TECHNICAL REPORT. May 13, 2015

Transcription

1 Page 1 of 146 TECHNICAL REPORT LAND-BASED STATUS TEST OF THE JFE BALLASTACE BALLAST WATER MANAGEMENT SYSTEM AND COMPONENTS AT THE GSI TESTING FACILITY May 13, 2015 Research Team: Allegra Cangelosi, NEMWI, Principal Investigator Meagan Aliff, NRRI, UMD Lisa Allinger, NRRI, UMD Mary Balcer, PhD, LSRI, UWS Kimberly Beesley, LSRI, UWS Allegra Cangelosi, NEMWI Lana Fanberg, LSRI, UWS Steve Hagedorn, LSRI, UWS Lindsey Krumrie, NEMWI Travis Mangan, NEMWI Nicole Mays, NEMWI Christine Polkinghorne, LSRI, UWS Kelsey Prihoda, LSRI, UWS Joe Radniecki, AMI Engineering Euan Reavie, PhD, NRRI, UMD Deanna Regan, LSRI, UWS Elaine Ruzycki, NRRI, UMD Heidi Saillard, LSRI, UWS Heidi Schaefer, LSRI, UWS Tyler Schwerdt, AMI Engineering Michael Stoolmiller, PhD, University of Oregon Matthew TenEyck, LSRI, UWS

2 Page 2 of 146 Technical Report: Land-Based Status Test of the JFE BallastAce Ballast Water Management System and Components at the GSI Testing Facility Date of issue of draft GSI findings: December 19, 2014 Date of issue of final report: May 13, 2015 X Approved for Release by: Ms. Allegra Cangelosi GSI Principal Investigator and Director Great Ships Initiative Northeast-Midwest Institute 50 F St. NW, Suite 950 Washington, DC acangelo@nemw.org X Approved for Release by: Mr. Shigeki Fujiwara Senior Researcher Water Treatment & Fluid Dynamics Research Group Research Center of Engineering Innovation JFE Engineering Corporation 2-1,Suehiro-cho, Tsurumi-ku, Yokohama, Japan mailto:fujiwara-shigeki@jfe-eng.co.jp

3 LIST OF ACRONYMS GSI/LB/QAQC/TR/JFE Page 3 of 146 %D: Percent Difference %T: Percent Transmittance µm: Micrometer BMDS: Ballast Management Discharge Standard BWMS: Ballast Water Management System CFU: Colony Forming Unit CV: Coefficient of Variation DBP: Disinfection Byproduct DI: Deionized DOC: Dissolved Organic Carbon DOM: Dissolved Organic Matter DSH: Duluth Superior Harbor ETV: Environmental Technology Verification FS: Filter System GLRI: Great Lakes Restoration Initiative GSI: Great Ships Initiative HMI: Human Machine Interface ID: Internal Diameter LAN: Local Area Network LSRI: Lake Superior Research Institute MARAD: United State Maritime Administration MM: Mineral Matter ND: No Data NEMWI: Northeast Midwest Institute NM: Not Measured NPOC: Non-Purgeable Organic Carbon NRRI: Natural Resources Research Institute PI: Principal Investigator PLC: Programmable Logic Controller POC: Particulate Organic Carbon POM: Particulate Organic Matter PSC: Percent Similarity QA: Quality Assurance QA/QC: Quality Assurance/Quality Control QAPP: Quality Assurance Project Plan QC: Quality Control RDTE: Research, Development, Testing, and Evaluation RPD: Relative Percent Difference SD: Secure Digital SEM: Standard Error of the Mean SOP: Standard Operating Procedure SP: Sample Port TOC: Total Organic Carbon TQAP: Test/Quality Assurance Plan TRC: Total Residual Chlorine TRO: Total Residual Oxidants TSS: Total Suspended Solids UMD: University of Minnesota-Duluth

4 USCG: United States Coast Guard USEPA: United States Environmental Protection Agency UV: Ultraviolet UWS: University of Wisconsin-Superior WET: Whole Effluent Toxicity YSI: Yellow Springs Instruments GSI/LB/QAQC/TR/JFE Page 4 of 146

