Water Purification System for a Laboratory Facility. Millipore Corporation Bioscience Division Christopher Yarima Mike Kelly

Transcription

1 Water Purification System for a Laboratory Facility Millipore Corporation Bioscience Division Christopher Yarima Mike Kelly

2 Outline Contaminants in Water Pure Water Applications and Quality Standards Water Purification Technologies Key Water Purification System Design Steps Systems Questions

3 Water Chemistry Contaminants

4 Ground & Surface Water Surface Water - Lower in dissolved ions - Higher in organic materials - Higher in particulates -Higher in biological material Ground Water - Higher in dissolved ions - Lower in organic materials - Lower in particulates -Lower in biological Material

5 Contaminants in Potable Water Inorganic Ions Organics Particles (Colloids) Microorganisms (Endotoxin) H H H-C-C-OH H H Cations Na+ Ca+2 Natural Tannic Acid Humic Acid Anions Cl- HCO-3 Man Made Pesticides Herbicides Non Dissolved Solid Matter (Small deformable solids with a net negative charge) Bacteria, Algae, Microfungi (Lipopolysaccharide fragment of Gram negative bacterial cell wall)

6 Measurement of Contaminant level Contaminant Inorganic Ions Organics Particles (Colloids) Bacteria Endotoxin Measurement Conductivity (Resistivity) Total Oxidizable Carbon (T.O.C.) Silt Density Index / Fouling Index Colony count on 0.45 μm membrane. -Rabbit Inoculation test -LAL Test Unit μs/cm MΩ.cm ppb (μg/l) Rate of pluggage of 0.45 μm membrane. cfu/ml Endotoxin units/ml

7 Measurement Units Thickness of a Human hair = 90 microns Smallest visible particle = 40 microns 1 Micron = 10-6 Meters Smallest bacteria = 0.22 micron ppm : Parts per Million = mg/liter ppb : Parts per Billion = microgram/liter ppt : Parts per Trillion = nanogram/liter 1 ppb = 1 Second in 32 Years.!!!

8 Water Standards

9 Standards and Common Terms Ultrapure Type 1 Ultrapure/Reagent Grade Critical Applications Water for HPLC,GC, HPLC,AA, ICP-MS, for buffers and culture media for mammalian cell culture & IVF, reagents for molecular biology... Pure Type II Pure/Analytical Grade Standard Applications Buffers, ph solutions,culture media preparation,clinical analysers and weatherometers feed. Type III Pure/Laboratory Grade General Applications Glassware rinsing, heating baths, humidifiers and autoclaves filling

10 Laboratory Water Purity Specifications Consolidated Guidelines Contaminant Parameter (units) Type 1 Type 2 Type 3 Ions Resistivity (MΩ-cm) > 18.0 > 1.0 > 0.05 Silica (ppb) < 10 < 100 < 1000 Organics TOC (ppb) < 20 < 50 < 200 Particles particles > 0.2 um (#/ml) < 1 NA NA Bacteria Bacteria (cfu/ml) < 1 < 100 < 1000 Endotoxin (EU/ml) < NA NA Regulatory Agencies with Published Standards: ASTM: American Society for Testing and Materials CLSI: Clinical and Laboratory Standards Institute (previously NCCLS: National Committee for Clinical Laboratory Standards) CAP: College of American Pathologists ISO: International Organization for Standardization USP: United States Pharmacopoeia EU: European Pharmacopoeia

11 ASTM Standards for Laboratory Reagent Water Contaminant Parameter (units) Type 1 Type 2 Type 3 Ions Resistivity (MΩ-cm) > 18.0 > 1.0 > 4.0 Silica (ppb) < 3 < 3 < 500 Organics TOC (ppb) < 100 < 50 < 200 Particles particles > 0.2 um (#/ml) < 1 NA NA Bacteria Bacteria (cfu/ml) 10/ / /10 ml ml ml Endotoxin (EU/ml) < NA ASTM: American Society for Testing and Materials

