Kris Arvid Berglund
University Distinguished Professor of Forestry and Chemical Engineering
Michigan State University
East Lansing, MI 48824 USA and
Professor of Biochemical &
Chemical Process Engineering
Luleå University of Technology
SE971 87 Luleå SWEDEN

MSU/ LTU ARTISAN DISTILLING PROGRAM
• Established to promote the establishment and expansion of artisan distillers
• Activities include: education, service, and research
• Designed as a dedicated program for distilled spirits

FACILITIES
• Michigan Brewing Company-houses program, alternating premises license
• A150l Christian Carl still equipped with a three tray side column and a packed column is for high rectification work. (120l to be added at LTU)
• A 450l Christian Carl still for stripping and botanicals
• An 800l, 38-tray Christian Carl still (on line in March
2009)
• A 10l Christian Carl still for experimental work
• Comprehensive analytical instrumentation: GC,
HPLC, Anton Paar DMA 5000 densitometer

EDUCATIONAL ACTIVITIES
• Workshops- two day
– MSU, Webberville, MI
– WSU, Mt. Vernon, WA
– Cornell University, Geneva, NY
• Coursework at MSU, CHE 491
• Book entitled, “Artisan Distilling” on CD-
ROM, internet download (free) at www.artisandistilling.org

RESEARCH ACTVITIES
• Develop quality indicators- congener monitoring and control
• Control of regulated compounds
• Yeast screening for congeners
• Activated carbon finishing

• The agency that licenses at the Federal level is Alcohol and Tobacco Tax and
Trade Bureau, the Department of Treasury
(TTB), not the Bureau of Alcohol, Tobacco and Firearms, the Department of
Homeland Security (BATF).
• All spirits are defined in the Code of
Federal Regulations-27 CFR Part 5.21
• Make sure anything you wish to make is defined!

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Class 1; neutral spirits or alcohol.
Class 2; whisky.
Class 3; gin.
Class 4; brandy.
Class 5; blended applejack.
Class 6; rum.
Class 7; tequila.
Class 8; cordials and liqueurs.
Class 9; flavored brandy, flavored gin, flavored rum, flavored vodka, and flavored whisky.
Class 10; imitations.
Class 11; geographical designations.
Class 12; products without geographical designations but distinctive of a particular place.

DISTILLATION- MOTIVATION
• Concentrate aromas, flavors, and alcohol
• Several operational parameters possible
• Remove the negative compounds

• A process involving an equilibrium between two phases - liquid and vapor.
• For a pure compound, a sharp boiling point usually exists.
• For a mixture, however, a phase equilibrium exists over a range of temperatures.

UNIQUE VLE OF ETHANOL-
WATER SOLUTIONS
• For ideal mixtures, the mvc is always at a higher concentration in the vapor phase than the lvc
• The boiling point of the mixture should be a continuously increasing value as the concentration of the lvc is increased
• This is not the case for ethanol-water
• The boiling point has a minimum value for a mixture
• This is called a minimum boiling azeotrope

Boiling Point Diagram
101
96
91
86 mixture vapor
DEW CURVE
81
BUBBLE CURVE liquid
76
0 0.2
0.4
0.6
Mole Fraction
0.8
1

Boiling Point Diagram Near Azeotrope
80
79.8
79.6
79.4
79.2
79
78.8
78.6
78.4
78.2
78
0.5
0.6
0.7
AZEOTROPE
0.8
Mole Fraction
0.9
1

Ethanol Water VLE
1
0.8
0.6
0.4
0.2
0
0
INCREASING TEMP.
0.2
0.4
0.6
Liquid Mole Fraction EtOH
0.8
1

COMPARISON
OF UNITS- MOLE,
WEIGHT, AND
VOLUME FRACTIONS
1
0.8
0.6
0.4
0.2
0
0
EtOH Water VLE
VOLUME
WEIGHT
MOLE
0.2
0.4
0.6
Liquid Phase
0.8
1

• Simple batch- no rectification
• Alambic- some rectification
• Column- active rectification

BATCH DISTILLATION
• Use “cuts”
• “Heads”- remove acetaldehyde, methanol
• “Hearts”- product rich in aromas and flavors
• “Tails”- fusel oils, dilute

RECTIFICATION- EQUILIBRIUM
CONTACT
• Rectification is the result of equilibrium contact between two phases
• The liquid and vapor leaving the contact are in equilibrium
• Rectification, also called enrichment, results in a higher concentration than would occur in a single equilibrium contact
L n-1
, x n-1
L n
, x n
V
V n
, y contact n+1 n
, y n+1 n

SIMPLE BATCH (RAYLEIGH)
DISTILLATION

Ethanol Water VLE
1
0.8
0.6
0.4
0.2
0
0
2
1
0.2
0.4
0.6
Liquid Mole Fraction EtOH
0.8
1

