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Pharmaceutical Processing News
News Release from: Trelleborg Sealing Solutions | Subject: Seal testing for CIP SIP
Edited by the Processingtalk Editorial
Team on 27 December 2005
Tests on CIP/SIP sealing materials
Acronyms may be short in the chemical processing, food and pharmaceutical industries, but they pose big sealing challenges: a review by Dr Burkhard Ledig, CPI Global Technical Manager
The acronyms may be short in the chemical processing, food and pharmaceutical industries, but they pose big sealing challenges CIP (Cleaning in Place) uses chemicals lethal to the majority of elastomer seals, while SIP (Sterilisation in Place) employs superheated steam up to 140C with an even greater deteriorating affect
This article was originally published on Processingtalk on 3 Dec 2003 at 8.00am (UK)
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The main conclusion of the Busak+Shamban 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 CHEMIACALS.
Automated CIP or SIP systems ensure safe and efficient processing, prevent toxic contamination of products and minimise 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 140C.
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 sterilisation at temperatures up to 140C.
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.
However, the Busak+Shamban tests showed the following.
* Silicon rubber (VMQ) is not suitable for most CIP and SIP applications including alkaline media or under hot steam sterilisation 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 sterilisation processes.
PERFORMANCE IN SIP STERILISATION PROCESSES.
After CIP cleaning, many process plants employ a sterilisation stage with steam, typically in the range 125C up to 140C and for this reason, the steam resistance of the elastomers used must always be considered.
The conclusions of Busak+Shamban on performance of elastomer materials in steam.
* At 125C up to 140C FKM and HNBR are already beyond their performance limits.
* In the presence of atmospheric oxygen and steam, EPDM is resistant up to 150C whereas without oxygen, temperatures of up to 200C are achievable.
* FFKM, Perfluoroelastomer offers the best temperature resistance with some grades capable of operating in temperatures up to 230C.
* Steam temperatures are increasing up to and beyond 150C: 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 Busak+Shamban 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 maximised, it is vital to work with a sealing supplier who can offer a range of tested and proven materials, such as Busak+Shamban.
Busak+Shamban 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 maximise seal life in any aggressive sealing environment it is recommended that manufacturers and users contact Busak+Shamban, who can provide the best sealing recommendation and collaborate in specific testing, if appropriate.
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 sterilisation.
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 80C.
* Acidic CIP formulations based on nitric acid or sulphuric acid; concentration of 2%, temperature 80C.
* Disinfectant alkaline CIP formulations based on sodium hypochlorite and active chlorine; concentration of 3%, temperature 80C.
* Disinfectant acidic CIP formulation based on peracetic acid and hydrogen peroxide; concentration of 2%, temperature 80C.
* Disinfectant spray injection media based on hydrogen peroxide with a concentration of 1%, temperature 80C.
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.
DETAIL OF TEST RESULTS BY MATERIAL AND MEDIA.
Alkaline CIP formulations based on caustic soda liquor and surfactants; concentration of 4%, temperature 80C.
* EPDM1 Not recommended: 8% shrinkage due to surfactants, which extracted constituents from the seal.
* EPDM2 Strongly recommended: Volume change minimal.
* FKM1 and 2: Unsuitable, Destroyed by sodium hydroxide.
* HNBR: With reserves: 5% volume change but other results in alkali show limited performance.
* FFKM Strongly recommended: Best sealing material in this media on all three parameters - practically unchanged.
Acidic CIP formulations based on nitric acid or sulphuric acid; concentration of 2%, temperature 80C.
* EPDM1 and 2: Strongly recommended, Practically no volume change.
* FKM1 and 2: Unsuitable: Extreme volume increase.
* HNBR: Unsuitable: Swelled by almost 100%.
* FFKM Strongly recommended: Practically no volume change.
Disinfectant alkaline CIP formulations based on sodium hypochlorite and active chlorine; concentration of 3%, temperature 80C.
* EPDM1 and 2: Strongly recommended, Minimal volume change.
* FKM1: With reserves: Volume change of 6%.
* FKM2: Strongly recommended: Minimal volume change.
* HNBR: Unsuitable: Volume change significantly higher than other materials.
* FFKM Strongly recommended: Minimal volume change.
Disinfectant acidic CIP formulation based on peracetic acid and hydrogen peroxide; concentration of 2%, temperature 80C.
* EPDM1 Unsuitable: 8% volume increase.
* EPDM2 Strongly recommended: Fully inert, the most cost-effective material for this media.
* FKM1 and 2: Unsuitable: Volume change exceeded 65% probably due to absorption of acetic acid.
* HNBR: Unsuitable: Significant volume change.
* FFKM: Strongly recommended: Minimal volume change.
Disinfectant spray injection media based on hydrogen peroxide with a concentration of 1%, temperature 80C.
* EPDM1 and 2: Unsuitable, Volume increase of 20% and surfaces became sooty.
* FKM1 and 2: Unsuitable, Volume change of between 15 and 22%.
* HNBR: Unsuitable, High volume increase.
* FFKM Strongly recommended: Fully inert, the only sealing material suitable for this media.
RESULT TABULATION: Data in the order: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.
Profile of author: Dr Burkhard Ledig is CPI Global Technical Manager at Busak+Shamban.
He studied chemistry at Marburg and since 1997, he has worked for Busak+Shamban, 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.
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