12 CLSI*, water quality specifications CLSI guidelines should be read to understand scope and detail for each requirement CLRW; Clinical Laboratory Reagent Water SRW; Special Reagent Water CLRW water quality with additional quality parameters and levels defined by the laboratory to meet the requirements of a specific application For example: CLRW quality with low silica and CO 2 levels Instrument Feed Water Contaminant Parameter (units) CLRW Ions Resistivity (MΩ-cm) > 10.0 Organics TOC (ppb) < 500 Bacteria Bacteria (cfu/ml) <10 Particles include 0.22 micron filter Confirm use of CLRW quality with manufacturer Water quality must meet instrument manufacturers specifications Also defined: Commercially bottled purified water, autoclave and wash water and water supplied by a method manufacturer (use as diluent or reagent) *CLSI: Clinical and Laboratory Standards Institute (previously NCCLS)

13 US and European Pharmacopoeia Pure Water Purified and Highly Purified Water* USP Purified EU Purified EU Highly Purified Conductivity: <1.3 us/cm at 25 o C <4.3 us/cm at 20 o C <1.1 us/cm at 20 o C TOC: < 500 ppb < 500 ppb <500 ppb Bacteria: <100 cfu/ml <100 cfu/ml <10 cfu/100 ml Endotoxin: N/A N/A <0.25 EU/ml * Overview of USP28 and EP 4th edition, (refer to detailed specifications for exact norms).

14 Purification Technologies Overview of Key Technologies Advantages/Disadvantages Summary

15 Purification Technologies Filtration Depth and Screen Filters Activated Carbon and chlorine removal Mineral scale control Softening and Sequestering Distillation Reverse Osmosis Deionization Electrodeionization Ultraviolet light

16 Depth & Screen Filters Glass Fiber SEM Depth filters = matrix of randomly oriented fibers in a maze of flow channels. Durapore Membrane - SEM Screen filters = rigid, uniform continuous mesh of polymeric material with pore size precisely determined during manufacture. 2 types of filters: depth & screen (or membrane) filters. Depth filters : for RO protection from fouling (high particle capacity). Membrane filters : for retention of small amounts (quick clogging) of small particulates like bacteria. Additional treatment: Depth filters : for heavily loaded feed water with particles (SDI over specification). Screen filters : for a final low pore size filtration downstream the system. Charge filters : for pyrogen removal, in-line distribution loop

17 Purification Technologies Filtration Summary Depth Filters Random Structure Nominal retention rating Works by entrapment within depths of filter media High dirt holding capacity Screen/Membrane Filters Uniform Structure Absolute retention rating Works largely by surface sieving Low dirt holding capacity

18 Activated Carbon Granules or beads of carbon activated to create a highly porous structure with very high surface area Activation can be heat or chemical Pore sizes typically <100 to 2000 Å Surface area typically 500 to >2000 m2/gram Removal of organics by adsorption Removal of chlorine by adsorptionreduction

19 Mineral Scale Control Calcium and carbonate ions are common in tap water supplies Scale forms when concentration exceeds solubility limits and CaCO3 precipitates as a solid Higher concentrations increase risk of scale formation Higher ph and higher temperature increase risk of scale formation Important in domestic water systems and purification technologies Ca ++ + CO = 3 CaCO (S) 3 CO = 3 Ca ++ Calcium carbonate scale CO = 3 CO = 3 CO = 3

20 Scale Control Ion-exchange Softening "Hard water" Ca Cl - Cation Exchange Resin Mg Cl - R Na Na R R Na Na R R R Ca Mg R R 4 Na Cl - "Soft water"

21 Scale Control Ion-exchange Softener Regeneration Regenerated resin R Na Na R R Na Na R Na + Cl - Mg CL - Ca Cl - EXCESS Na + Cl - R Ca R R Mg R Exhausted resin conc. NaCl Softeners are regenerated using a concentrated brine flush

22 Scale Control Chemical Sequestering Chemical sequestering weakly binds calcium ion preventing calcium and carbonate ions from forming scale Liquid and solid chemical options available Solid polyphosphate shown as example illustration Ca ++ + CO = 3 δ _ CaCO (S) 3 CO = 3 CO = 3 Ca ++ CO = 3 δ _ CO = 3 Polyphosphate chain

23 Double Distillation Principal Recondense by cooling vapor Cooling water jacket Benefits Removes wide class of contaminants Bacteria / pyrogen-free Low capital cost Limitations High maintenance High operating cost Heat to vapor Low resistivity Organic carryover Low product flow High waste water flow Water storage

