(a) Identification test. Add a few drops of concentrated nitric acid to about 10 mg of brucine alkaloid. A vivid red color is produced. Dilute the red solution with a few drops of water and add a few drops of freshly made dilute stannous chloride solution. A reddish purple (violet) color is produced.
(b) Melting point. 178 [deg]1 [deg]C. Dry the alkaloid in an oven for one hour at 100 [deg]C., increase the temperature to 110[deg] and dry to a constant weight before taking melting point.
Note. Brucine alkaloid tetrahydrate melts at 105 [deg]C. while the anhydrous form melts at 178 [deg]C.
(c) Strychnine test. Brucine alkaloid shall be free of strychnine when tested by the method listed under Brucine Sulfate, N.F. IX.
Note. If the brucine contains as much as 0.05 percent strychnine, a clear distinctive violet color, characteristic of strychnine, will be obtained.
(d) Sulfate test. No white precipitate is formed that is not dissolved by hydrochloric acid when several drops of a 1 N barium chloride solution are added to 10 ml of a solution of the alkaloid. [T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001] Sec. 21.100 n-Butyl alcohol.
(a) Acidity (as acetic acid). 0.03 percent by weight maximum.
(b) Color. Colorless.
(c) Dryness at 20 [deg]C. Miscible without turbidity with 10 volumes of 60[deg] B[eacute]1. gasoline.
(d) Odor. Characteristic odor.
(e) Specific gravity at 20 [deg]/20 [deg]C. 0.810 to 0.815. [T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001] Sec. 21.101 tert-Butyl alcohol.
(a) Acidity (as acetic acid). 0.003 percent by weight maximum.
(b) Color. Colorless.
(c) Distillation range. When 100 ml of tertiary butyl alcohol are distilled, none should distill below 78 [deg]C. and none above 85 [deg]C. More than 95 percent should distill between 81 [deg]-83 [deg]C.
(d) Dryness at 20 [deg]C. Miscible without turbidity with 19 volumes of 60[deg] B[eacute]1. gasoline.
(e) Freezing point (first needle). Above 20 [deg]C.
(f) Identification test. Place five drops of a solution containing approximately 0.1 percent tertiary butyl alcohol in ethyl alcohol in a test tube. Add 2 ml of Denige's reagent (dissolve 5 grams of red mercuric oxide in 20 ml of concentrated sulfuric acid; add this solution to 80 ml of distilled water, and filter when cool). Heat the mixture just to the boiling point and remove from the flame. A yellow precipitate forms within a few seconds.
(g) Nonvolatile matter. Less than 0.005 percent by weight.
(h) Odor. Characteristic odor.
(i) Residual odor after evaporation. None.
(j) Specific gravity at 25 [deg]/25 [deg]C. 0.780 to 0.786. [T.D. ATF-133, 48 FR 24673, June 2, 1983. Redesignated by T.D. ATF-442, 66 FR 12854, Mar. 1, 2001]