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An Overview of Package and Seal Integrity Testing
An Overview of Package and Seal Integrity Testing
Darrell R. Morrow, PhD
Leak Detection Associates, Inc.Blackwood, New Jersey
Package/Seal Integrity TestingVia Helium Leak Detection Methods
Package/Seal Integrity TestingVia Helium Leak Detection Methods
HELIUM LEAK DETECTION – A Well-Established, “Old” Technology
Many Industries, Such As Automotive, Electronic & Aerospace, Have Employed Helium Leak Detection For Many Years.
The Primary Focus For These Applications Has Been The Integrity Of Sealed Mechanical Systems; For Example, Brake Line Seals & O-Ring Seals.
Package/Seal Integrity TestingVia Helium Leak Detection Methods
Package/Seal Integrity TestingVia Helium Leak Detection Methods
SEAL INTEGRITY MONITORING OF “CONSUMER” PACKAGING – A Validated, “New” Application.
Some Pharmaceutical & Medical Device Companies Have Been Employing Integrated Seal Integrity Monitoring Systems For Up To Seven (7) Years.
As An “End-Use Performance Test”, These New Applications Have Been Extended To Include:
Design & Development Stability Pack-Out Verification Clinical Trial Pack-Out Verification Tooling Validation Process Validation
Gas/Vapor Barrier Requirements
Gas/Vapor Barrier Requirements
Gas and vapor transport can occur via permeation or leakage.
The total rate of gas/vapor transport is determined by the total number of holes; regardless of size.
Individual gross leaks, due to their size, are readily detectable by most leak test methods.
Gross “leaks” due to a multitude of “fine” leaks are not readily detectable by most leak test methods.
Sterility/Microbial Barrier Issues
Sterility/Microbial Barrier Issues
Microbial transport can occur only via leakage.
The total rate of microbial transport is determined by the total number of holes with dimensions > the minimum.
Leaks corresponding to the minimum size needed to block aqueous-borne microbes are not readily detectable by most leak test methods [single “hole” leak rate < ~1E-6 cc-atm/sec.].
Leak Detection Test MethodsComparative Sensitivities
Leak Detection Test MethodsComparative Sensitivities
10-1 10-2 10-3 10-4 10-5 10-6 10-7 10-8 10-9 10-10
Leak Rate (cc/s)
TEST METHOD/TECHNOLOGY
D3078 - VACUUM BUBBLEVacuum Level = 15" HgVacuum Level = 21" HgVacuum Level > 21" Hg
D3078 - DYE PENETRATIONVacuum Level = 15" HgVacuum Level = 21" Hg
Vacuum Level > 21" Hg
Pressure Decay
Carbon Dioxide Sensor
Gas Pressure - Bubble @ 10" H2O
@ 20" H2O
Helium Tracer- Mass Spectrometer Sniffer Mode Hard Vacuum Mode
Pharmaceutical/Device Industry Needs
Verify quality of seals and (overall) packaging for stability pack-out samples.
Insure integrity of seals and (overall) packages for clinical trials and production run product.
Insure medication shelf life.
Helium Leak Testing: Vacuum ModeHelium Leak Testing: Vacuum Mode Packages containing helium can be checked
for gross, fine and ultra-fine leaks using a vacuum chamber attached to a helium leak detector [“Hard” Vacuum Method].
The range of Helium leak rates detectable spans from low sensitivity (gross leak) values - E-1 - E-4 cc-atm/sec - to medium sensitivity (fine leak) values - E-5 - E-7 cc-atm/sec - to high sensitivity (ultra-fine leak) values - E-8 - E-10 cc-atm/sec.
Gas/Vapor/Microbial Sensitive Products
Active Ingredient Products (Gas/Vapor) A product’s micro-environment must be protected
against gas/vapor loss or gain, as needed. The barrier performance (integrity) of the package
combined with external environmental conditions determine a product’s shelf life.
Sterile Products The package’s integrity controls microbial
ingress of the package and resultant loss of
product sterility.
LDA Sims 1282+ UnitSIMSSeal Integrity Monitoring System
HSAMHead Space (Gas)Analysis Module
VTFM Vacuum Test Fixture Module
30+ years - packaging expertise 8+ years - leak testing experience
Helium Leak Testing Packaging Using a SIMS Unit
Procedure
Helium is flooded at the point of the packaging
machine/line process immediately prior to sealing
the blister/pouch/card/vial.
Helium is, thereby, captured in the head space of
the blister/pouch/card/vial.
Helium Leak Testing Packaging Using a SIMS Unit
Test Method Filled/sealed blisters/pouches/cards/vials are
taken from the production line. Each sample is placed inside a VTFM chamber
connected to the integrated helium leak
detection system (SIMS 1282+). The VTFM chamber encapsulates the entire
package ensuring that any He molecules
escaping from the package are captured by the
sensor.
Helium Leak Testing Packaging Using a SIMS Unit
Results The leak detector is connected to a computer
(integrated into the system).
The true leak rate is calculated by the software
taking into account the helium concentration
inside each package; as measured by the HSAM.
The test can be non-destructive, or destructive
for the packages and the product, depending on
materials & form
Advantages of He Leak Rate Methods and Instrumentation
Measurement Quality A package-specific vacuum chamber allows the
measurement of leak rates of test packages
without vacuum-induced failures.
The final result takes into account the helium
concentration inside the package, thereby providing
the actual leak rate (normalized to one atmosphere
driving force) for comparison against a pre-set
pass/fail (P/F) criterion; dictated by the product.
Advantages of Helium Leak Rate Methods and
Instrumentation Measurement quality
The helium concentration inside each test package
is measured (quantified) via a fixture (HSAM)
which measures the helium concentration with a
calibrated probe.
Gross leaks (>E-4 cc-atm/sec) are detected using
pre-determined settings which identify spikes of
helium during the test.
Advantages of He Leak Rate Methods and Instrumentation
Measurement Quality/Sensitivity
Empty (no Helium) packages are identified by the
absence of any signal above background due to a
lack of helium in the package.
Fine (& Ultra-Fine) leaks (<E-5 to E-9 cc-atm/sec) are
readily detectable using the Hard Vacuum Mode.
When you require high quality seals and a high
quality package, you need Helium leak detection
technology & leak testing instrumentation.
SIMS 180 TD+
The End – OF LOW SENSITIVITY PACKAGE
INTEGRITY TESTS
The Beginning - OF HIGH SENSITIVITY
PACKAGE INTEGRITY TESTS