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									Microconstituents – Emerging Contaminants

            Joint Water Resources Symposium
        New York Water Environment Associations
    New York Section American Water Works Association
               In Honor or Edwin C. Tifft, Jr.

                      Syracuse, NY
                    November 14, 2007

                 Joseph G. Cleary, P.E., BCEE
                          Principal
                       HydroQual, Inc.
                        Mahwah, NJ
           Presentation Outline

•   WEF’s Community of Practice Activities
•   Microconstituents - What’s Included?
•   Terminology / Name Changes / Key Messages
•   Treatment Technologies
•   Approach to Develop Best Solution
•   Case Studies
•   Summary
WEF Community of Practice
       Activities
   Why are Microconstituents a Concern?


• Better analytical methods and more monitoring are finding
  them in numerous receiving waters
• Feminized fish discovered in Europe in mid 1990s
• Steroids are implicated in Europe in late 1990s
• Treatment studies on POTWs (2002-2003) show POTWs are a
  collection point and one source to receiving waters
• USGS study of 139 streams in 2002 detected pharmaceuticals
  in 80% of samples
• More media coverage & public awareness and concerns.
WEF Community of Practice (CoP)


• Began at WEFTEC 2005 in
  Washington DC
• Deals with hot topics
• Broad, diverse membership – a
  benefit and challenge
• 150 Members and growing
           WEF Key Messages


• Committed to sharing clear, factual
  information
• Advancing understanding
• Pursuing sound, sustainable solutions
• Focusing on source control
        Two Fundamental Challenges


1.   Technical challenges due to scientific
     uncertainties
2.   Communication challenges related to public
     fears and perceptions.
WEF Community of Practice (CoP)


Identified work products
  • Technical Practice Updates
  • Public & Press Communications
  • Glossary of Terms
  • Name for the issue
  WEFs Public Communication’s Role


Staff Products include:
• Key Messages
• Fact Sheets
• Illustrations
• Finding Expert Spokespersons
• Building Consensus
Varying Communication Challenges
           Include:


What to call the compounds
without negatively branding them
as a “worry” or “concern”?

Media accounts and technical
publications already using a
multiplicity of terms
      Varying Communication Challenges
                 Include:

Scientists wanting to communicate with
precision to scientists

WEF needs also to communicate with the
scientific community, its membership and the
general public

The required vernacular must vary to suit the
audience – so the language must be tailored
    Communication Challenge


Second challenge - Technical and
communications experts
  • Different audiences
  • Different vocabulary
  • Different approaches
Microconstituents - What’s
       Included?
Micro Constituents in Water: Where Do
         They Come From?




             Courtesy of CH2M Hill
Reference: Kobylinski, Hunter and
Scruggs, 2005
                  New Emerging Compounds
HYDROPHILIC                              benzene, naphthalene
                                             sulfonates
                            surfactants
                        perfluorinated            pharmaceuticals
                                                betablockers, antibiotics,
                      compounds (PFOA)
                                                     contrast media,
                                                analgesics, antiepileptics,
    POLARITY




               corrosion inhibitors             parasiticides, babiturates,
                e.g. benzotriazole                       opioides
                      NDMA              phosphoric ester
                                         flame retardants
                                                                   estrogenes
                MTBE
                                          UV filter         from Walter Giger,
                              musk fragrances               in Ternes und Joss,
                                                            IWA Publishing, 2006
                                  Volatility
LIPOPHILIC           VOLATILE                      NON VOLATILE
                New Emerging Compounds
       conc. 6.0                                                       diclofenac                                                             March
                                                                                                                                                                                                             contrast media
      in µg/L                                                                                                                                 May
               5.0
                                                                                                                                              September
               4.0                                                     carbamazepine

               3.0                                                                                                                 betablocker


               2.0   antibiotics
                                                                                                                                                                                    musk frag.
               1.0

               0,0




                                                                                                                                                                                                                                        Iomeprol
                                    Sulfamethoxazole




                                                                                                                   Carbamazepine
                                                                                                  Clofibric acid
                                                       Roxithromycin




