Monitoring for Reliability and Process Control of Potable Reuse Applications Using On-Line Sensors

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1 Monitoring for Reliability and Process Control of Potable Reuse Applications Using On-Line Sensors August 12, 2015 WateReuse Webcast Series 2015 by the WateReuse Research Foundation

2 About WateReuse The WateReuse Research Foundation builds support for water reuse through research and education. More Information Research Reports 2

3 A Few Notes Before We Get Started Today s webcast will be 60 minutes. There is 1 (one) Professional Development Hour available. A PDF of today s presentation can be downloaded when you complete the survey at the conclusion of this webcast. Links to view the recording and to download the presentation will also be ed later. If you have questions for the presenters, please send a message by typing it into the chat box located on the panel on the left side of your screen. If you would like to enlarge your view of the slides, please click the Full Screen button in the upper right corner of the window. To use the chat box, you must exit full screen. 3

4 Today s Presenters Moderator Dr. Phil Rolchigo Pentair Dr. Ian Pepper University of Arizona Dr. Shane Snyder University of Arizona 4

5 Monitoring for Reliability and Process Control of Potable Reuse Applications WRRF Project 11-01, Webcast, 12 th August 2015 Ian Pepper, Ph.D. Professor & Co-Director Soil, Water, and Environ. Science Shane Snyder, Ph.D. Professor & Co-Director Chem. & Environ. Engineering

6 Acknowledgements Dr. Hye-Weon Yu (U. Arizona) Hach Corporation S::CAN Corporation Xylem Agilent Technologies Utility/Agency Partners WEST Center Partners

7 Industries That Rely on Sensors I. Transportation and Military (aircraft, trains, guidance) II. Medical and Health-Care (diagnostics, drug delivery) III. Security and Enforcement (airport security/customs)

8 Sensor Applications for Water I. Ensuring water quality & treatment integrity (RO credit) II. Optimization of chemical dosing & mixing (cost savings) III. Speed & automation (process control and labor savings)

9 Online monitoring system Questions when planning a monitoring and control system Analytical parameters Location of sensors Type of communication signals and sensor outputs Process control and regulatory compliance (Alert system)

10 Smart Water/Energy Network

11 Literature Review

12 What is the IDEAL Sensor? High-throughput by distribution of miniaturized sensors Integration from sample pretreatment and concentration to sensing system Real-time In-line Practical Application Activation, Regeneration, & Calibration Of sensing probes Long-term Multi-target Costeffectiveness

13 Accuracy Critical Aspects Consistency/Precision Sensitivity Range Often choice of sensor is a tradeoff between several of the above characteristics. For example, moderate accuracy over a large range may be preferable to great accuracy over a very small range. archive.senseit.org

14 Sensor Types

15 Physical/Chemical sensor A device that transforms chemical information, ranging from the concentration of a specific sample component to total composition analysis, into an analytically useful signal

16 Ion-selective electrode (ISE) Measures the activity of an ion in a solution by measuring the electric potential formed across a membrane when the electrode is submerged in the solution H + (ph meter), NH 4+, K +, Ag +, Cd +2, Ca +2, Cu +2, Pb +2, Cl -, CN -, F -, I -, NO 3-, ClO 4-, Br - An ion selective polymeric membrane is often made by mixing an ionophore (e.g. valinomycin, a natural occurring antibiotic) with PVC and a plasticizer (to make the rigid plastic more flexible)

17 Organic parameters

18 Professor Yoon: University of Arizona Microbial Sensors

19 Biosensor Analytical device that combines a biological sensing element with a transducer to produce a signal proportional to the analyte concentration Ultra-Sensitive Electrical Biosensor for Instant Diagnostic Devices

20 Animal Bioassays Some assays are available as on-line monitors

21 Lab-on-a-chip (LOC) A microfluidic device that integrates one or several laboratory functions, such as sampling, mixing, reaction, and separation into a small single chip (only millimeters to a few square centimeters in size) scopeblog.stanford.edu

22 Tissue on a Chip

23 Sensors are at the forefront of a multidisciplinary science that marries the biological world and the electronic world

24 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01)

