Latest developments in HEPA/ULPA filters In situ leak testing

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Latest developments in HEPA/ULPA filters In situ leak testing J.M. Vanhée, Product Manager Clean Process Camfil Farr France Latest developments in HEPA/ULPA filters In situ leak testing Filter Control :: EN1822 vs ISO - EN 14644-3,, Bleed Trough issue Terminal Diffuser Improvement to prevent leaks and facilitate terminal filter controls (PHARMASEAL) High Temperature HEPA filter improvement to avoid leaks due to expansion - 1 -

MPPS (Most Penetrating Particle Size) Filter Efficiency (%) Total Efficiency 4 effects combined Minimum Eff. Diffusion MPPS Interception Sifting +inertia 10nm 0,1µm 0,2µm 1 µm 10 µm Particle diameter Particle > MPPS... is stopped more efficiently Particle < MPPS... ALSO!!! Filter Efficiency Measurement depends on Challenge Test Aerosol PARTICLE SIZE EN1822 MIL STD 209 MPPS 0,1 < Ø < 0,2 µm DOP Ø = 0.3 µm EUROVENT NaCl = cube 0,35 µm ISO EN 14644-3 Ø = 0.5-0.7 µm - 2 -

EN1822 Classification MPPS based (0.1-0.2µm) HEPA/ULPA panel filter scanning on automatic and reliable test rig,factory made by producer Leak level linked to filter class filter probe ISO-EN 14644-3 B.6 Installed filter system leakage test confirm filter system is properly installed and that leaks have not developed during use absence of leakage, introducing an aerosol challenge upstream of the filters and scanning immediately downstream of the filters and support frame. leak test complete filter installation : filter media, frame, gasket and grid system. The installed filter system leak test should not be confused with the efficiency test of individual filters at the place of manufacture. portions of ISO-EN 14644-3 are adapted from IEST-RP-CC034-3 -

ISO-EN 14644-3 B.6.2 Procedures for installed filter system leakage scan test with an aerosol photometer Challenge Aerosol features Size 0,5 μm to 0,7 μm (geometric standard deviation of up to 1,7) Concentration 10 mg/m3 and 100 mg/m3 recommended > 20mgm3 and < 80 mg/m3 B.6.2.7 Acceptance criteria Designated leaks = reading greater than 10 4 (0,01 %) of the upstream challenge aerosol concentration. Alternative acceptance criteria may be agreed between the customer and the supplier. Installed filter system leakage test... In real life In some cases, GOOD FILTERS according to EN1822 fail the in situ <0.01% leak test! It is the so called Bleed Through issue Can be due to : Operating errors induction effects, pollution, bad 100% sampling... Airflow velocity Challenge aerosol size - 4 -

Filter «BLEED-THROUGH» Over-Velocity HEPA/ULPA Panel Filter standard nominal front velocity = 0,45m/s Used velocity > 0,45m/s... 0,9 to 1 m/s => efficiency Example H14 H13 To avoid Bleed Trough due to over front velocities Specify High Airflow HEPA/ULPA panel filters that are EN 1822 tested at high airflow ex. standard 610x610 mm MD = 600m3/h high airflow series MD= or MG=2000m3/h - 5 -

What is the actual size of aerosols used for In-Situ leak controls? Photometer can t measure particle sizes? Analysis of Aerosol generators currently used Camfil Farr Laboratories have made the measurement of aerosol produced by 2 currently used thermal aerosol generators with 3 types of oils. CONCLUSION : Mean mass diameter is close to 0.25µm, instead of 0.5-0.7 µm - 6 -

