EUROPEAN PHARMACOPOEIA 6.

0 Silica, colloidal hydrated

01/2008:0434 01/2008:0738
corrected 6.0 corrected 6.0

SILICA, COLLOIDAL ANHYDROUS SILICA, COLLOIDAL HYDRATED

Silica colloidalis anhydrica Silica colloidalis hydrica
SiO2 Mr 60.1
[63231-67-4]
[7631-86-9]
DEFINITION DEFINITION
Colloidal anhydrous silica contains not less than 99.0 per Colloidal hydrated silica contains not less than 98.0 per cent
cent and not more than the equivalent of 100.5 per cent of and not more than the equivalent of 100.5 per cent of SiO2
SiO2, determined on the ignited substance. (Mr 60.1), determined on the ignited substance.

CHARACTERS CHARACTERS
A light, fine, white or almost white, amorphous powder, with A white or almost white, light, fine, amorphous powder,
a particle size of about 15 nm, practically insoluble in water practically insoluble in water and in mineral acids, with the
and in mineral acids except hydrofluoric acid. It dissolves in exception of hydrofluoric acid. It dissolves in hot solutions
hot solutions of alkali hydroxides. of alkali hydroxides.
IDENTIFICATION IDENTIFICATION
About 20 mg gives the reaction of silicates (2.3.1). A. About 20 mg gives the reaction of silicates (2.3.1).
TESTS B. When heated in an oven at 100 °C to 105 °C for 2 h, it
shows a loss of mass not less than 3.0 per cent.
pH (2.2.3). Shake 1.0 g with 30 ml of carbon dioxide-free
water R. The pH of the suspension is 3.5 to 5.5. TESTS
Chlorides (2.4.4). To 1.0 g add a mixture of 20 ml of dilute Solution S. To 2.5 g add 50 ml of hydrochloric acid R and
nitric acid R and 30 ml of water R and heat on a water-bath mix. Heat on a water-bath for 30 min, stirring from time
for 15 min, shaking frequently. Dilute to 50 ml with water R to time. Maintain the original volume by adding dilute
if necessary, filter and cool. 10 ml of the filtrate diluted to
hydrochloric acid R. Evaporate to dryness. Add to the
15 ml with water R complies with the limit test for chlorides residue a mixture of 8 ml of dilute hydrochloric acid R and
(250 ppm). 24 ml of water R. Heat to boiling and filter under reduced
Heavy metals (2.4.8). Suspend 2.5 g in sufficient water R to pressure through a sintered-glass filter (16) (2.1.2). Wash
produce a semi-fluid slurry. Dry at 140 °C. When the dried the residue on the filter with a hot mixture of 3 ml of dilute
substance is white, break up the mass with a glass rod. Add hydrochloric acid R and 9 ml of water R. Wash with small
25 ml of 1 M hydrochloric acid and boil gently for 5 min, quantities of water R, combine the filtrate and washings and
stirring frequently with the glass rod. Centrifuge for 20 min dilute to 50 ml with water R.
and filter the supernatant liquid through a membrane filter. pH (2.2.3). Suspend 1.0 g in 30 ml of a 75 g/l solution of
To the residue in the centrifuge tube add 3 ml of dilute potassium chloride R. The pH of the suspension is 4.0 to 7.0.
hydrochloric acid R and 9 ml of water R and boil. Centrifuge
for 20 min and filter the supernatant liquid through the same Water-absorption capacity. In a mortar, triturate 5 g with
membrane filter. Wash the residue with small quantities of 5 ml of water R, added drop by drop. The mixture remains
water R, combine the filtrates and washings and dilute to powdery.
50 ml with water R. To 20 ml of the solution add 50 mg Substances soluble in hydrochloric acid. In a platinum
of ascorbic acid R and 1 ml of concentrated ammonia R. dish, evaporate to dryness 10.0 ml of solution S and dry to
Neutralise with dilute ammonia R2. Dilute to 25 ml with constant mass at 100 °C to 105 °C. The mass of the residue
water R. 12 ml of the solution complies with limit test A for is not more than 10 mg (2.0 per cent).
heavy metals (25 ppm). Prepare the standard using lead Chlorides (2.4.4). Heat 0.5 g with 50 ml of water R on a
standard solution (1 ppm Pb) R. water-bath for 15 min. Dilute to 100 ml with water R and
Loss on ignition. Not more than 5.0 per cent, determined on centrifuge at 1500 g for 5 min. 10 ml of the supernatant
0.200 g by ignition in a platinum crucible at 900 ± 50 °C for solution diluted to 15 ml with water R complies with the
2 h. Allow to cool in a desiccator before weighing. limit test for chlorides (0.1 per cent).
ASSAY Sulphates (2.4.13). Dilute 2 ml of solution S to 100 ml with
distilled water R. 15 ml of the solution complies with the
To the residue obtained in the test for loss on ignition
limit test for sulphates (1 per cent).
add 0.2 ml of sulphuric acid R and sufficient alcohol R to
moisten the residue completely. Add 6 ml of hydrofluoric Iron (2.4.9). To 2 ml of solution S add 28 ml of water R.
acid R and evaporate to dryness on a hot-plate at 95 °C 10 ml of the solution complies with the limit test for iron
to 105 °C, taking care to avoid loss from sputtering. Wash (300 ppm).
down the sides of the dish with 6 ml of hydrofluoric acid R Heavy metals (2.4.8). To 20 ml of solution S add 50 mg of
and evaporate to dryness. Ignite at 900 ± 50 °C, allow to hydroxylamine hydrochloride R and 1 ml of concentrated
cool in a desiccator and weigh. ammonia R. Adjust to pH 3.5 by adding dilute ammonia R2,
The difference between the mass of the final residue and the monitoring the pH potentiometrically. Dilute to 25 ml with
mass of the residue obtained in the test for loss on ignition water R. 12 ml of the solution complies with limit test A for
gives the amount of SiO2 in the quantity of the substance heavy metals (25 ppm). Prepare the standard using lead
to be examined used. standard solution (1 ppm Pb) R.

