Skip to main content

Distillation Experiments and Observations

  • Chapter
  • First Online:
Whisky Science
  • 2454 Accesses

Abstract

This chapter reviews some general observations about whisky distillation, and describes a few published experiments designed to assess chemical changes that occur during distillation, and how a still’s construction influences its distillates.

I have known a case where a distillery was making a whiskey which was not what was desired. There were a lot of experiments made; finally, a couple of feet were cut out of the height of the head, and they made entirely different whiskey simply by the cutting out. – Philip Schidrowitz, 1909 [37, ¶4078]

This is a preview of subscription content, log in via an institution to check access.

Access this chapter

Chapter
USD 29.95
Price excludes VAT (USA)
  • Available as PDF
  • Read on any device
  • Instant download
  • Own it forever
eBook
USD 89.00
Price excludes VAT (USA)
  • Available as EPUB and PDF
  • Read on any device
  • Instant download
  • Own it forever
Softcover Book
USD 119.99
Price excludes VAT (USA)
  • Compact, lightweight edition
  • Dispatched in 3 to 5 business days
  • Free shipping worldwide - see info
Hardcover Book
USD 179.99
Price excludes VAT (USA)
  • Durable hardcover edition
  • Dispatched in 3 to 5 business days
  • Free shipping worldwide - see info

Tax calculation will be finalised at checkout

Purchases are for personal use only

Institutional subscriptions

Notes

  1. 1.

    Leppänen et al. credit a 1978 Finnish masters thesis by A. Aejmelaeus for original work on this problem.

References

  1. Adam T, Duthie E, Feldmann J (2002) Investigations into the use of copper and other metals as indicators for the authenticity of Scotch whiskies. J Inst Brew 108:459–464

    Article  CAS  Google Scholar 

  2. Adams A, De Kimpe N (2006) Chemistry of 2-acetyl-1-pyrroline, 6-acetyl-1,2,3,4-tetrahydropyridine, 2-acetyl-2-thiazoline, and 5-acetyl-2,3-dihydro-4H-thiazine: extraordinary Maillard flavor compounds. Chem Rev 106:2299–2319

    Article  CAS  PubMed  Google Scholar 

  3. Adams AB (1910) The distillation of whiskey. J Ind Eng Chem 2:34–43

    Article  CAS  Google Scholar 

  4. Allen AH (1891) The chemistry of whisky and allied products. J Soc Chem Ind 10:305–314

    Google Scholar 

  5. Allen AH (1897) The chemistry of whisky. J Fed Inst Brew 3:24–48

    CAS  Google Scholar 

  6. Anon (1755) Serious reflections on the manifold dangers attending the use of copper vessels and other utensils of copper and brass, in the preparations of all such solids and liquids as are designed for food to human bodies: in a letter to a friend. M. Cooper, London

    Google Scholar 

  7. Anon (1870) Distillation of Kentucky whiskey. Intern Revenue Record 11:117

    Google Scholar 

  8. Anon (1901) Injurious constituents in potable spirits. Nature 563(1638):491–492

    Google Scholar 

  9. Anon (1901) Topics of the times. New York Times, p 8

    Google Scholar 

  10. Anon (1909) The royal commission on whisky and other potable spirits. Brit Med J 2(2537):399–404

    Article  Google Scholar 

  11. Anon (1912) The toxic factor in tobacco. Lancet 180(4643):547–548

    Article  Google Scholar 

  12. Anon (1934) Monthly review. The Scottish section. J Inst Brew 40:30–31

    Google Scholar 

  13. Aya I, Nariai H, Kobayashi M (1980) Pressure and fluid oscillations in vent system due to steam condensation (I). Experimental results and anlysis model for chugging. J Nucl Sci Technol 17:499–515

    Article  CAS  Google Scholar 

  14. Aya I, Kobayashi M, Nariai H (1983) Pressure and fluid oscillations in vent system due to steam condensation (II). High-frequency component of pressure oscillations in vent tubes under chugging and condensation oscillation. J Nucl Sci Technol 20:213–227

