standard testing procedure glass ampoule

1.0 OBJECTIVE
1.1 To lay down a procedure for Analysis of Glass Ampoule

2.0 SCOPE
2.1 This procedure is applicable to the Analysis of Ampoule in quality control laboratory

3.0 RESPONSIBILITY
3.1 Q.C- Chemist

4.0 ACCOUNTABILITY
4.1 Head-Quality Assurance

5.0 Description:– Visually check the appearance of the sample like colour, shape and physical condition of the sample.

6.0 Shades of colours used: – Visually match the colours used in the sample by shade card provided by the party.
7.0 Printing Quality:– Visually match the printing matter and quality of printing matter used in the sample against the approved standard.
8.0 Total Height:- Take the above five samples and check the height with the Help of calibrated scale and report in mm.
9.0 Body Wall Thickness:– Take the above five samples and check the width with the help of calibrated scale and report in mm.
10.0 Base to Construction Height:– Take the above five samples and check the height with the help of calibrated scale and report in mm.
11.0 Body Outer Diameter:- Take the above five samples and check the height with the help of calibrated scale and in mm.
12.0 Neck Diameter:- Take the above five samples and check the height with the help of calibrated scale and report in mm.
13.0 Arsenic:- Glass ampoules should comply with the following test. Carry out the lest on ampoules the inner and outer surfaces

of which are washed five times with freshly distilled water. Prepare a test solution as described in the test for

Hydrolytic resistance for an adequate number of ampoules to produce 50 ml. Pipette 10 ml of the test solution from

the combined contents of all acid and evaporate to dryness on a water-bath the ampoules into a flask, add 10 ml of nitric.

Dry the residue in an oven at 1300C for 30 minutes. Cool, add to the residue 10.0 ml of hydrazine-molybdate reagent,

swirl to dissolve and heat under reflux on a water bath for 20 minutes. Cool to room temperature.

Determine the absorbance of resulting solution at the maximum at about 840 nm, using 10.0 ml – of hydrazine molybdate reagent as the blank.

The absorbance of the test solution does not exceed the absorbance obtained by repeating the determination

using 0.1 ml of arsenic standard solution (10 ppm As) in place of the test solution (0.1 ppm)
14.0 Hydrolytic Resistance:- The test to be done for defining the type of glass are given in Table 1.

Table 1

Type of container	Test to be done
Type I and II glass containers to distinguish from type III glass containers.	Test 1 (Surface test)
Type I and Type II glass containers where it is necessary to determine whether the high hydrolytic resistance is due to the chemical composition or the surface treatment.	Test 1 and 2

Test 1 :- Carry out the determination on the unused containers. The number of containers to be

examined and the volumes of test solution to be used are given in Table 2.

Nominal capacity of Container (ml)	Number of containers to be used	Volume of test solution to be used for titration (ml)
Up to 3	At least 20	25.0
5 or less	At least 10	50.0
6 to 30	At least 5	50.0
More than 30	At least 3	100.0

Remove any debris or dust from the containers. Rinse each container at least twice with water at room temperature.

Just before the test rinse each container with freshly prepared distilled water and allow to drain.

Complete the cleaning procedure from the first rinsing is not less than 25 minutes and mot more

than 25 minutes. Fill the containers to the brim with freshly prepared distilled water, empty them and determine the average overflow volume.

Heat closed ampoules on a water bath or in air oven at about 500C. prepared distilled water to the maximum volume

compatible with sealing them by fusion of the glass and seal them. Fills bottles or vials to 90% of their calculated overflow

volume and cover them with borosilicate glass dishes or aluminium foil previously rinsed with freshly prepared distilled water.

Close the autoclave, displace the air by passage of steam for 10 minutes, raise the temperature from 1000C to 1210C over 20 minutes,

maintain a temperature of 1210C for 60 minutes and reduce the temperature from 1210C to 1000C over 40 minutes, venting to prevent vacuum.

Remove the containers from the autoclave and cool them in a bath of running tap water. Carry out the following titration

within 1 hour of removing the containers from the autoclave . Combine the liquids from the containers being examined,

measure the volume of test solution specified in Table 2 into a conical flask and add 0.15 ml of methyl red solution for

each 50 ml of liquid. Titrate with 0.01M hydrochloric acid taking as the end-point the colour obtained by repeating

the operation using the same volume of freshly prepared distilled water. The difference between the preparations represents

the volume of 0.01 M hydrochloric acid required by the test solution.
Calculate the volume of 0.01M hydrochloric acid required for each 100 ml of test solution, if necessary. The result is not greater than the value stated in Table3.

Capacity of container [Corresponding to 90% Average overflow volume (ml)]	Volume of 0.01 M hydrochloric acid per 100 ml of test solution
	Type I or II glass (ml)	Type III glass (ml)
Not more than I	2.0	20.0
More than 1 but not more than 2	1.8	17.6
More than 2 but not more than 5	1.3	13.2
More than 5 but not more than 10	1.0	10.2
More than 10 but not more than 20	0.80	8.1
More than 20 but not more than 50	0.60	6.1
More than 50 but not more than 100	0.50	4.8
More than100 but not more than 200	0.40	3.8
More than 200 but not more than 500	0.30	2.9
More than 500	0.20	2.2

Test 2:
Examine the number of containers indicated in Table 2. Rinse the containers twice with water and then fill completely with a 4% V/V solution hydrofluoric acid and allow to stand at room temperature for 10 minutes. Empty the containers and rinse carefully five times with water. Carry out the procedure described under Hydrolytic resistance. Compare the results with the limiting values given in Table 3. For Type I glass the values obtained with the hydrofluoric acid-treated containers are closely similar to those stated in the Table for Type I or Type II glass. For Type II glass the values obtained with the hydrofluoric acid-treated containers greatly exceed those given in the Table for I or Type II glass and are similar to those given for Type III glass.

15.0 ABBREVIATION

Sr. No.	Abbreviation used	Full form of abbreviation used
1.0	STP	Standard Testing Procedure
2.0	QA	Quality assurance
3.0	PM	Packaging Material
4.0	cm	Centimeter