General Notices (1) apply to all monographs and other texts 2877
Silica, dental type EUROPEAN PHARMACOPOEIA 6.0

Loss on ignition. Not more than 20.0 per cent, determined 50.0 ml with water R. Dilute 5.0 ml of the supernatant to
on 0.200 g in a platinum crucible by heating at 100 °C to 50.0 ml with water R and filter through a membrane filter
105 °C for 1 h and then at 900 ± 50 °C for 2 h. (nominal pore size 0.45 µm).
Reference solution. Dissolve 0.50 g of anhydrous sodium
ASSAY
sulphate R and 0.062 g of sodium chloride R in water R
To the residue obtained in the test for loss on ignition add and dilute to 1000.0 ml with water R. Dilute 5.0 ml of this
0.2 ml of sulphuric acid R and a quantity of alcohol R solution to 50.0 ml with water R.
sufficient to moisten the residue completely. Add 6 ml of
Column :
hydrofluoric acid R and evaporate to dryness at 95 °C to
105 °C, taking care to avoid loss from sputtering. Wash — material : non-metallic ;
the inside of the dish with 6 ml of hydrofluoric acid R and — size : l = 0.25 m, Ø = 4.6 mm ;
evaporate to dryness again. Ignite at 900 ± 50 °C, allow to — stationary phase : suitable anion-exchange resin
cool in a desiccator and weigh. The difference between the (30-50 µm).
mass of the final residue and that of the mass obtained in Mobile phase : dissolve 0.508 g of sodium carbonate R and
the test for loss on ignition corresponds to the mass of SiO2 0.05 g of sodium hydrogen carbonate R in water R, then
in the test sample. dilute to 1000 ml with the same solvent.
Flow rate : 1.2 ml/min.
01/2008:1562 Detection : conductivity detector.
corrected 6.0 Injection : 25 µl.
Retention time : sulphates = about 8 min.
SILICA, DENTAL TYPE Limit :
— sulphates : not more than the area of the corresponding
Silica ad usum dentalem peak in the chromatogram obtained with the reference
DEFINITION solution (4.0 per cent, expressed as sodium sulphate).
Amorphous silica (precipitated, gel or obtained by flame Iron (2.4.9) : maximum 400 ppm.
hydrolysis). Dilute 2 ml of solution S to 40 ml with water R.
Content : 94.0 per cent to 100.5 per cent of SiO2 (ignited Heavy metals (2.4.8) : maximum 25 ppm.
substance). To 20 ml of solution S, add 50 mg of hydroxylamine
CHARACTERS hydrochloride R and 1 ml of concentrated ammonia R.
Adjust to pH 3.5 by adding dilute ammonia R2, monitoring
Appearance : white or almost white, light, fine amorphous the pH potentiometrically. Dilute to 25 ml with water R.
powder. 12 ml of the solution complies with test A. Prepare the
Solubility : practically insoluble in water and in mineral reference solution using lead standard solution (1 ppm
acids. It dissolves in hydrofluoric acid and hot solutions of Pb) R.
alkali hydroxides.
Loss on ignition : maximum 25.0 per cent, determined on
IDENTIFICATION 0.200 g in a platinum crucible by heating at 100-105 °C for
About 20 mg gives the reaction of silicates (2.3.1). 1 h and then at 1000 ± 50 °C for 2 h.

