Water purification solutions Razmišljate li o kvaliteti vode u Vašem laboratoriju? Osijek, 06.10.2011. Prehrambeno-tehnološki fakultet u Osijeku Jasenka Ivanković, Merck d.o.o. Zagreb
Agenda - Water purification fundamentals - Water contaminants - Quality monitoring - Purification techniques - Standards and norms - Pure water production and storage, ultrapure water production Presentation title in footer 00 Month 0000
Natural water sources Sea Water Iced Water Ground Water Lake Water Swamp Water River Water Presentation title in footer 00 Month 0000
Water contaminants groups + - INORGANIC IONS ORGANICS PARTICLES / COLLOIDS MICROORGANISMS DISSOLVED GASES Presentation title in footer 00 Month 0000
From natural water to pure & ultrapure water Natural water contains 5 main classes of contaminants These contaminants, if they may have negative effects on human health, are removed down to a safety level by Water Companies Potable tap water still contains some of these contaminants, at levels that are not harmful for humans However, even at that level, these contaminants can be detrimental to laboratory instruments & experimentations These contaminants should therefore be monitored and removed to acceptable levels by appropriate techniques. When their effect on experimentation is unknown, they should be removed as much as possible (precaution principle) Presentation title in footer 00 Month 0000
Water purification techniques + - Contaminants Removal By Still DI EDI RO UF MF AC UV 254 185 Presentation title in footer 00 Month 0000
Distillation Benefits Limitations Removes a large percentage of all types of contaminants Produces water with resistivity between 0.2 and 1 MegOhm.cm @ 25 C and TOC between 50 and 100 ppb Average investment Well known and perceived as easy to operate Not all contaminants are removed and several are generated during the process No control of water quality High operating costs due to electric heating (0.8KW/L) and water cooling (15 L tap water /L distilled water produced) Not ecologically friendly Regular maintenance (acid cleaning) or pretreatment (DI) is actually required to ensure optimum performance Presentation title in footer 00 Month 0000
Deionization with single use mixed bed resin Benefits Effective at removing ions (Resistivity : 1-10 Megohm.cm with a single pass through the resin bed) Easy to use (simply open the tap and get the water) Limitations Does not eliminate particles, organic materials or microorganisms. Limited capacity depending on binding sites density and accessibility : requires good quality feed water to prevent premature exhaustion. Capacity related to flow rate Incorrect resin selection or multiple regeneration will cause water contamination by organic,particulate. Presentation title in footer 00 Month 0000
Electrodeionisation (EDI) Benefit s Very efficient removal of ions and small MW charged organics (R> 5 MegOhm.cm @ 25 C) Low energy consumption High water recovery Low operating cost Low maintenance No particulates or organic contamination (smooth, continuous regeneration by weak electric current) Moderate investment Limitations Requires good quality (RO) feed water to prevent plugging (particulates), fouling (organic, colloids) of ion-exchange resin beads. Solution required to prevent scaling at the cathode (early solution = softener) CO2 not totally removed if at high level in feed water. Presentation title in footer 00 Month 0000
Reverse Osmosis Benefits Removes a fair percentage of all types of water contaminants (ions, organics, pyrogens, viruses, bacteria, particulates, colloids) Low operating costs due to low energy needs No need for strong acid and bases cleaning ; minimum maintenance Good control of operating parameters. Water consumption 2 to 10 times lower than stills (recovery up to 66%). Presentation title in footer 00 Month 0000 Limitations Not enough contaminants are removed to satisfy Type II requirements. Reverse Osmosis membranes are subject to plugging (particulates), fouling (organic,colloids), piercing (particle, chemical attack) and scaling (CaCO3) in the long run if not properly protected
Ultrafiltration Benefits Effective removal (>90%) of all organic molecules with molecular weight above the NMWL. Very efficient at removing pyrogens and Rnases (if validated) and viruses as well as particles. No risk of scaling ; limited risk of fouling. Low use of water and energy Low maintenance ; procedures well documented / accepted. Limitations Almost no rejection of ions, gases and low molecular weight organics (tightest UF membranes have a 1,000 dalton cut-off BioPak Presentation title in footer 00 Month 0000
