Standard test procedure for Rubber Stopper

Description:

Examine 5 rubber stoppers visually for general appearance and record the observation.

Specification: 20 mm grey colour Butyl Rubber Stopper

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Identification:

Take rubber stopper strip with a cross-section of 1 mm² to 5 mm² and stretch by hand to at least twice its original length. Having been stretched to twice its length for l minute.

Specification: It contracts to less than 1.2 times its original length within 30 s.

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Physical Dimensions

Collar Diameter:

Instrument: Vernier caliper

Measure the at least 5 Nos. of 20 mm butyl rubber stopper collar diameter by vernier caliper and take a Average.

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Neck Diameter:

Instrument: Vernier caliper

Measure the at least 5 Nos of 20 mm butyl rubber stopper collar diameter by vernier caliper and take a Average.

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Thickness of collar:

Instrument: Vernier caliper

Measure the at least 5 Nos of 20 mm butyl rubber stopper collar diameter by vernier caliper and take a Average.

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Total Height:

Instrument: Vernier caliper

Measure the at least 5 Nos of 20 mm butyl rubber stopper collar diameter by vernier caliper and take a Average.

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Physicochemical Tests :

Appearance of solution :

Preparation of Sample solution :

Wash the closures by agitation in a 0.2 % w/v solution of an anionic surface – active agent for 5 minutes at room temperature. Rinse five times with water, place a number of the washed closures corresponding to a surface area of about 100 cm², in a suitable container of borosilicate glass or inert material, add 200 mL of water per 100 cm², surface area of the closure and weigh. Cover the mouth of the container with aluminium foil or a borosilicate glass beaker & heat in an autoclave so that a temperature of 119°C to 123°C is reached within 20 to 30 minutes & maintain at that temperature for 30 minutes. Cool to room temperature over about 30 minutes & make up to the original weight with water for injection. Shake & immediately separate the solution from the closure by decantation. Prepared blank in the same manner using 200 mL of

water without the closure. Shake & immediately separate the solution from the closure by decantation.

Specification:

Not more opalescent than Reference Suspension C for closures. Solution S is considered clear ifits clarity is the same as that of water when examined as described above, or if its opalescence is not more pronounced than that of Reference Suspension A.

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Acidity & Alkalinity: 

Procedure:

Take 20 mL of Solution S, add 0.1 mL of bromothymol blue solution. If the solution is yellow, titrate with 0.01 N sodium hydroxide until a blue endpoint is reached. If the solution is blue, titrate with 0.01 N hydrochloric acid until a yellow If the solution is green, it is neutral and no titration is required.

Blank Correction—Test 20 mL of Blank similarly. Correct the results obtained for Solution S by subtracting or adding the volume of titrant required for the blank, as appropriate.

Specification:

Not more than 0.3 mL of 0.01 N sodium hydroxide produces a blue color, or not more than 0.8 mL of 0.01 N hydrochloric acid produces a yellow color, or no titration is required.

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Light Absorption :

Procedure:

Carry out the test within 4 hrs of preparing solution S. Filter solution S through a membrane filter with a nominal pore size of 0.45 µm & reject the first few ml of the filtrate. Measure the light absorption of the filtrate in the range 220 to 360 nm, using as the blank a solution prepared in the same manner as solution A using 200 mL of water, without the closure.

Specification:

The A absorbance’s do not exceed 4.0.

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Reducing Substance:

Procedure:

Carry out the test within 4 hrs of preparing solution A. To 20 mL of solution S, add 1 mL of diluted sulphuric acid and 20 mL of 0.002 M Potassium Permangnate. Boil for 3 minutes. Cool, add 1 g of potassium iodide & titrate immediately with 0.01 M sodium thiosulphate Using 0.25 mL of starch solution, added towards the end of the titration, as indicator. Repeat the operation using 20 mL of the blank prepared in the light absorption.

Specification:

The difference between the titration volume is not more than 7.0 mL.