TESTS ASSAY
To the residue obtained in the test for loss on ignition add
Solution S. To 2.5 g add 50 ml of hydrochloric acid R and 0.2 ml of sulphuric acid R and a quantity of ethanol (96 per
mix. Heat on a water-bath for 30 min, stirring from time to cent) R sufficient to moisten the residue completely. Add
time. Evaporate to dryness. Add to the residue a mixture of 6 ml of hydrofluoric acid R and evaporate to dryness at
8 ml of dilute hydrochloric acid R and 24 ml of water R. 95-105 °C, taking care to avoid loss from sputtering. Wash
Heat to boiling and filter under reduced pressure through the inside of the crucible with 6 ml of hydrofluoric acid R
a sintered-glass filter (16) (2.1.2). Wash the residue on the and evaporate to dryness again. Ignite at 900 ± 50 °C, allow
filter with a hot mixture of 3 ml of dilute hydrochloric acid R to cool in a desiccator and weigh. The difference between
and 9 ml of water R. Wash with small quantities of water R, the mass of the final residue and that of the mass obtained
combine the washings and the filtrate, then dilute to 50 ml in the test for loss on ignition corresponds to the mass of
with water R. SiO2 in the test sample.
pH (2.2.3) : 3.2 to 8.9.
Suspend 5 g in a mixture of 5 ml of a 7.46 g/l solution of 01/2008:2208
potassium chloride R and 90 ml of carbon dioxide-free corrected 6.0
water R.
Chlorides. Liquid chromatography (2.2.29) as described in SILICA, HYDROPHOBIC COLLOIDAL
the test for sulphates.
Retention time : chlorides = about 4 min. Silica hydrophobica colloidalis
Limit :
DEFINITION
— chlorides : not more than the area of the corresponding
Colloidal silicon dioxide partly alkylated for hydrophobation.
peak in the chromatogram obtained with the reference
solution (0.3 per cent). Content : 99.0 per cent to 101.0 per cent SiO2 (ignited
substance).
Sulphates. Liquid chromatography (2.2.29).
Test solution. To 0.625 g of the substance to be examined CHARACTERS
add 30 ml of water R and boil for 2 h. Allow to cool and Appearance : light, fine, white or almost white, amorphous
quantitatively transfer to a 50 ml graduated flask. Dilute to powder, not wettable by water.

2878 See the information section on general monographs (cover pages)