    CAS  Google Scholar 

  15. Baker RH, Barkenbus C (1937) Whisky verdigris analysis. Ind Eng Chem 29:755–757

    Article  CAS  Google Scholar 

  16. Barnard A (2008) The whisky distilleries of the United Kingdom. Birlinn, Edinburgh (Reprints of articles from Harper’s Weekly gazette, 1887)

    Google Scholar 

  17. Bathgate GN (2003) History of the development of whiskey distillation. In: Russell I (ed) Whisky: technology, production and marketing, Academic Press, New York, p 1–26

    Google Scholar 

  18. Beck H, Glienke N, Möhlmann C (1997) Combustion and explosion characteristics of dusts. Tech. Rep. 13/97, Berufsgenossenschaftliches Institut für Arbeitssicherheit—BIA

    Google Scholar 

  19. Boucherie A (1819) The art of making whiskey. Worsley & Smith, Lexington

    Google Scholar 

  20. Boure JA, Bergles AE, Tong LS (1973) Review of two-phase flow instability. Nucl Eng Des 25:165–192

    Article  CAS  Google Scholar 

  21. Brooks MR, Crowl DA (2007) Flammability envelopes for methanol, ethanol, acetonitrile and toluene. J Loss Prev Process Ind 20:144–150

    Article  CAS  Google Scholar 

  22. Brunton SL, Tunnicliffe FW (1900) Concerning certain apparently injurious constituents of potable spirits. Lancet 156(4032):1643–1644

    Article  Google Scholar 

  23. Buttery RG, Stern DJ, Ling LC (1994) Studies on flavor volatiles of some sweet corn products. J Agric Food Chem 42:791–795

    Article  CAS  Google Scholar 

  24. Byrn ML (1871) The complete practical distiller, 8th edn. Henry Carey Baird, Philadelphia

    Google Scholar 

  25. Carter-Tijmstra JE (1990) Whisky flavour analysis. In: Campbell I (ed) Proceedings of the third aviemore conference on malting, brewing and distilling. Institute of Brewing, London, p 468–471

    Google Scholar 

  26. Chevance F, Guyot-Declerck C, Dupont J, Collin S (2002) Investigation of the β-damascenone level in fresh and aged commercial beers. J Agric Food Chem 50:3818–3821

    Article  CAS  PubMed  Google Scholar 

  27. Chin H-W, Lindsay RC (1994) Ascorbate and transition-metal mediation of methanethiol oxidation to dimethyl disulfide and dimethyl trisulfide. Food Chem 49:387–392

    Article  CAS  Google Scholar 

  28. Coghe S, Martens E, D’Hollander H, Dirinck PJ, Delvaux FR (2004) Sensory and instrumental flavour analysis of wort brewed with dark specialty malts. J Inst Brew 110:94–103

    Article  CAS  Google Scholar 

  29. Conner J, Jack F, Walker D (2010) 2-Acetyl-1-pyrroline, a contributor to cereal and feinty aromas in Scotch whisky. In: Walker GM, Hughes PS (eds) Distilled spirits. New horizons: energy, environment and enlightenment. Proceedings of the worldwide distilled spirits conference. Nottingham University Press, Nottingham, p 263–268

    Google Scholar 

  30. Coronado CJR, Carvalho JA Jr, Andrade JC, Mendiburu AZ, Cortez EV, Carvalho PS, Gonçalves B, Quintero JC, Gutiérrez Velásquez EI, Silva MH, Santos JC, Nascimento MAR (2014) Flammability limits of hydrated and anhydrous ethanol at reduced pressures in aeronautical applications. J Hazard Mater 280:174–184

    Article  CAS  PubMed  Google Scholar 

  31. Crampton CA, Tolman LM (1908) A study of the changes taking place in whiskey stored in wood. J Amer Chem Soc 30:98–136

    Article  CAS  Google Scholar 

  32. de Krasinski J, Fan Y (1984) Some viscoelastic aspects of liquid foams of high void fraction and possibilities of their applications. In: XVIth International Congress of Theoretical and Applied Mechanics (ICTAM), p 463

    Google Scholar 

  33. Department of Justice (1909) Proceedings before and by direction of the President concerning the meaning of the term whisky. U.S. Government Printing Office, Washington, DC

