Calcium Carbonate

001-1706PDG.

pdf

1 Calcium Carbonate
2
3
4 CaCO3: 100.09 [471-34-1]
5 Calcium Carbonate contains not less than 98.5% and not more than 100.5% of CaCO3,
6 calculated on the dried basis.
7
8 Identification
9 (1) Neutralize 10 mL of the sample solution obtained in the Purity (2) with ammonia
10 TS: the solution yields a white precipitate with ammonium oxalate TS. The separated
11 precipitate does not dissolve in dilute acetic acid, but dissolves in dilute hydrochloric acid.
12 (2) Carbonates effervesce upon addition of dilute hydrochloric acid, generating a gas,
13 which produces a white precipitate immediately, when passed into calcium hydroxide TS.
14
15 Purity
16 (1) Acid-insoluble substances --- To 5.0 g of Calcium Carbonate add 50 mL of water,
17 then add 20 mL of hydrochloric acid dropwise with stirring, boil for 5 minutes, cool, add
18 water to make 200 mL, and filter through filter paper for quantitative analysis. Wash
19 the residue until the last washing shows no turbidity with silver nitrate TS, and ignite
20 the residue together with the filter paper: the mass of the residue is not more than 10.0
21 mg.
22 (2) Chloride --- Dissolve 5.0 g of Calcium Carbonate in 80 mL of 2 mol/L acetic acid TS.
23 When the effervescence ceases, boil for 2 minutes. After cooling add 2 mol/L acetic acid
24 TS to make 100 mL, filter, if necessary, through a sintered glass filter, and use this
25 solution as the sample solution. Transfer 10 mL of the sample solution to a Nessler tube,
26 add 6 mL of dilute nitric acid and water to make 50 mL, and use this solution as the test
27 solution. Transfer 0.45 mL of 0.01 mol/L hydrochloric acid Standard Solution for
28 Volumetric Analysis to another Nessler tube, add 6 mL of dilute nitric acid and water to
29 make 50 mL, and use this solution as the control solution. When the test solution is not
30 clear, filter both solutions using the same procedure. Add 1 mL of silver nitrate TS to the
31 test solution and to the control solution, mix well, and allow to stand for 5 minutes
32 protecting from light. Compare the opalescence developed in both solutions against a
33 black background by viewing downward or transversely. The opalescence developed in
34 the test solution is not more than that of the control solution (not more than 0.032 %).
35 (3) Sulfate --- Transfer 2 mL of the sample solution obtained in (2) to a Nessler tube,
36 add 1 mL of dilute hydrochloric acid and dilute with water to make 50 mL, and use this

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001-1706PDG.pdf
37 solution as the test solution. Transfer 0.5 mL of 0.005 mol/L sulfuric acid Standard
38 Solution for Volumetric Analysis to another Nessler tube, add 1 mL of dilute hydrochloric
39 acid and water to make 50 mL, and use this solution as the control solution. When the
40 test solution is not clear, filter both solutions according to the same procedure. Add 2 mL
41 of barium chloride TS to the test solution and to the control solution, mix well, and allow
42 to stand for 10 minutes. Compare the white turbidity produced in both solutions against
43 a black background by viewing downward or transversely. The turbidity produced in the
44 test solution is not thicker than that of the control solution (not more than 0.24 %).
45 (4) Iron --- To 0.10 g of Calcium Carbonate add 10 mL of dilute hydrochloric acid, and
46 dissolve by warming if necessary. Dissolve 0.5 g of L-tartaric acid, and add one drop of
47 phenolphthalein TS. Add ammonia TS dropwise until the solution develops a pale red
48 color. Add 20 mL of acetic acid-sodium acetate buffer solution for iron limit test, pH 4.5,
49 and designate this solution as the test solution. Prepare the control solution as follows:
50 To 2.0 mL of Standard Iron Solution add 10 mL of dilute hydrochloric acid, and proceed
51 as directed for the test solution. Transfer the test solution and the control solution to
52 separate Nessler tubes, to each add 2 mL of a solution of L-ascorbic acid (1 in 100), mix
53 well, and allow to stand for 30 minutes. Add 1 mL of a solution of 2,2’-bipyridyl in ethanol
54 (95) (1 in 200), add water to make 50 mL, and allow to stand for 30 minutes. Then
55 compare the colors developed in both solutions against a white background. The test
56 solution has no more color than the control solution (not more than 200 ppm).
57 (5) Barium --- Mix 1.0 g of Calcium Carbonate with 10 mL of water, add dropwise 4 mL
58 of hydrochloric acid with stirring, boil for 5 minutes, cool, add water to make 40 mL,
59 filter and use this filtrate as the sample solution. Use a platinum wire of about 0.8 mm
60 in diameter and of the end part of it being straight for flame coloration test. Immerse the
61 end of the platinum wire into the sample solution to about 5 mm in length, remove from
62 the sample solution gently, and test by putting the end part in a colorless flame, keeping
63 the platinum wire horizontal: no green color appears.
64 (6) Magnesium and alkali metals --- Dissolve 1.0 g of Calcium Carbonate in a mixture
65 of 20 mL of water and 10 mL of dilute hydrochloric acid, boil, neutralize with ammonia
66 TS, and add ammonium oxalate TS until precipitation of calcium oxalate is completed.
67 Heat the mixture on a water bath for 1 hour, cool, dilute with water to 100 mL, shake
68 well, and filter. To 50 mL of the filtrate in a tared platinum dish, add 0.5 mL of sulfuric
69 acid, evaporate to dryness, and ignite at 600℃ to constant mass: the mass of the residue
70 is not more than 5.0 mg.
71 (7) Arsenic --- Moisten 0.40 g of Calcium Carbonate with 1 mL of water, then dissolve
72 in 4 mL of dilute hydrochloric acid, use this solution as the test solution, and perform
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001-1706PDG.pdf
73 the test (not more than 5 ppm).

