Kris Arvid Berglund

How Artisan Distillation Works Kris Arvid BerglundUniversity Distinguished Professorof Forestry and Chemical EngineeringMichigan State UniversityEast Lansing, MI 48824 USAandProfessor of Biochemical & Chemical Process EngineeringLule University of TechnologySE-971 87 Lule SWEDEN

MSU/ LTU ARTISAN DISTILLING PROGRAMEstablished to promote the establishment and expansion of artisan distillersActivities include: education, service, and researchDesigned as a dedicated program for distilled spirits

FACILITIESMichigan Brewing Company-houses program, alternating premises licenseA150l 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 botanicalsAn 800l, 38-tray Christian Carl still (on line in March 2009)A 10l Christian Carl still for experimental workComprehensive analytical instrumentation: GC, HPLC, Anton Paar DMA 5000 densitometer

EDUCATIONAL ACTIVITIESWorkshops- two dayMSU, Webberville, MIWSU, Mt. Vernon, WACornell University, Geneva, NYCoursework at MSU, CHE 491Book entitled, Artisan Distilling on CD-ROM, internet download (free) at www.artisandistilling.org

RESEARCH ACTVITIESDevelop quality indicators- congener monitoring and controlControl of regulated compoundsYeast screening for congenersActivated carbon finishing

Some definitionsThe 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 5.21Make sure anything you wish to make is defined!

Recognized classes of spiritsClass 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- MOTIVATIONConcentrate aromas, flavors, and alcoholSeveral operational parameters possibleRemove the negative compounds

DISTILLATIONA 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 SOLUTIONSFor ideal mixtures, the mvc is always at a higher concentration in the vapor phase than the lvcThe boiling point of the mixture should be a continuously increasing value as the concentration of the lvc is increasedThis is not the case for ethanol-waterThe boiling point has a minimum value for a mixtureThis is called a minimum boiling azeotrope

