11.1.

18
AOAC Official Method 920.195
Silica in Water
Gravimetric Method
First Action 1920
Final Action
Make preliminary examination, using 100–250 mL specimen, to
determine approximate amount of Ca and Mg present, in order to
determine amount of specimen to be evaporated for final analysis.
Evaporate amount of spec imen equivalent to 0.1–0.6 g CaO or
0.1–1 g Mg2P2O7 (usually 1–5 L). Acidify specimen with HCl and
evaporate on steam bath to dry ness in Pt dish. Continue dry ing ca
1 h. Thoroughly moisten residue with 5–10 mL HCl. Let stand
10–15 min and add enough H2O to bring soluble salts into solution.
Heat on steam bath until salts dissolve. Filter to remove most of SiO2
and wash thoroughly with hot water. Evaporate filtrate to dryness
and treat residue with 5 mL HCl and enough H2O to dissolve soluble
salts, as before. Heat, filter, and wash thoroughly with hot water.
Designate filtrate as Solution X.
Transfer the 2 residues to Pt crucible, ignite, heat over blast lamp,
and weigh. Moisten contents of crucible with few drops H2O, add
few drops H2SO4 and few mL HF, and evaporate on steam bath under
hood. Repeat treatment if all SiO2 is not volatilized. Dry carefully on
hot plate, ignite, heat over blast lamp, and weigh. Difference
between the two weights is weight SiO2. Add weight residue (Fe2O3
+ Al2O3) to that of Al2O3 and Fe2O3 obtained in 920.196 (see
11.1.19). [If residue weighs >0.5 mg, BaSO4 may be present in
specimen. If so, make necessary correction and add to weight Fe2O3
and Al2O3 in 920.196 (see 11.1.19).]

 2005 AOAC INTERNATIONAL