standard testing procedure croscarmellose sodium

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standard testing procedure croscarmellose sodium

Storage Requirements:
Store protected from light and moisture.

Sampling:
Sample from each container / bag, if the consignment is of 03 or less than three containers / bags. If the number of containers / bags is more than 03and are up to 100, sample at randomly using the formula root (n) +1 where n is the number of containers/bags in the consignment. For the consignment of more than 100 containers/bags, sample additional containers/bags for every 100 containers/bags and thereafter. Collect a minimum of 5g from each of the randomly selected containers/bags in to individually no toxic, self sealing transparent polyethylene bearing ‘Sample For Analysis label kept in another transparent self sealing polythene bag. After completion of sampling return rest sample on the same container. Collect control sample in Pet bottle/Glass bottle.

Quantity of Composite Sample:

50 g

Quantity of Control Sample:

2 X 50 g

Description: A white or greyish-white powder.

Solubility: Slightly soluble in water; insoluble in ethanol, ether and in other organic solvents.

Identification:

The substance under examination absorbs the methylene blue and settles as a blue, fibrous mass.
A reddish-violet colour develops at the interface.
The solution prepared from the sulphated ash in the test for Heavy metals gives reaction (a) of sodium salts.

pH: 5.0 to 7.0

Degree of substitution. Titrate with 0.1M sodium hydroxide until the colour turns to violet.

Sodium chloride and sodium glycollate: The sum of the percentage contents of sodium chloride and sodium glycollate is not more than 0.5 per cent, calculated on the dried basis.

Water soluble substances: NMT 10.0 per cent.

Heavy Metals: NMT 20ppm

Settling volume. The substance is homogeneously distributed

Microbial contamination: Total microbial count, not more than 103 bacteria and 102 fungi per gram.

Sulphated ash: NMT 14.0 to 28.0 % w/w

Loss on Drying: NMT 10.0 % w/w at 105º for 6 hours.
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Description: A white or greyish-white powder.

Solubility: Slightly soluble in water
Insoluble in ethanol, ether and in other organic solvents.

Identification:

A. Shake 1g with 100ml of 0.0004 per cent w/v solution of methylene blue and allow to settle. The
Substance under examination absorbs the methylene blue and settles as a blue fibrous mass.
B. Shake 1g with 50ml of water. Transfer 1 ml of the mixture to a test-tube, add 1 ml of the mixture to a
Test-tube, add 1 ml of water and 0.05 ml of a freshly prepared 4.0 per cent w/v solution of œ–
Napthol in methanol. Incline the test –tube and add carefully 2 ml of sulphuric acid down the side so
That it forms a lower layer .A reddish –violet colour develops at the interface.
C. The solution prepared from the sulphated ash in the test for Heavy metals gives reaction (a) of
Sodium salts.

pH: 5.0 to 7.0, determined on 1.0 per cent w/v solution in carbon dioxide-free water.

Degree of substitution.
Take 1.0 g in 500ml conical flask, add 300ml of a 10 per cent w/v solution of sodium chloride, 25.0 ml of 0.1 M sodium hydroxide, stopper the flask and allow to stands for 5 minutes, shaking occasionally, Add 0.05ml of m-cresol purple solution and about 15ml of 0.1M hydrochloric acid from a burette. Insert the stopper and shake. If the solution is violet, add 0.1M hydrochloric acid in 1ml portions until the solutions becomes yellow, shaking after each addition. Titrate with 0.1M sodium hydroxide until the colour turns to violet.

Calculate the number of mill equivalents (M) of base required for the neutralization equivalent to 1g of dried substance.

Sodium chloride and sodium glycollate:
The sum of the percentage contents of sodium chloride and sodium glycollate is not more than 0.5 per cent, calculated on the dried basis.

Sodium chloride:
Place 5.0 g in a 250ml conical flask, add 50ml of water and 5 ml of strong hydrogen peroxide solution and heat on a water-bath

for 20 minutes stirring occasionally to ensure total hydration. Cool, add 100ml of water and 10ml of nitric acid. Titrate

with 0.05 M silver nitrate determining the end point potentiometrically. Using a silver indicator electrode and a

double junction reference electrode containing a 10 per cent w/v solution of potassium nitrate in the outer jacket and a standard filling solution in the inner jacket and stirring constantly.

1 ml of 0.05M silver nitrate is equivalent to 0.002922 g of NaCl.

Reporting: Report in %.

Sodium glycollate:
Place 0.5g of the substance under examination in a 100ml beaker. Add 5ml of glacial acetic acid and 5ml of water and stir

to ensure total hydration (about 15 minutes). Add 50ml of acetone and1g of sodium chloride. Stir for several minutes to

ensure complete precipitation of the carboxymethyl- cellulose. Filter through a fast filter paper impregnated with

acetone into a volumetric flask, rinse the beaker and filter with 30 ml of acetone and dilute the filtrate to 100.0 ml

with the same solvent. Allow to stand for 24 hours without shaking. Use the clear supernatant to prepare the test solution.

Reference solution: Dissolve 0.1g of glycolic acid in 100ml of water. Use the solution within 30 days.

Transfer 1.0 ml, 2.0 ml, 3.0 ml and 4.0ml of the solution to separate volumetric flasks; dilute

the contents of each flask to 5.0 ml with water, add 5ml of glacial acetic acid, dilute to 100.0 ml with acetone and mix.

Transfer 2.0 ml of the test solution and 2.0 ml of each of the reference solutions to separate 25ml volumetric flasks.

Heat the uncovered flasks for 20 minutes on water –bath to eliminate acetone. Allow to cool and add 5.0ml of 2.7-dihydroxynaphthalene

solution to each flask. Mix, add a further 15.0ml of 2, 7-hydroxynaphthalene solution and mix again. Close the flasks with

aluminum foil and heat on a water-bath for 20 minutes. Cool and dilute to 25.0 ml with sulphuric acid.

Measure the absorbance of each solution at 540 nm . Prepare a blank using 2.0 ml of a solution containing 5 per cent v/v each

of glacial acetic acid and water in acetone. Prepare a standard curve using the absorbance obtained with the reference solutions.

From the standard curve and the absorbance of the test solution, determine the mass, in milligrams, of glycolic acid in the

substance under examination, and calculate the content of sodium glycollate from the expression;

Water soluble substances:
Disperse 10.0g in 800.0 ml of water and stir for 1 minute and stir for 1 minute every 10 minutes during the first 30 minutes. Allow to stand for 1 hour and centrifuge,

if necessary. Decant 200.0ml of the supernatant liquid onto a fast filter paper in a vacuum filtration funnel, apply to dryness and dry the residue at 100° to 105° for 4 hours.

Heavy Metals:
To the residue obtained in sulphated ash add 1ml of hydrochloric acid and evaporate on a water-bath. Take up the residue in 20ml of water, 12ml of

the solution complies with the limit test for heavy metals, Method (10 ppm). Prepare the reference solution using lead standard solution (1 ppm Pb).

Settling volume:
Place 75 ml of water in a 100ml graduated cylinder and add 1.5g of the substance under examination in 0.5g portions, shaking vigorously

after each addition. Dilute to 100.0 ml with water and shake again until the substance is homogeneously distributed. Allow to stand for 4 hours.

Microbial contamination:
Total microbial count, not more than 103 bacteria and 102 fungi per gram, determined by plate count. 10g is free from E. coli.

Sulphated ash:
Determined on 2.0g, using a mixture of equal volumes of sulphuric acid and water, and calculated on the dried basis.
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