4/1/22, 5:45 PM Method of Analysis for Colloidal Silicon Dioxide : Pharmaceutical Guidelines

-->

Method of Analysis for Colloidal Silicon Dioxide

Learn how to analyse Colloidal Silicon Dioxide in pharmaceutical laboratory.

1. Description
Light, fine, white amorphous powder. It has a particle size of about 15 nm.

2. Solubility
Practically insoluble in water and in mineral acid with exception of hydrofluoric acid Dissolves in hot solutions of alkali hydroxides. When 1
g is shaken vigorously with 20 ml of carbon tetrachloride for 3 minutes, a transparent gel is produced

3. Identification
Reaction of Silicates
Reagent required

Sodium fluoride

Sulphuric acid

Procedure: Weight about 20 mg. of the sample and transfer into a platinum crucible. Add 10 mg. of sodium fluoride and few drops of
sulphuric acid. Mix by means of a copper wire to obtain the thin slurry. Cover the crucible with a thin transparent plate of plastic under
which a drop of water is suspended. Warm the crucible gently, within a short time; a white ring is formed around the drop of water.

4. pH
Limit: Between 3.5 and 5.5

Procedure: Weigh 1.0 g. the sample in a 100 ml beaker, add 30 ml of water and disperse the substance by shaking the solution well. Measure
the pH of the suspension.

5. Chloride
Limit: Not more than 250 ppm

Reagent required

Nitric acid

0.1M Silver nitrate

Chloride standard solution (25 ppm Cl)

Standard solution: Transfer 10 ml of chloride standard solution (25 ppm Cl) into a clean and dried Nessler cylinder, add 5 ml of water. Add 10
ml dilute nitric acid and make the volume to 50 ml with water.

Sample solution: Weigh 1.0 g sample into a 50 ml volumetric flask, add a mixture of 20 ml of 2M HNO3 and 30 ml of water. Heat the flask on
a water bath for 15 minutes with frequent shaking. Cool the flask to room temperature. Make up the volume to 50 ml with water, if
necessary, filter and cool. Transfer the filtrate into a clean and dried Nessler cylinder.

Procedure: Add 1 ml of 0.1 M silver nitrate, mix and allow standing for 5 minutes protected from light. When viewing transversely against a
black background the opalescence if any, produced in the sample solution is less than that produced in the standard solution.

6. Arsenic
Limit: Not more than 8 ppm

Reagent required

Lead acetate cotton

3M hydrochloric acid

Arsenic standard solution (10 ppm As)

1M potassium iodide

Zinc granules

Mercuric chloride paper

Hydrochloric acid

Sample Preparation: Weigh 2.5 g. of the sample and transfer it to a 250 ml round bottom flask, add 50 ml of 3M hydrochloric acid and reflux
for 30 minutes using water condenser. Cool, filter with the aid of suction, and transfer the filtrate to a 100 ml volumetric flask. Wash the filter
and flask with several portions of hot water and add the washings to the flask. Cool, dilute to volume with water and mix. To 50 ml of the
solution, add 3 ml of hydrochloric acid.

Standard Preparation: Transfer 1 ml of arsenic standard solution (10 ppm as) into arsenic test apparatus bottle and dilute to 50 ml with
water.

Procedure: In each of the arsenic test apparatus bottles, add 5 ml of 1M potassium iodide and 10 g. Zinc granules. Immediately assemble the
apparatus and immerse the bottles in a water-bath at a temperature such that a uniform evolution of gas is maintained. After 40 minutes,
any stain produced on the mercuric chloride paper with the sample preparation is not more intense than that is obtained by standard
preparation.