                                                                                                                                                                      Propranolol




                                                                                                                                                                                                                          Diatrizoate
                                                                                     Diclofenac




                                                                                                                                                         Metoprolol
                                                                        Ibuprofen




                                                                                                                                                                                     Galaxolide



                                                                                                                                                                                                              Iopamidol
                     Trimethoprim




                                                                                                                                   Atenolol

                                                                                                                                               Sotalol




                                                                                                                                                                                                  Tonalide
360‘000 Pop. Equiv.
Nitrification/Denitrification                                                       Ternes et al., Chemosphere 2007
    Diversity of Endocrine Disruptor
  Compounds (Falconer (2003) and Wren (2001))
Pesticides   2,4-D             Chlordane              DDT                  Endosulfan
&            Endrin            Heptachlor             Methoxychlor         Toxaphane
Herbicides   Vinclozolin       Atrazine               Simazine             Dieldrin
             Lindane


Persistent   Dioxins           Furans                 P-nonylphenol’s      PBB
             PCP               Hexachlorobenzene      Tributyl tin         Octachlorostyrene
Industrial
             Phthalates        Bisphenol A                                 PCB’s
Chemicals

Heavy        Cadmium           Lead                   Mercury
Metals

Hormones     Synthetic:        17-Ethinylestradiol   Diethylstilbestrol   Estrone
             Biological:       17-Estradiol          Estriol              Phytosterols
                               Progesterone           Testerone            Coumestans
             Plant secondary                          Sesquiterpenes
             metabolites
                               Lignans                Isoflavonoids
Why are Microconstituents a Concern?

• A review by the World Health Organization has
  concluded that low-level environmental exposure to
  Endocrine Disruptors has not yet been demonstrated
  to cause harm to human health (Damstra et al.,
  2002).
• Uptake of Endocrine Disruptors by humans from
  treated drinking water is relatively low in comparison
  to other sources such as food (GWRC, 2003).
  Terminology / Name
Changes / Key Messages
         WEF Terminology Challenges

Nov 2005
Endocrine Disrupting Compounds (EDC)
(goal was communicating with WEF membership)

Feb 2006
Compounds of Emerging Concern (CEC)
(because not just about endocrine issues)

Oct 2006
Compounds of Potential Concern
(how to respond to the public – diligence in studying the issue)
            Terminology Challenge

May 2007
More discussion about alarming the public – when we don’t
have a basis to ring the alarm bells

                     Micro-constituents

No, not little voters but really small things in the water
environment that we can now detect (at ppb and ppt) and we
don’t know enough about.
              WEF Key Messages

These compounds are referred to in a multiplicity of
ways including micro-constituents, trace constituents
compounds of emerging concern, etc.

WEF is calling them micro-constituents. We continue
to study them as a prudent, conservative course of
action reflecting our commitment to continue to assess
the potential impact on human health and the
environment.
              WEF Key Messages

Low levels of compounds remain but in
concentrations that we believe are safe to return to the
environment

There are differing levels of Wastewater Treatment and
Water Treatment

We are studying the issue of even the trace amounts
of these chemicals that remain after wastewater
treatment
           WEF Key Messages


• Treated wastewater is not the only pathway
  for these substances to enter the
  environment
• Many items we can detect have beneficial
  effects (i.e. medicines and pest control)
• Some improvement quality & longevity of life
        WEF Key Messages


• Effects depend on:

    - Nature of compound
    - Type of exposure
    - Concentration
    - Quantity/duration of exposure
       Some Facts to Keep in Mind


• Some compounds are naturally occurring
• Society chooses to ingest, bathe in and
  apply constituents at much higher
  concentrations than ever found in the
  environment
Treatment Technologies
Physical/Chemical Properties – Keys to
             Treatment
   Water Solubility (mg/L)
   Henry’s Constant (atm m3/mole)
   Octonal Water Coefficient Log Kow (Partitioning to
    Solids)
   Vapor Pressure, Vp
   Distribution Coefficient, Kd
   Biotransformation Ratio (K bio in soil, water, sludge and
    sediment)
   Biodegradability
   Photolysis Rate
   Oxidation Rate
   Reduction Rate               Reference: Williams, 2006
Applicable Treatment Technologies for
                EDCs