    Google Scholar 

  34. Deshpande NS, Barigou M (2000) The flow of gas-liquid foams in vertical pipes. Chem Eng Sci 44:4297–4309

    Article  Google Scholar 

  35. Deshpande NS, Barigou M (2001) Foam flow phenomena in sudden expansions and contractions. Int J Multiphase Flow 27:1463–1477

    Article  CAS  Google Scholar 

  36. Duplais M (1871) Alcoholic liquors (trans: McKennie M). Henry Carey Baird, Philadelphia

    Google Scholar 

  37. Duplais P, McKennie M (1871) A treatise on the manufacture and distillation of alcoholic liquors. Henry Carey Baird, Philadelphia

    Google Scholar 

  38. Flora LF, Wiley RC (1974) Sweet corn aroma, chemical components and relative importance in the overall flavor response. J Food Sci 39:770–773

    Article  CAS  Google Scholar 

  39. Ford H (1914) The case against the little white slaver, vol 1. Henry Ford, Detroit

    Google Scholar 

  40. Gardiner BS, Dlugogorski BZ, Jameson GJ (1999) Prediction of pressure losses in pipe flow of aqueous foams. Ind Eng Chem Res 38:1099–1106

    Article  CAS  Google Scholar 

  41. Gijs L, Perpète P, Timmermans A, Collin S (2000) 3-methylpropionaldehyde as precursor of dimethyl trisulfide in aged beers. J Agric Food Chem 48:6196–6199

    Article  CAS  PubMed  Google Scholar 

  42. Goodykoontz JH, Dorsch RG (1967) Local heat-transfer coefficients and static pressures for condensation of high-velocity steam within a tube. Tech. Rep. TN D-3953, NASA Lewis Research Center

    Google Scholar 

  43. Gray SF (1828) The operative chemist. Hurst, Chance, and Co., London

    Google Scholar 

  44. Guymon JF (1974) Chemical aspects of distilling wines into brandy. In: Webb A (ed) Chemistry of winemaking. American Chemical Society, Washington, DC

    Google Scholar 

  45. Hall H (1813) Hall’s distiller. John Bioren, Philadelphia

    Google Scholar 

  46. Harrison B, Fagnen O, Jack F, Brosnan J (2011) The impact of copper in different parts of malt whisky pot stills on new make spirit composition and aroma. J Inst Brew 117:106–112

    Article  CAS  Google Scholar 

  47. Hastie SH (1925) The application of chemistry to pot still distillation. J Inst Brew 31:198–215

    Article  CAS  Google Scholar 

  48. Hastie SH (1926) Character in pot still whisky. J Inst Brew 32:209–220

    Article  Google Scholar 

  49. Hastie SH, Dick WD (1928) Character in pot still whisky. J Inst Brew 34:477–494

    Article  CAS  Google Scholar 

  50. Heitz JE (1960) Measurement of vapor-liquid equilibria for acetaldehyde-ethanol-water mixtures. Am J Enol Vitic 11:19–29

    CAS  Google Scholar 

  51. Howie D, Swan JS (1984) Compounds influencing peatiness in Scotch malt whisky flavour. In: Nykänen L, Lehtonen P (eds) Proceedings of the Alko symposium on flavour research of alcoholic beverages. Helsinki, Foundation for Biotechnical and Industrial Fermentation Research, Helsinki, p 279–290

    Google Scholar 

  52. Ikari A (1970) On the behavior of minute amount component in simple distillation of aqueous solution of ethanol. Kagaku Kōgaku 34:1185–1192

    Article  CAS  Google Scholar 

  53. Ikari A, Ayabe N (1969) On the vapor-liquid equilibrium of minute amount components–Water-ethanol systems containing a minute amount of 1-butanol. Kagaku Kōgaku 33:157–162

    Article  CAS  Google Scholar 

  54. Ikari A, Kubo R (1975) Behavior of various impurities in simple distillation of aqueous solution of ethanol. J Chem Eng Jpn 8:294–299

    Article  CAS  Google Scholar 

  55. Ikari A, Tōya S (1971) Simple distillation of aqueous solution of ethanol containing a minute amount of furfural. Kagaku Kōgaku 35:1131–1135

    Article  CAS  Google Scholar 

  56. Isoe S, Katsumiura S, Sakan T (1973) The synthesis of damascenone and β-damascone and the possible mechanism of their formation from cartenoids. Helv Chim Acta 56:1514–1516

