Distilled Alcoholic Beverages – Distilled Spirits

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DISTILLED ALCOHOLIC BEVERAGES

DISTILLED SPIRITS

Ethanol

Colorless
mixed with water in every ratio.
Density = 0.79 g/ml at 20 C.
energy of combustion 7000 kcal/kg
boiling point is 78.31 C
85% metabolized in the liver, remaining 15 % lost by respiration, sweating and urination
etheric oils in ethanol is related with its poisoning effect
lethal dosage is 3 g ethanol / kg body weight

Methanol

Flammable
Colorless
Heat of combustion: 5360 kcal/kg.
mixed with water, and ethanol in every ratio.
During alcohol fermentation

Pectin Methanol

Pectinesterase ( opt. PH =5-6)
When pH is reduced, formation of methanol is reduced.
Heating fruit must to 85 C for 90 minutes reduces methanol formation by 40-90 %.
Methanol is poisonous for human
almost impossible to produce methanol free drinks.

Factors that cause to increase methanol content of alcoholic beverages are;

insufficient heating of must
some contaminating molds ( ie Batryis cineroe ) breakdowns pectins
existence of heat resistance pectinesterases
if must contacts more with skin and stem, methanol production will increase
In the body, methanol is converted to formaldehyde first and than formic acid, which is poisonous.
Methanol is less effective to make people drunk compared to ethanol.
It is a very good solvent for lipids, so it quickly affects control nervous system and eyes.
Limiting values for methanol is; < 0.35 % at USA and 1.5 % at EC and in Turkish drinks less than 0.3 %.
Nitrosamines and ethyl carbamate are natural carcinogenic compounds, which develop during the kilning and distilling processes respectively.
Very low levels of nitrosamines are specified (none or 1 ppb max.).
Glycosidic nitrile is also specified at very low levels (3.0 g t−1 of malt) because it is the precursor of ethyl carbamate.

Factors affecting ethanol fermentation :

-oxygen ( during initial stage of fermentation aeration is necessary )
-CO2 ( if P CO2 is too high ( ie 20 atm ) fermentation completely stops.
-temperature ( 25-30 C is good for microbial growth but 30-37 C are better for ethanol production )
-pH ( weak acidic medium is good for ethanol production, optimum pH is 3.8-4.2 )
-inoculation rate ( 1-2 % is optimum )
-sugar concentration ( culture should stand very high osmotic pressure )

Distillation

simple distillation : ( single stage batch distillation , equipment is called still, imbik in turkish)
10 % ethanol 32.7 % 58.3 %
1st distillation 2nd 3rd
74.8 % 83.2 % 87.3 % ethanol
4th 5th
Continuous ( column ) distillation: Better separation of higher alcohol occurs due to higher ethanol concentration an specific decantators used.)
After distillation residual material with no alcohol left is called as stillage (şilempe in Turkish)
We can not produce ethanol with concentration over 97.2 % because we get azeotrope formation at that concentration ( where Tx and Ty lines intersects, xi =yi, on temperature % ethanol graph.

Absolute ethanol production

Interactions between the components of the solution create properties unique to the solution, as most processes entail nonideal mixtures, where Raoult’s Law does not hold.
Such interactions can result in a constant-boiling azeotrope which behaves as if it were a pure compound (i.e., boils at a single temperature instead of a range).
At an azeotrope, the solution contains the given component in the same proportion as the vapor, so that evaporation does not change the purity, and distillation does not effect separation.
Ethanol and water form an azeotrope of 95% at 78.2°C.
there exist some techniques to break the azeotrope to give a pure distillate.
This set of techniques are known as azeotropic distillation.
by “jumping” over the azeotropic composition (by adding an additional component to create a new azeotrope, or by varying the pressure).
Others work by chemically or physically remove or sequester the impurity. For example, to purify ethanol beyond 95 %, a drying agent or a dessicant such as potassium carbonate can be added to convert the soluble water into insolublewater of crystallization .

