AOAC Official Method 939.06 Beta-Ionone in Flavor Extracts and Toilet Preparations Crystallographic Method I
First Action 1939
Final Action
(Applicable to pure solutions containing £100mgin 5mLalcohol.) Place 5 mL alcoholic sample containing 10–100 mg b-ionone in 125 mL Erlenmeyer. Add 95–100 mg solid m-nitrobenzhydrazide and dissolve by warming on steam bath, taking precautions to prevent loss of alcohol through evaporation. Add 5mLH2O, and if solution becomes cloudy, warm until clear. Remove from steam bath, add 0.2 mL CH3COOH, stopper flask lightly, and place on wooden surface to prevent too rapid cooling.
If ³20 mg of b-ionone is present, crystals begin to form within 30 min after solution reaches room temperature. Let stand in room ³2 h (overnight does no harm) and add 5 mL H2O dropwise, mixing solution continuously during addition by rotating flask. Stopper, let stand in room ³1 h and refrigerate overnight (£48 h). Filter through fine fritted glass crucible, wash with 30mLdilute alcohol (3 + 7), using wet policeman to remove precipitate adhering to flask, and dry at 100°C. Weight precipitate ´0.541 = weight b-ionone. Identify crystals microscopically, 939.08 (see 36.6.07).
References: JAOAC 22, 383(1939); 23, 572(1940).
CAS-14901-07-6 (b-Ionone)
