavours, there is subtraction, in- sirable. Toasting in front of electrically immature flavours are slower to go and
mature flavours take longer to develop.
Oak still rules This is best tracked by looking at the
colour which is extracted. By carefully
choosing the US cooperage supplying
the used bourbon casks, it is possible to
get a level of activity to suit the product
you are trying to mature. After all, if you
have to hold stock for a statutory three
years there is little point in procuring
casks which will have moderated the
new-make flavours in two!
In the old days exhausted casks
would be destined for the garden centre
but now they can go through a dechar/
char process where the old layer is
scoured off down to bare wood and the
surface then charred again with suf-
ficient heat to damage the upper wood
layer to allow a further few fillings. Con-
In Scotland at and Arran and the currently closed Bladnoch distillery ditioning with sherry used to be popular

DISTILLATION l
but today if you have both grain and malt with oxygen which diffuses through the
whiskies, the newly-charred cask is just oak to produce desirable flavour conge-
refilled with grain spirit. Otherwise they ners such as acetals.
might be used for a ‘finishing’ period Furthermore, the concentration
with matured whisky to condition the of ethanol, increased by loss of water
wood. There is obviously a limit to suc- to the atmosphere or decreased by
cessive dechars before the structural the loss of ethanol if the humidity is
integrity of the stave is compromised. high, will complicate the reaction even
Balance is essential. A heavily peat- more. For a more detailed review of
ed Islay may still dominate the finished the reactions which take place, Ian
product even after long maturation Hornsey published a survey in last
in a highly active cask. Conversely, a April’s Brewer and Distiller International
delicate Lowland would be swamped by and John Conner’s chapter in Inge
the use of first-fill sherry casks leaving Russell’s Whisky Technology: Production
a cask flavour masking any contribution and Marketing is invaluable.
of the stills themselves. Having said New make is typically cut to
that the heavy sweetness from sherry 63-64%ABV into cask, there may be
is popular with some customers but it temptation to increase this to save on Learning more about maturation conditions.
should not be overbearing. barrels and warehouse space but such The front and rear elevations of Buffalo
spirit matures more slowly so it will Trace’s experimental 150 cask Warehouse X at
Frankfort in Kentucky
Over 500 components have to be in cask for longer. Casks may
Industry guru Alan Rutherford points be held on their bilges (bellies to the to explore some of the storage issues.
out that mature whisky contains over brewer) two high in traditional ware- Warehouse X is comprised of four in-
500 identifiable molecular compo- houses or else on steel racks as high dependently operating chambers that
nents, although it is likely that fewer as your building costs and fork lift truck allow specific variables like natural
than a hundred of these have a primary reach will allow. More and more will light, temperature, humidity and air-
influence on organoleptic character. be conveniently stored on their ends flow to be tested. There is only space
These compounds, or congeners, (heads to the brewer) on pallets per- for 150 casks but it uses $1m worth of
include higher alcohols, aldehydes, es- haps five high or six high. Temperature monitoring equipment.
ters, nitrogen and sulphur compounds, seems to be important and warehouses After a couple of years, results are
carbonyls, phenols and lactones. He should be as full as possible to reduce said to be encouraging, yielding ‘inter-
groups the long slow chemical reac- fluctuations but casks on the top- esting experimental insights’. Sazerac
tions occurring during maturation into most rows will get a lot hotter even in CEO Mark Brown does not believe
three general categories. Scotland unless the ceiling is specially rapid aging is the solution to current
Firstly, the removal of undesirable insulated. Even in Scotland a steady shortages but he has launched Whis-
or immature components such as heavy 2% of volume is lost to the angels every key Thief – a bourbon with added oak
sulphur compounds by absorption on year meaning that after ten years only inserted into the barrel. Such contact
to the oak/char surface and to a lesser 85% of the volume will remain but the is said to double the age profile of the
extent by evaporation (light carbonyls) loss of water being relatively greater product. Meanwhile Buffalo Trace is to
through the porous wood. Then desir- will usually slightly elevate the %ABV. spend $200million on capacity expan-
able components such as lactones mi- sion at its Frankfort base in Kentucky.
grate from the oak to the spirit. Finally Experimental warehouse
there is chemical interaction within the Sazerac opened its Buffalo Trace Reducing the raw new-make
spirit between organic compounds and Experimental Warehouse X in late 2013 flavours
A large company like Diageo with 28
malt distilleries has to know the char-
acter of the various new-make prod-
ucts in formulating a wood manage-
ment policy. These flavours may range
from perfumed, appley, grassy or fruity
to cereal, sulphury, feinty or smokey.
This immaturity is attenuated to yield
a desirable product over time before
the whisky is deemed saleable and
can be passed on for blending. Newer
producers should look at the materials
and processes which might lead to the
new-make product being more pun-
gent, sulphury and feinty thus needing
a longer maturation period.
One Speyside distiller I spoke to was
most affronted when I suggested his
new-make was pungent, raw or feinty.
Three casks sit in the firing chamber at various stages of the charring and heat treatment as Clearly he has a finely-tuned process,
part of cask rejuvenation he thought he would get the sack if

