Transcript Millipore Corporation Lab Water Division Jeff Denoncourt

Water Purification System for a
Laboratory Facility
Millipore Corporation
Bioscience Division
Christopher 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
Organics
HH
H-C-C-OH
Cations
Anions
Na+
Cl-
Ca+2
HCO-3
Natural
Man Made
Tannic Acid
Pesticides
Humic Acid
Herbicides
HH
Particles
Non Dissolved Solid Matter
(Colloids)
(Small deformable solids with a net negative
charge)
Microorganisms
Bacteria , Algae , Microfungi
(Endotoxin)
(Lipopolysaccharide fragment of Gram
negative bacterial cell wall)
Measurement of Contaminant level
Contaminant Measurement Unit
Inorganic Ions
Conductivity
(Resistivity)
μs/cm
MΩ.cm
Organics
Total Oxidizable
Carbon (T.O.C.)
ppb (μg/L)
Particles (Colloids)
Silt Density Index /
Fouling Index
Rate of pluggage of
0.45 μm
membrane.
Bacteria
Colony count on 0.45 cfu/ml
μm membrane.
Endotoxin
-Rabbit Inoculation
test
-LAL Test
Endotoxin units/ml
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. !!!
Water Standards
Standards and Common Terms
Ultrapure/Reagent Grade
Critical Applications
“Ultrapure”
Type 1
Water for HPLC,GC, HPLC ,AA , ICP-MS, for
buffers and culture media for mammalian cell
culture & IVF, reagents for molecular biology...
Pure/Analytical Grade
Standard Applications
“Pure”
Type II
Buffers, pH solutions,culture media
preparation ,clinical analysers and
weatherometers feed.
Pure/Laboratory Grade
General Applications
Type III
Glassware rinsing, heating baths,
humidifiers and autoclaves filling
Laboratory Water Purity Specifications
Consolidated Guidelines
Contaminant Parameter (units)
Resistivity (M-cm)
Ions
Organics
Particles
Bacteria
Type 1 Type 2 Type 3
> 18.0
> 1.0
> 0.05
< 10
< 20
<1
< 100
< 50
NA
< 1000
< 200
NA
<1
< 0.001
< 100
NA
< 1000
NA
Silica (ppb)
TOC (ppb)
particles > 0.2 um (#/ml)
Bacteria (cfu/ml)
Endotoxin (EU/ml)
• 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)
Resistivity (M-cm)
Ions
Organics
Particles
Bacteria
Silica (ppb)
TOC (ppb)
particles > 0.2 um (#/ml)
Bacteria (cfu/ml)
Endotoxin (EU/ml)
Type 1 Type 2 Type 3
> 18.0
> 1.0
> 4.0
<3
< 100
<1
<3
< 50
NA
< 500
< 200
NA
10/1000
ml
< 0.03
10/100
ml
0.25
100/10
ml
NA
ASTM: American Society for Testing and Materials
CLSI*, water quality specifications
CLSI guidelines should be read to understand scope and detail for each requirement
• CLRW; Clinical Laboratory Reagent Water
Contaminant
Parameter (units)
CLRW
Ions
Organics
Bacteria
Particles
> 10.0
Resistivity (M-cm)
TOC (ppb)
< 500
Bacteria (cfu/ml)
<10
include 0.22 micron filter
• 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: Clinical and Laboratory Standards Institute
(previously NCCLS)
US and European Pharmacopoeia Pure Water
Purified and Highly Purified Water*
Conductivity:
USP Purified
EU Purified
EU Highly Purified
<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
N/A
N/A
<0.25 EU/ml
Endotoxin:
* Overview of USP28 and EP 4th edition, (refer to detailed specifications for exact norms).
Purification Technologies
Overview of Key Technologies
Advantages/Disadvantages
Summary
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 adsorptionreduction
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++ + CO3=
CaCO3(S)
Calcium carbonate scale
CO3=
CO3=
Ca++
CO3=
CO3=
Scale Control – Ion-exchange Softening
"Hard water"
Cation
Exchange Resin
Ca++ + 2 ClMg++ + 2 ClR
Na Na
R
R
Na Na
R
R
Ca
R
R
Mg
R
4 Na+ + 4 Cl"Soft water"
Scale Control
Ion-exchange Softener Regeneration
Regenerated resin
Mg++ + 2 CLCa++ + 2 ClEXCESS Na+ Cl-
R
Na Na
R
R
Na Na
R
R
Ca
R
R
Mg
R
Na+
Cl-
conc. NaCl
Exhausted resin
Softeners are regenerated using a concentrated “brine” flush
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++ + CO3=