    Article  CAS  Google Scholar 

  57. Joint FAO/WHO Expert Committee on Food Additives (1999) Furfural. WHO Food Additives Series 42. 51st Joint FAO/WHO Expert Committee on Food Additives, Geneva

    Google Scholar 

  58. Jones K, Wills R (1966) Separation and composition of a Scotch whisky fusel oil. J Inst Brew 72:196–201

    Article  CAS  Google Scholar 

  59. Kadir S, Decloux M, Giampaoli P, Joulia X (2008) Liquid-liquid equilibria of the ternary systems 3-methyl-1-butanol +  ethanol +  water and 2-methyl-1-propanol +  ethanol +  water at 293.15 K. J Chem Eng Data 53:910–912

    Article  CAS  Google Scholar 

  60. Kahnjahn D, Jarms U, Maier HG (1997) Hydroxymethylfurfural and furfural in coffee and related beverages II. Coffee. Dtsch Lebensmitt Rundsch. 93:44–46

    Google Scholar 

  61. Lahey RT Jr, Podowski MZ (1989) On the analysis of various instabilities in two-phase flows. Multiph Sci Technol 4:183–370

    Article  CAS  Google Scholar 

  62. Leppänen O, Ronkainen P, Denslow J, Laasko R, Lindeman A, Nykänen I (1983) Polysulphides and thiophenes in whisky. In: Piggott JR (ed) Flavour of distilled beverages: origin and development. Ellis Horwood, Chichester, p 206–214

    Google Scholar 

  63. Li X, Wang X, Evans GM, Stevenson P (2011) Foam flowing vertically upwards in pipes through expansions and contractions. Int J Multiphase Flow 37:802–811

    Article  CAS  Google Scholar 

  64. Lindet ML (1890) Sur la présence du furfural dans les alcools commerciaux. C R Hebd Seances Acad Sci 111:236–237

    Google Scholar 

  65. MacKenzie WM, Clyne AH, MacDonald LS (1990) Ethyl carbamate formation in grain based spirits Part II. The identification and determination of cyanide related species involved in ethyl carbamate formation in Scotch grain whisky. J Inst Brew 96:223–232

    CAS  Google Scholar 

  66. MacWilliam IC (1968) Wort composition—a review. J Inst Brew 74:38–54

    Article  CAS  Google Scholar 

  67. Mapes JJ (1841) On the effects of arts, trades, and professions, as well as habits of living, on health and longevity. no. XII. Am Rep Arts Sci Manuf 3(6):401–413

    Google Scholar 

  68. Masuda M, Nishimura K (1980) Occurrence and formation of damascenone in alcoholic beverages. J Food Sci 45:396–397

    Article  CAS  Google Scholar 

  69. Maxwell R (1743) Select transactions of the honourable the society of improvers in the knowledge of agriculture in Scotland. Sands, Brymer, Murray and Cochran, Edinburgh

    Google Scholar 

  70. McNulty WJ (1923) Smuggling whisky from Canada. Curr Hist Forum 18:123–125

    Google Scholar 

  71. M’Harry S (1809) The practical distiller. John Wyeth, Harrisburgh

    Google Scholar 

  72. Nakamura H (1963) Studies on the manufacture of distillated liquor. Part I. Changes of the components during distillation and a cutting method of potable alcohol of raw whisky. Kagaku Kōgaku 37:309–314

    CAS  Google Scholar 

  73. Nedjma M, Hoffmann N (1996) Hydrogen sulfide reactivity with thiols in the presence of copper(II) in hydroalcoholic solutions or Cognac brandies: formation of symmetrical and unsymmetrical dialkyl trisulfides. J Agric Food Chem 44:3935–3938

    Article  CAS  Google Scholar 

  74. Nettleton JA (1913) The manufacture of whisky and plain spirit. G. Cornwall & Sons, Aberdeen

    Google Scholar 

  75. Nicol D (2014) Batch distillation. In: Russell I, Stewart G (eds) Whisky technology, production and marketing, 2nd edn, Academic Press, New York, p 155–178