Bleed Though due to in-situ Challenge Aerosol size MPPS leak rate (EN 1822) As on site particle size is too small, a leak free filter can be considered wrongly failing on site Conclusion SITUATION On site controls are most of the time stronger than ISO-EN 14644-3 requirement : This is due to the use of thermal generators that generate challenge aerosol between 0.2-0.3µm (close to MPPS) instead of 0.5-0.7µm Consequently as acceptance criteria is 0.01%, In situ Problems can occur with : H13 : leak rate < 0.25% @ MPPS according EN1822 H14 : leak rate < 0.025% @ MPPS according EN1822 TO AVOID THIS PROBLEM Camfil Farr guaranties H14 MEGALAM leak rate < 0.01% @ MPPS instead of standard 0.025% Specify U15 filters (standard leak rate < 0.0025% << 0.01%) - 7 -

Latest developments in HEPA/ULPA filters In situ leak testing Filter Control : EN1822 vs ISO - EN 14644-3, Bleed Trough issue Terminal Diffuser Improvement to prevent leaks and facilitate terminal filter controls (PHARMASEAL) High Temperature HEPA filter improvement to avoid leaks due to expansion (TERMIKFIL) PHARMASEAL An innovative solution for ducted ceiling terminal HEPA/ULPA filtration For Pharmaceutical Industry and Biotechnology facilities 1 - Design : ZERO leak policy 2 - Full filter control equipped 3 - Individual Isolation possibility - 8 -

PHARMASEAL A solution that has already proved itself Examples of recent projects Amgen Puerto Rico 700 Amgen Rhode Island 600 Idec California 600 Wyeth BioPharma Missouri 90 Bayer California 290 Lilly Indianapolis 300 Merck North Carolina 200 Berlix *Schering Oregon 250 Cangene Canada 90 Wyeth PR & Ireland 180 PHARMASEAL ZERO Leak policy : by design More security fixed interfaces => fully continuous welded inlet collar hood mobile interfaces => gel seal filter bubble tight damper - 9 -

PHARMASEAL ZERO leak policy : by factory control + tracability Zero leak proof by facts : each PHARMASEAL is leak tested under pressure at 750Pa Unique Serial Numbers are assigned to each hood after leak testing and provide traceability. PHARMASEAL Fully equipped for GMP Tests (EMERY test, pressure drop, airflow, velocity) (1) Control ports immediate access => hinged grille => captive 1/4 turn fastener (1) (1) (2) Everything managed from room side => dedicated control panel => tests ports => filter clamping => damper adjustment (2) - 10-

PHARMASEAL Fully Equipped for Filter GMP controls All centralised on a ergonomic device => Injection + control from room side => Only 1 single person can test filter Quick and airtight connection => stainless steel quick disconnect ports (1) (2) EMERY test really performed in compliance with rules => aerosol dispersion ring (3) NO EMERY IN HVAC DUCTING => Fire safety Aerosol Input (2) 100%(1) Diffusion ring(3) (2) PHARMASEAL Easy and Secured filter installation and replacement No clamping effort nor complexity => pre-positioned retaining rotating tables (1) Immediate perfect filter positioning => filter guides as standard (2) No leak nor by-pass risks => gel seal / knife edge sealing technology (3) (3) (2) (1) - 11-

PHARMASEAL Individual Isolation Possibility Bubble Tight Damper Visible and precise adjustment from room side Full balancing capabilities Airtight individual isolation Camfil Farr bubble tight damper knife edge damper position indicator gel PHARMASEAL Individual Isolation Possibility Bubble Tight Damper ADVANTAGES Filter Maintenance diffuser isolated => no non filtered air supplied into the room during filter maintenance => no contamination => no need heavy room decon procedure can be done without stopping HVAC Local filter decontamination with decon shroud Room decontamination Reduces Downtime & Expenses Camfil Farr bubble tight damper - 12-