7. Heavy metals
Limit: Not more than 25 ppm

Reagent required

https://www.pharmaguideline.com/2008/06/method-of-analysis-for-colloidal-silicon-dioxide.html 1/3
4/1/22, 5:45 PM Method of Analysis for Colloidal Silicon Dioxide : Pharmaceutical Guidelines

Strong ammonia

2M ammonia

Thioacetamide reagent

Acetate buffer pH 3.5

Lead standard solution (1 ppm Pb)

2M Hydrochloric acid

1M Hydrochloric acid

Phenolphthalein solution
Sample Preparation: Weigh 2.5 g. of the sample in a 100 ml beaker; add sufficient water to produce a semi-fluid slurry. Dry at 140°c. When
the dried substance is white, break up the mass using a glass rod. Add 25 ml of 1M HCl, boil gently for 5 minutes, stirring frequently with the
glass rod and transfer the solution into the centrifuge tube. Centrifuge for 20 minutes and filter the supernatant liquid through the
membrane filter. To the residue in the centrifuge tube, add 3 ml of 2M hydrochloric acid and 9 ml of water. Boil, Centrifuge for 20 minutes
and filter the supernatant liquid through the same membrane filter. Wash the residue with small quantities of water. Collect the combined
filtrates and washings and dilute to 50 ml with water. Pipette out 20 ml of the solution and transfer it into 25 ml volumetric flask. Add 50
mg. of L-ascorbic acid and 1 ml of strong ammonia solution, neutralize with 2M ammonia and dilute to 25 ml with water. Pipette out 12 ml of
above solution and transfer it into 50 ml Nessler cylinder.

Standard Solution: Take 10 ml of Lead standard solution (1 ppm Pb) into 50 ml Nessler cylinder and dilute to 10 ml with water. Add 2 ml of
the test solution and mix.

Procedure: To both the cylinders add 2 ml of acetate buffer pH 3.5, mix and add 1.2 ml of thioacetamide reagent, mix, allow to stand for 2
minutes. Any color produced in the sample solution is not more intense than that produced in the standard solution.

8. Loss on ignition
Limit: Not more than 5.0%

Procedure: Ignite a clean platinum crucible at 900°c for 30 minutes, cool and weigh the crucible. Transfer about 200 mg. of the sample into
the crucible and record the weight. Ignite the crucible along with the sample at 900°c for 2 hours. Cool the crucible to room temperature in a
desiccator and record the weight.

Calculation

                                   W2 – W3

%Loss on ignition = --------------- X 100

                                   W2 – W1

Where:

W1 = Weight of empty platinum crucible

W2 = Weight of crucible + sample

9. Assay
Limit: Not less than 99.0% and Not more than 100.5% of SiO2, calculated with reference to the ignited substance.

Reagent required

Hydrofluoric acid

Sulphuric acid

Ethanol (95%)

Procedure: To the residue obtained in the test “Loss on ignition”, add 0.2 ml of sulphuric acid and sufficient ethanol (95%) to moisten the
residue completely, add 6 ml of hydrofluoric acid. Evaporate to dryness in a well-ventilated hood on a hot plate at 95°c to 105°c, avoiding loss
from sputtering. Wash the sides of the dish with 6 ml of hydrofluoric acid, evaporate to dryness in a well-ventilated hood, ignite at 1000°c,
allow to cool in a desiccator and weigh the crucible (W4). The difference between the weight of the final residue and that of the residue
obtained in the test for loss on ignition represents the amount of SiO2 in the amount of the sample taken for the test for Loss on ignition.

Calculation

                      (W3 – W1) – (W4 – W1)

% Assay = ---------------------------------- x 100

                              (W3 – W1)

Where,

W1 = Weight of empty platinum crucible.

W3 = Weight of crucible + sample. (After ignite)

W4 = Weight of crucible + sample. (After treatment of hydrofluoric acid)

Ankur Choudhary is India's first professional pharmaceutical blogger, author and founder of Pharmaceutical Guidelines, a widely-read
pharmaceutical blog since 2008. Sign-up for the free email updates for your daily dose of pharmaceutical tips.

Need Help: Ask Question

https://www.pharmaguideline.com/2008/06/method-of-analysis-for-colloidal-silicon-dioxide.html 2/3
4/1/22, 5:45 PM Method of Analysis for Colloidal Silicon Dioxide : Pharmaceutical Guidelines

 
Copyright © 2008-2022
Pharmaceutical Guidelines

Setup ❘ Terms of Use ❘ FAQ

https://www.pharmaguideline.com/2008/06/method-of-analysis-for-colloidal-silicon-dioxide.html 3/3