Post on 22-Dec-2015
Water Purification System for a Laboratory Facility
Millipore CorporationBioscience DivisionChristopher Yarima
Mike Kelly
Outline
Contaminants in Water
Pure Water Applications and Quality Standards
Water Purification Technologies
Key Water Purification System Design Steps Systems
Questions
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
Contaminants in Potable Water
Inorganic Ions Cations
Na+
Ca+2
Anions
Cl-
HCO-3
Organics Natural
Tannic Acid
Humic Acid
Man Made
Pesticides
Herbicides
Particles
(Colloids)
Non Dissolved Solid Matter
(Small deformable solids with a net negative charge)
Microorganisms
(Endotoxin)
Bacteria , Algae , Microfungi
(Lipopolysaccharide fragment of Gram negative bacterial cell wall)
H H
H-C-C-OH
H H
Endotoxin units/ml-Rabbit Inoculation test-LAL Test
Endotoxin
cfu/mlColony count on 0.45 μm membrane.
Bacteria
Rate of pluggage of 0.45 μm membrane.
Silt Density Index / Fouling Index
Particles (Colloids)
ppb (μg/L) Total Oxidizable Carbon (T.O.C.)
Organics
μs/cmMΩ.cm
Conductivity (Resistivity)
Inorganic Ions
UnitMeasurementContaminant
Measurement of Contaminant level
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. !!!
Measurement Units
Standards and Common Terms
Ultrapure/Reagent GradeCritical Applications
Water for HPLC,GC, HPLC ,AA , ICP-MS, for buffers and culture media for mammalian cell
culture & IVF, reagents for molecular biology...
Pure/Analytical GradeStandard Applications
Buffers, pH solutions,culture media preparation ,clinical analysers and weatherometers feed.
Pure/Laboratory GradeGeneral Applications
Glassware rinsing, heating baths, humidifiers and autoclaves filling
Type 1
Type II
Type III
“Pure”
“Ultrapure”
Laboratory Water Purity SpecificationsConsolidated Guidelines
Contaminant Parameter (units) Type 1 Type 2 Type 3Ions Resistivity (M-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 < 1000Endotoxin (EU/ml) < 0.001 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
ASTM Standards for Laboratory Reagent Water
Contaminant Parameter (units) Type 1 Type 2 Type 3 Ions Resistivity (M-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) 10/1000 ml
10/100ml
100/10ml
Endotoxin (EU/ml) < 0.03 0.25 NA
ASTM: American Society for Testing and Materials
• 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 CO2 levels
• Instrument Feed Water• 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*, water quality specifications CLSI guidelines should be read to understand scope and detail for each requirement
Contaminant Parameter (units) CLRW
Ions Resistivity (M-cm) > 10.0 Organics TOC (ppb) < 500 Bacteria Bacteria (cfu/ml) <10 Particles include 0.22 micron filter
*CLSI: Clinical and Laboratory Standards Institute(previously NCCLS)
US and European Pharmacopoeia Pure Water
Purified and Highly Purified Water*
USP Purified EU Purified EU Highly Purified
Conductivity: <1.3 uS/cm at 25oC <4.3 uS/cm at 20oC <1.1 uS/cm at 20oC
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).
