Dry tests on empty rigid packaging - ASTM D4991

The ASTM D4991 test is used to carry out leakage tests on empty rigid containers containing liquid or viscous products.

This method applies to empty containers. It is used to check the integrity of the packaging without its contents. It should be used during the design phase of the packaging and its closure system.

As a laboratory, we are well aware of the importance of this type of test. We are fully conversant with testing protocols and guide companies through the implementation of these processes.

Control Sensei offers you the peace of mind of knowing that all your needs will be met.

We will be in constant communication throughout the testing process. Where packaging does not meet requirements, we will help you find solutions.

Summary of ASTM D4991 test method

The ASTM D4991 integrity test recommends not using a simple water bath to carry out the test, but a solution made up of 50% water and 50% ethylene glycol (C2H6O2).

This will ensure that the boiling temperature remains high enough not to disrupt the test with spurious bubbles. Ethylene glycol has a boiling temperature of around 200°C (424°F).

Test procedure in accordance with ASTM D4991

To carry out this test, the chamber is filled with a solution of water and etylene glycol.

The solution is prepared to remove the dissolved air. The mixture is subjected to an extreme vacuum of -950 mbar for 10 minutes. This allows the air dissolved in the mixture to be evacuated.

The empty containers are all hermetically sealed to the same specifications (tightening torques, caps, seals, etc.).

A minimum of 3 identical samples must be tested at the same time.

The rigid containers are then placed in the vacuum chamber, immersed and subjected to depressurisation.

The method recommends increasing the vacuum to -950 mbar.

Once the target vacuum has been reached, the vacuum must be maintained for at least 10 minutes.

For plastic packaging, the test time will be 30 minutes.

Interpreting the results.

Observe the samples for any columns of bubbles that might indicate the presence of a leak.

Once the time has elapsed, gradually return to atmospheric pressure and keep the samples immersed for at least 30 seconds at atmospheric pressure.

Once the 30 seconds have elapsed, check that there is no liquid inside the packs.

If no bubbles appear during the test and there is no liquid inside your packaging, the test is conclusive.

ASTM D4991 tests apply to the following products:

  • 🏭 Industrial liquids
  • ☠️ Hazardous and non-hazardous liquids
  • 🫙 Rigid containers
  • 🍾 Beverages (non-carbonated)
  • 🧴Perfume bottle / Fragrance
  • 💅 Liquid cosmetics in bottles or flasks
  • 💊 Pharmaceuticals
  • 🧪 Chemical products packed in rigid containers
  • 🛁 Personal care, health & hygiene
  • 🪣 Domestic cleaning

Our solution fits your needs

Our vacuum chambers are hermetically sealed, so you can maintain a vacuum for as long as you need.

Our test programmes have been adapted to make it easier to carry out the test. The input screen allows you to enter the starting altitude and the arrival altitude instead of entering the vacuum.

They make it easy to perform ASTM D4991 tests.

Other test methods