Membrane (Screen) Microfiltration Benefits 100 % removal of all contaminants (particulates, bacteria)larger than pore size. Integrity test available Sterilizing filtration (0.22 um membranes - LRV > 7) Minimum maintenance : simply replace when required. High flow rates are achievable at low pressure Efficiency independent of flow rate. Limitations Minimum effect on other contaminants Surface retention : may be subject to fouling/ plugging Presentation title in footer 00 Month 0000
Activated Carbon Benefits Effective removal of a large range of organic substances (even of low molecular weight) by non specific binding (Van der Waals forces) or chlorine reduction Large capacity due to high developed surface Limitations Very little effect on other contaminants (except some particulates removed by depth filtration) Once all active sites are occupied, an equilibrium is established and organics are released. Bacteria may develop after several months. Efficiency depending on flow rate Presentation title in footer 00 Month 0000
UV Technology (185 + 254 nm) Benefits Conversion of traces of organic contaminants to charged species and ultimately CO2 (185 + 254) Limited destruction of microorganisms and viruses (254) Limited energy use Easy to operate Limitations Polishing technique only: may be overwhelmed if organics concentration in feed water is too high Organics are converted, not removed. Limited effect on other contaminants Good design required for optimum performance. Presentation title in footer 00 Month 0000
Technologies & Contaminants Removal IONS ORGANICS PARTICLE COLLOIDS BACTERIA GASES STILL DI RO UF MF AC UV Contaminant still 100% present (not removed) Contaminant completely (100%) removed
Main water purity criteria resistivity and TOC Presentation title in footer 00 Month 0000
Conductivity / resistivity measurement Conductivity and resistivity used to define the overall ionic purity/contamination Conductivity X = F c i z i µ i Conductivity (Siemens/cm) Faraday constant Concentration of each ionic species (eq/ml) Valence Mobility Ω -1.cm -1.s -1 [H + ] = [OH - ] = 10-7 M Minimum theoretical conductivity is 0.055 µs.cm -1 at 25 C Resistivity R = 1 X Maximum theoretical resistivity is 18.2 MΩ.cm at 25 C Presentation title in footer 00 Month 0000
Ultrapure water resistivity = f (t C) 18.2 Resistivity (MΩ.cm) 100 90 80 70 60 50 40 30 20 10 0 Presentation title in footer 00 Month 0000 It is important to notify the temperature at which conductivity or resistivity measures are performed as those values are strongly dependent on temperature. At 25 C, ultrapure water resistivity = 18.2 MΩ.cm 0 20 40 60 80 100 120 25 C At 10 C, ultrapure water resistivity = 43.4MΩ.cm Temperature ( C)
Millipore resistivity meter: a unique design Electrodes Support block Thermistor Concentric electrodes design ensures reproducible manufacturing and stable cell constant. No dead legs: immediate response Made of high quality 316 L stainless steel Low cell constant (0.01 cm -1) for accuracy Protected thermistor Thermistor sensitivity = 0.1 C Electronic autotest Alarms if defective parts Presentation title in footer 00 Month 0000
Millipore Built-in Resistivity Meters Design allows to perform suitability test as required by USP ( 645) Resistivity meter calibrated with traceability to internationally recognized primary standards Concentric electrodes design for cell constant stability Patented cell design US Patent Number: 0405347000 low cell constant (0.01 cm-1) Delivered with certificate of calibration Presentation title in footer 00 Month 0000
Why TOC? Because no correlation between resistivity & TOC level in ultrapure water + sugar Monitoring Municipal tap water Polishing Reverse Storage Unit osmosis reservoir No UV 20 1200 High purity water Resistivity, megohm.cm 18 16 14 12 10 8 0 0 30 60 90 120 150 180 210 240 Time, minutes 1000 800 600 400 200 TOC, ppb Presentation title in footer 00 Month 0000
Organics detection by TOC Monitor Built-in calibrated TOC Monitor TOC USP suitability testing: USP < 643> Presentation title in footer 00 Month 0000
TOC Monitor Calibration Certificate - 1 Presentation title in footer 00 Month 0000
Conclusion We have reviewed 2 water analytical methods that are well adapted to measure the ABSENCE of specific contaminants types in ultrapure water Resistivity measure allows to ensure on-line and in real time that ionic contamination of ultrapure water is below 1 µg/l level TOC measure allows to ensure that organic contamination is below the 5 µg/l level Both methods, in order to deliver significant results, require: Proper design : adequate measure + alarms if defective measure Proper calibration Respect of established norms Merck Millipore meters meet those criteria and deliver therefore valid assurance of water quality Presentation title in footer 00 Month 0000
