Design and Construction of USP
Purified Water Systems
William V. Collentro
Feed Water Analysis
USP Purified Water System –
Feed Water Analysis
• Official Monograph
– United States EPA NPDWR
– Equivalent European Regulations
– Equivalent Japanese Regulations
– World Health Organization Reference
USP Purified Water System –
Feed Water Analysis
• United States EPA – National Primary
Drinking Water Regulations (NPDWR)
–Regulated Items
–Total Viable Bacteria
–“Private” Water Supplies
USP Purified Water System –
Feed Water Analysis
• Regulated Items - Microorganisms
– Cryptosporidium
– Giardia lamblia
– Legionella
– Total Coliform
– Turbidity
– Viruses
USP Purified Water System –
Feed Water Analysis
• Regulated Items – Disinfection Byproducts
–Bromate
–Chlorite
–Haloacetic Acids (HAA5)
–Total Trihalomethanes (TTHMs)
USP Purified Water System –
Feed Water Analysis
• Regulated Items – Disinfectants
–Chlorine
–Chloramines
–Chlorine Dioxide
USP Purified Water System –
Feed Water Analysis
• Regulated Items – Inorganic Chemicals
–
–
–
–
–
–
–
–
Antimony
Arsenic
Asbestos
Barium
Beryllium
Cadmium
Total Chromium
Copper
USP Purified Water System –
Feed Water Analysis
• Regulated Items – Inorganic Chemicals
–
–
–
–
–
–
–
–
Cyanide
Fluoride
Lead
Mercury
Nitrate
Nitrite
Selenium
Thallium
USP Purified Water System –
Feed Water Analysis
• Regulated Items – Organic Chemicals (53
Total)
–
–
–
–
–
–
–
Sewage/Wastewater Treatment
Herbicides
Landfill Leachates
Chemical/Industrial Facility Waste
Fumigants
Petroleum /Refinery Waste
Insecticides
USP Purified Water System –
Feed Water Analysis
• Regulated Item – Radionuclides
– Alpha Particles
– Beta Particles and Photon Emitters
– Radium 226
– Uranium
USP Purified Water System –
Feed Water Analysis
• Total Viable Bacteria
– No limit in NPDWR
– Total Coliform (Confirmed as Fecal Coliform or E.
coli, used as indicator)
– “Action Limit” of 500 cfu/ml in non enforceable
General Information Section of USP
– TVB may only indicate a fraction of viable
organisms present
USP Purified Water System –
Feed Water Analysis
• Regulated Items - Testing
– Municipality?
– Pharmaceutical Facility?
– Compliance?
– Obligation?
– Consequences?
Periodic Monitoring
USP Purified Water System –
Periodic Monitoring
• General Monitoring – Storage and Distribution
System
• Point-of-Use TVB
• Online Conductivity
• Online TOC
USP Purified Water System –
Periodic Monitoring
• General Monitoring – Water Purification
System
• Final TVB
• Inline RO Feed Water and Product Water
Conductivity plus % Rejection of Ions
• Inline Post RO Polishing Conductivity
USP Purified Water System –
Periodic Monitoring
• Frequent Monitoring – Water Purification
System
• Silt Density Index (Test Kit)
• Total Hardness (Test Kit)
• Chlorine (Test Kit)
USP Purified Water System –
Periodic Monitoring
• Less Frequent Monitoring – Water Purification
System
• Inline ORP for Reducing Agent Injection
Monitoring
• Inline Total Hardness Monitor
• Inline Chlorine Monitor
USP Purified Water System –
Pretreatment Periodic Monitoring
Raw Water
Post
Multimedia
Post Activated
Carbon
Post UV
Post Lead
Water
Softener
Post Polish
Water
Softener
Post Cartridge
Filter
NPDWR Tests
X
-
-
-
-
-
-
TVB
X
X
X
X
X
X
X
BET
X
-
X
-
-
-
X
Chlorine
X
X
X
-
-
-
-
TOC
X
X
X
-
-
-
-
TSS
X
X
X
-
X
X
-
Total Hardness
X
-
X
-
X
X
-
Total Iron
X
X
X
-
X
X
-
Turbidity
X
X
-
-
-
-
-
SDI
-
-
-
-
-
-
X
USP Purified Water System –
RO/Polishing Periodic Monitoring
Post RO Break
Tank
Post RO
Post CEDI
Post UV
Post Final
Filter
TVB
X
X
X
X
X
BET
X
X
-
-
-
pH
X
X
-
-
-
TOC
X
X
X
X
X
Carbon
Dioxide
X
X
-
-
-
USP Purified Water System –
Periodic Monitoring
• Summary
• Monitoring of Pretreatment and Ion Removal
steps identifies a problem before it effects pointof-use values.