25 Systems Evaluated Evaluation of online sensor monitoring system Scale Processes Water source Lab Pilot Full O 3, UV/H 2 O 2, RO, GAC O 3, UV/H 2 O 2 UF/RO GMF, MF, O 3 /H 2 O 2 MF, RO, UV/H 2 O 2 MF, RO, UV/H 2 O 2 Two wastewater reclamation facilities (Arizona, United States) Tucson Water Sweetwater Recharge Infiltration Systems (Arizona, United States) Beenyup Wastewater Treatment Plant and Advanced Water Recycling Plant (Perth, Australia) Sacramento Regional Wastewater Treatment Plant (California, United States) West Basin Municipal Water District (California, United States) Orange County Water District Groundwater Replenishment System (California, United States)

26 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) Indicator An individual compound or microorganism, occurring at a quantifiable level, whose behavior in the unit process is thought to be representative of TOrCs or microorganisms Surrogate A bulk parameter, whose measurement characterizes the performance of a unit process in removing a target contaminant J.E. Drewes et al., WateReuse Foundation (2008) Chemical indicator Microbial indicator Bacteria MS2 virus Spore Metabolic biomarkers (ATP, NADP(H)) General parameters (ph, temperature, conductivity, turbidity) Organic parameters (TOC, DOC, UVA 254, fluorescence) Inorganic parameters (Chlorine, NO 2, NO 3 )

27 Surrogates

28 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01)

29 False positives False negatives Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) SENSOR ISSUES Sensitivity of detection Detection of chemical and microbial contaminants via a realtime trigger Identification of treatment failures Integration of software data management, e.g., Labview Sensor maintenance & cost evaluation Self-monitoring

30 Sensor Performance Working range Limit of linearty (LOL, R 2 >0.95) Limit of quantitation (LOQ, S/N=10) Limit of detection (LOD, S/N=3) Sensor performance (1) Limit of detection (LOD) (2) Working range - Limit of quantitation (LOQ) - Limit of linearity (LOL) (3) Response time (4) Accuracy (%Recovery) (5) Precision (%RSD) (6) Correlation coefficient to reference method (R 2 )

31 Reuse Water Testing

32 UVT/UVA UV absorbance & UV transmittance (λ=254 nm) UVA = 2 log 10 UVT R 2 (Online/Offline data) RealUVT 0.99 IQ 0.99

33 On-line TOC

34 On-line TOC Limits for Optical

35 Lab Scale Configuration Online data acquisition system Feed water tank (Secondary treated effluent) Cartridge filter (10 µm-filtration) FM Untreated flow FM FM FM FM FM FM FM FM FM FM Waste H 2 O 2 UV reactor (Low pressure) Treated flow Manifold Sampling point for offline analysis

36 Lab-scale Testing (1) Ozonation Ozonation is an effective water treatment technology for oxidation of trace organic contaminants such as endocrine-disrupting chemicals (EDC) and residuals of pharmaceutical and personal care products (PPCPs) In addition to direct oxidation of these pollutants by ozone (O 3 ), ozone decomposition produces hydroxyl radicals ( OH) that readily degrade many organic compounds present in water Direct reaction with O 3 M Low molecular organic compound OH Radical reaction

37 Lab-scale Testing (1) Ozonation Ozone generator Ozone absorption contactor

38 Lab-scale Testing (1) Ozonation Online sensor response

39 Lab-scale Testing (1) Ozonation Classification of TOrCs Reactivity Ozone OH ko3 (M-1s-1) k OH (M-1s-1) Group1 High High >10^5 >5*10^9 Group2 Moderate High 10<kO3<10^5 >5*10^9 Attenuation of TOrCs by ozonation Group3 Moderate Moderate 10<kO3<10^5 10^9<kOH<5*10^9 Group4 Low Moderate <10 10^9<kOH<5*10^9 Group5 Low Low <10 <10^9 Group1 Group2 Group3 Group4 Group5 Carbamezapine Atenolol DEET Meprobamate TCEP Diclofenac Caffeine Diphenhydramine TCPP Naproxen Gemfibrozil Ibuprofen Sulfamethoxazole Primidone Triclosan Trimethoprim