Laboratory grade water norms Different laboratory water grades have been defined by different regulatory bodies: ASTM, ISO, USP, CLSI, CAP The grades correspond to both applications & specifications Their role is both technical & economical - Technical: select the adequate water quality for a specific application - Economical: avoid selecting a quality that is too high for an application as the cost of laboratory grade water production increases with the water quality Presentation title in footer 00 Month 0000
Water Quality Specifications Contaminant Parameter & unit Type 1 Type 2 Type 3 Ions Resistivity (M Ω.cm) > 18.0 > 1.0 > 0.05 Organics TOC (ppb) < 10 < 50 < 200 Particulates Particulates > 0.2 < 1 NA NA µm (units / ml) Silica Silica (ppb) < 10 < 100 < 1000 Bacteria Bacteria (cfu/ml) < 0.1 < 100 < 1000 Type 1 water HPLC and IC mobile phase preparation; blanks and sample dilution in GC, HPLC, AA, ICP-MS and other advanced analytical techniques ; preparation of buffers and culture media for mammalian cell culture, IVF, reagents for molecular biology... Complies with ASTM Type 1, ISO 3696 Grade 1, Pharmacopeiea
Type 3 water - basic laboratory applications Water baths Rotavapors Presentation title in footer 00 Month 0000 Autoclaves
Type 2 water - regular laboratory applications Titrators Presentation title in footer 00 Month 0000 ph Meters Regular lab solutions such as buffers Glassware Washers
Type 1 water - critical laboratory applications Molecular Biology Elemental Trace Analysis Cell Culture HPLC Presentation title in footer 00 Month 0000
Production of Pure Water Type 3 and Type 2
Тype 3 water - pure water - RiOs systems Technologies: Pretreatment + Reverse Osmosis (+ UV optional) Systems: RiOs (3,5,8 and16 l/h) and Large RiOs (30, 50, 100, 150 and 200 l/h) Applications: Type 3 Laboratory-grade water is used in laboratories mainly for non-critical applications such as: - Glassware rinsing - Feed water for humidifiers, autoclaves, washing machines - Feed water for Milli-Q ultrapure water systems
RiOs principles Conductivity cells Optional on-line UV Lamp (254 nm) Storage Reservoir Pump MILLIPORE Tap Water Type 3 Water 1. Progard pretreatment pack to protect the RO membrane: Activated Carbon (+ silver) against chlorine Polyphosphate against scaling Depth Filter against particulates Recovery Loop RO Reject Drain 2. RO Cartridge (including sanitization port): Removes all types of contaminants up to 98% (except gasses) Tank Point Of Use
Type 2 Water Systems & Applications Technologies: Pretreatment RO EDI or DI UV Type 2 Water Systems: Elix 3, 5,10,15, 20,35,70,100 RiOs-DI 3 UV Applications: Microbiology Media preparation Feed to clinical analyzers Chemical reactions run in water Weatherometers Washing machines Histology Feed to Ultrapure (Type 1) Milli-Q water systems
Electro - deionization (Elix technology) EDI module - Ion selective membranes - Ion exchange resins - Continuous current RO water 10-20µS A C A C H + Na + Cl - OH - Anode + Cl - H + Cl - Na + Na+ OH - - Cathode Cl - Na + Cl - Na+ Reject A - Anionic Membrane C - Cationic Membrane Product Resistivity: > 10 MOhm.cm TOC: < 30 ppb
ELIX Water System Principles Conductivity cells Optional on-line UV Lamp (254 nm) Storage Reservoir Pump Resistivity cell MILLIPORE Tap Water Type 3 Type 2 Water Water 1.Progard pretreatment pack to protect the RO membrane: Activated Carbon (+ silver) against chlorine Polyphosphate against scaling Depth Filter against particulates Recovery Loop RO Reject Drain 2. RO Cartridge (including sanitization port): Removes all types of contaminants up to 98% (except gasses) EDI Reject 3. EDI Module Removes remaining ions & small charged organic molecules 5 < R < 15 MΩ.cm Type 2 Point Of Use
ELIX Advantage System Principles On-line UV Lamp (254 nm) Storage Reservoir MILLIPORE Tap Water Type 3 Water Type 2 Water Recovery Loop Drain Recirculation Loop POD-Pak E-POD
2- ELIX E-POD Feature E-POD = Elix water Point Of Delivery Benefits for User 1. Improved bacterial water quality ᅳ ᅳ ᅳ Less than 0.1 cfu/ml (with final filter) Recirculation on UV light 254 nm Recirculation up to the point of use POU (no dead volume) 2. Ergonomic design & ease of use ᅳ ᅳ ᅳ ᅳ ᅳ Pressurized Type 2 water dispensing up to 2L/min Adapted for manual rinsing as well as vessel filling Volumetric dispensing available & easily accessible Monitoring at a glance on the POD screen (quality, volume ) Printing Function 3. Versatility for multiple applications or users ᅳ ᅳ ᅳ POD-Paks = several POU filters available for specific quality Up to 3 E-PODs connected to the same system No need to carry water around anymore!