74
75 Loss on drying Not more than 1.0% (2 g, 200℃, 4 hours)
76
77 Assay Weigh accurately about 0.12 g of Calcium Carbonate and dissolve in 20 mL of
78 water and 3 mL of dilute hydrochloric acid. Add 80 mL of water, 15 mL of a solution of
79 potassium hydroxide (1 in 10) and 0.05 g of NN indicator, and titrate immediately with
80 0.05 mol/L disodium dihydrogen ethylenediamine tetraacetate Standard Solution for
81 Volumetric Analysis until the color of the solution changes from red-purple to blue.
82 Each mL of 0.05 mol/L disodium dihydrogen ethylenediamine tetraacetate Standard
83 Solution for Volumetric Analysis
84 ＝ 5.005 mg of CaCO3
85
86 Reagents
87 Dilute hydrochloric acid Dilute 23.6 mL of hydrochloric acid with water to make
88 100mL (10%).
89 Silver nitrate TS Dissolve 17.5 g of silver nitrate in water to make 1000 mL (0.1
90 mol/L). Preserve in light-resistant containers.
91 Dilute nitric acid Dilute 10.5 mL of nitric acid with water to make 100 mL (10%).
92 2 mol/L Acetic acid TS Dilute 12 g of acetic acid (100) with water to make 100 mL.
93 Barium chloride TS Dissolve 12 g of barium chloride dihydrate in water to make 100
94 mL (0.5 mol/L).
95 Phenolphthalein TS Dissolve 1 g of phenolphthalein in 100 mL of ethanol (95).
96 Acetic acid-sodium acetate buffer solution for iron limit test, pH 4.5 Dissolve 75.4 mL
97 of acetic acid (100) and 111 g of sodium acetate trihydrate in 1000 mL of water.
98 Ammonia TS To 400 mL of ammonia solution (28) add water to make 1000 mL (10%).
99 Standard Iron Solution Weigh exactly 86.3 mg of ammonium iron (III) sulfate
100 dodecahydrate, dissolve in 100 mL of water, and add 5 mL of dilute hydrochloric acid
101 and water to make exactly 1000 mL. Each mL of this solution contains 0.01 mg of iron
102 (Fe).
103 Ammonium oxalate TS Dissolve 3.5 g ammonium oxalate monohydrate in water to
104 make 100 mL (0.25 mol/L)
105 2,2’-Bipyridyl （2,2’-Bipyridine, α,α’-Dipyridyl） C10H8N2 [JIS K 8486,Special
106 class]
107 White or faintly colored crystals. Freely soluble in ethanol (95), in diethyl ether, in
108 chloroform and in benzene, and sparingly soluble in water.
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001-1706PDG.pdf
109 Melting point: 69.5 - 72℃.

110 Purity (1) Clarity of solution―Dissolve 0.5 g of 2,2’-Bipyridyl in ethanol (95) to make 10
111 mL: the solution is clear.
112 (2) Iron―Not more than 0.001 %
113 Residue on ignition―not more than 0.1 %
114 Sensitiveness―Measure exactly 5 mL of standard iron solution (0.01 mg Fe/mL) , add
115 water to make 10 mL and add 3 mL of ammonium acetate solution (1 in 4). Adjust the
116 pH of this solution to 3.5 to 5.0 with approximately 3 mL of a mixture of water and acetic
117 acid (2:1), add 0.5 mL of hydroxylammonium chloride solution (1 in 10), shake well and
118 allow to stand for 10 minutes. To this solution add exactly 0.5 mL of a solution, prepared
119 by dissolving 0.100 g of 2,2’-bipyridyl in ethanol (95) to make 100 mL, and add water to
120 make exactly 20 mL. Determine the absorbance of this solution at the wavelength of
121 maximum absorption at about 520 nm in a 1-cm cell using a blank solution prepared in
122 the same manner as directed in the above except adding the standard iron solution (0.01
123 mg Fe/mL) as the control solution: the absorbance is not less than 0.32.
124 NN indicator Mix 0.5 g of 2-hydroxy-1-(2-hydroxy-4-sulfo-1-naphthylazo)-3-naphthoic
125 acid with 50 g of anhydrous sodium sulfate, and triturate until the mixture becomes
126 homogeneous.
127
128

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001-1706PDG.

73 the test (not more than 5 ppm).

109 Melting point: 69.5 - 72℃.

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