40 Lab-scale Testing (1) Ozonation Online sensor response vs. Attenuation of TOrCs UVA decrease UVT increase

41 Lab-scale Testing (2) UV/H 2 O 2 AOP Direct photolysis: TOrCs absorb light energy in the UV spectra range, which raises the molecule to an excited state and results in photochemical transformation and degradation OH oxidation: When hydrogen peroxide (H 2 O 2 ) is added to the water that is irradiated by UV, hydroxyl radicals are formed and quickly react with the TOrCs through electron transfer

42 Lab-scale Testing (2) UV/H 2 O 2 AOP Online sensor response Chemical based-toc sensor Optical based-toc sensor Fragmentation and transformation of the organic compounds from high to low molecular weight

43 Lab-scale Testing (2) UV/H 2 O 2 AOP Online sensor response

44 Lab-scale Testing (2) UV/H 2 O 2 AOP UV dose

45 Lab-scale Testing (2) UV/H 2 O 2 AOP Attenuation of TOrCs UV dose UV dose UV dose UV dose

46 Lab-scale Testing (2) UV/H 2 O 2 AOP Yu et al., Water Research 81 (2015)

47 Lab-scale Testing (2) UV/H 2 O 2 AOP Yu et al., Water Research 81 (2015)

48 Lab-scale Testing (2) UV/H 2 O 2 AOP Yu et al., Water Research 81 (2015)

49 Lab-scale Testing (2) UV/H 2 O 2 AOP Online sensor response vs. Attenuation of TOrCs Yu et al., Water Research 81 (2015)

50 Recent Publication: UV/H 2 O 2 AOP

51 Lab-scale Testing (3) Reverse osmosis (RO) filtration Failure of the RO Process and Increased Salt Passage Increased salt passage could result from mechanical leaks, faulty O-ring seals, cracked tubes, or punctured membranes, and centerfold cracking. Membrane damage can result from: i) membrane oxidation by oxidizing chemicals; ii) membrane surface abrasion by crystalline or sharp-edged metallic suspended solids in the feed water; or iii) membrane rupture in the edges of glue lines by permeate backpressure. SSSS ppppppp % = 1 ssss rrrrrrrrr 100 reverseosmosispros.com = TTT pppppppp TTT ffff 100

52 Lab-scale Testing (3) Reverse osmosis (RO) filtration

53 Lab-scale Testing (3) Reverse osmosis (RO) filtration

54 Online sensor response Lab-scale Testing (3) Reverse osmosis (RO) filtration

55 Lab-scale Testing (3) Reverse osmosis (RO) filtration

56 Lab-scale Testing (1) Granual activated carbon (GAC) Rapid Small Scale Column Testing (RSSCTs) Bench-scale tool to accurately predict GAC performance in a short period of time

57 UV254 and TF as surrogate indicators Linear regression model WWTP Contaminant Removal (%) Reduction in UV 254 Absorbance (%) Increase in BV Reduction in Total Fluorescence (%)

58 Lab-scale Testing (1) Granual activated carbon (GAC)

59 Recent Publication: Granual activated carbon (GAC)

60 Powdered Activated Carbon < Different Water > TF is the integration of fluorescence intensity over excitation and emission wavelengths < Different PAC >

61 PARAFAC modeling for PAC To investigate correlation between TOrCs removal and each fluorescent organic fraction removal. Ref: Murphy, K.R., Stedmon, C.A., Graeber, D. and Bro, R. (2013) Fluorescence spectroscopy and multi-way techniques. PARAFAC. Analytical Methods 5(23),

62 PARAFAC modeling for PAC Little difference between fluorescent components, but good correlation established for each component

63 Lab-scale Testing (3) Reverse osmosis (RO) filtration Online sensor response vs. Attenuation of TOrCs

64 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) REAL-TIME DETECTION OF BACTERIA IN WATER Issues related to detection of bacteria - Culturable populations versus viablebut-non-culturable (VBNC) - Ability to regrow - Repair mechanisms following UV disinfection

65 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) Microbial real-time sensors evaluated in: - Distilled water (spiked contaminants) - Tap water (spiked contaminants) - Secondary treated wastewater effluents (natural existing microbial contaminants)

