Dibasic Calcium Phosphate

Dibasic Calcium Phosphate

(Calcium Hydrogen Phosphate Dihydrate,

CaHPO4,2H20 172.1

DEFINITION
Content
98.0 per cent to 105.0 per cent.
CHARACTERS
Appearance
White or almost white, crystalline powder.
Solubility
Practically insoluble in water and in ethanol (96 per cent). It dissolves in dilute hydrochloric acid and in
dilute nitric acid.
IDENTIFICATION
A. Dissolve with heating 0.1 g in 10 mL of dilute hydrochloric acid R. Add 2.5 mL of dilute ammonia R1,
shake and add 5 mL of a 35 g/L solution of ammonium oxalate R. A white precipitate is produced.
B. Dissolve 0.1 g in 5 mL of dilute nitric acid R, add 2 mL of ammonium molybdate solution R and heat at
70 °C for 2 min. A yellow precipitate is produced.
C. It complies with the limits of the assay.
TESTS
Solution S
Dissolve 2.5 g in 20 mL of dilute hydrochloric acid R, filter if necessary and add dilute ammonia R1 until a
precipitate is formed. Add just sufficient dilute hydrochloric acid R to dissolve the precipitate and dilute to
50 mL with distilled water R.
Acid-insoluble substances
Maximum 0.2 per cent.
Dissolve 5.0 g in 40 mL of water R, add 10 mL of hydrochloric acid R and heat to boiling for 5 min. Cool,
then collect the insoluble substances using ashless filter paper. Wash with water R until turbidity is no
longer produced when silver nitrate solution R2 is added to the filtrate. Ignite at 600 ± 50 °C. The residue
weighs not more than 10 mg.
Carbonates
Shake 0.5 g with 5 mL of carbon dioxide-free water R and add 1 mL of hydrochloric acid R. No
effervescence is produced.
Chlorides
Test solution Dissolve 0.20 g in a mixture of 20 mL of water R and 13 mL of dilute nitric acid R, dilute
to 100 mL with water R and filter if necessary. Use 50 mL of this solution.
Reference solution To 0.70 mL of 0.01 M hydrochloric acid , add 6 mL of dilute nitric acid R and
dilute to 50 mL with water R.
Add 1 mL of silver nitrate solution R2 to the test solution and to the reference solution and mix. After
standing for 5 min protected from light, any opalescence in the test solution is not more intense than that
in the reference solution.
Fluorides
Maximum 100 ppm.
Potentiometry (2.2.36, Method II).
Chelating solution Dissolve 45 g of cyclohexylenedinitrilotetra-acetic acid R in 75 mL of sodium

hydroxide solution R and dilute to 250 mL with water R.
Test solution Dissolve 1.000 g in 4 mL of hydrochloric acid R1, add 20 mL of chelating solution, 2.7
mL of glacial acetic acid R and 2.8 g of sodium chloride R, adjust to pH 5-6 with sodium hydroxide
solution R and dilute to 50.0 mL with water R.
Reference solution Dissolve 4.42 g of sodium fluoride R, previously dried at 300 °C for 12 h, in water
R and dilute to 1000.0 mL with the same solvent. Dilute 50.0 mL of this solution to 500.0 mL with total-
ionic-strength-adjustment buffer R (200 ppm F).
Indicator electrode Fluoride-selective.
Reference electrode Silver-silver chloride.
Carry out the measurement on 20.0 mL of the test solution. Add at least 3 times 0.10 mL of the reference
solution and carry out the measurement after each addition. Calculate the concentration of fluorides
using the calibration curve.
Sulfates
Test solution Dissolve 0.5 g in a mixture of 5 mL of water R and 5 mL of dilute hydrochloric acid R
and dilute to 100 mL with water R. Filter if necessary. To 20 mL of this solution, add 1 mL of dilute
hydrochloric acid R and dilute to 50 mL with water R.
Reference solution To 1.0 mL of 0.005 M sulfuric acid , add 1 mL of dilute hydrochloric acid R and
dilute to 50 mL with water R. Filter if necessary.
To the test solution and to the reference solution, add 2 mL of a 120 g/L solution of barium chloride R
and allow to stand for 10 min. Any opalescence in the test solution is not more intense than that in the
reference solution.
Arsenic (2.4.2, Method A)
Maximum 10 ppm, determined on 2 mL of solution S.
Barium
To 0.5 g, add 10 mL of water R and heat to boiling. While stirring, add 1 mL of hydrochloric acid R
dropwise. Allow to cool and filter if necessary. Add 2 mL of a 10 g/L solution of dipotassium sulfate R and
allow to stand for 10 min. No turbidity is produced.
Iron (2.4.9)
Maximum 400 ppm.
Dilute 0.5 mL of solution S to 10 mL with water R.
Heavy metals (2.4.8)
Maximum 40 ppm.
Dilute 10 mL of solution S to 20 mL with water R. 12 mL of the solution complies with test A. Prepare the
reference solution using lead standard solution (1 ppm Pb) R.
Loss on ignition
24.5 per cent to 26.5 per cent, determined on 1.000 g by ignition to constant mass at 800-825 °C.
ASSAY
Dissolve 0.4 g in 12 mL of dilute hydrochloric acid R and dilute to 200 mL with water R. To 20.0 mL of this
solution add 25.0 mL of 0.02 M sodium edetate, 50 mL of water R, 5 mL of ammonium chloride buffer
solution pH 10.7 R and about 25 mg of mordant black 11 triturate R. Titrate the excess of sodium edetate
with 0.02 M zinc sulfate. Carry out a blank titration.
1 mL of 0.02 M sodium edetate is equivalent to 3.44 mg of CaHPO 4,2H2O.

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Dibasic Calcium Phosphate

(Calcium Hydrogen Phosphate Dihydrate,

98.0 per cent to 105.0 per cent.

White or almost white, crystalline powder.

C. It complies with the limits of the assay.

Maximum 0.2 per cent.

Maximum 0.25 per cent.

Maximum 100 ppm.

Potentiometry (2.2.36, Method II).

Chelating solution Dissolve 45 g of cyclohexylenedinitrilotetra-acetic acid R in 75 mL of sodium

Indicator electrode Fluoride-selective.

Reference electrode Silver-silver chloride.

Maximum 0.5 per cent.

Arsenic (2.4.2, Method A)

Maximum 10 ppm, determined on 2 mL of solution S.

Maximum 400 ppm.

Dilute 0.5 mL of solution S to 10 mL with water R.

Heavy metals (2.4.8)

1 mL of 0.02 M sodium edetate is equivalent to 3.44 mg of CaHPO 4,2H2O.

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