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47.3.

17
AOAC Official Method 905.03
Fluorides (Soluble) in Food
Hydrofluoric Acid Test
First Action 1905
Final Action

(a) Not applicable in presence of silicates.After thoroughly


mixing test sample, transfer to beaker 150 mL, or equivalent
amount of aqueous extract in case of solid foods, and boil, adding
5 mL 10% K2SO4 solution and 10 mL 10% Ba(CH3COO)2 solution.
Collect precipitate (BaF2) in compact mass (centrifuge may be
used advantageously) and wash on small filter. Transfer to Pt
crucible and ignite.
Carefully dip cleaned glass plate, while hot, in mixture of equal
parts of carnauba wax and paraffin, and let cool. Make distinctive
mark through wax with sharp instrument, taking care not to scratch
surface of glass.

Add few drops H2SO4 to residue in crucible and cover crucible


with waxed plate, having mark over center of crucible and making
sure edge of crucible is in close contact with plate. Keep top surface
of plate cool, and heat crucible 1 h at as high temperature as
practi ca ble without melting wax (electric stove gives most
satisfactory form of heat). If fluorides are present, distinct etching is
apparent on exposed glass.
(b) Applicable in presence of silicates.Mix small amount of
precipitated SiO2 with precipitated BaF2, (a), and proceed as in
975.28B or C (see 47.3.19). [This method is valuable for foods
which contain considerable amount of SiO2 in the ash. Under these
circumstances H2SO4 liberates SiF4, which would escape detection
in (a).]
References: Chem. News 91, 39(1905)
Ann. Rept. Mass. State Bd. Health (1905) p. 498.

2005 AOAC INTERNATIONAL