Calcium hydrogen phosphate dihydrate

EUROPEAN PHARMACOPOEIA 8.0

01/2013:0116 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
CALCIUM HYDROGEN PHOSPHATE solution to 500.0 mL with total-ionic-strength-adjustment
DIHYDRATE
buffer R (200 ppm F).
Indicator electrode : uoride-selective.
Calcii hydrogenophosphas dihydricus
Reference electrode : silver-silver chloride.
Carry out the measurement on 20.0 mL of the test solution.
CaHPO4,2H2O
Mr 172.1 Add at least 3 times 0.10 mL of the reference solution and
carry out the measurement after each addition. Calculate the
[7789-77-7]
concentration of uorides using the calibration curve.
DEFINITION
Sulfates : maximum 0.5 per cent.
Content : 98.0 per cent to 105.0 per cent.
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
CHARACTERS
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
Appearance : white or almost white, crystalline powder.
Solubility : practically insoluble in water and in ethanol (96 per with water R.
Reference solution. To 1.0 mL of 0.005 M sulfuric acid, add
cent). It dissolves in dilute hydrochloric acid and in dilute
1 mL of dilute hydrochloric acid R and dilute to 50 mL with
nitric acid.
water R. Filter if necessary.
IDENTIFICATION
To the test solution and to the reference solution, add 2 mL
A. Dissolve with heating 0.1 g in 10 mL of dilute hydrochloric 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
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 intense than that in the reference solution.
precipitate is produced.
Arsenic (2.4.2, Method A): maximum 10 ppm, determined
B. Dissolve 0.1 g in 5 mL of dilute nitric acid R, add 2 mL
on 2 mL of solution S.
of ammonium molybdate solution R and heat at 70 C for
Barium. To 0.5 g, add 10 mL of water R and heat to boiling.
2 min. A yellow precipitate is produced.
While stirring, add 1 mL of hydrochloric acid R dropwise.
C. It complies with the limits of the assay.
Allow to cool and lter if necessary. Add 2 mL of a 10 g/L
solution of dipotassium sulfate R and allow to stand for 10 min.
TESTS
No turbidity is produced.
Solution S. Dissolve 2.5 g in 20 mL of dilute hydrochloric
Iron (2.4.9) : maximum 400 ppm.
acid R, lter if necessary and add dilute ammonia R1 until a
Dilute 0.5 mL of solution S to 10 mL with water R.
precipitate is formed. Add just sufcient dilute hydrochloric
Heavy metals (2.4.8): maximum 40 ppm.
acid R to dissolve the precipitate and dilute to 50 mL with
distilled water R.
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
Acid-insoluble substances : maximum 0.2 per cent.
using lead standard solution (1 ppm Pb) R.
Dissolve 5.0 g in 40 mL of water R, add 10 mL of hydrochloric
Loss on ignition : 24.5 per cent to 26.5 per cent, determined
acid R and heat to boiling for 5 min. Cool, then collect the
on 1.000 g by ignition to constant mass at 800-825 C.
insoluble substances using ashless lter paper. Wash with
water R until turbidity is no longer produced when silver
ASSAY
nitrate solution R2 is added to the ltrate. Ignite at 600 50 C.
Dissolve 0.4 g in 12 mL of dilute hydrochloric acid R by heating
The residue weighs not more than 10 mg.
on a water bath if necessary and dilute to 200 mL with water R.
Carbonates. Shake 0.5 g with 5 mL of carbon dioxide-free
To 20.0 mL of this solution add 25.0 mL of 0.02 M sodium
water R and add 1 mL of hydrochloric acid R. No effervescence
edetate, 50 mL of water R, 5 mL of ammonium chloride buffer
is produced.
solution pH 10.7 R and about 25 mg of mordant black 11
Chlorides : maximum 0.25 per cent.
triturate R. Titrate the excess of sodium edetate with 0.02 M
Test solution. Dissolve 0.20 g in a mixture of 20 mL of water R zinc sulfate. Carry out a blank titration.
and 13 mL of dilute nitric acid R by warming if necessary,
1 mL of 0.02 M sodium edetate is equivalent to 3.44 mg
dilute to 100 mL with water R and lter if necessary. Use
of CaHPO4,2H2O.
50 mL of this solution.
FUNCTIONALITY-RELATED CHARACTERISTICS
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. This section provides information on characteristics that are
recognised as being relevant control parameters for one or
Add 1 mL of silver nitrate solution R2 to the test solution and more functions of the substance when used as an excipient
to the reference solution and mix. After standing for 5 min
(see chapter 5.15). Some of the characteristics described in
protected from light, any opalescence in the test solution is
the Functionality-related characteristics section may also be
not more intense than that in the reference solution.
present in the mandatory part of the monograph since they
Fluorides : maximum 100 ppm.
also represent mandatory quality criteria. In such cases, a
cross-reference to the tests described in the mandatory part is
Potentiometry (2.2.36, Method II).
included in the Functionality-related characteristics section.
Chelating solution. Dissolve 45 g of cyclohexylenedinitrilotetra- Control of the characteristics can contribute to the quality
acetic acid R in 75 mL of sodium hydroxide solution R and
of a medicinal product by improving the consistency of the
dilute to 250 mL with water R.
manufacturing process and the performance of the medicinal
Test solution. Dissolve 1.000 g in 4 mL of hydrochloric acid R1, product during use. Where control methods are cited, they are
add 20 mL of chelating solution, 2.7 mL of glacial acetic acid R recognised as being suitable for the purpose, but other methods
and 2.8 g of sodium chloride R, adjust to pH 5-6 with sodium can also be used. Wherever results for a particular characteristic
are reported, the control method must be indicated.
hydroxide solution R and dilute to 50.0 mL with water R.