l DISTILLATION
Maturation in action it wasn’t and the spirit was not ready

Maturation effects on the 1096th day after filling. Others
might choose to alter the wash condi-
tions considering the wort clarity and
concentration, totally enclosed or open,
stainless or pitch pine fermenters, pitch
rate, type of yeast used, pitch tem-
Character
Distillery Character Interactive

Spirit
perature, wort oxygenation and period

in fermenter. All will alter the volatile
Immaturity Maturity compounds present in the wash.
Within the still, the ‘copper conversa-
Subtractive Additive
tion’ is critical as active sites on the sur-
face will remove sulphury compounds.
Time These active sites will get used up like a
This diagram from Diageo illustrates how the maturation process attenuates the raw spirit spent Brillo pad and need rejuvenation
immaturity over time, the distillery character interacts with the wood which also develops by resting the still, opening the hatch to
maturity traits – all over time
allow air inside and also having a gap be-
Maturation effects - Maturation effects -
tween one distillation and another. There
initial high level of immaturity low level of initial maturity must be some mileage in the nano par-
ticle copper surfaces espoused by Italy’s
Green Engineering (Brewer and Distiller
International, June 2016) as surface area
Character
Character
Spirit
Distillery Character A Distillery Character A

Spirit
for reaction is increased dramatically.

Distillery Character B Distillery Character B Still design with respect to the angle of
Immaturity Immaturity the lyne arm, the reflux geometry in the
neck and the temperature of operating
Time Time
the condensers so that if they run hotter
These slides show higher levels of immature character take longer to attenuate with the vapour condensing further down
the worm so that there is more spirit
Maturation effects - Maturation effects - vapour ‘conversation’.
exhausted cask highly active cask Then there is the generosity of the
cuts from foreshots to spirits and then
to feints. Whether there are separate
Character
Character
tanks for foreshots and feints and

Spirit

Spirit
the way these recoveries at different

Distillery Character B Distillery Character B ethanol concentrations react with the
Immaturity Immaturity still all have an effect. It has always
Time Time amazed a humble brewer how these
An exhausted cask will remove immaturity far more slowly than a reactive one unwanted compounds go round and
round the process yet somehow the
levels remain in balance and you do
Maturation effects - Maturation effects -
exhausted cask highly active cask not get the accumulated methanol
from operations since stills were
legalised in 1823!
Scotland is a relatively small area
Character
Character
Spirit

Spirit
compared to the United States or Canada

Maturity where temperatures can easily range
Distillery Character B Distillery Character B
Maturity
from 30oC in summer to -30oC in winter.
Eight thousand feet up in the Rockies in
Time Time
Colorado will see a 20% evaporative loss;
Similarly, the maturity level in an exhausted cask will build more slowly than in a highly there you will see casks covered in large
reactive one plastic sheets and misters trying to keep
the atmospheric moisture up. There
Maturation effects - Maturation effects - are over a hundred Coloradoan craft
exhausted cask highly active cask distillers, situated over 5000 feet above
sea level, tackling challenges unknown
at sea level but with many Americans
Character
Character
tracing their ancestry back to Scottish

Spirit

Spirit
immigrants, the draw to produce a tradi-

Distillery Character B Maturity
Immaturity tional Scotch is high indeed.
Immaturity
Maturity
Time Time Oak is big business
Putting the two effects together, you can see the slow loss of immaturity and the slow gain of The Scotch Whisky Association reckons
mature character in an exhausted cask compared to the more rapid reduction in raw flavour and there are 20 million casks matur-
increase in mature flavour to a higher level if the cask is more active ing spirit in Scotland. I am told that a