66 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) 1) Real-Time Detection via Multi-Angle Light Scattering MALS (BioSentry) Unique light-scattering patterns generated by laser beam passing through water Four channels classify microbes on basis of size and shape into - Bacteria - Spores - Protozoa - Unknown category

67 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) REAL-TIME SENSORS FOR MICROBES Detection of Microbial Contaminants: BioSentry

68 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) BioSentry Detection of Escherichia coli

69 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) BioSentry Results for E.coli Concentration measured (org/ml) 1.00E E E E E E E E+00 DI Water E. coli with media Cultural AODC BioSentry Target Concentration BioSentry output coincides well with all concentrations

70 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) ISSUES WITH MALS Turbidity Does not distinguish viable versus nonviable cells

71 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) REAL-TIME DETECTION VIA FLUORESCENCE EMISSION (Instant BioScan) Detection of universal bio-markers - NADH and Riboflavin - Fluorescence under UV illumination at 405 nm gives viable count Laser light scattering gives total count (biological and colloidal)

72 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) MICROBIAL CONTAMINANTS THE RMS SYSTEM: Instant BioScan Real-Time Monitoring System Delivering instant detection and enumeration of microorganisms and inert particles Manufacturer: Instant BioScan

73 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) Instant BioScan Response to unfiltered Tucson Tap Water RMS BioCount (cells/ml) Instant BioScan Analysis: Unfiltered Tucson Tap Water Instant BioScan Response to filtered Tucson Tap Water RMS BioCounts (cells/ml) HPC HPC HPC Minutes into Experiments Filtered Tap Water

74 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) DETECTION OF BACTERIA IN SECONDARY TREATED EFFLUENT Fluorescence from NADH and Riboflavin unsuccessful REASON: Fluorescence excitation emission of biomarkers overlap with natural organic matter (NOM)

75 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) The FL-EEM (Fluorescence excitation emission) of either E. coli & NOM

76 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) INSTANT BIOSCAN Gives viable counts Useful in water with low NOM eg. back-end of advanced treatment train

77 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) REAL-TIME DETECTION VIA ATP PRODUCTION LUMINULTRA (Hach) Surrogate for total microbial load Based on adenosine triphosphate (ATP) production Mg 2+ ATP + O 2 + luciferin AMP + PPi + oxyluciferin + light luciferase Light detected via luminometer Bacterial cell contains 1 femtogram ATP Test assay duration < 5 minutes

78 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) LUMINULTRA: Advantages Real-time assay 2 minutes Detects total microbial load including culturable and VBN microbes Field-ready (portable)

79 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) LUMINULTRA Useful surrogate for total microbial load Essentially real-time assay Not on-line, but cost-effective such that batch tests can be run multiple times daily

80 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) DETERMINATION OF MICROBIAL NUMBERS Where RLU = Relative Light Units

81 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) DETECTION OF INCREMENTAL MEMBRANE FAILURE VIA LUMINULTRA Reverse osmosis utilized to generate RO permeate and brime (salt) Two secondary treated effluents subjected to reverse osmosis Failure mode simulated by blending permeate with increasing amounts of brine Seven different ratios

82 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) Raw microbial counts in blends of Brine: Permeate representing incremental failure. GV Ina Target blending ratio (%Brine:%Permeate) Salt passage (%) LuminUltra (ME/100 ml) HPC (Counts/100 ml) Total coliform (MPN/ 100mL) E.coli (MPN/ 100mL)

83 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) Correlation of LuminUltra values with increasing salt passage.

84 Pilot-scale Testing (1) Tucson Water Sweetwater Tucson Water Sweetwater Recharge Infiltration Systems O 3 /UV pilot facility Online sensor system

