With so much tequila on the market, there's no reason to compromise. Devote an evening to reposado, or rested, tequilas, which have aged in wood for up to a year. Ones to seek out (all from Mexico): Herradura ($$), Chinaco ($$), and Patrón ($$$). Throw in some José Cuervo ($$) and see what happens.
Rum, while increasingly trendy, is still pretty limited brand-wise. If you're tasting dark rums, be sure to sample from the various islands: Mount Gay Eclipse (Barbados $), Rhum Barbancourt Estate Reserve (aged in oak, Haiti, $$), and Myers Legend Rum Aged 10 Years (Jamaica $$). A newcomer on the light rum front is 10 Cane (Trinidad $$), made from first-pressed sugarcane. Compare it with Bacardi, of course (Puerto Rico $).
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Entire books are devoted to Scotch, and you'll want to pick one up before embarking on a proper tasting. You might consider a mind-blowing bottle of Suntory Single Malt 18-year-old Black Label (Japan $$$), which Bill Murray hawks in Lost in Translation. But Suntory 12-year-old (Japan $) is a third the price, and excellent as well.
An all-American bourbon tasting is an opportunity to sample the many small-batch, single-barrel whiskeys hitting the shelves. Try the superb Pappy Van Winkle 15-year-old ($$$) or Knob Creek 9-year-old ($$) against good ol' Jim Beam ($$) and Jack Daniel's ($$).
Here's the host's protocol, per Blue: Lay out a tall, narrow glass (such as a highball or champagne flute) for each guest. Provide room-temperature spring water for sipping and rinsing between tastes, as well as paper and pens.
To keep bias at bay, pour each guest's portion (small sips, now) in another room, out of sight, or decant the spirits into clean, unlabeled glass bottles. Either way, introduce each as a number (and don’t forget to make a key!), then unveil their true identities after the tasting.
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