All about coffee by William H. Ukers

14. _Caffein--The Fendler and Stüber Method--Tentative_

Pulverize the coffee to pass without residue through a sieve having circular openings 1 mm. in diameter. Treat a 10-gram sample with 10 grams of 10-percent ammonium hydroxid and 200 grams of chloroform in a glass-stoppered bottle and shake continuously by machine or hand for one-half hour. Pour the entire contents of the bottle on a 12.5-cm. folded filter, covering with a watch glass. Weigh 150 grams of the filtrate into a 250-cc. flask and evaporate on the steam bath, removing the last chloroform with a blast of air. Digest the residue with 80 cc. of hot water for ten minutes on a steam bath with frequent shaking, and let cool. Treat the solution with 20 cc. (for roasted coffee) or 10 cc. (for unroasted coffee) of 1-percent potassium permanganate and let stand for 15 minutes at room temperature. Add 2 cc. of 3-percent hydrogen peroxid (containing 1 cc. of glacial acetic acid in 100 cc.). If the liquid is still red or reddish, add hydrogen peroxid, 1 cc. at a time, until the excess of potassium permanganate is destroyed. Place the flask on the steam bath for 15 minutes, adding hydrogen peroxid in 0.5-cc. portions until the liquid becomes no lighter in color. Cool and filter into a separatory funnel, washing with cold water. Extract four times with 25 cc. of chloroform. Evaporate the chloroform extract from a weighed flask with aid of an air blast and dry at 100° C. to constant weight (one-half hour is usually sufficient). Weigh the residue as caffein and calculate on 7.5 grams of coffee. Test the purity of the residue by determining nitrogen and multiplying by 3.464 to obtain caffein.