4.8.03 AOAC of Fi Cial Method 927.02 Cal Cium in An I Mal Feed
4.8.03 AOAC of Fi Cial Method 927.02 Cal Cium in An I Mal Feed
4.8.03 AOAC of Fi Cial Method 927.02 Cal Cium in An I Mal Feed
03
AOAC Official Method 927.02
Calcium in Animal Feed
Dry Ash Method
First Action 1927
Final Action 1945
(Applicable to mineral feeds only.)
Weigh 2 g finely ground test portion into SiO2 or porcelain dish
and ignite in furnace to C-free ash, but avoid fusing. Boil residue in
40 mL HCl (1 + 3) and few drops HNO3. Transfer to 250 mL
volumetric flask, cool, dilute to volume, and mix thoroughly. Pipet
25 mL clear liquid into beaker, dilute to ca 100 mL, and add 2 drops
methyl red, 984.13B(c) (see 4.2.09). Add NH4OH (1 + 1) dropwise
to pH 5.6, as shown by in ter me di ate brown ish-orange. If
overstepped, add HCl (1 + 3) with dropper to orange. Add 2 more
drops HCl (1 + 3). Color should now be pink (pH 2.5–3.0), not
orange. Dilute to ca 150 mL, bring to boil, and slowly add, with
con stant stir ring, 10 mL hot sat u rated (4.2%) so lu tion of
(NH4)2C2O4. If red changes to orange or yellow, add HCl (1 + 3)
dropwise until color again changes to pink. Let stand overnight for
precipitate to settle. Filter supernate through quantitative paper,
Gooch, or fritted glass filter (fine Pyrex is preferable), and wash
precipitate thoroughly with NH4OH (1 + 50). Place paper or crucible
with precipitate in original beaker, and add mixture of 125 mL H2O
and 5 mL H2SO4. Heat to 70°C and titrate with 0.02M KMnO4,
940.35 (see A.1.10), to first slight pink. Presence of paper may cause
color to fade in few s. Correct for blank and calculate percent Ca.
CAS-7440-70-2 (calcium)