5 EXECUTIVE SUMMARY GSI/LB/QAQC/TR/JFE Page 5 of 146 This Great Ships Initiative (GSI) technical report describes outcomes from freshwater, landbased, empirical status tests to support developer driven improvement of the JFE BallastAce Ballast Water Management System (BWMS). Tests took place at the GSI Land-Based Research, Development, Testing and Evaluation (RDTE) Facility (hereafter GSI Facility) located in the Duluth-Superior Harbor (DSH) of Lake Superior (Superior, Wisconsin, USA) during September and October 2014 and comprised three stages: 1. Operational and biological performance evaluation of three alternate filter systems (FSs) (hereafter JFE FS Intercomparison Test); 2. Evaluation of the operational, water chemistry/water quality and biological efficacy of three versions of the prototype JFE BallastAce BWMS; and 3. Durability testing of the F Panel FS (hereafter JFE F Panel Durability Test). All three sets of tests took place under controlled conditions. The JFE FS Intercomparison and BallastAce BWMS Status Test occurred in the context of challenge conditions stipulated in the United States Environmental Protection Agency (USEPA) Environmental Technology Verification (ETV) Program s Generic Protocol for the Verification of Ballast Water Treatment Technology, version 5.1 (USEPA, 2010), hereafter ETV Land-Based Protocol. The JFE F Panel Durability Test took place under ambient conditions. In the JFE FS Intercomparison Test, three alternative FS were evaluated: two candle-type FSs (referred to as the K Candle and F Candle, respectively), and the F Panel FS. Four test cycles comparing performance of the three FS were conducted at a rate of one comparative test cycle per day. In each test cycle, each FS was operated for the period of time necessary to process its nominal hourly capacity. Augmented DSH water was drawn through the GSI Facility at the developer-specified flow rate (varied by FS) with a target inlet pressure of 2 bar (29 psi) for a period of approximately one hour. Operational measurements included pre- and post-fs flow rate, backflush volume and rate, and differential pressure. Pre- and post-fs water quality and biological samples were also collected and analyzed. Results from this test indicate that the K Candle FS had higher differential pressure and more water lost to backflush than the F Candle and F Panel FSs, which performed similarly with respect to these parameters. However, the K Candle FS also removed solids most effectively (the F Candle and F Panel FSs performed similarly with respect to solids removal). With respect to organisms, in the 50 µm size class the three FSs performed similarly. The F Candle FS discharge had total densities ranging from 141,000/m 3 to 259,000/m 3, the K Candle FS discharge contained total densities of 8,860/m 3 314,152/m 3, and the F Panel FS discharge had total densities ranging from 41,700/m 3 to 238,000/m 3. Likewise, post-fs densities of organisms in the > 10 µm and < 50 µm size class ranged from 1,406 to 2,989 total cells/ml across test cycles and FSs. The JFE BallastAce BWMS Status Test evaluated the biological and chemical performance of three versions of the prototype JFE BallastAce BWMS against the U.S. Coast Guard (USCG) Ballast Water Discharge Standard (BWDS):

