03b - Distillation Of Brandy.docx

Distillation of Brandy BIOPROCESS LABORATORY By M.Sc. Ashanty Piña

Objectives 1. To apply knowledge obtained about distillation part A session to manufacture a distilled product. 2. To identify the foreshot, heads, middle run, and tails of ethanol distillation from fermented mash.

Background Distillation is the centuries old process used to produce alcohol. In it, heat is used to separate the components of a liquid, or mash, and as vaporization takes place, the vapors are cooled so they condense into neutral spirits with little color, aroma, or flavor. The distiller then blends this neutral spirit with other alcohol or flavorings and may or may not leave it to mature (age) until the desired flavor and aroma is achieved before bottling. Brandy and clear, colorless grappa are two examples of spirits distilled from wine. Brandy was first discovered in the middle of the thirteenth century in France as an attempt to produce a medicinal drink. Brandy is now made around the world wherever grapes are grown. After two distillations, the clear, colorless alcohol is given its distinctive nutty brown color and flavor by aging in wood barrels. The longer a brandy ages, the more “refined” the flavor is judged to be (Mario, 2010) When elaborating liquor through distillation, the different volatile compounds in the mash begin to vaporize around their specific boiling temperatures. Some of these volatile compounds present in fermented mash, and their boiling points at 1 atm, are:  Acetone (56.5°C)  1-propanol (97°C)  Methanol (64°C)  Water (100°C)  Ethyl acetate (77.1°C)  Butanol (116°C)  Ethanol (78°C)  Amyl alcohol (137.8°C)  2-propanol (82°C)  Furfural (161°C) When distilling, the distiller tries to separate isolate the condensed alcohol from methanol, fusel alcohols, and other compounds. During distillation, the first volatiles to be collected are usually methanol and acetone, called the heads. Fusel alcohols are concentrated in the tails at the end of the distillation run and are characterized by their oily consistency (Hazelwood et al., 2008).

Materials and Methods Materials (per team): 2 burette stands 4 three-fingered clamps 1 Quick Fit refrigerant, large 2 Quick Fit two-mouth round flasks, 5000-6000mL 1 Quick Fit Y-connection 1 beaker, 100mL 3 Erlenmeyer flask, 250mL 4 Erlenmeyer flask, 25 ml 2 thermometers 1 Abbe refractometer

2 thermal sink 5 pasteur pipettes 2 graduated cylinder, 500mL 2 brandy flasks with cork 2 security bulbs 1 recirculating immersion pump Iced water 2 rubber hoses 1000 mL of table (red) wine Página | 1

Procedure: 1. Set up as the same apparatus you used for Distillation part A. Use running, cold, recirculating water as refrigerant. 2. Fill the two-mouthed Quick Fit flask halfway up with table wine, remember to measure the amount to confirm volume, and analyze IR of initial wine. 3. Place a thermometer into one of the mouths of the Quick Fit flask using a thermal sink until the bulb is submerged halfway into the liquid 4. Place the other thermometer into the top of the Y connection using the other thermal sink, so that the bulb is at the height of the exit to the refrigerant. 5. Heat until the wine begins to boil, record the temperature and investigate what was the barometric pressure for that day. 6. Once you begin collecting distillate, sample it every 2-3 minutes and record the temperature when you sampled. Use different Pasteur pipettes to avoid cross-contaminating your samples. 7. Measure the refractive index of your distillate samples. Analyze the refraction index of these samples. 8. Compare the alcohol composition of your sample with the refraction index curves built before on Distillation part A. 9. Identify the ranges of boiling temperatures and composition of the distillate. Separate in fractions according with the ethanol distillation terms foreshots, heads, middle run, and tails. Research the composition and temperature difference on each. 10. Measure how much you obtain of each fraction, and save. 11. Once you know at what temperatures you have your foreshots, heads, and tails, make a brandy with a 40°G.L. (abv) that contains only the middle run and bottle your liquor. If required, use the tails fraction to complete and make your brandy, however be aware that tails usually bring strong flavors in liquors.

Results and Discussion For your introduction:  Liquid-vapor equilibrium, partial pressures  Laws of Dalton, Raoult, and Henry  Research on brandy manufacturing.  Measurement of alcoholic content in beverages, ABV, degrees Gay-Lussac, and examples of beverages and their alcohol content (at least 5).  The concepts of foreshot, head, middle run, and tail in alcohol distillation. For your results:  Report the tables where you show temperature, ethanol content, and whether that value is a foreshot, head, middle run, or tail.  Calculate and report the distillation efficiency (how much alcohol was recovered vs what is supposed to be contained in wine)  Calculate, report, and discuss the brandy production process efficiency

Conclusions Questionnaire 1) Describe the process to make whiskey.

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References Barbosa-Canovas, G. and Ibarz, A. 2003. Unit Operations in Food Engineering. CRC Press. New York, USA. Charm. S. 1978. Fundamentals of Food Engineering. AVI Publishing Co. Connecticut, USA. Hazelwood, L.A.; Daran, J.-M.; van Maris, A. J. A.; Pronk, J. T., and Disckinson, J.R. 2008. The ehrlich pathway for fusel alcohol production: a century of research on Saccharomyces cerevisiae metabolism. Appl. Environ. Microbiol. 74 (8): 2259-2266. Mario. 2010. Liquor Distillation from Wine. Article Gold. http://www.articlegold.com/Article/Liquor-DistillationFrom-Wine/10956. Accessed: 04/Oct/2010. Urquiza, M. 1987. Experimentos de Fisicoquímica. ITESM Campus Monterrey. Nuevo León, México.

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