24 Natural Osmosis Pure water will pass though the membrane trying to dilute the contaminants Osmotic Pressure Water Plus Contaminants Pure Water ~100 ppm NaCl = 1 psi of osmotic pressure Semi-Permeable Reverse Osmosis Membrane

25 Reverse Osmosis Pressure applied in the reverse direction exceeding the osmotic pressure will force pure water through the membrane A reject line is added to rinse contaminants to drain Pressure Water Plus Contaminants Pure Water Reject Semi-Permeable Reverse Osmosis Membrane

26 Reverse Osmosis Summary Benefits All types of contaminants removed: ions, organics - pyrogens, viruses, bacteria, particulates & colloids. Low operating costs due to low energy needs. Minimum maintenance (no strong acid or bases cleaning) Good control of operating parameters. Ideal protection for ion-exchange resin polisher: a large ionic part already removed ( resin lifetime), particulates, organics, colloids also eliminated (no fouling). Limitations Not enough contaminants removed for Type II water. RO membrane sensitivity to plugging (particulates), fouling (organic,colloids), piercing (particle, chemical attack) and scaling (CaCO 3 ) in the long run if not properly protected. Need of right pressure (5 bars) & right ph for proper ion rejection. Flow fluctuation with pressure and temperature. Membrane sensitivity to back pressure Preservative rinsing needed Need optimized reject

27 Ion Exchange Cation Exchange Resin R -SO - 3 H+ + Na + R -SO - 3 Na+ + H + IX resin (+) Ion (-) H 2 O Particulate Colloid (-) Organics R -NH 4 OH - + Cl - R -NH 4 Cl - + OH - Fines (-) Anion Exchange Resin Benefits Effective at removing ions Resistivity 1-10 MΩ.cm with a single pass through the resin bed. Resistivity 18 MΩ.cm with proper pretreatment Easy to use: Simply open the tap and get water Low capital cost Limitations Limited or no removal of particles, colloids, organics or microorganisms Capacity related to flow rate and water ionic content Regeneration needed using strong acid and base Prone to organic fouling Multiple regenerations can result in resin breakdown and water contamination Risk of organic contamination from previous uses

28 Electrodeionization (EDI, CDI, ELIX, CIX) Waste + H + H + RO Feed Water Ion Exchange Resin A C A C Na + Cl - Cl - Cl- Na + Cl - Na + Cl - OH - Na + OH - Na + - Conductive Carbon Beads Product Continuous deionization technique where mixed bed ion-exchange resins, ion-exchange membranes and a small DC electric current continuously remove ions from water (commercialize by Millipore in mid 80 s) Performance enhancements: Ion-exchange added to waste channels improve ion transfer and removal. Conductive beads aded to cathode electrode channel reduces risk of scale and use of a softener Cations driven toward negative electrode by DC current Anions driven toward positive electrode by DC current Alternating anion permeable and cation permeable membranes effectively separate ions from water RO feed water: Avoids plugging, fouling and scaling of the EDI module

29 Electrodeionization Benefit Very efficient removal of ions and small MW charged organic (Resitivity > 5 MΩ-cm) Low energy consumption Typical <100 watt light bulb High water recovery No chemical regeneration Low operating cost Low maintenance No particulates or organic contamination (smooth, continuous regeneration by weak electric current) Limitations Good feed water quality required to prevent plugging and fouling of ion-exchange and scaling at cathode electrode RO feed water ideal New enhancements minimize risk of scale. Weakly charged ions more difficult to remove Dissolve CO 2 and silica Moderate capital investment

30 UV Lamps (254 and 185 nm) Relative Bactericidal Effect 100% 80% 60% 40% 20% 0% nm UV Light Wavelenght (nm) 2 O O * 3 O 2 UV (185 ) 2 O 3 UV (254) UV (254) 4 OH * 2 O H 2 O H 2 O CH 3 OH + 2 OH * HCHO + 2 H 2 O HCOOH + 2 OH * H 2 O 2 OH * CO H 2 O The UV rays between 200 and 300 nm destroy the micro-organisms by breaking the DNA chains. The optimal wavelength for DNA damage is 260 nm. 254 nm radiation is quite close to the optimum germicidal action efficiency (about 80%) and can therefore be successfully used to destroy bacteria. 254 UV does not oxidize organics UV energy catalyzes production of hydroxyl radicals (OH*). These hydroxyl radicals generate reactions which oxidize organic compounds. As the oxidation of organics progresses, reaction products become more polar (charged). These charged species are removed by a special ion exchange polishing cartridge