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
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
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 adsorption-reduction
Mineral Scale Control
COCO33==
CaCa++++
COCO33== COCO33
==
COCO33==
CaCa++++ + CO + CO33== CaCOCaCO33
(S)(S) Calcium carbonate scale
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++ + 2 Cl-
NaR Na R
NaR Na R
4 Na+ + 4 Cl-
Ca
R
R
R
R
"Hard water"
"Soft water"
Cation Exchange Resin
Mg
Mg++ + 2 Cl-
Scale Control – Ion-exchange Softening
Cl-NaR Na R
NaR Na R
Mg++ + 2 CL-
Ca++ + 2 Cl-
EXCESS Na+ Cl-
Na+
Ca
MgR
R
R
R
Softeners are regenerated using a concentrated “brine” flush
conc. NaCl
Regenerated resin
Exhausted resin
Scale ControlIon-exchange Softener Regeneration
COCO33==
CaCa++++
COCO33== COCO33
==
COCO33==
CaCa++++ + CO + CO33== CaCOCaCO33
(S)(S)_
_
Polyphosphate chain
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
Heat to vapor
Recondenseby cooling vapor Cooling water
jacket
Double Distillation Principal
Benefits
Removes wide class of contaminants
Bacteria / pyrogen-free
Low capital cost
Limitations
High maintenance
High operating cost
Low resistivity
Organic carryover
Low product flow
High waste water flow
Water storage
Pure Water
Semi-PermeableReverse Osmosis
Membrane
WaterPlus
Contaminants
Osmotic Pressure
Natural Osmosis
~100 ppm NaCl = 1 psi of osmotic pressure
• Pure water will pass though the membrane trying to dilute the contaminants
PureWater
Semi-PermeableReverse Osmosis
Membrane
WaterPlus
Contaminants
Reverse Osmosis
Pressure
Reject
• 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
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 (CaCO3) 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
Ion Exchange
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
IX resin (+)
Ion (-)
Particulate
Colloid (-)
Organics
Fines (-) R - NH4OH- + Cl- R - NH4 Cl- + OH-
R - SO-3 H+ + Na+ R - SO-
3 Na+ + H+
Cation Exchange Resin
Anion Exchange Resin
H2O
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
Electrodeionization (EDI, CDI, ELIX, CIX)
Conductive Carbon Beads
A C A C
Na+
Na+
Na+
Na+
H+
H+
OH-
OH-Cl--
Na++
Cl-
Cl-
Cl-
Cl-
-+
WasteProduct
RO Feed WaterIon Exchange Resin
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
ElectrodeionizationBenefit
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 CO2 and silica
Moderate capital investment
Inor
gani
csO
rgan
ics
Bacte
riaPar
ticul
ates
2311BD10
Contaminant Removal Efficiency
Distillation
Carbon
Microporous Filtration
Electrodeionization
Ultraviolet light
Reverse Osmosis
Ultrapure Ion Exchange
Ultrafiltration
Water Purification System DesignMulti-Step Purification Process
Reverse Osmosis
Remove up to 99% of feed
water contaminants
Progard PackPretreatment
pack RO cartridge
protection
Elix TechnologyElectrodeionization
Consistent production
of high resistivity and low TOC water
UV LampProduction of water with low
levels of Bacteria
RO systems
RO + EDI systemsBoth
Type III Type II Low Bacteria Tap water
ProductWater1 2 3 4
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
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
Define the pure water requirements and specifications
Design the distribution loop
Design the makeup system and storage tank
Review and Finalize specifications and design
Design ProcessKey Steps
DishwasherDirect Feed
UltrapurePolishingfor HPLC
GeneralGlassware
Rinsing
pump
UV
sterilefiltration
monitoring
TapWater
PureWater
Storage
1
2
3
4
Defining the pure water requirements and specifications
What purity level?
How much water?
When is it needed?
Where is it needed?
DishwasherDirect Feed
UltrapurePolishingfor HPLC
GeneralGlassware
Rinsing
Design Process: Step 11
DishwasherDirect Feed
UltrapurePolishingfor HPLC
GeneralGlassware
Rinsing
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?
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?
DishwasherDirect Feed
UltrapurePolishingfor HPLC
GeneralGlassware
Rinsing
Definition of the needsQuestions to select the right configuration and design
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?