    Google Scholar 

  76. Ohtake K, Yamasaki H, Kojima K (1995) Evaluation of mass-transfer by mist as a new parameter in the control of wash distillation. In: Campbell I, Priest FG (eds) Proceedings of the fourth aviemore conference on malting, brewing, and distilling, 1994. Institute of Brewing, London, p 202–208

    Google Scholar 

  77. Perry DR (1986) Whisky maturation mechanisms. In: Campbell I, Priest FG (eds) Proceedings of the 2nd Aviemore Conference on Malting, Brewing, and Distilling. Institute of Brewing, London, p 409–412

    Google Scholar 

  78. A Physician (1834) Desultory notes on the origin, uses, and effects of ardent spirit. Adam Waldie, Philadelphia

    Google Scholar 

  79. Poisson L, Schieberle P (2008) Characterization of the most odor-active compounds in an American bourbon whisky by application of the aroma extract dilution analysis. J Agric Food Chem 56:5813–5819

    Article  CAS  PubMed  Google Scholar 

  80. Pope S (2016) The first tank crews. Helion & Co Ltd., Solihull

    Google Scholar 

  81. Porter AL (1830) The chemistry of the arts, vol 2. Carey & Lea, Philadelphia

    Google Scholar 

  82. A practical liquor manufacturer (1857) The Bordeaux wine and liquor dealer’s guide. Dick & Fitzgerald, New York

    Google Scholar 

  83. Preyer ER (1901) Whiskey. Information and guide for the liquor business. Edgar R. Preyer, New York

    Google Scholar 

  84. Pryde J, Conner J, Jack F, Lancaster M, Meek L, Owen C, Paterson R, Steele G, Strang F, Woods J (2011) Sensory and chemical analysis of ‘Shackelton’s’ Mackinlay Scotch whisky. J Inst Brew 117:156–165

    Article  CAS  Google Scholar 

  85. Reaich D (1999) The influence of copper on malt whisky character. In: Campbell I (ed) Proceedings of the fifth Aviemore conference on malting, brewing and distilling. Institute of Brewing, London, p 141–152

    Google Scholar 

  86. Redlich O, Kister AT (1948) Algebraic representation of thermodynamic properties and the classification of solutions. Ind Eng Chem 40:345–348

    Article  Google Scholar 

  87. Roberts DD, Acree TE (1995) Developments in the isolation and characterization of β-damascenone precursors from apples. In: Rouseff RL, Leahy MM (eds) Fruit flavors. Biogenesis, characterization, and authentication. American Chemical Society, Washington, p 190–199

    Google Scholar 

  88. Ronkainen P (1973) The formation of volatile sulphur compounds during pressure cooking of grain/water mixtures. J Inst Brew 79:200–202

    Article  CAS  Google Scholar 

  89. Ronkainen PP, Denslow J, Leppänen OA (1973) The gas chromatographic analysis of some volatile sulfur compounds. J Chromatogr Sci 11:384–390

    Article  CAS  Google Scholar 

  90. Royal Commission (1908) Minutes of evidence taken by the Royal Commission on Whiskey and Other Potable Spirits. Jas Treuscott & Sons, London

    Google Scholar 

  91. Schidrowitz P, Kaye F (1906) The distillation of whisky. J Inst Brew 12:496–517

    Article  Google Scholar 

  92. Schieberle P (1995) Quantitation of important roast-smelling odorants in popcorn by stable isotope dilution assays and model studies on flavor formation during popping. J Agric Food Chem 43:2442–2448

    Article  CAS  Google Scholar 

  93. Shinkle CA (1912) American commercial methods of manufacturing preserves, pickles, canned foods, etc. Herald Leader Press, Menominee

    Google Scholar 

  94. Smith SB, Owsley HC (eds) (1980) The papers of Andrew Jackson. Volume 1, 1770–1803. University of Tennessee Press, Knoxville

    Google Scholar 

  95. Stenhouse J (1870) Ueber Furfuranilin und Furfurtoluidin. Liebigs Ann Chem 156:197–205

    Article  Google Scholar 

  96. Sundholm G (1964) Vapour-liquid equilibria of six organic compounds present in impurity concentrations in ethanol-water mixtures. Finska Kemistsamfundets Meddelanden 73:1–15