Boiling Point Diagram
101
96
91
86
81
76
0 mixture
0.2
2 vapor
1 liquid
0.4
0.6
Mole Fraction
0.8
1

DIRECT FIRED STILL (ALAMBIC)
Some vapor condenses to liquid and returns to the pot

INDIRECT STEAM HEATING
(ALAMBIC)
Some vapor condenses to liquid and returns to the pot
Steam
Figure courtesy of
Christian Carl Ing. GmbH

INDIRECT HEATING WITH
RECTIFICATION
INCREASING
TEMPERATURE
DOWN THE
COLUMN,
HIGHEST
TEMPERATURE
IS IN THE POT
Figure courtesy of
Christian Carl Ing. GmbH

•
Figure courtesy of
Christian Carl Ing. GmbH

Top View
SIEVE TRAY
Condensed
Liquid
Vapor
Side View
Condensate Return

BUBBLE CAP TRAY
Condensed
Liquid
Vapor
Condensate Return

BATCH COLUMN STILL
Partial condensor
D, x
D
L
Reflux ratio
R

L
D
Boiler

Ethanol Water VLE
1
0.8
0.6
0.4
1
0.2
2
3
4
5
6
0
0
X
FEED 0.2
0.4
0.6
Liquid Mole Fraction EtOH
0.8
x
DIST 1
The number of trays needed for a specific separation is determined by stepping off……..

Boiling Point Diagram
101
96 vapor
91
86
81
76
0 mixture
0.2
1
2 liquid
0.4
0.6
Mole Fraction
3
4
5
0.8
1

Ethanol Water VLE
1
0.8
0.6
0.4
1
1
2
2
3
3
0.2
0
0 0.2
0.4
0.6
Liquid Mole Fraction EtOH
0.8
1
If the reflux ratio is constant, the product concentration will decrease during the batch

Ethanol Water VLE
1
0.8
0.6
0.4
1
1
2
2
3
3
0.2
0
0 0.2
0.4
0.6
Liquid Mole Fraction EtOH
0.8
1
Since the concentration in the pot decrease during a bath, in order to keep the product concentration high, the reflux must be increased

REFLUX IS INCREASED BY INCREASING COOLING
WATER FLOWRATE TO PARTIAL CONDENSER
TEMPERATURE
SENSOR
WATER TO
CONDENSER
T
Figure courtesy of
Christian Carl Ing. GmbH

FLAVOR COMPOUNDS (CONGENERS) IN
DISTILLED SPIRITS
2200
2000
1800
1600
1400
1200
1000
Methanol
Higher alcohols
Carbonyl compounds
Ethyl acetate
Other esters
800
600
400
200
0
Fr en ch
C og na c
W in e al co ho l
Po m ace Plu m
M ira be lle
C he rry
W ill ia m s
Po m e
C al va
G er m an do
ra s sp be rry
Fr en ch
ra
U
Ssp be rry bo n-
W hi sky hi ske y
Bo ur tch
B le nd ed
W
Sco
G in
Vo dka

TYPICAL COMPOUNDS BY GC
Chemical Name RetentionTime (min) Boiling point (deg. C)
Acetaldehyde 2.5
20.8
Acetone
Ethyl Formate
Ethyl Acetate
3.4
3.6
4.5
56.2
54.0
77.0
Methanol
Ethanol
1-propanol
Isopentanol
4.7
5.8
8.7
64.7
78.0
97.0
(isoamyl alcohol)
Benzaldehyde
16.3
33.0
132.0
179.0

1000 t s l o m v
500
0
0
50
Methanol
Ethanol
Ethanol t l s m v o 25
Acetone
Acetaldehyde
1-Propanol
0
0
Isoamyl Alcohol
Ethyl Acetate
5
Minutes
Benzaldehyde
1-Propanol
10
20
Minutes
30 40
10

ETHANOL RESULTS FROM PLUM
DISTILLATION
90
HEADS HEARTS TAILS
80
70
60
50
0 2000 4000
Distillate Volume (mL)
6000 8000

CONGENER CONCENTRATIONS IN
PLUM DISTILLATES
0.45
Congener Concentration vs Distillate Volume
HEADS
2 Trays with Catalytic Converter
HEARTS TAILS
0.60
0.20
0.15
0.10
0.05
0.00
-0.05
0
0.40
0.35
0.30
0.25
1000 2000 3000
Distillate Volume (mL)
4000 5000
0.35
0.30
0.25
0.20
0.15
0.10
0.55
0.50
0.45
0.40
Acetaldehyde
Ethyl Acetate
1-Propanol
Iso Amyl Alcohol
M ethanol

CONTACT
Prof. Kris Arvid Berglund
Email: berglund@msu.edu
Email: kris.berglund@ltu.se
www.artisandistilling.org

• Christian Carl Ing. GmbH
• Project GREEEN, State of
Michigan
• Michigan State University
• Luleå University of Technology