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Heavy Metals:

Procedure:

Proceed as directed for Method I under. Prepare the Test Preparation using 10.0 mL of Solution S.

Specification:

The colour of the solution in Test solution is not darker than that of the solution from the standard solution and the intensity of the color solution of the Monitor Preparation is equal to or greater than that of the standard preparation.

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Ammonium:

Procedure:

Alkaline Potassium Tetraiodomercurate Solution:

Prepare a 100 mL solution containing 11 g of potassium iodide and 15 g of mercuric iodide in water. Immediately before use, mix 1 volume of this solution with an equal volume of a 250 g per L solution of sodium hydroxide.

Test Solution:

Dilute 5 mL of Solution S to 14 mL with water. Make alkaline if necessary by adding 1 N sodium hydroxide, and dilute with water to 15 mL. Add 0.3 mL of Alkaline Potassium Tetraiodomercurate Solution and close the container.

Ammonium Standard Solution:

Prepare a solution of ammonium chloride in water (1 ppm NH4). Mix 10 mL of the 1 ppm ammonium chloride solution with 5 mL water and 0.3 mL of Alkaline Potassium Tetraiodomercurate Solution. Close the container.

Specification:

After 5 minutes, any yellow color in the Test Solution is no darker than the Ammonium Standard Solution (no more than 2 ppm of NH4 in Solution S)

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Volatile sulphides :

Procedure:

Place closure, cut if necessary, with a total surface of 20 ± 2 cm² in a 100 mL conical flask & add 50 mL of a 20 g per L solution of citric acid. Place a piece of lead acetate paper over the mouth of the flask & maintained the paper in position by placing over it an inverted weighing bottle. Heat in an autoclave at 121 ± 2°C for 30 minutes. Any black stain on the paper is not more intense than that of standard prepared at the same time in the same manner using 0.154 mg of sodium sulphide & 50 mL of a 2 % w/v solution of citric acid.

Specification:

Any black stain on the paper produced by the test solution is not more intense than that produced by the control substance.

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Functionality Tests:

Penetrability:

Procedure:

Fill 10 suitable vials to the nominal volume with water, fit the closures to be examined and secure with a cap. Using a new hypodermic needle as described above for each closure, pierce the closure with the needle perpendicular to the surface.

Specification: The force for piercing is no greater than 10 N (1kgf) for each closure, determined with an accuracy of ± 0.25 N (25 gf).

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Fragmentation:

Procedure:

Closures for Liquid Preparation–

Fill 12 clean vials with water to 4 mL less than the nominal capacity. Fit the closures to be  examined, secure with a cap, and allow to stand for 16 hours.

Closures for Dry Preparations–

Fit closures to be examined into 12 clean vials, and secure each with a cap.

Procedure:

Using a hypodermic needle as described above fitted to a clean syringe, inject into each vial 1 mL of water while removing 1 mL of air. Repeat this procedure four times for each closure, piercing each time at a different site. Use a new needle for each closure, checking that it is not blunted during the test. Filter the total volume of liquid in all the vials through a single filter with a nominal pore size no greater than 0.5 μm. Count the rubber fragments on the surface of the filter visible to the naked eye.

Specification:

There are no more than five fragments visible. This limit is based on the assumption that fragments with a diameter >50 μm are visible to the naked eye. In case of doubt or dispute, the particles are examined microscopically to verify their nature and size.

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Self-Sealing Capacity:

Procedure :

Fill 10 suitable vials with water to the nominal volume, close the vials with the ‘prepared’ Closure & secure with a cap. For each closure use a new hypodermic needle with an external diameter of 0.8 mm & pierce the closure 10 times, piercing each time at a different site. Immerse the vials upright in a 0.1 % w/v solution of methylene blue & reduce the external pressure by 27 KPa for 10 minutes. Restore the atmospheric pressure & leave the vials immersed for 30 minutes. Rinse the outside of the vials. None of the vials contains any trace of coloured solution.  

Specification:

None of the vials contain any trace of blue solution

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