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