AOAC Official Method 934.04 Saccharin in Nonalcoholic Beverages
First Action 1934
Final Action
Add 2mLHCl to 50mLtest portion in separator. Extract with two 50 mL portions ether. Filter ether extracts through cotton, and wash combined filtrates with ca 5 mL H2O containing 1 drop HCl. Separate ether layer and evaporate to dryness on H2O bath. Add 5mLNH3-freeH2Oand 6mLHCl to residue, and evaporate solution to ca 1 mL on hot plate, stirring constantly. Again add 5 mL NH3-free H2O and 6 mL HCl, and evaporate to ca 1 mL. Dilute to
50 mL with NH3-free H2O and dilute 2 mL of this solution to 25 mL withNH3-freeH2O. Add 1mLNessler reagent. (Dissolve 100 g HgI2 and 70 g KI in small amount H2O. Add slowly, with stirring, to cooled solution of 160 gNaOHin 500mLH2O, and dilute to 1 L. Reagent is stable 1 year if stored in Pyrex container out of direct sunlight.
Reagent should give characteristic color, but no precipitate,with 0.04mgNH3-N in 50mLH2Oin 10 min.) Compare withNH4Cl standards in usual manner; 0.2921 g NH4Cl = 1 g saccharin, insoluble form (C7H5NO3S), and 1.317 g Na salt (C7H4NNaO3S×2H2O).
For convenience prepare NH4Cl standard equivalent to 200 mg/g insoluble form of saccharin.
References: Z. Nahr. Genussm. 18, 577(1909).
JAOAC 17, 193(1934); 18, 56(1935); 21, 184(1938).
CAS-81-07-2 (saccharin)
CAS-6155-57-3 (sodium saccharin, dihydrate)