DISTILLATION l
commercial rental for a cask is around degradation products (such as vanillin, istic of aged product’. A 1976 patent
£15 per year. Applying that figure syringaldehyde and coniferaldehyde) from Belarus proposes that staves are
across the industry shows how storage provide floral, spicy, smooth, mellow placed in a vessel under vacuum for
alone amounts to a not inconsiderable attributes to flavour and aroma. Tannin half an hour to remove most of the air
sum. The whisky market worldwide is contributes to bitterness and astrin- from within; gaseous NH3 is introduced
around 11.5% of the total spirits market gency. Subtractive reactions include under a pressure of 1bar and the
(3127m 9L cases), so add the brandy evaporation of volatile compounds staves are held for 0.5-5 h at 20-35°C
and rum casks, all the wine casks and such as ethanol, acetaldehyde and in an alkaline medium, in which oxida-
even Tabasco, Worcestershire Sauce dimethylsulfide. tion with O2 is carried out at 20-35°C
and maple syrup barrels, you have an Oxidations involve ethanol to for 0.5-3 days. Excess NH3 is removed
awful lot of wooden containers. acetaldehyde and dimethylsulfide to under vacuum.
Today the brewing contribution is dimethyl sulfoxide and ethanolysis John continues: “From a Scotch
negligible with traditional producers like of acrolein to 1,1,3-triethoxypropane. whisky perspective, there are two prob-
St Austell, Wadworth and Sam Smiths Productive or interactive reactions lems with the first method. A big stick-
as well as kolsch makers in Cologne include oxidation of acetaldehyde to ing point is that most Scotch whisky
still using a few casks. It is thus hardly acetic acid, esterification of acetic acid is matured in used casks and this is
surprising that one of the earlier papers to ethyl acetate. Acetal formation from virtually impossible to mimic using oak
exploring rapid maturation appeared in acetaldehyde and ethanol, oxidation sticks. The chips provide a rapid and
a journal called Forestry back in 1985. and esterification of lignin degradation almost complete extraction whereas
Oak is a large industry. A tree might take products and water-ethanol interac- the physical structure of the stave plays
80-120 years growing tightly together to tions through hydrogen bonding lead- an important role in regulating the
ensure a tall straight trunk. The timber ing to the formation of stable clusters extractives that dissolve in the spirit.
below the first branch is taken and that of water and ethanol and an increase “Also, we have very limited informa-
might only yield enough wood to make in viscosity. Stable clusters of water tion on how wood extractives change
two or three casks. English oak is said and ethanol are thought to contribute over the course of maturation. Without
to be too knotty although that did not to the ‘mellowness’ of the spirit. this knowledge it is impossible to say
seem to bother Admiral Nelson and the Maturation enriches the sensorial whether the various methods in use
shipbuilders at Chatham Dockyard. characteristics of the product through accelerate these reactions, so what you
The vast majority of casks used for reduction of DMDS and DMTS from have added is extract and not mature
whiskey are sourced from the USA. grain and ‘nutty, cereal, oily or feinty’ character.
Stateside regulations demand that characters of new-make spirit. All this I have similar reservations about
whiskey be matured in a new cask, complexity suggests that any attempts the methods used to reduce immature
which leads to the availability of a at acceleration are not likely to deliver characteristics. “Again we do not know
large number of second-hand casks. an absolute match to any traditionally enough about these reactions to say
The Scotch industry has based its matured product. whether they are accelerated by the
strategy around this continuous supply. John Conner, the Scotch Whisky various methods. Increasing the energy
Another April 1st post in 2014 sug- Research Institute’s maturation guru input in whatever form or the use of
gested that Diageo and Brown Forman divides the approaches into three. catalysts may not just accelerate reac-
were tussling with US regulators (The First is what amounts to the addition tions that would naturally have taken
Alcohol and Tobacco Tax and Trade of wood extracts and this can take a place, but the chemist in me can’t help
Bureau – TTB) over the definition of multitude of forms depending on the thinking it could help others over
Tennessee whiskey with B-F wanting required character: American v French their activation energy barrier
to allow the second use of a cask. oak, the degree of toast, staves, cubes and put in motion reactions that
This would solve any US cask or chips and whether soaked in wine. wouldn’t normally occur.”
shortages but the supply of cheap The use of ultrasonics is simply a IBD whisky tutor Brian Eaton
casks for Diageo’s 30 Scottish plants way of increasing the rate of extrac- adds: “There are other matura-
would dry up – putting pressure on us- tion. The second camp concentrates on tion effects that cannot easily be
ing casks more economically. A scary the removal of immature characters mimicked – the loss of volatiles
spoof perhaps, but could it happen? and a variety of techniques appear to and oxidation. This was shown
be used – activated charcoal, light and
Speeding things up metal catalysts.
We have had a thorough look at the Lastly there are one or two patents
challenges of more traditional cask espousing the ammonium ion but Dr
maturation, so how can this be accel- Conner is at a loss to think of any rea-
erated? Imitating maturation is rather son this would promote a naturally oc-
challenging in view of complex multi curring reaction. The patent describes
stage and subtle processes. A quick the background as ‘alkaline distillation
recap might be helpful. causing protein hydrolysis and amino
During maturation, additive, sub- acid deamination, the resulting NH3+
tractive and productive mechanisms ions react with the naturally present
operate which change the colour and aldehydes to form ammonium alde-
the flavour of the new-make spirit. The hydes. These in turn enter into aldol
Tuthilltown Distillery in New York State were early
main groups of compounds extracted condensations with the esters and/ exponents of maturation in smaller casks using 3, 5, 10 and
by spirit from oak are hemicelluloses, or the congener molecules to give the 14 gallon barrels. Even the bottle for its Baby Hudson is
lignins, tannins, and lactones. Lignin complex aldehyde mixture character- small at 375mL

