An Overview of Package and Seal Integrity Testing Darrell R. Morrow, PhD Leak Detection Associates,...

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