• Aerobic Biological Treatment Processes including
  Nitrogen Removal (e.g. Activated Sludge, Membrane
  Bioreactors)
• Chlorination (e.g. bleach, alkaline chlorination)
• Advanced Oxidation (UV/Peroxide, Ozone/Peroxide,
  UV/Ozone
• Carbon Adsorption
• Membrane Filtration and Reverse Osmosis
• Thermal Oxidizers
• Anaerobic Biological Treatment
Summary of Poseidon Project in Europe
         (Thomas Ternes)
• PPCPs and Estrogens removal focus in Europe
• Membranes & Ozonation in combination with Activated
  Sludge & Biofilters were evaluated
• Sludge treatment and urine separation was evaluated
• Sorption is an important mechanism for hydrophobic and
  positively charged compounds
• Biodegradation is a key mechanism
• Stripping was not effective
• Chemical oxidation was an effective polishing step for some
  PPCPs
• Some PPCPs are degraded in anaerobic sludge digestion
• Available process models can be used using rate
  coefficients developed
                                  Activated Sludge
Process Wastewater




      EQ
     Tank          Jet Aeration




                                  Aeration Tank #1

 Denitrification
                                                             Clarifier            Effluent
   Selector

                                  Aeration Tank #2
                                                                   Waste Activated Sludge


                   Jet Aeration

                                   Return Activated Sludge                   Filter
                                                                             Press
Membrane Bioreactor Process
Fixed Film Technology
          Other Treatment Studies

• MLE Plant in San Diego (WERF Study, Oppenheimer,
  2005)
• Six full-scale WWTPs in the U.S. and two pilot scale
  MBRs (WERF Study, Oppenheimer, 2006)
• Half of the 20 PPCPs were removed to greater than 80%
  at SRT <5 days
• No additional removal was attributed to MBR, media
  filters or longer HRTs
• Removal of musk fragrances required SRTs of at least
  25 days
    Results from Two-Stage MBR & Ozone
           Treatment in Pilot Study

      API(1)          DL(2)          Influent            MBR Permeate           Ozone Effluent
                               Average     Range       Average     Range      Average      Range
17-α-estradiol        0.23      0.36     ND(3) – 1.1    0.18     ND – 0.41     ND           ND
17-β-estradiol        0.23       1.7     0.62 – 2.6     0.30     ND – 0.68     ND           ND
17-α-dihydroequilin   0.23       1.7     0.22 – 6.4     0.30     ND – 0.63     ND           ND
Estrone               0.23       3.8      2.8 – 4.9     3.30     0.54 – 6.0    0.20     0.17 – 0.25

   (1)   APIs concentrations are listed in g/L
   (2)   DL: Detection limit
   (3)   ND: Not detected


   Reference: Helmig, Edward et al., WEFTEC 2005
                                Ozone Treatment

                                              O
        HOOC                                          H
                 H     Cl            H2N      S       N
                 N                            O                                                 N
                                                          N    O
                                                                                            O       NH2
                Cl
            Diclofenac                Sulfamethoxazole                             Carbamazepine

                 CH3
                       OH                                 R1

                            C   CH

                                             HO                    OR2
                                                          OH                           N
                                                                           HO
                                                                           O      O
                                                                                            Huber et al., 2003,
HO
                                                      O                                     Env.Sci.Technol.
                                                  O                O            OCH3


                                                                                       OH
                                                                       O

     17 a-Ethinylestradiol                            Roxithromycin
WEF Technical Practice Update on Treatment

  • EDC Committee Formed @ WEFTEC October 2005
  • List of TPUs was developed ( 13 topics)
  • Treatment was done first
  • Draft for comment in January 2006
  • Review meeting in February 2006
  • Committee name changed to “Contaminants of
    Emerging Concern” now “Microconstituents”
  • Comments received in March 2006 on Treatment
    White Paper – Change to Technical Practice Update
  • Final draft April 2007
  • Final version now on WEF website along with
    others
What Has Been Done and What Do We Know