Storage and distribution - Types 3 & 2 (pure) water Best practices for laboratory water storage
The storage challenge Your needs The options you have What is this water used for? Any quality requirements? How much water do you need, when? Do you need to distribute the water to a bench, an instrument? etc 1.Size of reservoir and of system 2. Right storage solution to maintain the best quality 3. Options to get pure water where and when you need it
Small Storage Reservoir offer
Summary: Storage & Distribution Good Practices Intermittent recirculation while limiting temperature build up Recirculation Loop. UV 254 nm Lamp in the Tank (ASM) Sanitary overflow + vent filter. Conical bottom tank for complete emptying Maintains water quality during non-use periods. Avoids stagnation and maintains water quality. Prevents biofilm formation Reduces need for chemical sanitisation Introduction of clean filtered air during drawoff of water. Easy to clean
Production of ultrapure water Type 1
Ultrapure water adapted to each application Tap water Pure water Type 3 or 2 Pretreatment step Polishing step Ultrapure water Type 1 Nuclease-free water Water for trace ion analysis Water for organic analysis Low bacteria water
STANDBY READY C M Ω.cm@ Ω 25 C ΩΩ ppb TO C L STANDBY READY C M Ω.cm@ Ω 25 C ΩΩ ppb TO C L STANDBY READY C M Ω.cm@ Ω 25 C ΩΩ ppb TO C L New Concept Several water qualities One central purification unit and several point-of-use purifiers Screen filter Ultrafilter Activated Carbon Standard high purity water Water with no bacteria by-products (endotoxins, nucleases, ) Water with very low volatile organic pollutants
Q-POD Dispenser The most critical purification step for the user application comes last
POD-Pak polishers for any application
Type 1 Water Systems and Applications Type 1 Water Systems: Milli-Q Integral (with TOC monitor) Milli-Q Direct (with TOC indicator) Direct-Q 3 UV Milli-Q Advantage A10 (with TOC monitor) Applications: HPLC and IC mobile phase preparation Blanks and sample dilution in GC, HPLC, AA, ICP-MS and other advanced analytical techniques Preparation of buffers and culture media for mammalian cell culture, IVF, reagents for molecular biology
Gradient profiles - water with various TOC levels 20 ppb 13 ppb 9 ppb 5 ppb 2 ppb Increasing TOC levels result in more extraneous peaks and shifts of the baseline Important to know what s the TOC level of the water you use in your mobile phase!
Water contaminants: Summary of effects on HPLC performance Contaminants Effects on HPLC Improper check valve operation Particles Damage to pump and injector Plugging of frits and column Organics Ions Bacteria Ghost peaks Increased background noise Drifting baselines Some ions absorb in the UV range (e.g., NO 3-, NO 2- ) With MS detectors: Na +, K + adduct peaks Plugging of frits and columns Ghost peaks
Summary of ISO 11131-1 : Type 2 water quality recommended for microbiology media preparation Since 99% of the culture media is water, water quality is critical. It should be: free of nutrients free of toxic substances resistivity > 0.3 MΩ.cm (< 10 µs/cm) low concentration of chlorine low concentration of heavy metals low microbial count
Water systems designed to serve your needs
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