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How Artisan Distillation Works 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 SE-971 87 Luleå SWEDEN

Kris Arvid Berglund

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  • 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

    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

    00

    00

    00

    00

    00

    00

    00

    Mole Fraction

    Boiling Point

    Boiling Point Diagram Near Azeotrope

    x EtOHwt. fractvol. fract.T BoilingV-xV-yW-xW-yMole-xMole-y

    000100000000

    0.0190.0470.0587195.50.058710.410520.0470.3430.0190.17

    0.07210.1660.20399890.203990.694920.1660.6190.07210.3891

    0.09660.2150.2625686.70.262560.737560.2150.6650.09660.4375

    0.12380.2650.3213885.30.321380.763740.2650.6940.12380.4704

    0.16610.3380.4049284.10.404920.791960.3380.7260.16610.5089

    0.23770.4440.5213282.70.521320.815250.4440.7530.23770.5445

    0.26080.4740.5516182.30.551610.823760.4740.76350.26080.558

    0.32730.5550.6332981.50.633290.838880.5550.7810.32730.5826

    0.39650.6270.7024380.70.702430.855410.6270.8010.39650.6112

    0.50790.7250.7910979.80.791090.878850.7250.830.50790.6564

    0.51980.7350.7997879.70.799780.885990.7350.8390.51980.6599

    0.57320.7740.8330379.30.833030.892290.7740.8470.57320.6841

    0.67630.8420.8883578.740.888350.916910.8420.8790.67630.7385

    0.74720.8830.9199278.410.919920.933270.8830.9010.74720.7815

    0.89430.9560.9719278.150.971920.971920.9560.9560.89430.8943

    11178.3111111

    y EtOHwt. Fract.vol. fract.T boiling

    000100

    0.170.3430.4105295.5

    0.38910.6190.6949289

    0.43750.6650.7375686.7

    0.47040.6940.7637485.3

    0.50890.7260.7919684.1

    0.54450.7530.8152582.7

    0.5580.76350.8237682.3

    0.58260.7810.8388881.5

    0.61120.8010.8554180.7

    0.65640.830.8788579.8

    0.65990.8390.8859979.7

    0.68410.8470.8922979.3

    0.73850.8790.9169178.74

    0.78150.9010.9332778.41

    0.89430.9560.9719278.15

    11178.3

    Liquid Phase

    Vapor Phase

    EtOH Water VLE

  • TYPES OF DISTILLATIONSimple batch- no rectification

    Alambic- some rectification

    Column- active rectification

  • BATCH DISTILLATIONUse cutsHeads- remove acetaldehyde, methanolHearts- product rich in aromas and flavorsTails- fusel oils, dilute

  • RECTIFICATION- EQUILIBRIUM CONTACT Rectification is the result of equilibrium contact between two phasesThe liquid and vapor leaving the contact are in equilibriumRectification, also called enrichment, results in a higher concentration than would occur in a single equilibrium contact

  • SIMPLE BATCH (RAYLEIGH) DISTILLATION

  • 12

    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

  • vaporliquidmixture12

    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

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

  • Classic cognac distillation

  • INDIRECT STEAM HEATING (ALAMBIC)Some vapor condenses to liquid and returns to the pot

    SteamFigure courtesy of Christian Carl Ing. GmbH

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

  • RECTIFICATION COLUMNS

    Figure courtesy of Christian Carl Ing. GmbH

  • SIEVE TRAY

  • BUBBLE CAP TRAY

  • BATCH COLUMN STILLBoilerPartialcondensorD, xDLRefluxratio

  • 123456XFEEDxDISTThe number of trays needed for a specific separation is determined by stepping off..