_
CaCO3 (S)
CO3=
CO3=
Ca++
CO3=

_
CO3=
Polyphosphate chain
Double Distillation Principal
Benefits
Recondense
by cooling vapor
Cooling water
jacket

Removes wide class of
contaminants

Bacteria / pyrogen-free

Low capital cost
Limitations
Heat to
vapor

High maintenance

High operating cost

Low resistivity

Organic carryover

Low product flow

High waste water flow

Water storage
Natural Osmosis
• Pure water will pass though the membrane trying to dilute the contaminants
Osmotic
Pressure
Water
Plus
Contaminants
~100 ppm NaCl
= 1 psi of osmotic pressure
Pure
Water
Semi-Permeable
Reverse Osmosis
Membrane
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
Reject
Pure
Water
Semi-Permeable
Reverse Osmosis
Membrane
Reverse Osmosis Summary
Limitations
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).

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
Cation Exchange Resin
R - SO-3 H+ + Na+
R - SO-3 Na+ + H+
IX resin (+)
Ion (-)
Particulate
H2O
Colloid (-)
Organics
R - NH4OH- + Cl-
R - NH4 Cl- + OH-
Fines (-)
Anion Exchange Resin
Benefits

Effective at removing ions

Easy to use: Simply open the tap and get water
Low capital cost




 Resistivity 1-10 MΩ.cm with a single pass
through the resin bed.
 Resistivity 18 MΩ.cm with proper pretreatment


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)
RO Feed Water
Ion Exchange Resin
+
A
C
A
Na+
-
C
Cl-
OHNa+
H+ Cl-
Waste




Na+ Cl-
(commercialize by Millipore in mid 80’s)
Conductive
Carbon
Beads
Performance enhancements:
Cl-- Na+
H+ Cl-
Continuous deionization technique
where mixed bed ion-exchange
resins, ion-exchange membranes and
a small DC electric current
continuously remove ions from water
OHNa+
Product
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
Electrodeionization
Benefit

Very efficient removal of ions
and small MW charged organic
(Resitivity > 5 MΩ-cm)

Low energy consumption

Limitations

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)

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
Contaminant Removal Efficiency
Distillation
Reverse Osmosis
Ultrapure Ion Exchange
Electrodeionization
Ultraviolet light
Carbon
Ultrafiltration
Microporous Filtration
2311BD10
Water Purification System Design
Multi-Step Purification Process
RO systems
RO + EDI systems
Progard Pack
Pretreatment
pack
RO cartridge
protection
1
Tap water
Reverse
Osmosis
Remove up to
99% of feed
water
contaminants
Both
Elix Technology
UV Lamp
Electrodeionization
Consistent
production
of high resistivity
and low TOC water
Production of
water with low
levels of
Bacteria
2
3
Type III
Type II
4
Low Bacteria
Product
Water
Water Purification System
Overview 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
Design Process
Key Steps
Dishwasher
Direct Feed
1
Define the pure water requirements and
specifications
Ultrapure
Polishing
for HPLC
monitoring
2
Design the distribution loop
3
Design the makeup system and storage tank
UV
pump
sterile
filtration
Tap
Water
4
General
Glassware
Rinsing
Review and Finalize specifications and design
Pure
Water
Storage
1
Design Process: Step 1

Defining the pure water requirements and
specifications


Dishwasher
Direct Feed
What purity level?
How much water?

When is it needed?

