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Sealing Challenges In The Pharmaceutical Industry

Wed, 09/05/2007 - 5:17am
Testing shows differences in materials and seal life

by Dr. Burkhard Ledig
CPI Global Technical Manager

The acronyms may be short in the pharmaceutical, chemical processing, and food industries, but they pose big sealing challenges. CIP, Cleaning in Place, uses chemicals lethal to the majority of elastomer seals, while SIP, Sterilization in Place employs superheated steam up to 140C with an even greater deteriorating affect. In addition to this, for some applications, the seals must meet the strict requirements for FDA approval.

Trelleborg Sealing Solutions, by working closely with major customers in the chemical industry, saw and responded to the trend for increasingly aggressive chemicals and processes. To extend seal life and reduce downtime, they tested existing materials and developed new compounds to cost-effectively meet performance requirements and approvals. The main conclusion of the Trelleborg Sealing Solutions research, the first of its kind within the industry, was that by matching the right sealing compound to a specific application, this could be achieved.

Specifying the right material when CIP and SIP is used is not a simple matter. In fact, test results proved that some elastomer types recommended in DIN 11864 and DIN 11851, applying to fittings for connections in process equipment usually subject to CIP and SIP, were unsuitable or not wholly suitable for sealing with these cleaning regimes. And FFKM, perfluoroelastomer, not given as a recommended material for sealing within the standards, was universally suitable even at elevated temperatures.
CIP chemicals
Automated CIP or SIP systems ensure safe and efficient processing, prevent toxic contamination of products and minimize re-contamination of the process. To achieve cleaning efficiency and effectiveness, a complex mixture of chemicals is required.

CIP cleaning media includes the following:
• Alkaline CIP mixtures based on sodium hydroxide and surfactants used to remove organic and fatty contamination, emulsions and gels.
• Acid CIP mixtures based on nitric acid and phosphoric acid or sulphuric acid used to remove inorganic sediments in tanks, tubes, fermentation or similar equipment.
• Alkaline CIP disinfecting mixtures based on sodium hypochlorite and active chlorine.
• Acid CIP disinfecting mixture based on per-acetic acid and hydrogen peroxide used on surfaces based on activated oxygen.
• Intensive disinfecting media based on hydrogen peroxide and surfactants added to alkaline CIP media to remove those residues requiring an oxidation stage.

These chemical media do not affect processing equipment manufactured from stainless steel but severe damage may be caused to elastomeric seals, especially in applications where thermal load and pressure are involved.

Seal materials must be chemically resistant to the product processed, CIP media used and also the harsh SIP sterilisation process using superheated steam up to 140°C. They need to withstand abrasion by any solids contained in the product and have a low level of extractables. Seal surfaces must be easy to clean and sterilise and if required, the material should have FDA approval.
Standards applying to seals
Standards do not really help in deciding which materials to specify for seals. They only offer general information and refer just to groups of elastomeric materials and their compliance with FDA standard 21 CFR 177.2600. No specific characteristics are defined, such as vulcanising system or shore hardness, nor are indications given regarding chemical resistance to common CIP media or performance in steam sterilization at temperatures up to 140°C.

The standards DIN 11864 and DIN 11851, covering fittings for the food, chemical and pharmaceutical industry on aseptic and stainless steel connections, recommend Ethylene Propylene Diene Rubber (EPDM), Hydrogenated Acrylonitrile Butadiene Rubber (HNBR), Silicone Rubber (VMQ) and Fluoroelastomer (FKM) as materials for elastomeric seals used in sterilising technology. For some applications, these materials must also comply with the relevant FDA regulation under 21 CFR 177.2600.
Summary of Trelleborg Sealing Solutions Test Results
However, the Trelleborg Sealing Solutions tests showed the following:
• Silicon rubber (VMQ) is not suitable for most CIP and SIP applications including alkaline media or under hot steam sterilization conditions.
• Generally, HNBR is not suitable in any CIP media.
• The FDA compliant FKM materials showed significant weaknesses in alkaline-based media as well as acidic media, including the per-acetic acid and hydrogen peroxide mix due to their polar nature.
• EPDM was established as an excellent sealing material for aseptic technology but some formulations are less suited to 'intensive' CIP additives.
• FFKM, Perfluoroelastomer showed most resistance in CIP media, especially at elevated temperatures. It is universally suited for CIP applications and SIP sterilization processes.
Performance in SIP Sterilization Processes
After CIP cleaning, many process plants employ a sterilization stage with steam, typically in the range 125°C up to 140°C and for this reason, the steam resistance of the elastomers used must always be considered.