Alcohol yields from different substrates

100 kg substrate ethanol (liter)
sucrose 58-64
molasses 29-32
sour cherry 5-8
apple 5-7
fresh grape 8-12
raisin 31-37
fig(dried) 30
starch 60-66
rice 42-47
wheat 37-41
potato 10-14

Alcohol scales used

Gay-lussac English proof American proof
EU,Turkey (sikes)
10 17.5 20
20
30
40
50 87.5 100 (you can have flame with it )
60
100 175 200 (pure ethanol)
Distilled alcoholic drinks(> 15 % ethanol) also called as distilled spirits or spirits
Distilled alcoholic beverages can be classified as;
aged ones ( usually more than a year ) : brandy, cognac, whisky, rum , arak
not aged ones : rakı, gin, vodka, snaps, tekila, mescal

RAKI PRODUCTION

It is called araki in Arabic, means one that makes you sweat.
Aniseed ( Pimpinella anisum ) is added to ethanol from agricultural products goes through distillation.

Main component of etheric essence of aniseed is anethol.

It is white colored solid at room temperature, does not dissolve in water, requires organic solvent. That is why when we add water to dilute rakı, it becomes white.

Ouzo :Greek drink with aniseed
Anis : French rakı
Gin: Produced from barley malt and corn and flavored with Juniper berries which is fruit of Juniperus communis tree ( ardıç in Turkish)

VODKA

The word vodka or wodka means ‘little water’. It is derived from the Russian word voda. Today the Russians refer to it as vodoshka
fairly tasteless, neutral spiritfrom the fermentation and distillation of grain.
other raw materials; potatoes, sugarbeet, grapes, or cassava .
producers ; own, secret, ways of filtering concerned about the contact time of the spirit with the charcoal.
a single filter or a series of filters.
The choice of charcoal affects the final product.
regenerate the charcoal using steam or discard

European Community, the minimum alcohol 37.5% (vv),

higher-strength vodkas from eastern Europe, e.g., 45–55%.

Turkish vodka : 40 % ethanol ( from barley malt + grain or potato ) + 3 g / sugar + 0.1 % ethylacetate

RUM

the fermented products of sugarcane (Saccharum spp.), that is to say fresh juice, molasses (the thick brown liquid separated from raw sugar at the end of the sugar manufacturing process), and syrup obtained from sugarcane juice concentration
The fermented liquid must be distilled under 96% ethanol
Rum was first a drink for slaves and seamen.
Jamaica, Cuba and Portorico
in the 1980s ; most consumed drink ( in front of whisky and vodka)
Nowadays, after vodka and whisky, rum is the third spirit consumed through the world
Light rum, of which Bacardi is the market leader
More than 95% of the rum produced in the world is derived from molasses
Light ( silver ) rum; short aging, filtering to remove color after aging
Agricultural Amber(Gold) Rum:
Amber rum is stored for 18 months in oak tun
Agricultural Aged(Dark) Rum:
Dark Rum (Rhum Vieux), in an oak barrel a minimum of 3 years ( up to 6 years)
solera’
BRANDY
Initially wine was distilled as a preservation method and as a way to make the wine easier for merchants to transport.
It was also thought that wine was originally distilled to lessen the tax which was assessed by volume. The intent was to add the water removed by distillation back to the brandy shortly before consumption.
It was discovered that after having been stored in wooden casks, the resulting product had improved over the original distilled spirit.
the distillation process leads to the formation and break-up of dozens of aroma compounds fundamentally altering the composition of the distillate.
This is why unaged wine spirits (unaged brandy) diluted back to wine alcohol strength tastes nothing like the original wine.
Grape brandy
four main subtypes of grape brandies.
Cognac comes from the Cognac region in France, and is double distilled using pot stills. Aged > 2.5years
VS (Very Special) or *** (three stars), stored at least two years in cask.
VSOP (Very Superior Old Pale), stored at least four years in cask.
XO (Extra Old), stored at least six years in cask.
Armanac is made from grapes of the Armagnac region in Southwest of France .It is single continuous distilled in a copper stills and aged in oak casks
kanyak (in Turkish)

produced at Çanakkale factory. Yapıncak, dökülgen and karasakız type grapes are used. Small amount of pekmez, tartaric acid and vanillin is added. ( 41 % ethanol )

…

DISTILLED ALCOHOLIC BEVERAGES

DISTILLED SPIRITS

Ethanol

Colorless

mixed with water in every ratio.