• Frequency of the monitoring program established
for each application
• Regulatory concerns
Sanitization Provisions
USP Purified Water System –
Sanitization Provisions
• Frequency
– Determined by microbial monitoring
– Must include storage, distribution, ion removal,
and pretreatment
– Employs chemical and thermal methods
– Ineffectiveness of Steam
– Biofilm requires chemical sanitizing agent
USP Purified Water System –
Sanitization Provisions
• Fundamentals
– TVB destruction a function of concentration and
time for chemical sanitization
– TVB destruction a function of temperature and
time for hot water with 65°C lowest temperature
– Dead Leg for thermal sanitization
– Dead leg for chemical sanitization
USP Purified Water System –
Sanitization Provisions
• Fundamentals
– Removal of Biofilm
– Activated Carbon Issues
– RO Waste Recirculation Issues
– Pretreatment and Ion removal Recirculation Issues
– Hot water sanitizable ion removal systems
– Pretreatment must be included
USP Purified Water System –
Sanitization Provisions
• Execution - Pretreatment
– Hot Water Sanitizable Activated Carbon
– Chemical Sanitization with 1% solution of
Hydrogen Peroxide and Peracidic Acid (except
activated carbon unit)
– Replace activated carbon media every 6-12
months
– Dynamic-Stagnant-Dynamic Procedure
USP Purified Water System –
Sanitization Provisions
• Execution – Ion Removal
– Continuous operation (make-up and recirculation)
– Hot Water Sanitization Provisions (entire system)
– RO membrane rotation every 6 months
– Chemical Sanitization with 1% solution of
Hydrogen Peroxide and Peracidic Acid annually
– Dynamic-Stagnant-Dynamic Procedure
USP Purified Water System –
Sanitization Provisions
• Execution – Storage & Distribution
– Ozonation
– Periodic Hot Water
– Membrane Filtration discouraged
– Chemical Sanitization with 1% solution of
Hydrogen Peroxide and Peracidic Acid annually
– Dynamic-Stagnant-Dynamic Procedure
Validation Criteria
Validation Criteria
• Commissioning Documentation
– Reference in IQ and OQ
– “Credit” for inspection and testing
– Factory Acceptance Test (FAT) Documentation
– Turnover Packages (TOP)
– Coordination
– Interface
Validation Criteria
• IQ Format
– Unit operation based with all support
documentation for components and accessories
verified. Support documents in document or as
an appendix/attachment. Provides understanding
of component by individuals preparing, reviewing,
and executing IQ
– Component based program for items such as
valves, gauges, pumps, etc. Poor tool for
individuals to understand the system.
Validation Criteria
• IQ Information
– Limits on material? The more information
available, the better. If a accessory breaks, it must
be replaced. The model number, serial number,
and/or manufacturer may change or no longer
exists. “Cut sheets” of accessories provide an
excellent vehicle for identifying a “like-for-like”
replacement which significantly reduces the
“Change Control” effort.
Validation Criteria
• IQ Information
– All support information should reference the
original manufacturer’s part number. Project
specifications should clearly state that the name
of the manufacturer as well as the part number be
provided. The vast majority of this information is
“coded” to the water purification equipment
manufacturer’s model number, useless for
replacement on a “like-for-like” basis.
Validation Criteria
• OQ Information
– Prepared and executed in an integrated basis.
Individual Unit Operation will impact the
operation of other components.
– Execution must provide exact operating condition.
As an example, if media is not installed in a
pretreatment component during execution of a
FAT, execution (partial) may be required after
installation and start-up.