• Many studies have demonstrated that activated
  sludge processes have the potential to remove a
  large fraction of several suspected EDCs, often to
  below detection limits (Ying, 2002).
• Johnson and Darton (2003) state that the EDCs
  generally implicated in endocrine disruption in fish –
  the estrogens E1, E2, EE2, and NP – are all
  “inherently biodegradable”
What Has Been Done and What Do We Know
                        (continued)



• Siegrist estimates that about a 10 to 15 day SRT would
  be required for appreciable EDC removal (Siegrist et al.,
  2005).
• Estrogens can be eliminated in WWTPs by applying a
  nitrification/denitrification step (SRTs 15 days), or by
  effluent ozonation, nanofiltraton, or activated carbon.
• Anaerobic sludge digestion leads to a degradation of
  some PPCPs.
What Has Been Done and What Do We Know
                          (continued)


• Substances that are difficult to biodegrade may be oxidized by
  AOPs, and the oxidized byproducts may be more amenable to
  biodegradation (Ried and Mielcke, 2003).
• Advanced oxidation process (AOP) are combinations of UV
  plus hydrogen peroxide, ozone plus hydrogen peroxide, and
  UV plus ozone, that are specifically designed to increase the
  formation of powerful hydroxyl radicals to oxidize EDCs and
  provide disinfection. Ozone shows similar potential to the
  AOPs for EDC removal.
What Has Been Done and What Do We Know
                       (continued)


• 100% removal of EDCs from WWTP effluent will not be
  possible, so the goal should be reduction to levels with
  no adverse environmental effects.
• Source control (e.g., ecolabelling) and source
  separation (e.g., urine or rain water segregation) are
  important measures for reducing the PPCP load
  entering the environment.
         What is Needed or Not Known?



• Toxicological and other environmental impacts are not known
  for most EDCs.
• Risk assessment studies are needed to develop appropriate
  regulatory actions (Schoenberg, Helmig et al., 2005).
• Fate studies are needed describing removals of compounds
  and pathways: biodegradation/biotransformation, partitioning
  to solids, volatilization.
        What is Needed or Not Known?
                         (continued)



• Analytical procedures are needed to detect lower levels of
  estrogens and to distinguish between various forms.
• Research to better understand the performance of engineered
  and natural treatment systems for reduction of these
  compounds (Oppenheimer et al., 2005).
• The hazard potential of the byproducts formed through
  treatment with advanced oxidation requires additional
  investigation.
  Integrated / Holistic
Approach to Develop Best
        Solution
                     Urban Water Cycle

    Industry



                   STP




                     Irrigation
Water/Sediment      (soil/aquifer)

                   “Run off“
                            infiltration
             bank filtrate groundwater



                 Waterworks                Drinking water
Integrated vs. End-of-Pipe Approach

                                              End of Pipe Approach




             Production



                                  Secondary                     To POTW
                                                  Tertiary
                                 Wastewater
                                                Wastewater
  Raw                             Treatment
                                                 Treatment
 Water
 Supply


                                   Sludge
             Utilities
                                                         Brine Disposal



                          Water Reuse


   Well
  Water
 Supply
             Collaborative Team
              Approach is Best

• Mobilize a Team – Include People Closest to
  Problems and Stakeholders
• Include Production, Water and Wastewater
  Operations, Environmental Compliance
  Managers
• Outside Consultant
• Commitment of Management and Team
• Frequent Communications and Meetings
                     Approach
                  Sequence of Tasks

• Flow Balance & Wastewater Characteristics
•   Design Basis (flow & wasteloads)
•   Screen Technologies
•   Develop Initial Alternatives
•   Alternative Comparison (cost & non-costs criteria)
•   Narrow List of Alternatives
•   Treatability Studies & Process Modeling
•   Refine Comparison
•   Select Best Solution
Case Studies
                        Case Study #1