1742

See the information section on general monographs (cover pages)

Calcium lactate, anhydrous

EUROPEAN PHARMACOPOEIA 8.0

The following characteristics may be relevant for calcium

hydrogen phosphate dihydrate used as filler in tablets and
capsules.
Particle-size distribution (2.9.31 or 2.9.38).
Bulk and tapped density (2.9.34).
Powder ow (2.9.36).

CALCIUM

Heavy metals (2.4.8): maximum 20 ppm.

Dissolve 1.0 g in 10 mL of hydrochloric acid R1 and evaporate
to dryness on a water-bath. Dissolve the residue in 20 mL of
water R and lter. 12 mL of the ltrate complies with test A.
Prepare the reference solution using lead standard solution
(1 ppm Pb) R.

ASSAY
To 1.500 g in a mortar, add 20-30 mL of water R and 0.5 mL of
01/2008:1078 phenolphthalein solution R. Titrate with 1 M hydrochloric acid
by triturating the substance until the red colour disappears.
The nal solution is used in the tests for carbonates.
HYDROXIDE
1 mL of 1 M hydrochloric acid is equivalent to 37.05 mg
of Ca(OH)2.

Calcii hydroxidum
Ca(OH)2
[1305-62-0]

01/2008:2118
corrected 6.0

Mr 74.1

DEFINITION
Content : 95.0 per cent to 100.5 per cent.