l DISTILLATION
ture identical or artificial and referred

to as GRAS (Generally Recognised
as Safe). Several of the components
imitate the composition of congeners
formed during fermentation which
would be released into the spirit.
These would be esters notably ethyl
acetate ethyl caproate, ethyl caprylate,
ethyl caprate, ethyl laurate, isoamyl
acetate and phenylethyl acetate,
which impart diverse fruity and flow-
ery notes. Small amounts of other
chemical compounds such as higher
alcohols/fusel oils, fatty/organic acids
and aldehydes are also incorporated to
provide a balanced product character
and palate appeal.
Flavour houses can supply treat-
ments containing some of the critical
components developed during the
maturation process such as furfural,
vanillin, lactone, eugenol, guaiacol etc,
but incorporating tannin and phenolic
aldehydes such as coniferaldehyde,
sinapaldehyde and syringaldehyde
in appropriate proportions is often a
limiting factor.
Staves, cubes and chips

Innerstave products are typical of oak inserts: Most accelerators will use wood in the
staves installed in a vessels, a fan of slats for form of staves, cubes or chips. There
suspension in a cask, a nylon bag of ‘blocks’, a is a choice of oak and toasting. Andre
chain of toasted laths fits into the barrel and Alcarde at Brazil’s Sao Paulo University
oak cubes
tested chips with cachaça and found it
pop-up all over the country they also made no difference whether the oak
adapted this method. Ralph and Gable was American or European but toast-
Erenzo at Tuthilltown Distillery started to ing levels did. Wood to make a matrix
use three- and five-gallon casks allowing of staves within a tank or just cubes or
a few years back with shrink-wrapping them to bring their Hudson Baby Bour- chips are available from Independent
of casks in Scotland with the aim of bon whiskey to a colour and taste profile Stave, Oak Wise and Innerstave.
minimising alcohol loss – the whisky at a decent level in under six months. A This latter company, based in Cali-
did not mature well. It has also been lot of distillers are using the micro-oxy- fornia, is typical, with a choice of oaks
found recently that stacking casks genation method – again inspired again and toast levels – toasted staves can
on pallets instead of on their bel- from the wine industry. Those micro- be mounted inside tanks where 1.7 m2
lies increases the time required for oxygenators are not that expensive to will mimic a 225L cask, they can be in
maturation by about a month per year, buy. They pump medical oxygen into the the form of a fan of 22 laths measuring
presumably due to poorer air flow barrels in intervals to oxidise the spirit 28x2x5/16” which can be dangled in on
around the cask. So it is not just about like it would over the years. a chain. Shorter laths can be drilled
adding wood character.” Another method is the pressure and linked so that a chain of 17 can
cooker invented by Tom Lix at Cleve- be used and each mimics a third of a
What has been tried? land Whiskey. He puts some wood barrel. Half-inch cubes suspended in a
There are lots of cautions out there but chips and staves in his spirit in a big nylon mesh bag with a drawstring and
perhaps you would expect those con- pot and alternates the pressure low a sack with 6.3m2 surface will treat 600
nected with an industry where there is and high over several days.” gallons within the year. Chips the size
tremendous heritage and a strict legal Smaller casks alter the surface to of broken matchsticks are used at 10
time limit to be apprehensive but let’s volume ratio. Buffalo Trace reported to 20 pounds per 600 gallons, they too
see what has been tried. Bozzy Karasu back in 2012 that trials with small can be contained in a nylon bag.
takes up the story: “To start with, using casks (5, 10 and 15 gallons) over six Infusion Spirals, part of the Barrel
any cask size smaller than standard years were not successful citing a lack Mill Cooperage, increase the surface
53-gallon barrel is for one goal only: of depth of flavour. area by milling a spiral configuration
accelerated maturation. It is a method At the budget end of the market in into 48-inch long poles around 30mm in
perfected over the years in the wine India, commercial flavours are added diameter. Five in a mesh bag will treat
industry and they have been pretty to molasses-based neutral spirit to 1000 gallons. Nine-inch lengths can