DishwasherDirect Feed
UltrapurePolishingfor HPLC
GeneralGlassware
Rinsing
1Defining the pure water requirements and specifications
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
Step 2: Designing the Distribution Loop 2
“Satellite” Units
Distribution Loop Layout Options:Multiple Loop and make-up systems and POU systems
2
Design Considerations; Avoid Dead legs
“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”
Ø 0.59”
Maximum dead leg = 6 times the pipe diameter
Ø 0.59” X 6 = 3.5”
Maximum dead length of 3.5 inches
Maximum length 6X pipe diameter(our example max is 3.5 inches)
2
Design Considerations; Flow VelocityDesign Considerations; Flow Velocity
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
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
2
Define Loop Purification and Monitoring Equipment
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)
2
Loop Bacteria Sampling
Designed for sanitary sampling (bacteria and endotoxin)
Mid-stream sampling
Zero-Dead leg when closed
Sanitize easily in place
Direct attachment to samplers
Designed for sanitary sampling (bacteria and endotoxin)
Mid-stream sampling
Zero-Dead leg when closed
Sanitize easily in place
Direct attachment to samplers
Sanitary Sampling Valve
2
Determine the Distribution Pump Requirements 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
2
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
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
90o
elbow2 feet
1 foot
2
Example: 2 ft + 1 ft + (1) 90o elbow
90o elbow = 2 equivalent feet of pipe
2 + 1 + 2 eq-ft = 5 feet total length
Distribution SystemsDistribution SystemsWater Flow Dynamics; Pressure dropWater Flow Dynamics; Pressure drop
Distribution SystemsDistribution SystemsWater Flow Dynamics; Pressure dropWater Flow Dynamics; Pressure drop
Determining pressure drop through additional loop equipment Refer to manufacturers specifications UV lamps: Typically 2 to 3 psi Filters and housings:
Pressure loss data
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
2
Determine the Distribution Pump Requirements 2Type in the yellow cells.
External diameter (in) 1 1/4
Internal diameter (in) 1.28nominal
pipe PNExt Ø inch
thick.Nominal inside Ø
151/2 25 0.79 0.098 0.59
Total length of the loop (ft) 2000 1/2 25 0.79 0.098 0.59Fittings (eq. length in m of PVC tube) Qty Eq. 3/4 25 0.98 0.106 0.79
Elbows 90° 90 315 1 16 1.26 0.118 0.95Long Elbows 90° 0 0 1 1/4 16 1.57 0.146 1.28
Elbows 45° 0 0Tees (straight) 30 75 POU Qty
Tees (90°) 0 0 15 gpm 1Ball valves in line 5 2 gpm
Union fittings 15 60 gpmTotal eq. length (in ft of pipe) 452 gpm
Total length of the pipe (pipe + fittings) (ft) 2452 gpm
47.5 psi 483.8 f/s 3.8
psi0
47.53.00.000100
25.00 0.0
85.5
86 psi15 gpm
100%
0 pgm0 gpm15 gpm
Flowrate Table
Total Pressure Drop
Total Instant. Q15 gpm0 gpm
Flowrate in the loop (gal/min)(see Flowrate Table)
0 gpm
Instant. Q
Simult. use factor
details
from above
Accessories
Super-QDI tanks
5 µm loop filterUV Lamp
Case Study Pressure drop and Pump Requirement Calculations
Highest elevation difference (ft)
Required Velocity : 4 ± 1 f/s
Adjusted pressure on BPRother (to be specified) details
0.22 loop filterother (to be specified)
Loop pressure dropPump feed pressure
Velocity and Pressure drop Table Piping Loop
Distribution Pump specs Table( Pressure drop of loop and accessories )
Velocity OK
Diameter of PP pipe(Ashai-America)
Velocity Total flowrate in the loop 15 gpm
Sum of Total instant. Q
15 gpm198 feetRequired pressure @ distribution pump outlet
Required flowrate @ distribution pump outlet
Total pressure drop in the Loop
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
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
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
Pump performance curve
15 GPM and 180 feet of head (~78 psi) shown as an example
Select the pump that meets the minimum requirements
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
Step 3 - Design the Makeup Purification System and Storage Tank
3
Makeup System Sizing and Quality
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
3
Sizing Makeup System and Tank
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.
1500 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
3
Sizing the makeup system is done in conjunction with the storage tank
Sizing Examples:
Determine the pretreatment needed for the makeup water system
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
3
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
Design Process Step 4 4
Outline
Contaminants in Water
Pure Water Applications and Quality Standards
Water Purification Technologies
Key Water Purification System Design Steps Systems
Questions ???