An Overview of Package and Seal Integrity Testing

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An Overview of Package and Seal Integrity Testing

• Darrell R. Morrow, PhD
• Leak Detection Associates, Inc.
• Blackwood, New Jersey

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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.

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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

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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.

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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 gt 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 lt 1E-6 cc-atm/sec..

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Leak Detection Test MethodsComparative
Sensitivities
TEST METHOD/TECHNOLOGY D3078 - VACUUM
BUBBLE Vacuum Level 15" Hg Vacuum Level 21"
Hg Vacuum Level gt 21" Hg D3078 - DYE
PENETRATION Vacuum Level 15" Hg Vacuum Level
21" Hg Vacuum Level gt 21" Hg
Pressure Decay Carbon Dioxide Sensor Gas
Pressure - Bubble _at_ 10" H2O _at_ 20"
H2O Helium Tracer- Mass Spectrometer
Sniffer Mode Hard Vacuum Mode
10-1 10-2 10-3 10-4 10-5 10-6 10-7
10-8 10-9 10-10 Leak Rate (cc/s)
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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.

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Helium 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.

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Gas/Vapor/Microbial Sensitive Products

• Active Ingredient Products (Gas/Vapor)
• A products 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 products shelf life.
• Sterile Products
• The packages integrity controls microbial
• ingress of the package and resultant loss of
• product sterility.

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LDA Sims 1282 Unit
SIMS Seal Integrity Monitoring System
HSAM Head Space (Gas) Analysis Module
VTFM Vacuum Test Fixture Module

• 30 years - packaging expertise
• 8 years - leak testing experience

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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.

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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.

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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

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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.

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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 (gtE-4 cc-atm/sec) are detected using
• pre-determined settings which identify spikes of
• helium during the test.

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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 (ltE-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.

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The End OF LOW SENSITIVITY PACKAGE
INTEGRITY TESTSThe Beginning - OF HIGH
SENSITIVITY PACKAGE INTEGRITY
TESTS