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    1.3.04 AOAC Official Method 917.02 Calcium in Liming Materials

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    1.3.04 AOAC Official Method 917.02 Calcium in Liming Materials

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    Anju Doraisamy
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    AOAC91702

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    1.3.04 AOAC Official Method 917.02 Calcium in Liming Materials

    Uploaded by

    Anju Doraisamy

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    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
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    1.3.

    04 filtrates and washings from both precipitations for determination of


    AOAC Official Method 917.02 Mg, 919.01B (see 1.3.05).
    Calcium in Liming Materials Complete determination by one of following methods and report
    Gravimetric Method as percent CaO:
    First Action 1917 (a) Ignite precipitate in crucible, either over S-free blast lamp, or
    Final Action 1965 in electric furnace at 950°C, to constant weight, cool in desiccator,
    and weigh as CaO.
    Concentrate combined filtrates and washings from 917.01 (see (b) Incinerate filter over low flame, mix ignited precipitate with
    1.3.03) to ca 50 mL; make slightly alkaline with NH4OH (1 + 1); finely pulverized and dried mixture of equal parts of (NH4)2SO4 and
    while still hot, add saturated (NH4)2C2O4 solution dropwise as long NH4Cl, and drive off excess sulfate by carefully heating upper portion
    as any precipiate forms, and then enough excess to convert Mg salts of crucible. Complete ignition, cool in desiccator, and weigh as CaSO4.
    also to oxalate. Heat to bp, let stand 3 h, decant clear solution through (c) Perforate apex of cone; wash CaC2O4 precipitate into beaker
    filter, pour 15–20 mL hot H2O on precipitate, and again decant clear used for precipitation; then wash filter with hot H2SO4 (1 + 4), and ti-
    solution through filter. Dissolve any precipitate remaining on filter trate at 85°–90°C with 0.1M KMnO4.
    by washing with hot HCl (1 + 9) into original beaker, wash 6 times
    with hot H2O, and then reprecipitate at bp by adding NH4OH and a References: U.S. Geol. Survey Bull. 700, p. 106.
    little saturated (NH4)2C2O4 solution. Let stand as before, filter Ind. Eng. Chem. 9, 1114(1917).
    through same filter, and wash with hot H2O until Cl-free. Reserve CAS-1305-78-8 (calcium oxide)

    © 2000 AOAC INTERNATIONAL

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