successful with it. make cheaper whiskies. These added form a chain inside a long nylon bag
When craft distilleries started to flavours are classified as natural, na- and six of them are said to mature 70

DISTILLATION l
day inside a bottle of neutral spirit to with a cask of the

make a passable whisky. You can buy a same brew flown
750mL oak bottle from Amazon to keep out from Burton.
your vodka in and surprise granddad In the whiskey
at Christmas! Thousand Oaks Bar- world, Jefferson
rels in Virginia will make you a cask Bourbon recreated
from one litre size upwards and also the route used 150
supply a range of essences if you really years ago from
want to cheat! Independent Stave can Louisville down the
make casks with up to five different Mississippi across
types of oak wood to give you the best to Florida and north
of all woody worlds and Makers Mark to the East Coast –
offers private customers the chance and went on to take
to formulate their own barrel in a new a cask between five
program called Private Barrel. continents cross-
A number of distillers use chips ing the equator
within a conventional cask. Copper Fox four times to see
in Virginia which incidentally floor-malts whether ten months
its own barley, pops a mesh bag of oak on water would en-
Joe Paglioni’s Oak Bottle claims to ‘infuse’ and apple chips into the bourbon barrel hance seven years
spirits with the same amount of flavour as
with the whiskey. After the year, the chip in a warehouse on C&C Shine’s Californian moonshine
lengthy barrel ageing
bag is removed and reused, then the dry land. (from a Kentucky recipe) came with
gallons. Different oak sources and toast- whiskey is transferred into another bar- French whiskey a toasted oak rod. This is placed in
ings can be used together. The company rel which is heated and then rolled, still maker Black Moun- the bottle which can be regularly
also makes smaller diameter spirals hot, to ensure that the alcohol achieves tain strapped a 280L tasted to assess how long it takes
which can be inserted into bottles. maximum penetration into the charred cask to the deck of a to obtain the wood flavour you like
Time and Oak sell small toasted internal layers of the barrel. After sailing vessel which took tourists around
sticks branded Whiskey Elements cooling, the process is repeated several the Bay of Biscay. It was on board for six
which are cut to increase surface area times over the next few months until the months. A 300L cask of Jack Daniel’s
and apparently need only to spend a spirit is ready for bottling cocktail as formulated by the Savoy in
London was on the open deck of the
The effect of long journeys Queen Mary II for a 41,000mile trip lasting
Agitation could be a factor. There have four months. Last year Suntory put some
been various publicity stunts like Pete whisky (not in barrels) on the Interna-
Brown trying to take a cask of Burton tional Space Station in a maturation
IPA to Calcutta until it disgorged its experiment echoing the Ardbeg exercise
contents all over his hotel room in which kept vials of Islay congeners grav-
Brazil. The idea was to take the beer ity free for three years. The continuing
on a six-month journey and compare it saga allowed the release of several top
end offerings celebrating the 90-min-
ute circumnavigation of the weightless
Time and Oak claims its Whiskey Elements containers – we await the results.
sticks add the effects of three years of ageing Going not quite as high we have
to any whisky in just 24 hours seen Montanya Rum matured at 8,900
feet up in the Rockies inspired by some
Columbian rum which was kept at
17,000 feet. A day at Crested Butte in
Colorado can see temperature fluc-
Oak spirals from Infusion Spirals… tuations of 40oC! Meanwhile, Cayman
Spirits Company’s Seven Fathoms
Rum matures at a depth of 42 feet
under the Caribbean Sea. The motion
of the tides gently rocks the casks
and the company keeps the location a
closely guarded secret.
We know the wood ‘breathes’
allowing oxygen and other molecules
out, so is the micro movement allow-
ing the layer of liquid close to the stave
to mix with the body of the cask and
avoid concentrations which might slow
reactions. How many distillers roll
their casks before sampling? Is there
A bottle spiral kit you can use in spirits, beers a concentration gradient in the liquid
or cocktails or oak chips from Add Oak towards the wood surface?