Where is it needed?
Ultrapure
Polishing
for HPLC
General
Glassware
Rinsing
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?


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?




General rinsing/washing to sensitive trace analysis,…?
Ionic, Organic, and Microbiological Quality?
Are there alert and action levels?
Are there standard specifications to follow?
How much water? When? Where?
Dishwasher
Direct Feed
Ultrapure
Polishing
for HPLC
General
Glassware
Rinsing
1
Definition of the needs
Questions to select the right configuration and design


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?
Dishwasher
Direct Feed
Ultrapure
Polishing
for HPLC
General
Glassware
Rinsing
Defining the pure water requirements and specifications



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?
Dishwasher
Direct Feed
Ultrapure
Polishing
for HPLC
General
Glassware
Rinsing
1
Step 2: Designing the Distribution Loop

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
2
Distribution Loop Layout Options:
Gravity Feed
2
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
Distribution Loop Layout Options:
Multiple Loop and make-up systems and POU systems
“Satellite” Units
2
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”
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)
Design 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
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

2
Loop Water Purity Monitoring
–
–
–
–
–
Resistivity
TOC
Bacteria
Temperature
Sanitant Monitors (Ozone)
2
Loop Monitoring
Sanitary Sampling Valve
TOC
Resistivity
Loop Bacteria Sampling
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
2
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
2
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
1 foot
Example:
2 ft + 1 ft + (1) 90o elbow
90o elbow = 2 equivalent feet of pipe
2 + 1 + 2 eq-ft = 5 feet total length
2 feet
90o
elbow
Distribution Systems
Water 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
20 inch Code-0 Durapore
2
Determine the Distribution Pump Requirements
2
Case Study Pressure drop and Pump Requirement Calculations
Velocity and Pressure drop Table Piping Loop
Type in the yellow cells.
External diameter (in)
1 1/4
Internal diameter (in)
Flowrate in the loop (gal/min)
(see Flowrate Table)
Total length of the loop (ft)
Fittings (eq. length in m of PVC tube)
Qty
Elbows 90°
90
Long Elbows 90°
0
Elbows 45°
0
Tees (straight)
30
Tees (90°)
0
Ball valves in line
5
Union fittings
15
Total eq. length (in ft of pipe)
Total length of the pipe (pipe + fittings) (ft)
1.28
Total Pressure Drop
Velocity
Required Velocity : 4 ± 1 f/s
nominal
pipe
15
1/2
1/2
3/4
1
1 1/4
0.79
0.098
0.59
0.79
0.098
0.59
0.98
0.106
0.79
1.26
0.118
0.95
1.57
0.146
1.28
Flowrate Table
Instant. Q POU Qty Total Instant. Q
15
gpm
1
15 gpm
gpm
0 gpm
gpm
0 gpm
gpm
0 pgm
gpm
0 gpm
Sum of Total instant. Q
15 gpm
47.5 psi
48
Simult. use factor
100%
3.8 f/s
3.8
Total flowrate in the loop 15 gpm
Velocity OK
2000
Eq.
315
0
0
75
0
2
60
452
2452
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)
other (to be specified)
Adjusted pressure on BPR
Highest elevation difference (ft)
0
Total pressure drop in the Loop
Required pressure @ distribution pump outlet
Required flowrate @ distribution pump outlet
Diameter of PP pipe
(Ashai-America)
Nominal
Ext Ø
PN
thick.
inch
inside Ø
psi
0
47.5
3.0
0.0
0
0
10
0
from above
details
details
25.0
0.0
85.5
86 psi
15 gpm
198 feet
15 gpm
25
25
25
16
16
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
Step 3 - Design the Makeup Purification
System and Storage Tank

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
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
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.


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
Determine the pretreatment needed for
the makeup water system

Determine feed flow rate base on the make-up system water
recovery rate


Complete feed water analysis


Feed Flow Rate = RO Product / RO recovery rate
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
Design Process Step 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

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 Corporation
Bioscience Division
Christopher Yarima
Mike Kelly