PHARMASEAL A Bio-Pharma GMP designed 1 2 3 4 5 General Immediate access to filter and all controls from roomside => hinged grille Filter installation and replacement No clamping effort nor complexity => pre-positioned retaining rotating tables Immediate perfect filter positioning => filter guides as standard No leak nor by-pass risks => gel seal / knife edge sealing technology Filter GMP controls All centralised on a ergonomic device => integrated side control panel Quick and airtight connection => stainless steel quick disconnect ports EMERY test really performed in compliance with rules => aerosol dispersion ring Individual airflow adjustment Visible and precise adjustment from room side => damper position indicator Full balancing capabilities => guillotine damper Full balancing and airtight module isolation => Camfil Farr bubble tight damper QA evidences Full traceability items included => unique serial number, individual leak test, Latest developments in HEPA/ULPA filters In situ leak testing Filter Control : EN1822 vs ISO - EN 14644-3, Bleed Trough issue Terminal Diffuser Improvement to prevent leaks and facilitate terminal filter controls (PHARMASEAL) High Temperature HEPA filter improvement to avoid leaks due to expansion (TERMIKFIL) - 13-

End User s needs High Temperature : What does it mean? 350 C => Sterilization & Depyrogenation tunnels (destroy endotoxins) 230 C - 250 C => Sterilization & Depyrogenation static ovens 120 C => Granulation dryers < 70 C - 80 C => HVAC End User s needs : FDA / EUGMP Requirements Sterile Products EU / GMP : Class A = ISO5 operational => HEPA filtration FDA Guidelines Guidance for Industry Sterile Drug Products Produced by Aseptic Processing Current Good Manufacturing Practice September 2004 Class 100 (ISO5) Overall Efficiency > 99.97% 0.3µm Leak -free @ 0.01% with scanning of the filter face + frame HT FILTERS ARE SCANNED BY BIO-PHARMA CUSTOMERS - 14-

En User s needs : Where in its process? Static Ovens : 250 C FRSi HT HEPA Filters SOFILAIR HT230 End User s needs : Where in his process? Tunnels : 350 C Vials entry (HEPA Filtered zone) Entry zone Hot zone Cool zone Process Process AIR Process HT HEPA Fiers Vials washing Vials Heating 350 C (sterilization + depyrogenation) Vials Zone @ 350-15-

High Temperature : HEPA Filters requirements => components high temperature resistant <=> no degradation => filter assembling high temperature resistant <=> expansion => no particle shedding (out gassing) <=> burning cycle Filter Components 5 Main Components Frame Media Sealant Separator Gasket - 16-

High Temperature : What does that means for filters? TEMP Sealant LUT Gasket Frame Separ. MEDIA Media Filter 350 C Ceram. GF-HT 230 C / 250 C Silicon JOINT Glass Fibre Silicon CADRE SS Ceram. SS SEPAR. Alum Glass Glass Alum GF-HT FILTRE FRK, F-Series TERMIKFIL SOFILAIR-HT230 FRSi, K-Series 120 C < 70 C / 80 C PU PU PU/ EPDM PU / EPDM Metal Metal Plastic... Glass Alum Hot Melt GF GF SOFILAIR-HT120 Absolute SOFILAIR(80 C) Close Pleat MEGALAM 350-400 C CF Solutions Efficiency : Camfil Farr Guarantee FRK TERMIKFIL Prior to any Heating Factory certified H13 @ 20 C New > 99,95% MPPS Leak-Free : YES After initial on-site burn-in cycle 99.97% 0.3µm overall Leak-free : NO After Factory Heating (300 C) Factory certified > 99,99% 0.3µm Leak-Free : YES After initial on-site burnin cycle 99.99% 0.3µm overall Leak-free : YES - 17-

350 C HEPA Filtration : main problem / Leak-free : NO Torsional forces (expansion) => cracks between sealant and frame => leaks Differential expansions : sealant cracking => leak frame/sealant Palliative Solution dynamic seal BOSCH (Bausch+Ströbel, IMA,...) Spacers FRK - + + - 18-

Differential expansions : sealant cracking => leak frame/sealant Preventive Solution a high temp. consistent set Frame + Sealant + Media => TERMIKFIL ceramic frame glass fibre media ceramic sealant Latest developments in HEPA/ULPA filters In situ leak testing THANK YOU ANY QUESTIONS? J.M. Vanhée, Product Manager Clean Process Camfil Farr France - 19-