Density = 0.79 g/ml at 20 C.

energy of combustion 7000 kcal/kg

boiling point is 78.31 C

85% metabolized in the liver, remaining 15 % lost by respiration, sweating and urination

etheric oils in ethanol is related with its poisoning effect

lethal dosage is 3 g ethanol / kg body weight

Methanol

Flammable

Colorless

Heat of combustion: 5360 kcal/kg.

mixed with water, and ethanol in every ratio.

During alcohol fermentation

Pectin Methanol

Pectinesterase ( opt. PH =5-6)

When pH is reduced, formation of methanol is reduced.

Heating fruit must to 85 C for 90 minutes reduces methanol formation by 40-90 %.

Methanol is poisonous for human

almost impossible to produce methanol free drinks.

Factors that cause to increase methanol content of alcoholic beverages are;

insufficient heating of must

some contaminating molds ( ie Batryis cineroe ) breakdowns pectins

existence of heat resistance pectinesterases

if must contacts more with skin and stem, methanol production will increase

In the body, methanol is converted to formaldehyde first and than formic acid, which is poisonous.

Methanol is less effective to make people drunk compared to ethanol.

It is a very good solvent for lipids, so it quickly affects control nervous system and eyes.

Limiting values for methanol is; < 0.35 % at USA and 1.5 % at EC and in Turkish drinks less than 0.3 %.

Nitrosamines and ethyl carbamate are natural carcinogenic compounds, which develop during the kilning and distilling processes respectively.

Very low levels of nitrosamines are specified (none or 1 ppb max.).

Glycosidic nitrile is also specified at very low levels (3.0 g t−1 of malt) because it is the precursor of ethyl carbamate.

Factors affecting ethanol fermentation :

-oxygen ( during initial stage of fermentation aeration is necessary )

-CO2 ( if P CO2 is too high ( ie 20 atm ) fermentation completely stops.

-temperature ( 25-30 C is good for microbial growth but 30-37 C are better for ethanol production )

-pH ( weak acidic medium is good for ethanol production, optimum pH is 3.8-4.2 )

-inoculation rate ( 1-2 % is optimum )

-sugar concentration ( culture should stand very high osmotic pressure )

Distillation

simple distillation : ( single stage batch distillation , equipment is called still, imbik in turkish)

10 % ethanol 32.7 % 58.3 %

1st distillation 2nd 3rd

74.8 % 83.2 % 87.3 % ethanol

4th 5th

Continuous ( column ) distillation: Better separation of higher alcohol occurs due to higher ethanol concentration an specific decantators used.)

After distillation residual material with no alcohol left is called as stillage (şilempe in Turkish)

We can not produce ethanol with concentration over 97.2 % because we get azeotrope formation at that concentration ( where Tx and Ty lines intersects, xi =yi, on temperature % ethanol graph.

Absolute ethanol production

Interactions between the components of the solution create properties unique to the solution, as most processes entail nonideal mixtures, where Raoult’s Law does not hold.

Such interactions can result in a constant-boiling azeotrope which behaves as if it were a pure compound (i.e., boils at a single temperature instead of a range).

At an azeotrope, the solution contains the given component in the same proportion as the vapor, so that evaporation does not change the purity, and distillation does not effect separation.

Ethanol and water form an azeotrope of 95% at 78.2°C.

there exist some techniques to break the azeotrope to give a pure distillate.

This set of techniques are known as azeotropic distillation.

by “jumping” over the azeotropic composition (by adding an additional component to create a new azeotrope, or by varying the pressure).

Others work by chemically or physically remove or sequester the impurity. For example, to purify ethanol beyond 95 %, a drying agent or a dessicant such as potassium carbonate can be added to convert the soluble water into insolublewater of crystallization .

Alcohol yields from different substrates

100 kg substrate ethanol (liter)

sucrose 58-64

molasses 29-32

sour cherry 5-8

apple 5-7

fresh grape 8-12

raisin 31-37

fig(dried) 30

starch 60-66

rice 42-47

wheat 37-41

potato 10-14

Alcohol scales used

Gay-lussac English proof American proof

EU,Turkey (sikes)

10 17.5 20

20

30

40

Agricultural Amber(Gold) Rum:
Amber rum is stored for 18 months in oak tun

Agricultural Aged(Dark) Rum:
Dark Rum (Rhum Vieux), in an oak barrel a minimum of 3 years ( up to 6 years)