DEW CURVEBUBBLE CURVEvaporliquidmixture

Chart5

100100

95.595.5

8989

86.786.7

85.385.3

84.184.1

82.782.7

82.382.3

81.581.5

80.780.7

79.879.8

79.779.7

79.379.3

78.7478.74

78.4178.41

78.1578.15

78.378.3

Mole Fraction

Boiling Point, C

Boiling Point Diagram

Chart1

00

0.0190.17

0.07210.3891

0.09660.4375

0.12380.4704

0.16610.5089

0.23770.5445

0.26080.558

0.32730.5826

0.39650.6112

0.50790.6564

0.51980.6599

0.57320.6841

0.67630.7385

0.74720.7815

0.89430.8943

11

Sheet1

x EtOHy EtOHT Boiling

00100010010000

0.0190.1795.50.01995.595.50.0190.17

0.07210.3891890.072189890.07210.3891

0.09660.437586.70.096686.786.70.09660.4375

0.12380.470485.30.123885.385.30.12380.4704

0.16610.508984.10.166184.184.10.16610.5089

0.23770.544582.70.237782.782.70.23770.5445

0.26080.55882.30.260882.382.30.26080.558

0.32730.582681.50.327381.581.50.32730.5826

0.39650.611280.70.396580.780.70.39650.6112

0.50790.656479.80.507979.879.80.50790.6564

0.51980.659979.70.519879.779.70.51980.6599

0.57320.684179.30.573279.379.30.57320.6841

0.67630.738578.740.676378.7478.740.67630.7385

0.74720.781578.410.747278.4178.410.74720.7815

0.89430.894378.150.894378.1578.150.89430.8943

1178.3178.378.311

Sheet1

1

Liquid Mole Fraction EtOH

Vapor Mole Fraction EtOH

Ethanol Water VLE

Sheet2

Mole Fraction

Boiling Point, C

Boiling Point Diagram

Sheet3

AZEOTROPE

Chart7

79.879.8

79.779.7

79.379.3

78.7478.74

78.4178.41

78.1578.15

78.378.3

Mole Fraction

Boiling Point

Boiling Point Diagram Near Azeotrope

Chart1

00

0.0190.17

0.07210.3891

0.09660.4375

0.12380.4704

0.16610.5089

0.23770.5445

0.26080.558

0.32730.5826

0.39650.6112

0.50790.6564

0.51980.6599

0.57320.6841

0.67630.7385

0.74720.7815

0.89430.8943

11

Sheet1

x EtOHy EtOHT Boiling

00100010010000

0.0190.1795.50.01995.595.50.0190.17

0.07210.3891890.072189890.07210.3891

0.09660.437586.70.096686.786.70.09660.4375

0.12380.470485.30.123885.385.30.12380.4704

0.16610.508984.10.166184.184.10.16610.5089

0.23770.544582.70.237782.782.70.23770.5445

0.26080.55882.30.260882.382.30.26080.558

0.32730.582681.50.327381.581.50.32730.5826

0.39650.611280.70.396580.780.70.39650.6112

0.50790.656479.80.507979.879.80.50790.6564

0.51980.659979.70.519879.779.70.51980.6599

0.57320.684179.30.573279.379.30.57320.6841

0.67630.738578.740.676378.7478.740.67630.7385

0.74720.781578.410.747278.4178.410.74720.7815

0.89430.894378.150.894378.1578.150.89430.8943

1178.3178.378.311

Sheet1

1

Liquid Mole Fraction EtOH

Vapor Mole Fraction EtOH

Ethanol Water VLE

Sheet2

Mole Fraction

Boiling Point, C

Boiling Point Diagram

Sheet3

Mole Fraction

Boiling Point

Boiling Point Diagram Near Azeotrope

INCREASING TEMP.

Chart4

10

0.0190.17

0.07210.3891

0.09660.4375

0.12380.4704

0.16610.5089

0.23770.5445

0.26080.558

0.32730.5826

0.39650.6112

0.50790.6564

0.51980.6599

0.57320.6841

0.67630.7385

0.74720.7815

0.89430.8943

11

Liquid Mole Fraction EtOH

Vapor Mole Fraction EtOH

Ethanol Water VLE

Chart1

00

0.0190.17

0.07210.3891

0.09660.4375

0.12380.4704

0.16610.5089

0.23770.5445

0.26080.558

0.32730.5826

0.39650.6112

0.50790.6564

0.51980.6599

0.57320.6841

0.67630.7385

0.74720.7815

0.89430.8943

11

Sheet1

x EtOHy EtOHT Boiling

00100010010000

0.0190.1795.50.01995.595.50.0190.17

0.07210.3891890.072189890.07210.3891

0.09660.437586.70.096686.786.70.09660.4375

0.12380.470485.30.123885.385.30.12380.4704

0.16610.508984.10.166184.184.10.16610.5089

0.23770.544582.70.237782.782.70.23770.5445

0.26080.55882.30.260882.382.30.26080.558

0.32730.582681.50.327381.581.50.32730.5826

0.39650.611280.70.396580.780.70.39650.6112

0.50790.656479.80.507979.879.80.50790.6564

0.51980.659979.70.519879.779.70.51980.6599

0.57320.684179.30.573279.379.30.57320.6841

0.67630.738578.740.676378.7478.740.67630.7385

0.74720.781578.410.747278.4178.410.74720.7815

0.89430.894378.150.894378.1578.150.89430.8943

1178.3178.378.311

Sheet1

10

00

00

00

00

00

00

00

00

00

00

00

00

00

00

00

00

Liquid Mole Fraction EtOH

Vapor Mole Fraction EtOH

Ethanol Water VLE

Sheet2

00

00

00

00

00

00

00

00

00

00

00

00

00

00

00

00

00

Mole Fraction

Boiling Point, C

Boiling Point Diagram

Sheet3

COMPARISON OF UNITS- MOLE, WEIGHT, ANDVOLUME FRACTIONSVOLUMEWEIGHTMOLE

Chart2

000

0.410520.3430.17

0.694920.6190.3891

0.737560.6650.4375

0.763740.6940.4704

0.791960.7260.5089

0.815250.7530.5445

0.823760.76350.558

0.838880.7810.5826

0.855410.8010.6112

0.878850.830.6564

0.885990.8390.6599

0.892290.8470.6841

0.916910.8790.7385

0.933270.9010.7815

0.971920.9560.8943

111

Liquid Phase

Vapor Phase

EtOH Water VLE

Chart1

10

0.0190.17

0.07210.3891

0.09660.4375

0.12380.4704

0.16610.5089

0.23770.5445

0.26080.558

0.32730.5826

0.39650.6112

0.50790.6564

0.51980.6599

0.57320.6841

0.67630.7385

0.74720.7815

0.89430.8943

11

Sheet1

x EtOHy EtOHT Boiling

00100010010000

0.0190.1795.50.01995.595.50.0190.17

0.07210.3891890.072189890.07210.3891

0.09660.437586.70.096686.786.70.09660.4375

0.12380.470485.30.123885.385.30.12380.4704

0.16610.508984.10.166184.184.10.16610.5089

0.23770.544582.70.237782.782.70.23770.5445

0.26080.55882.30.260882.382.30.26080.558

0.32730.582681.50.327381.581.50.32730.5826

0.39650.611280.70.396580.780.70.39650.6112

0.50790.656479.80.507979.879.80.50790.6564

0.51980.659979.70.519879.779.70.51980.6599

0.57320.684179.30.573279.379.30.57320.6841