85 Pilot-scale Testing (1) Tucson Water Sweetwater Ozonation: Sensor signal as surrogate parameter

86 Pilot-scale Testing (1) Tucson Water Sweetwater Ozonation: Sensor signal vs. Attenuation of TOrCs

87 Pilot-scale Testing (1) Tucson Water Sweetwater UV/H 2 O 2 AOP: Sensor signal as surrogate parameter

88 Pilot-scale Testing (1) Tucson Water Sweetwater UV/H 2 O 2 AOP: Sensor signal vs. Attenuation of TOrCs

89 Pilot-scale Testing (2) Beenyup Advanced Water Recycling Plant (Perth, Australia) Analytical parameter On-line sensor Feedwater Ammonia HACH Amtax SC Turbidity HACH 1720 E Chlorine Prominent ORP Yokogawa UF filtrate pre H 2 SO 4 dosing Turbidity HACH Filtertrak 660 sc TOC GE Sievers 5310C UF filtrate post H 2 SO 4 dosing Ammonia/monochloramine HACH APA 6000 Turbidity, nitrate, TOC/DOC, UV254, ammonium, ph S::CAN ph, conductivity E&H Liquiline ORP Yokogawa RO feedwater Ammonia/monochloramine HACH APA 6000 ph, conductivity E&H Liquiline ORP Yokogawa RO permeate TOC GE Sievers 5310C Turbidity, nitrate, TOC/DOC, UV254, ammonium, ph S::CAN ph, conductivity E&H Liquiline ORP Yokogawa Treated water Ammonia/monochloramine HACH APA 6000 ph, conductivity E&H Liquiline ORP Yokogawa DO E&H Liquisys

90 Pilot-scale Testing (2) Beenyup Advanced Water Recycling Plant (Perth, Australia)

91 Pilot-scale Testing (3) Sacramento Regional Wastewater Treatment Plant (California, United States)

92 Full-scale Testing (1) West Basin Municipal Water District (California, United States)

93 Full-scale Testing (2) Orange County Water District Groundwater Replenishment System (California, United States) Process control by online sensor-based monitoring

94 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) OTHER SENSOR ISSUES Data Management Requirements: Implemented Ability to stream and collect data from multiple sensors simultaneously and 24/7 - Modified LabVIEW software - Centralized database - Data can be displayed numerically and graphically - Real-time data, past and present can be accessed - Can be exported to an Excel spreadsheet for further manipulation Data Management Requirements: Needed Develop an operational decision support tool: - SCADA system - Early detection of incremental treatment failure - Critical control points - Software development for self healing ie. WateReuse 14-01

95 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) OTHER SENSOR ISSUES: MAINTENANCE Real-time sensors require monitoring on a daily basis. Key online monitoring parameters include TOC, free chlorine, conductivity, ph/orp, turbidity and temperature. Maintenance requirements vary significantly depending on the parameters and the device. Maintenance scheduling requirements can be daily (D), weekly (W),monthly (M), quarterly (Q), semi-annually (SA), and annually (A). TOC instrumentation is the most labor/cost intensive. A skilled technician is required to reliably operate and maintain the instrumentation on a continuous daily basis.

96 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) EXAMPLE OF MAINTENANCE Sievers 5310C Online TOC Analyzer: Approximately $4000/year for consumables Replace reagent/acid(q), reagent/oxidizer (SA) Change the pump tubing (SA) Replace the resin bed (SA) Replace UV lamp (SA) Replace ICR degasser, chemical trap, and rebuild pump (A) Replace in-line particulate filter (A) Replace oxidizer syringe (A) Replace restrictor tubing (A) Locate and remove crystal blockages from restrictor tubing (D)(M) Interior view of TOC Analyzer

97 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) SUMMARY LAB EVALUATIONS Advanced treatment of reclaimed water successfully removes or inactivates chemical and microbial contaminants to acceptable levels Chemical based on-line sensors for TOC; and on-line sensors for conductivity and turbidity are useful on-line sensors for process control Best surrogates for trace organics: - Excitation Emission Matrix (EEM) and UV 254 Absorbance - Sensors: SaFire UV 254 Best surrogates/indicators for microbes - HPC E.coli total coliforms - Sensors/Assays: LuminUltra

98 Monitoring for Reliability and Process Control of Potable Reuse Applications (WateReuse 11-01) SUMMARY PILOT & FULL-SCALE EVALUATIONS On-line sensors effective for process control On-line fluorescence sensors and the LuminUltra real-time assay could be considered for process control at future plants Real-time monitoring feasible, but challenges still need to be overcome

99 For More Information: Ian Pepper: Shane Snyder: