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    D. Monographs: Test Solution

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    KAMAL BEHL
    Calcium carbonate is a fine white powder that is odorless and contains 98-102% calcium carbonate. It effervesces and dissolves when added to water and acetic acid. Impurities should not exceed 0.2% hydrochloric acid-insoluble substances, free alkali levels should not cause a pink color with phenolphthalein, and heavy metals should not exceed 20 μg/g of lead. The substance is also tested for limits of alkali metals and magnesium, barium, and arsenic. Loss on drying after heating to 200°C for 4 hours should not exceed 2%.

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    D. Monographs: Test Solution

    Uploaded by

    KAMAL BEHL
    33 views2 pages
    Calcium carbonate is a fine white powder that is odorless and contains 98-102% calcium carbonate. It effervesces and dissolves when added to water and acetic acid. Impurities should not exceed 0.2% hydrochloric acid-insoluble substances, free alkali levels should not cause a pink color with phenolphthalein, and heavy metals should not exceed 20 μg/g of lead. The substance is also tested for limits of alkali metals and magnesium, barium, and arsenic. Loss on drying after heating to 200°C for 4 hours should not exceed 2%.

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    Calcium carbonate is a fine white powder that is odorless and contains 98-102% calcium carbonate. It effervesces and dissolves when added to water and acetic acid. Impurities should not exceed 0.2% hydrochloric acid-insoluble substances, free alkali levels should not cause a pink color with phenolphthalein, and heavy metals should not exceed 20 μg/g of lead. The substance is also tested for limits of alkali metals and magnesium, barium, and arsenic. Loss on drying after heating to 200°C for 4 hours should not exceed 2%.

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    © All Rights Reserved
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    33 views2 pages

    D. Monographs: Test Solution

    Uploaded by

    KAMAL BEHL
    Calcium carbonate is a fine white powder that is odorless and contains 98-102% calcium carbonate. It effervesces and dissolves when added to water and acetic acid. Impurities should not exceed 0.2% hydrochloric acid-insoluble substances, free alkali levels should not cause a pink color with phenolphthalein, and heavy metals should not exceed 20 μg/g of lead. The substance is also tested for limits of alkali metals and magnesium, barium, and arsenic. Loss on drying after heating to 200°C for 4 hours should not exceed 2%.

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    of 2

    D.

    MONOGRAPHS

    Calcium Carbonate
    CaCO3

    Mol. Wt. 100.09


    471-34-1

    Content

    Calcium Carbonate, when dried, contains 98.0102.0% of calcium

    carbonate (CaCO3).
    Description

    Calcium Carbonate occurs as a fine white powder. It is odorless.

    Identification

    To 1 g of Calcium Carbonate, add 10 ml of water and 7 ml of

    diluted acetic acid (1 4). It effervesces and dissolves. This solution, after being
    boiled and neutralized with ammonia TS, responds to all tests for Calcium Salt as
    described in the Qualitative Tests.
    Purity

    (1)

    Hydrochloric acid-insoluble substances

    Not more than 0.20%.

    Weigh 5.0 g of Calcium Carbonate, add 10 ml of water, and add dropwise


    gradually 12 ml of hydrochloric acid while stirring, and add water to make 200 ml.
    Filter through a filter paper for quantitative analysis (5C), wash thoroughly the
    residue on the filter paper with boiling water until the washings do not respond to
    the test for Chloride, incinerate together with the filter paper, and weigh the residue.
    (2)

    Free alkali

    Weigh 3.0 g of Calcium Carbonate, add 30 ml of freshly boiled

    and cooled water, shake for 3 minutes, and filter the solution. Measure 20 ml of the
    filtrate, and add 2 drops of phenolphthalein TS. Even if a pink color develops, it
    disappears when 0.20 ml of 0.1 mol/l hydrochloric acid is added.
    (3)

    Heavy metals

    Not more than 20 g/g as Pb.

    Test Solution Weigh 1.0 g of Calcium Carbonate, dissolve in 8 ml of diluted


    hydrochloric acid (1 4), add water to make about 20 ml, and add dropwise
    ammonia TS while shaking until slight white turbidity appears. Add 2 ml of diluted
    acetic acid (1 20) and water to make 50 ml.

    Control Solution To 2 ml of Lead Standard Solution, exactly measured, add 2 ml


    of diluted acetic acid (1 20) and water to make 50 ml.
    (4)

    Alkali metals and magnesium

    Not more than 1.0%.

    Weigh 1.0 g of Calcium Carbonate, dissolve by gradually adding 30 ml of diluted


    hydrochloric acid (1 10), expel carbon dioxide while boiling. Cool, neutralize with
    ammonia TS, add 60 ml of ammonium oxalate solution (1 25), and heat on a water
    bath for 1 hour. After cooling, add water to make 100 ml, stir thoroughly, and filter.
    Measure 50 ml of the filtrate, add 0.5 ml of sulfuric acid, evaporate to dryness, and
    ignite to constant weight, and weigh the residue.
    (5)

    Barium

    Not more than 0.030% as Ba.

    Test Solution Weigh 1.0 g of Calcium Carbonate, dissolve in 8 ml of diluted


    hydrochloric acid (1 4), add water to make 20 ml.

    D. MONOGRAPHS
    Control Solution To 0.30 ml of Barium Standard Solution, add water to make 20
    ml.

    Procedure Add 2 g of sodium acetate, 1 ml of diluted acetic acid (1 20), and


    0.5 ml of potassium chromate solution (1 20) to the test solution, and allow to
    stand for 15 minutes. The solution is not more turbid than the control solution.
    (6)

    Arsenic

    Not more than 4.0 g/g as As2O3.

    Test Solution Weigh 0.50 g of Calcium Carbonate, moisten with 1 ml of water,


    and dissolve in 4 ml of hydrochloric acid (1 4).

    Apparatus Apparatus B.
    Loss on Drying
    Assay

    Not more than 2.0% (200, 4 hours).

    Weigh accurately about 1 g of Calcium Carbonate, previously dried,

    gradually dissolve in 10 ml of diluted hydrochloric acid (1 4), gradually added, add


    water to make exactly 100 ml, and use this solution as the test solution. Proceed as
    directed under Method 1 in Calcium Salt Determination.
    1 ml of 0.05 mol/l EDTA = 5.004 mg of CaCO3

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