1.0 OBJECTIVE:
1.1 To describe the procedure for the operation of the Leak Test Apparatus for determining the integrity of pharmaceutical packaging systems by detecting leakage under vacuum conditions.
2.0 SCOPE:
2.1 This SOP shall apply to the operation of the DBK Leak Test Apparatus for testing the integrity of pharmaceutical packaging materials and finished products, as applicable.
3.0 RESPONSIBILITIES:
3.1 Designee Production / Quality Assurance (QA) / Quality Assurance (QC):
3.1.1 Operation, cleaning and documentation.
3.1.2 Shall verify the instrument status before use.
3.1.3 Shall operate the instrument in accordance with this SOP.
3.1.4 Shall record the observations and test results.
3.1.5 Shall clean the instrument after completion of analysis.
3.2 Department Head:
3.2.1 Overall compliance.
3.3 QA Department:
3.3.1 Periodic verification and SOP compliance.
4.0 DEFINATIONS:
4.1 Leak Test: A test performed to evaluate the integrity of a packaging system by subjecting the sample to vacuum conditions and observing for leakage.
4.2 Vacuum: Pressure below atmospheric pressure generated within the desiccator during the leak test.
4.3 Desiccator: A transparent vacuum chamber used to accommodate the test sample during leak testing.
4.4 Vacuum Level: The degree of vacuum applied to the desiccator during the test, expressed in mmHg.
5.0 PROCEDURE:
5.1 Before Operation:
5.1.1 The designee shall verify that the instrument is clean, calibrated and labelled with a valid calibration status before use.
5.1.2 The designee shall ensure that the desiccator, lid, perforated separator plate, sealing gasket and vacuum tubing are clean, dry and free from any visible damage.
5.1.3 The designee shall ensure that the vacuum release valve is in the closed position before starting the test.
5.1.4 The designee shall verify that the vacuum pump is properly connected to the instrument.
5.1.5 The mains power supply shall be switched ON and the instrument shall be allowed to initialize.
5.1.6 The designee shall ensure that the instrument display is functioning properly before commencing the analysis.
5.2 Operation:
5.2.1 The desiccator shall be filled with sufficient purified water to completely immerse the test sample.
5.2.2 The test sample shall be placed inside the desiccator on the perforated separator plate and shall be completely immersed in water.
5.2.3 The desiccator lid shall be properly positioned and securely closed to obtain an airtight seal.
5.2.4 The required vacuum level shall be selected using the VACUUM selection switch.
5.2.5 The required holding time shall be selected using the TIMER selection switch.
5.2.6 The vacuum level and holding time shall be selected as specified in the approved analytical method or packaging specification.
5.2.7 The designee shall initiate the test by pressing the START switch.
5.2.8 The instrument shall generate and maintain the selected vacuum throughout the test period.
5.2.9 The designee shall observe the sample continuously for the presence of air bubbles throughout the test.
5.2.10 Upon completion of the preset holding time, the instrument shall stop automatically.
5.2.11 The vacuum shall be released gradually by operating the vacuum release valve.
5.2.12 The desiccator lid shall be opened only after complete release of the vacuum.
5.3 Observation and Interpretation:
5.3.1 The sample shall be examined for continuous air bubble formation during the application of vacuum.
5.3.2 Continuous air bubbles emerging from the package shall indicate leakage.
5.3.3 Isolated air bubbles generated during initial vacuum application shall not be considered as evidence of leakage unless continuous bubbling is observed.
5.3.4 The sample shall be visually examined for deformation, seal separation or any other packaging defects after completion of the test.
5.3.5 The acceptance criteria shall be as specified in the Batch Manufacturing Records (BPR).
5.4 Recording of Results:
5.4.1 The observations regarding leakage or absence of leakage shall be recorded.
5.4.2 The final test result shall be recorded as Pass or Fail in accordance with the approved acceptance criteria
5.5 Cleaning:
5.5.1 The test sample shall be removed from the desiccator after completion of the test.
5.5.2 The water shall be drained from the desiccator, where applicable.
5.5.3 The desiccator, lid and perforated separator plate shall be cleaned with purified water and wiped dry using a clean, lint-free cloth.
5.5.4 The sealing gasket shall be cleaned carefully to remove any residue and shall be inspected for damage before reuse.
5.5.5 The external surfaces of the instrument shall be cleaned using a clean, dry lint-free cloth.
5.5.6 Abrasive materials, excessive water or organic solvents shall not be used for cleaning the instrument.
5.5.7 The instrument shall be switched OFF after completion of cleaning.
5.5.8 The instrument usage shall be recorded in the instrument logbook.
6.0 REFERENCE:
6.1 Instrument User Manual
6.2 British Pharmacopoeia / US Pharmacopoeia
7.0 RECORDS:
Sr No. Title Nature of Document Document No.
NA NA NA NA
8.0 REVISION HISTORY:
Amendment Date: Update Summary Version No.
NA New SOP 01