    CAS  Google Scholar 

  97. Suomalainen H, Lehtonen M (1979) The production of aroma compounds by yeast. J Inst Brew 85:149–156

    Article  CAS  Google Scholar 

  98. Tylecote RF (1992) A history of metallurgy, 2nd edn. Institute of Materials, Brookfield

    Google Scholar 

  99. Udo M (2006) The Scottish whisky distilleries. Black & White, Edinburgh

    Google Scholar 

  100. van Beek S, Priest FG (2000) Decarboxylation of substituted cinnamic acids by lactic acid bacteria islated during malt whisky fermentation. Appl Environ Microbiol 66:5322–5328

    Article  PubMed  PubMed Central  Google Scholar 

  101. War Office (1916) Second Supplement. London Gazette Tue. 14th Nov. (29824):11055

    Google Scholar 

  102. War Office (1919) Fifth Supplement. London Gazette Fri. 30th May (31370):6800

    Google Scholar 

  103. Ward C (2003) The Glenkinchie story since 1723. Prestoungrange University Press, Presonpans

    Google Scholar 

  104. Wathen JW (1910) Distillery operation and control. In: Wiley HW (ed) Manufacture of denatured alcohol based on the operations of an experimental still at Washington, D. C., and a course of lectures delivered in connection therewith, Government Printing Office, Washington, DC, p 109–113

    Google Scholar 

  105. Watson DC (1983) A laboratory apparatus for distillation research. In: Priest FG, Campbell I (eds) Proceedings of the aviemore conference on malting, brewing and distilling. Institute of Brewing, London, p 249–255

    Google Scholar 

  106. Watson DC (1985) Current developments in the potable distilling industry. Crit Rev Biotechnol 2:147–192

    Article  CAS  Google Scholar 

  107. Weir RB (1984) Distilling and agriculture 1870–1939. Agric Hist Rev 32:49–62

    Google Scholar 

  108. Whitby BR (1992) Traditional distillation in the whisky industry. Ferment 5:261–267

    Google Scholar 

  109. Wiley HW (1906) Foreign trade practices in the manufacture and exportation of alcoholic beverages and canned goods. US Department of Agriculture, Bureau of Chemistry Bulletin No 102

    Google Scholar 

  110. Wiley HW (1919) Beverages and their adulteration. P. Blakiston’s Son, Philadelphia

    Google Scholar 

  111. Williams GC (1962) Vapor-liquid equilibria of organic homologues in ethanol–water solutions. Am J Enol Vitic 13:169–180

    CAS  Google Scholar 

  112. Williams LA, Knuttel WP (1983) Computer modeling of aroma compound behavior during batch distillation. In: Piggott JR (ed) Flavour of distilled beverages: origin and development. Ellis Horwood, Chichester, p 134–144

    Google Scholar 

  113. Winterhalter P, Sefton MA, Williams PJ (1990) Volatile C13-norisoprenoid compounds in Riesling wine are generated from multiple precursors. Am J Enol Vitic 41:277–283

    CAS  Google Scholar 

  114. Wright FB (1907) A practical handbook on the distillation of alcohol from farm products, 2nd edn. Spon & Chamberlain, London

    Google Scholar 

  115. Yoshihashi T, Huong NTT, Inatomi H (2002) Precursors of 2-acetyl-1-pyrroline, a potent flavor compound of an aromatic rice variety. J Agric Food Chem 50:2001–2004

    Article  CAS  PubMed  Google Scholar 

  116. Zabetakis MG (1965) Flammability characteristics of combustible gases and vapors. Bulletin 627, Bureau of Mines, US Department of the Interior, Washington, DC.

    Google Scholar 

  117. Zacarías I, Yáñez CG, Araya M, Oraka C, Olivares M, Uauy R (2001) Determination of the taste threshold of copper in water. Chem Senses 26:85–89

    Article  PubMed  Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Rights and permissions

Reprints and permissions

Copyright information

© 2019 Springer Nature Switzerland AG

About this chapter

Check for updates. Verify currency and authenticity via CrossMark

Cite this chapter

Miller, G.H. (2019). Distillation Experiments and Observations. In: Whisky Science. Springer, Cham. https://doi.org/10.1007/978-3-030-13732-8_6

Download citation

Publish with us

Policies and ethics