31 UV Technology ( nm) Benefit Conversion of traces of organic contaminants to charged species and ultimately CO 2 ( ) Limited destruction of microorganisms and viruses (254) Limited energy use Easy to operate Limitations Polishing technique only: may be overwhelmed if organic concentration in feed water is too high. Organics are converted, not removed. Limited effect on other contaminants. Good design required for optimum performance.

32 Contaminant Removal Efficiency Distillation Inorganics Organics Bacteria Particulates Reverse Osmosis Ultrapure Ion Exchange Electrodeionization Ultraviolet light Carbon Ultrafiltration Microporous Filtration 2311BD10

33 Water Purification System Design Multi-Step Purification Process RO systems RO + EDI systems Both Progard Pack Pretreatment pack RO cartridge protection Reverse Osmosis Remove up to 99% of feed water contaminants Elix Technology Electrodeionization Consistent production of high resistivity and low TOC water UV Lamp Production of water with low levels of Bacteria Product Water Tap water Type III Type II Low Bacteria

34 Water Purification System Overview of Design Considerations

35 Major phases in a project Definition of the needs Design of a total solution Budget estimation Tender (Bid) process Delivery of the units, accessories and consumables Installation Users training/commissioning Additional phases Preventive maintenance Full support for validation

36 Major phases in a project Definition of the needs Design of a total solution Budget estimation Tender (Bid) process Delivery of the units, accessories and consumables Installation Users training/commissioning Additional phases Preventive maintenance Full support for validation

37 Design Process Key Steps Dishwasher Direct Feed 1 Define the pure water requirements and specifications Ultrapure Polishing for HPLC General Glassware Rinsing 2 Design the distribution loop pump UV monitoring sterile filtration 3 4 Design the makeup system and storage tank Tap Water Review and Finalize specifications and design Pure Water Storage

38 Design Process: Step 1 1 Defining the pure water requirements and specifications What purity level? How much water? When is it needed? Where is it needed? Ultrapure Polishing for HPLC Dishwasher Direct Feed General Glassware Rinsing

39 1 Defining the pure water requirements and specifications What purity level? What labs and locations need purified water? What kind of work will be carried out in each lab, at each location? General rinsing/washing to sensitive trace analysis,? Are there instruments that will need pure water? Glassware washers, steam sterilizers, autoclaves..? Are there any maximum purity level requirements? What water quality is needed for each location? Ionic, Organic, and Microbiological Quality? Are there alert and action levels? Are there standard specifications to follow? How much water? When? Where? Ultrapure Polishing for HPLC Dishwasher Direct Feed General Glassware Rinsing

40 Definition of the needs Questions to select the right configuration and design 1 What purity level? How much water? When? Where? How much water is needed each day? In each lab, at each location,..? By the individual users, instruments, ultrapure polishing systems? How is the demand distributed during the day? Steady demand over the course of a day? Peak demands at certain times of the day? How many floors need water? Where is each location? Are there remote locations that need water? What are the distances between each location? Ultrapure Polishing for HPLC Dishwasher Direct Feed General Glassware Rinsing

41 Defining the pure water requirements and specifications 1 What purity level? How much water? When? Where? Additional questions: Does the equipment need to be validated? At all locations? Who will do the maintenance? Is a service/maintenance contact required? Are the water quality requirements similar between locations? How many researchers/scientists will work in each lab? Where can the equipment be located (space)? Where can piping be run? Are there plans for future expansion? Ultrapure Polishing for HPLC Dishwasher Direct Feed General Glassware Rinsing

42 Step 2: Designing the Distribution Loop 2 Define the distribution piping Design Layout Materials, welding method, valve type, pipe diameter Design Considerations Define Loop Purification and Monitoring Equipment Determine distribution pump performance Flow rate and pressure

