11.1.

23
AOAC Official Method 920.199
Calcium in Water
Gravimetric Method
First Action 1920
Final Action
Concentrate Solution Y, 920.196 (see 11.1.19), to 150–200 mL,
and to this solution, containing equivalent of ≤0.6 g CaO or 1 g
Mg2P2O7, add 1–2 g H2C2O4⋅2H2O and enough HCl (1 + 1) to clear
solution. Heat to bp and neutralize with NH4OH, stirring constantly.
Add NH4OH in slight excess and let stand 3 h in warm place. Filter
supernate and wash precipitate once or twice by decantation with
1% (NH4)2C2O4 solution. Dissolve precipitate in HCl (1 + 1), dilute
to 100–200 mL, add little more H2C2O4, and precipitate as above.
After letting precipitate stand 3 h, filter, wash with 1% (NH4)2C2O4
solution, dry, ignite, heat over blast lamp at ≥950°C and weigh as
CaO and SrO. From this weight subtract weight SrO equivalent to
the Sr, 911.03 (see 11.1.24). Difference is weight CaO. Calculate as
Ca. Designate combined filtrates and washings as Solution Z.
As check on CaO, evaporate to dryness filtrate from the Sr(NO3)2
in 911.03 (see 11.1.24), be gin ning “Fil ter, and wash with
ether–alcohol mixture . . .”. Dissolve the Ca(NO3)2 in H2O,
precipitate as oxalate, filter, wash, ignite at 950°C, and weigh as
CaO. CaO × 0.7147 = Ca.

 2005 AOAC INTERNATIONAL