l DISTILLATION
Agitation in action. reheated to 60-75oC to finish off the

operation.
Terrapure from Terrassentia based
in South Carolina makes claims for a
similar system which uses ultrasonics
and pumps new-make through an oxy-
genated chamber. It offers own-label
spirits to some 50 hotel and restaurant
chains but details of the actual process
are currently rather vague.
The Allegro process from Kairos
Global also offers a reaction vessel un-
der controlled temperature and oxida-
tion conditions passing spirit through
a comminuted wood matrix. Kairos
offers a service to match the ethyl
Jefferson took two casks from Louisville to New York by sea and then took another cask acetate in a matured product which
on a voyage visiting all continents crossing the equator four times. Seven Fathoms from might take four years by incorporating
the Cayman Islands is matured 42 feet down in the Caribbean an addition into the reaction.
The wine industry has tried passing
Listen to the music Thea One electric currents in the presence of
The boys at Tuthilltown There are a number of patents for oxygen through young acidic red wine
also installed sub-bass ultrasonic treatments to hurry the and reported more mellow and aro-
speakers into their molecules along a bit but apart from matic results. Three minutes produced
warehouses to give the Terrapure, tests do not seem to have the best wine while anything over eight
barrels some rumble got beyond the laboratory bench. There yielded a product worse than the con-
so that the magic at is one high-energy input system which trol. Pulsed electric currents have also
the air, wood and spirit is causing a bit of a stir despite the shown encouraging results. Rice wine
interfaces can be en- inventor getting a pretty rough ride at has been reportedly enhanced by both
hanced. Copper and Kings, an ADI symposium. γ-radiation and ultrasonic treatments.
a brandy distillery in Kentucky says its Bryan Davis has spent years inves- Any application to spirit maturation
casks prefer the works of Lenny Krav- tigating the aging of spirits. He first has yet to be published.
itz, The Doors and Bruce Springsteen founded an absinthe operation in Spain Bozzy gets the last word: “I have
to stretch their pores. New Zealand gin and moved back the States to make tasted hundreds of spirits that went
maker Rogue Society has also experi- whiskey at a plant called Lost Spirits through accelerated aging one way
mented using a local band and you get beside the Pacific at Monterey. He had or other; they have a different taste
a CD of the ‘music’ when you buy the a wooden still, obviously steam heated, profile you can get right away. But it is
Electric Wire Hustle X Rogue Society and the worm passed through his not necessarily bad. Anyway, they do
Gin Limited Edition. swimming pool so that he could have a taste different – exactly like small bar-
relaxing dip after the run! rel wines do. Distillers should not try
With the help of crowd funding he to match the flavour profile of longer
launched Lost Spirits Technology and maturation periods of Scotch distiller-
built a portable reactor which claims ies. It is a fight they cannot win. Noth-
to make a good quality spirit in just six ing can replace longer maturation in
days. He has impressive GC-MS charts bigger barrels in milder climates. They
to show that the peaks are all in the use a different method which leads to
right places. His board boasts some a different taste.
retired industry heavyweights, there “Be OK with it, craft distillers have
are five prototype installations chris- a six-month old whiskey matured in
tened Thea One in operation and he a different way and tastes different.
is in talks with another 65 distilleries It is a new product, maybe a new cat-
looking at forming a partnership. Thea egory – and they should work on how
One will produce over 500L of ‘20yo’ to make that unique product better. I
each week. think we have all learned that in this
New-make spirit and oak chips industry, we cannot replace time with
are put in the reactor. The process smart ideas.”
first involves a heating spell under
just 6psi top pressure at tempera- Acknowledgements
tures between 60-75oC. The spirit is The author would like to thank Bill
cooled and subjected to light ra- Owens, Margarett Waterbury, Gra-
diation from 400-1000nm passing ham Stewart, James MacTaggart,
over 2m lux hours. Putting a carboy Ian Palmer, Alan Winchester, Gary
Colonial American Inspired Rum at 62%ABV from the Lost in a Californian greenhouse for a Spedding, Binod Maitin and Douglas
Spirits Distillery in California – oak matured in the Lost week would pass just over 4m lux Murray for helpful direction during the
Spirits reactor (inset) hours. The light treated spirit is then preparation of this article.