43 Distribution Loop Layout Options: Gravity Feed 2

44 Distribution Loop Layout Options: Single Loop and make-up system Central Location 2

45 Distribution Loop Layout Options: Single Loop and Duplex-central make-up system 2

46 Distribution Loop Layout Options: Multiple Loop and make-up systems 2

47 Distribution Loop Layout Options: Multiple Loop and make-up systems and POU systems 2 Satellite Units

48 Design Considerations; Avoid Dead legs 2 6D rule CFR212 regulations of 1976 Good Engineering practice requires minimizing the length of dead legs and there are many good instrument and valve designs available to do so. 6D rule Ø0.59 Maximum dead leg = 6 times the pipe diameter Ø0.59 X 6 = 3.5 Maximum dead length of 3.5 inches Maximum length 6X pipe diameter (our example max is 3.5 inches)

49 Design Considerations; Avoid Dead legs 2 2D rule ASME Bioprocessing Equipment Guide of 1997 Good Engineering practice requires minimizing the length of dead legs and there are many good instrument and valve designs available to do so. 2D rule Ø0.59 Maximum dead leg = 2 times the pipe diameter Example: Ø0.59 X 2 = 1.2 Maximum dead length of 1.2 inches

50 Design Considerations; Flow Velocity 2 Design system for 3 to 5 f/s (~1 to 1.5 m/s) to: Maintain turbulent flow Minimize biofilm on internal walls Balance between velocity and pressure drop Higher velocity results in too high a pressure drop Requiring a larger pump and risk of increased water temperature

51 Design Considerations; Flow Velocity 2 Velocity through distribution pipe: 3 to 5 ft/sec design target, (~1 to 1.5 m/s) nominal OD OD ID Flow rates (GPM) at velocity: size mm inch inch 3 f/s 4 f/s 5 f/s 1/2" 20 mm /4" 25 mm " 32 mm /4" 40 mm /2" 50 mm Ashai Pro Line PP pipe

52 Define Loop Purification and Monitoring Equipment 2 Loop purification equipment to maintain water quality UV lamp»bacteria control»toc Reduction Filtration»Membranes for Bacteria and particle control»ultra-filtration for Pyrogen removal Deionization Ion removal Loop Water Purity Monitoring Resistivity TOC Bacteria Temperature Sanitant Monitors (Ozone)

53 Loop Monitoring 2 Sanitary Sampling Valve TOC Resistivity

54 Loop Bacteria Sampling 2 Sanitary Sampling Valve Designed for sanitary sampling (bacteria and endotoxin) Mid-stream sampling Zero-Dead leg when closed Sanitize easily in place Direct attachment to samplers

55 Determine the Distribution Pump Requirements 2 Pump selection is based on flow rate and pressure requirements Flow rate required defined in step 1 Pressure requirement Total Pressure requirement can be estimated by adding: piping pressure loss + loop equipment pressure loss + pressure due to elevation changes + pressure required at furthest point of use (25 psi typical) Select a pump that delivers the required flow rate and pressure Reduce pressure loss by increasing pipe diameter, (keeping balance with flow required and target velocity) For added reliability a duplex pumping system can be used

56 Distribution Systems Water Flow Dynamics; Pressure drop 2 Pressure drop through pipe: the resistance to water flow moving through a pipe (friction losses occurring along pipe walls and through fittings and valves) Key factors influencing pressure drop Pipe material, (surface roughness) Pipe diameter Pipe length Flow rate Determining pressure drop through pipe: Hazen-Williams formula for predicting pressure drop, (turbulent flow) Simplified: Hp = (L) x (Q) 1.85 /(d) 4.86 Hp= pressure drop in psi L = pipe length in feet Q = flow in GPM d = pipe inside diameter (friction factor included for smooth surfaces)

57 Distribution Systems Water Flow Dynamics; Pressure drop Determining pressure drop through fittings: Fittings; (elbows, tees, unions, etc..) Flow through fittings creates turbulence and adds to pressure drop Equivalent pipe length method most common Express each fitting as a length of pipe 2 1 foot Example: 2 ft + 1 ft + (1) 90 o elbow 90 o elbow = 2 equivalent feet of pipe eq-ft = 5 feet total length 2 feet 90 o elbow

58 Distribution Systems Water Flow Dynamics; Pressure drop 2 Determining pressure drop through additional loop equipment Refer to manufacturers specifications UV lamps: Typically 2 to 3 psi Filters and housings: Pressure loss data 20 inch Code-0 Durapore