CALCIUM LACTATE, ANHYDROUS

Calcii lactas anhydricus

CHARACTERS
Appearance : white or almost white, ne powder.
Solubility : practically insoluble in water.
IDENTIFICATION
A. To 0.80 g in a mortar, add 10 mL of water R and 0.5 mL of
phenolphthalein solution R and mix. The suspension turns
red. On addition of 17.5 mL of 1 M hydrochloric acid, the
suspension becomes colourless without effervescing. The
red colour occurs again when the mixture is triturated for
1 min. On addition of a further 6 mL of 1 M hydrochloric
acid and triturating, the solution becomes colourless.
B. Dissolve about 0.1 g in dilute hydrochloric acid R and
dilute to 10 mL with water R. 5 mL of the solution give
reaction (b) of calcium (2.3.1).
TESTS
Matter insoluble in hydrochloric acid : maximum 0.5 per
cent.
Dissolve 2.0 g in 30 mL of hydrochloric acid R. Boil the
solution and lter. Wash the residue with hot water R. The
residue weighs a maximum of 10 mg.
Carbonates : maximum 5.0 per cent of CaCO3.
Add 5.0 mL of 1 M hydrochloric acid to the titrated solution
obtained under Assay and titrate with 1 M sodium hydroxide
using 0.5 mL of methyl orange solution R as indicator.
1 mL of 1 M hydrochloric acid is equivalent to 50.05 mg
of CaCO3.
Chlorides (2.4.4): maximum 330 ppm.
Dissolve 0.30 g in a mixture of 2 mL of nitric acid R and 10 mL
of water R and dilute to 30 mL with water R.
Sulfates (2.4.13) : maximum 0.4 per cent.
Dissolve 0.15 g in a mixture of 5 mL of dilute hydrochloric
acid R and 10 mL of distilled water R and dilute to 60 mL with
distilled water R.
Arsenic (2.4.2, Method A) : maximum 4 ppm.
Dissolve 0.50 g in 5 mL of brominated hydrochloric acid R and
dilute to 50 mL with water R. Use 25 mL of this solution.
Magnesium and alkali metals : maximum 4.0 per cent
calculated as sulfates.
Dissolve 1.0 g in a mixture of 10 mL of hydrochloric acid R
and 40 mL of water R. Boil and add 50 mL of a 63 g/L solution
of oxalic acid R. Neutralise with ammonia R and dilute to
200 mL with water R. Allow to stand for 1 h and lter through
a suitable lter. To 100 mL of the ltrate, add 0.5 mL of
sulfuric acid R. Cautiously evaporate to dryness and ignite.
The residue weighs a maximum of 20 mg.
General Notices (1) apply to all monographs and other texts

C6H10CaO6

Mr 218.2

DEFINITION
Calcium bis(2-hydroxypropanoate) or mixture of calcium
(2R)-, (2S)- and (2RS)-2-hydroxypropanoates.
Content : 98.0 per cent to 102.0 per cent (dried substance).
CHARACTERS
Appearance : white or almost white, crystalline or granular
powder.
Solubility : soluble in water, freely soluble in boiling water, very
slightly soluble in ethanol (96 per cent).
IDENTIFICATION
A. Loss on drying (see Tests).
B. It gives the reaction of lactates (2.3.1).
C. It gives reaction (b) of calcium (2.3.1).
TESTS
Solution S. Dissolve 5.0 g with heating in carbon dioxide-free
water R prepared from distilled water R, allow to cool and
dilute to 100 mL with the same solvent.
Appearance of solution. Solution S is not more opalescent
than reference suspension II (2.2.1) and not more intensely
coloured than reference solution BY6 (2.2.2, Method II).
Acidity or alkalinity. To 10 mL of solution S add 0.1 mL of
phenolphthalein solution R and 0.5 mL of 0.01 M hydrochloric
acid. The solution is colourless. Not more than 2.0 mL of
0.01 M sodium hydroxide is required to change the colour of
the indicator to pink.
Chlorides (2.4.4) : maximum 200 ppm.
Dilute 5 mL of solution S to 15 mL with water R.
Sulfates (2.4.13): maximum 400 ppm.
Dilute 7.5 mL of solution S to 15 mL with distilled water R.
Barium. To 10 mL of solution S add 1 mL of calcium sulfate
solution R. Allow to stand for 15 min. Any opalescence in the
solution is not more intense than that in a mixture of 1 mL of
distilled water R and 10 mL of solution S.
Iron (2.4.9) : maximum 50 ppm.
Dilute 4 mL of solution S to 10 mL with water R.
Magnesium and alkali salts : maximum 1 per cent.
To 20 mL of solution S add 20 mL of water R, 2 g of ammonium
chloride R and 2 mL of dilute ammonia R1. Heat to boiling

1743