The conclusions of Trelleborg Sealing Solutions on performance of elastomer materials in steam:
• At 125°C up to 140°C FKM and HNBR are already beyond their performance limits.
• In the presence of atmospheric oxygen and steam, EPDM is resistant up to 150°C whereas without oxygen, temperatures of up to 200°C are achievable.
• FFKM, Perfluoroelastomer offers the best temperature resistance with some grades capable of operating in temperatures up to 230°C.
• Steam temperatures are increasing up to and beyond 150°C. Under these operating conditions, EPDM may reach its natural limit and in these cases, perfluoroelastomer is the best material.
Selecting For Chemical Compatibility
The results of Trelleborg Sealing Solutions research demonstrate that it is not simple to select the optimum seal material for a CIP or SIP application. Even materials that may appear similar react differently in chemical media. To ensure seal life is maximized, it is vital to work with a sealing supplier who can offer a range of tested and proven materials.

Trelleborg Sealing Solutions publish a chemical compatibility chart to help equipment manufacturers and processors select the right seal for an application. This gives details of the resistance of different materials in a variety of chemical media and offers an effective guide to initial compound selection. However to maximize seal life in any aggressive sealing environment it is recommended that manufacturers and users contact a supplier who can provide the best sealing recommendation and collaborate in specific testing, if appropriate.

Table of Results:
  EPDM 1 EPDM 2 FKM 1 FKM 2 HNBR FFKM
Alkaline CIP formulations 4 1 4 4 3 1
Acidic CIP formulations 1 1 4 4 4 1
Disinfectant alkaline CIP 1 1 3 1 4 1
Disinfectant acidic CIP 4 1 4 4 4 1
Disinfectant spray injection 4 4 4 4 4 2
Key:
1 - Strongly recommended
2 - Recommended
3 - Recommended with reserves
4 - Unsuitable
Details of Trelleborg Sealing Solutions tests
The following seal materials were tested:
• Two types of peroxide cross linked Ethylene Propylene Diene Rubber (EPDM)
• Two types of Fluoroelastomer (FKM), cross-linked with bisphenol
• A Hydrogenated Acrylonitrile Butadiene Rubber (HNBR), cross-linked with peroxide
• A FFKM Isolast® perfluoroelastomer, which conforms to FDA Guidelines 21 CFR 177.2400 (d) and 21 CFR 177.2600 (e, f)

Silicone rubber (VMQ) was not tested as initial experiments showed it not to be sufficiently resistant in alkaline media and under conditions of live steam sterilization.

The material test specimens were immersed in the following CIP media concentrations, at temperatures given for one week in accordance to DIN 53521:
• Alkaline CIP formulations based on caustic soda liquor and surfactants; concentration of 4%, temperature 80°C.
• Acidic CIP formulations based on nitric acid or sulphuric acid; concentration of 2%, temperature 80°C.
• Disinfectant alkaline CIP formulations based on sodium hypochlorite and active chlorine; concentration of 3%, temperature 80°C.
• Disinfectant acidic CIP formulation based on peracetic acid and hydrogen peroxide; concentration of 2%, temperature 80°C.
• Disinfectant spray injection media based on hydrogen peroxide with a concentration of 1%, temperature 80°C.

After the test period the hardness (shore A) and percentage weight change were measured along with the most important parameter, volume change.

Because of the dead-space-free installation of seals in sterile technology, narrow limits are set on volume change of the sealing material.

Recommendations for use dependent on volume change:
• Less than 5% - material suitable for sealing.
• More than 5% but 10% or less - material can only be used for sealing with reservations.
• More than 10% - material not suitable for sealing.

About the author: Dr. Burkhard Ledig is CPI Global Technical Manager at Trelleborg Sealing Solutions. He studied chemistry at Marburg and since 1997, he has worked for Trelleborg Sealing Solutions, where he has held various positions, including European Technical Manager Isolast. He conducts market projects for the company's Pharmaceuticals and Food and Chemicals and Process Technology divisions. He can be reached at Burkhard.ledig@trelleborg.com

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