59 Determine the Distribution Pump Requirements 2 Case Study Pressure drop and Pump Requirement Calculations Type in the yellow cells. Velocity and Pressure drop Table Piping Loop External diameter (in) 1 1/4 nominal pipe Diameter of PP pipe (Ashai-America) Ext Ø inch Nominal inside Ø Internal diameter (in) 1.28 PN thick. Flowrate in the loop (gal/min) 15 (see Flowrate Table) 1/ Total length of the loop (ft) / Fittings (eq. length in m of PVC tube) Qty Eq. 3/ Elbows Long Elbows / Elbows Flowrate Table Tees (straight) Instant. Q POU Qty Total Instant. Q Tees (90 ) gpm 1 15 gpm Ball valves in line 5 2 gpm 0 gpm Union fittings gpm 0 gpm Total eq. length (in ft of pipe) 452 gpm 0 pgm Total length of the pipe (pipe + fittings) (ft) 2452 gpm 0 gpm Sum of Total instant. Q 15 gpm Total Pressure Drop 47.5 psi 48 Simult. use factor 100% Velocity 3.8 f/s 3.8 Total flowrate in the loop 15 gpm Required Velocity : 4 ± 1 f/s Velocity OK Example worksheet tool Helps track and automatically calculate all key parameters Sizing and selection of correct pump is a key step in the design process Distribution Pump specs Table ( Pressure drop of loop and accessories ) Accessories Pump feed pressure Loop pressure drop UV Lamp 5 µm loop filter DI tanks Super-Q 0.22 loop filter other (to be specified) psi other (to be specified) Adjusted pressure on BPR 25.0 Highest elevation difference (ft) Total pressure drop in the Loop 85.5 from above details details Required distribution pump outlet Required distribution pump outlet 86 psi 15 gpm 198 feet 15 gpm

60 Determine the Distribution Pump Requirements 2 Pump performance curve 15 GPM and 180 feet of head (~78 psi) shown as an example Select the pump that meets the minimum requirements

61 Step 3 - Design the Makeup Purification System and Storage Tank 3 Select the make-up purification system to match the water quality required Size the makeup purification system to match the quantity required per day Size the storage tank to meet peak demands during the day Determine the pretreatment needed

62 Makeup System Sizing and Quality 3 Match to the quality requirement (defined in step 1) RO/EDI or RO/DI system for Type 2 pure water applications RO system for Type 3 more general applications Size the makeup system to match the quantity required per day (defined in step 1) Plans for future expansion? Are Duplex systems needed? Back-up for maintenance-down time. Option to add for future expansion

63 Sizing Makeup System and Tank 3 Sizing the makeup system is done in conjunction with the storage tank Sizing Examples: Company A needs water to clean vessels in the first two hours of the day shift. They need a total of 1200 Gallons in two hours Gallon Tank with 100 gph make-up rate Company B needs pure water to feed automated Filling machine. They need 200 gallons per hour for an 8 hour shift. 200 Gallon Tank with 200 gph make-up rate

64 Determine the pretreatment needed for the makeup water system 3 Determine feed flow rate base on the make-up system water recovery rate Feed Flow Rate = RO Product / RO recovery rate Complete feed water analysis conductivity, chlorine, fouling index, ph, hardness, alkalinity.. Select pretreatment options based on feed water analysis and manufacturers recommendations Multimedia Sand Particulate contamination Carbon Filters Chlorine and some organic removal Softeners Hard water (Mg ++ or Ca ++ contamination) Cartridge Filters Particulate and carbon options

65 Design Process Step 4 4 Step 4 - Finalize Design Prepare Process Flow Diagram (PFD), supporting documents and specifications Design Controls and Monitoring Review Validation requirements Review who will maintain the equipment Consider service/maintenance plans Review requirements, specifications, design, equipment and PFD with customer/client Update and Finalize design as needed

66 Outline Contaminants in Water Pure Water Applications and Quality Standards Water Purification Technologies Key Water Purification System Design Steps Systems Questions???

67 Water Purification System for a Laboratory Facility Thank You!! Millipore Corporation Bioscience Division Christopher Yarima Mike Kelly