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● BIOCHEMISTRY

Way through the wood

By Ian Hornsey generally being used for ageing being

U ntil the advent of plastic, wooden

bilge hoop chime

Parts of a cask Ceramic dolia, used to ferment and store wine

48 z Brewer and Distiller International April 2016 www.ibd.org.uk

to casks filled with firewood pitch and

www.ibd.org.uk Brewer and Distiller International April 2016 z 49

Cooperages of different ages

Wooden hoops; Northern Europe, 16th century

50 z Brewer and Distiller International April 2016 www.ibd.org.uk

major cell-wall components extractives

lignin hemicellulose cellulose phenolics fatty acids other extractibles

guaiacyl & hexoses, hexose: polyphenols simple phenols lactones

Oak heartwood components

www.ibd.org.uk Brewer and Distiller International April 2016 z 51

Tannins ellagitannins have been characterised in oak wood; castalagin;

hydrolysable tannins complex tannins condensed tannins

Recent advances in tannin chemistry have seen a reassess-

52 z Brewer and Distiller International April 2016 www.ibd.org.uk

likelihood of cask leakage and extract

www.ibd.org.uk Brewer and Distiller International April 2016 z 53

and heavy), an increase in concentra-

54 z Brewer and Distiller International April 2016 www.ibd.org.uk

by high levels of eugenol, 2-phenyle- acacia, cherry and mulberry (in

www.ibd.org.uk Brewer and Distiller International April 2016 z 55

Much has been researched

W ith this article I hope to provide

key element in the process of mak-

22 ❚ Brewer and Distiller International May 2015 www.ibd.org.uk

www.ibd.org.uk Brewer and Distiller International May 2015 ❚ 23

the maturing whisky. tion. Initially these casks were broken

24 ❚ Brewer and Distiller International May 2015 www.ibd.org.uk

ing maturation, this well known ﬁlter

www.ibd.org.uk Brewer and Distiller International May 2015 ❚ 25

whisky maturation process. Generally ditional ﬁlling stores and warehouses

The cooper – a master craftsman.

26 ❚ Brewer and Distiller International May 2015 www.ibd.org.uk

employed in Scotland compared to the

www.ibd.org.uk Brewer and Distiller International May 2015 ❚ 27

Is the oak industry under threat

Moving things along

By Roger Putman fortune, perhaps we should consider

H ence there has been a lot of inter-

36 z Brewer and Distiller International November 2016 www.ibd.org.uk

Brown spirits of course start off

www.ibd.org.uk Brewer and Distiller International November 2016 z 37

teraction and masking of low flavour heated elements provides a similar if

38 z Brewer and Distiller International November 2016 www.ibd.org.uk

www.ibd.org.uk Brewer and Distiller International November 2016 z 39

Maturation in action it wasn’t and the spirit was not ready

Distillery Character Interactive

perature, wort oxygenation and period

Distillery Character A Distillery Character A

for reaction is increased dramatically.

tanks for foreshots and feints and

Distillery Character A Distillery Character A

the way these recoveries at different