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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

Water Chemistry – Contaminants

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

Water Standards

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

Overview of Key Technologies

Advantages/Disadvantages

Summary


Filtration – Depth and Screen Filters

Activated Carbon and chlorine removal

Mineral scale control – Softening and Sequestering

Distillation

Reverse Osmosis

Deionization

Electrodeionization

Ultraviolet light


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

Water Purification SystemOverview of Design Considerations

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?



GeneralGlassware

Rinsing

Design Process: Step 11



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?



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?



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

2Distribution Loop Layout Options:Gravity Feed

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

2

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

2

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

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 Monitoring

TOC

Resistivity

2

Sanitary Sampling Valve

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 ???

Water Purification System for a Laboratory Facility

Thank You!! Millipore CorporationBioscience DivisionChristopher Yarima

Mike Kelly