    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

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    Liquid Mole Fraction EtOH

    Vapor Mole Fraction EtOH

    Ethanol Water VLE

    Sheet2

    00

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    Mole Fraction

    Boiling Point, C

    Boiling Point Diagram

    Sheet3

  • vaporliquidmixture12345

    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

    10

    00

    00

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    Liquid Mole Fraction EtOH

    Vapor Mole Fraction EtOH

    Ethanol Water VLE

    Sheet2

    00

    00

    00

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    00

    00

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    00

    00

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    00

    00

    00

    00

    00

    Mole Fraction

    Boiling Point, C

    Boiling Point Diagram

    Sheet3

  • If the reflux ratio is constant,the product concentrationwill decrease during the batch112233

    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

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    00

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    Liquid Mole Fraction EtOH

    Vapor Mole Fraction EtOH

    Ethanol Water VLE

    Sheet2

    00

    00

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    00

    00

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    00

    00

    00

    00

    00

    00

    00

    00

    00

    00

    00

    Mole Fraction

    Boiling Point, C

    Boiling Point Diagram

    Sheet3

  • Since the concentration in the pot decrease during a bath, in order to keep the product concentration high, the reflux must be increased 123123

    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

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    00

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    Liquid Mole Fraction EtOH

    Vapor Mole Fraction EtOH

    Ethanol Water VLE

    Sheet2

    00

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    00

    00

    00

    00

    00

    00

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    00

    00

    Mole Fraction

    Boiling Point, C

    Boiling Point Diagram

    Sheet3

  • REFLUX IS INCREASED BY INCREASING COOLING WATER FLOWRATE TO PARTIAL CONDENSER TTEMPERATURE SENSORWATER TO CONDENSERFigure courtesy of Christian Carl Ing. GmbH

  • FLAVOR COMPOUNDS (CONGENERS) IN DISTILLED SPIRITS

  • TYPICAL COMPOUNDS BY GC

    Sheet1

    Chemical NameRetentionTime (min)Boiling point (deg. C)

    Acetaldehyde2.520.8

    Acetone3.456.2

    Ethyl Formate3.654.0

    Ethyl Acetate4.577.0

    Methanol4.764.7

    Ethanol5.878.0

    1-propanol8.797.0

    Isopentanol (isoamyl alcohol)16.3132.0

    Benzaldehyde33.0179.0

  • TYPICAL GC RESULTS

  • ETHANOL RESULTS FROM PLUM DISTILLATIONHEADSHEARTSTAILS

    Chart1

    85

    87

    82

    80

    78

    76

    71

    64

    58

    1

    Distillate Volume (mL)

    Ethanol Conc. (% v/v)

    Sheet1

    All trays with CC40085All trays40084

    8008780086

    120082120085

    220080220084

    320078320081

    420076420075

    520071490065

    615064555055

    670058

    2 trays with CC400852 trays40085

    8008680085

    120086120083

    220084220080

    320080320070

    420064420050

  • CONGENER CONCENTRATIONS IN PLUM DISTILLATESHEADSHEARTSTAILS

    Chart1

    0.30269567710.57362318090.12438143560.08436951480.0212524377

    0.09051417370.50170066270.05749395790.10445260510.033395885

    0.02084552690.43965257460.01952761390.12698574270.0547523221

    0.00758602320.37569988360.00451826880.16787063520.1182030239

    0.0053004470.37500662560.00171381120.20602248570.241388246

    0.00492636740.4815596130.00550255070.15080878130.1153446981

    Acetaldehyde

    Methanol

    Ethyl Acetate

    1-Propanol

    Iso Amyl Alcohol

    Distillate Volume (mL)

    Congener Concentration (% v/v)

    Methanol Concentration (% v/v)

    Congener Concentration vs Distillate Volume 2 Trays with Catalytic Converter

    Sheet1

    Sheet1

    0.30269567710.57362318090.12438143560.08436951480.0212524377

    0.09051417370.50170066270.05749395790.10445260510.033395885

    0.02084552690.43965257460.01952761390.12698574270.0547523221

    0.00758602320.37569988360.00451826880.16787063520.1182030239

    0.0053004470.37500662560.00171381120.20602248570.241388246

    0.00492636740.4815596130.00550255070.15080878130.1153446981

    Acetaldehyde

    Methanol

    Ethyl Acetate

    1-Propanol

    Iso Amyl Alcohol

    Distillate Volume (mL)

    Congener Concentration (% v/v)

    Methanol Concentration (% v/v)

    Congener Concentration vs Distillate Volume 2 Trays with Catalytic Converter

    Sheet2

    Sheet3

  • CONTACT Prof. Kris Arvid BerglundEmail: [email protected]: [email protected]

    www.artisandistilling.org

  • ACKNOWLEDGEMENTSChristian Carl Ing. GmbHProject GREEEN, State of MichiganMichigan State UniversityLule University of Technology