Validation Criteria
• OQ Information – Considerations
– Fixed alarm and operating set points versus
adjustable set points
– Processor access levels
– Alarm set points and time delays
– Control set points and time delays
– View screen navigation
– “ALERM” banner display
– “OPERATOR OVERRIDE” banner display
Validation Criteria
• PQ Criteria
– Post start-up and commissioning
– 30 day sample period
– Sampling plan to duplicate water use
• “Working days”
• Attempt to duplicate water demand
• Attempt to duplicate actual conditions at individual
points-of-use
Validation Criteria
• PQ Criteria
– Every point-of-use every day if practical
– TOC “grab” samples from each points-of-use
– Conductivity “grab” samples from points-of-use
– Suggest transition for about 30-60 days after
successful execution
– Continues for one year period
– Monitoring never stops
Validation Criteria
• PQ Microbial Monitoring
– Duplicate sampling schedule over length of
intense monitoring program and less frequently
thereafter
– Different agar (PCA versus R2A)
– Different incubation temperatures (22°C and 3035°C)
– Extended incubation time period (3, 5, 8, and 10
days)
Validation Criteria
• PQ Microbial Monitoring
– EP Monograph Reference
– Verify enumeration parameters
– Bacteria identification
• MIS
• Riboprinter
– Gram Stain
– Objectionable organisms
– Summary Report
Operating Procedures
Standard Operating Procedures
• General Considerations
– Prepared, reviewed, and accepted before OQ
execution
– Verbatim compliance
– Keep as concise as possible
– Do not include maintenance procedures
– “Control” of copies important
– Formal training
Standard Operating Procedures
• General Considerations
– Video tape training sessions
– Training Manuals
– System P&IDs mounted in water system area
– Documentation of individual attending training
sessions
– Periodic retraining
– Personnel incident/excursion retraining
Preventative Maintenance
Program
Preventative Maintenance Program
• Objective
- Proactive not reactive
- Shutdown Considerations – frequency
- Cost of lost production time
- Cost of quarantine of product
- Cost of lost product
- “Micro delay”
Preventative Maintenance Program
• Pretreatment Component Example – Activated
Carbon Unit
Item
Suggested Frequency
Consequences
Media Replacement
Six Months
TOC and/or Chloramine Breakthrough
Sanitize Column
Internals
Six Months
Microbial Excursion
Replace Gaskets
Two Years
Leak/Shutdown
Access Gaskets
Six Months
Leak/Shutdown
Clean/Replace
Distributors
One Year
Failure – Media in Product Water
Instrument
Calibration
One Year
Improper System Operation
Replace Valve
Diaphragms
Two Years
Bypass/Cross Contamination
Preventative Maintenance Program
• Ion Removal Component Example – Reverse
Osmosis Unit
Item
Suggested
Frequency
Consequences
“Rotate RO
Membranes”
Six Months
Loss in Product Water Flow Rate and
Quality (Chemical and TVB)
Contract Clean Rotated
Membranes
Six Months
Loss in Product Water Flow Rate and
Quality (Chemical and TVB)
Chemical Sanitization
Six Months
TVB Excursions
Interconnector O-Rings
Six Months
Waste-to-Product Leak
End Fitting O-Rings
Six Months
Waste-to-Product Leak
Instrument Calibration
One Year
Loss of System Control
Replace
Interconnectors
One Year
Waste-to-Product Leak
Preventative Maintenance Program
• Ion Removal Component Example – Reverse
Osmosis Unit
Item
Suggested
Frequency
Consequences
Replace Feed Water
Pump Seals
Two Years
Pump Leak – Introduction of Air/Water –
TVB Increase
Vale Seals/Diaphragms
Two Years
Bypass
Sanitize Pressure
Vessels
Six Months
TVB Excursions
Change Prefilters
One Week
Foulant Increase Resulting in TVB Increase
Hot Water Sanitize (if
equipped)
Two Weeks
TVB Excursions
Replace “Rotated
Membranes”
Three Years
Loss in Product Water Flow Rate and
Quality (Chemical and TVB)
Preventative Maintenance Program
• Storage & Distribution Loop Example – USP
Purified Water Storage Tank (No Ozone)
Item
Suggested
Frequency
Consequences
Instrument Calibration
One Year
Loss of Level Control
Inspect Rupture Disc
Six Months
TVB Excursion
Replace Rupture Disc
One Year
TVB Excursions
Replace Hydrophobic
Vent Filter Cartridge
Six Months
TVB Excursion
Inspect Tank Interior
Six Months
Rouging/Biofilm
Replace Manway
Gasket
One Year
TVB Excursion/Leak
Preventative Maintenance Program
• Ion Removal Component Example – Reverse
Osmosis Unit
Item
Suggested
Frequency
Consequences
Repassivate
One -Two Years
Rouging – Biofilm – TVB Increase
Derouge & Repassivate
Two -Three Years
Rouging – Biofilm – TVB Increase
Hot Water Sanitization
One Week – One
Month
TVB Excursions
Chemical Sanitization
Six Months
Biofilm – TVB Excursion
Thank you!
Questions?