   Pharmaceutical Company in U.S.
   New Product from Europe – Chlorination (bleach) used for destruction
   Initial testing showed it was non-biodegradable, would pass through
    existing treatment plant and result in effluent toxicity violations.
   Treatability Studies were conducted to evaluate Advanced Oxidation
    treatment technology; UV/hydrogen peroxide, catalyst/UV/hydrogen
    peroxide, UV/ozone and UV/hydrogen peroxide/ozone.
   Two technologies also reduced effluent toxicity by 95% (UV/ozone and
    UV/ozone/hydrogen peroxide.
   Product was never brought to the plant from Europe.
Chemical Oxidation Technology Evaluation

Run Number   Treatment Process   Compound     Toxicity
                                 Reduction   Reduction


    1        UV, hydrogen          99.5%       58%
             peroxide
    2        Catalyzed UV,         99.8%      88.2%
             hydrogen peroxide
    3        UV, ozone             99.4%      99.1%


    4        UV, ozone,            99.5%       95%
             hydrogen peroxide
                    Case Study #2

   Pharmaceutical Company in Puerto Rico
   New Product
   “Active Pharmaceutical Ingredients” (API) in cleaning
    wastewaters
   Company had Corporate Guidelines (from Europe) for
    discharge to the Atlantic Ocean
   Discharge through POTW to Atlantic Ocean
   Best solution was holding tank with controlled release to
    POTW – no treatment was needed
                          EXAMPLE WATER BALANCE

                                           CTF – 2

                300,000
                gallons
                                           CTF – 1

                                                                                               CIP

                                          PROCESS – 2
                                                           41,000 gpd
                                                                                                     10,500 gpd
                             58,000 gpd
                                           COOLING – 2           17,000 gpd                          009
                                                                                 Wastewater                   43,000 gpd
PRASA 2                                                                          Treatment
                                                           15,000 gpd
                             21,000 gpd
              300,000                     COOLING – 1




                                                                                   8,000 gpd
92,000 gpd    gallons                                                                          1,500 gpd
                                                                   6,000 gpd

                                                                                                      Miscellaneous
                             2,500 gpd                    005
                                               Sanitary                           AHU
                                                                   2,500 gpd
                                                                                Condensate
               12,000
               gallons                                    18,000 gpd
                            25,000 gpd                          7,000 gpd
                                           PROCESS – 1


                                                                                Wastewater           001      12,500 gpd
 PRASA 1                                                                        Treatment
                             2,000 gpd
                                               Boiler
 31,000 gpd    50,000
               gallons
                             1,000 gpd    PROCESS – 1                                                                 Process User
                                                          004
                                                                    5,500 gpd                                         Utility User
                             5,500 gpd      Cafeteria
                                            Sanitary
                                                                                                                      Sanitary User
                              Case Study #3

   Pharmaceutical Company in Ireland.
   Considering production of an antifungal compound.
   Compound is relatively insoluble and non-biodegradable.
   Potential to accumulate in sludge and impact composting.
   Concern was potential impact on activated sludge plant and sludge
    composting at POTW.
   Treatability Studies simulated activated sludge and sludge composting
    to determine process impacts and concentrations present in sludge and
    compost material.
   There was no impact on activated sludge performance including
    nitrification.
   Mass balance showed 70% of compound was biodegradable.
   There was no impact on composting process.
Bench-Scale Anoxic and Aerobic Reactors
                                SUMMARY

   Microconstituents are now being detected more in water and wastewater.
   Analytical methods are “specialized”.
   Information is developing on treatment/destruction of Microconstituents in both
    POTWs and pharmaceutical wastewaters.
   Applicable treatment technologies include biological and advanced oxidation
    processes.
   EDCs removal in POTWs and Industrial Wastewater Plants varies based on
    wastewater characteristics and process design operating parameters such as
    sludge age.
   Treatability studies are very helpful for site-specific wastewater projects.
   Stay tuned as more “Technical Practice Updates” are developed by WEF and
    specially conferences are planned.
Thank you!


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