6 GSI/LB/QAQC/TR/JFE Page 6 of 146 The F Panel FS and injection of NEO-CHLOR DICD Granules at a target total residual oxidant (TRO) level of ~ 5 mg/l (3 test cycles); The F Panel FS and injection of TG BallastCleaner at a target TRO of ~ 5 mg/l (3 test cycles); and The F Panel FS and injection of TG BallastCleaner at a target TRO of ~ 20 mg/l (2 test cycles). For each test cycle, a single flow of DSH intake water, amended as needed to meet ETV requirements, was split with one half of the flow directed through the BWMS component combination (at a flow rate of 330 m 3 /hour for Test Cycles 1 6 and 200 m 3 /hour for Test Cycles 7 8) and into a treatment retention tank. The remaining flow was directed into a control retention tank. Following a two day retention period, the treated and untreated water was sequentially discharged. Pre-treatment intake, control discharge and treatment discharge flows were operationally tracked, and continuously sampled for later analysis of chemical and biological characteristics. Test cycles of the JFE BallastAce BWMS Status Test in which the BWMS was operated using NEO-CHLOR DICD Granules at a target TRO of ~ 5 mg/l (Test Cycles 1, 3, and 5) showed substantial reduction ( % relative to control) in discharge densities of live organisms in the 50 µm size class. Densities were still 37 to 50 times greater than the USCG BWDS, however. Live organism densities in the 10 µm and < 50 µm size class met the BWDS in two of the three test cycles. During Test Cycle 1, there were 197 live protist cells/ml, a difference likely related to a large colony of blue-green algae in one sample transect. On average, there was a 97 % reduction in total culturable heterotrophic bacteria in comparison to the control discharge. The concentrations of all classes of disinfection byproducts (DBPs) were elevated in the treatment discharge compared to the control discharge. The trihalomethanes had the highest concentration in treatment discharge, with an average of 214 µg/l in Test Cycle 1 and 155 µg/l in Test Cycle 5. In the two test cycles selected for whole effluent toxicity (WET) testing; Test Cycles 1 and 5, the only statistically significant (p<0.05) toxic effect was associated with reproduction in the 50 % and 100 % treatment groups of Test Cycle 1. Test cycles of the JFE BallastAce BWMS Status Test in which the BWMS was operated using TG BallastCleaner at a target TRO of ~ 5 mg/l, i.e., Test Cycles 2, 4, and 6, also showed substantial reduction (99.9 % compared to control) in densities of live organisms in the 50 µm size class. Live organism densities in treatment discharge for the 10 µm and < 50 µm size class met the BWDS for all three test cycles. On average, there was a 96 % reduction in total culturable heterotrophic bacteria in comparison to the control discharge. Again, there were elevated concentrations of all classes of DBPs measured in treatment discharge as compared to control discharge. The chlorate ion had the highest measured concentration in treatment discharge, with an average of 238 µg/l. The total trihalomethanes was the second highest class of DBPs, in terms of concentration in treatment discharge, with an average concentration of 147 µg/l. Test Cycle 4 was selected for WET testing; there was no statistically significant (p<0.05) toxic effect seen for any of the organisms tested. In Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test, the JFE BallastAce BWMS was operated using TG BallastCleaner as the active substance formulation at a higher target TRO

7 Page 7 of 146 (~ 20 mg/l). Discharge from both test cycles met the USCG BWDS for live organism densities in treatment discharge for the 50 µm, and 10 µm < 50 µm size classes. On average, there was a 99 % reduction in total culturable heterotrophic bacteria compared to the control discharge. There were substantially elevated concentrations of all classes of DBPs measured in the treatment discharge as compared to the control discharge, with the exception of the bromate ion. The chlorate ion had the highest measured concentration in treatment discharge, with an average of 1410 µg/l. The total trihalomethanes was the second highest class of DBPs, in terms of concentration in treatment discharge, with an average concentration of 459 µg/l. Test Cycle 7 was selected for WET testing; there was no statistically significant (p<0.05) effect seen for any of the organisms tested. The JFE F Panel Durability Test evaluated the operational performance of the F Panel FS over a single test cycle of 16 hours in duration (conducted over two, eight hour days) during a sea-tosea operation in which the BWMS programming was edited to run a backflush slightly more frequent than twice a minute. The number of backflushes during the test was the equivalent of two years of hypothetical normal BWMS operation on board a ship, according to developer estimates. After the test cycle was complete, the differential pressure between the inside and outside of the FS panel at the start and end of the cycle was compared. In addition, GSI personnel cleaned, dried, photographed and weighed the filter arm brush in order to quantify wear over time. The overall duration of the JFE F Panel Durability Test was hours over a two day period. During the test 2,705 m 3 of DSH water was filtered. The average differential pressure between the pre- and post-fs lines was 0.22 bar. The average post-treatment flow rate was 203 m 3 /hour, which was within 10 % of the target flow rate (i.e., 200 m 3 /hour). On average, the FS brushes weighed 4 mg less after completion of the JFE F Panel Durability Test, indicating that brush wear (as measured by weight loss) was minimal. Magnified images of randomly-selected FS brushes from each of the eight filter brush arms indicate that brush wear was not uniform over the entire length of the brush. However, even the areas of visible wear seemed relatively minimal and were limited to discoloration of the brush and fraying/bending of the brush hairs. Collectively, findings from the three sets of land-based tests GSI conducted of the various FS units and biocidal treatments proposed for use as part of the prototype BallastAce BWMS provide ample evidence to support developer driven improvement and development of the subject BWMS and its components.

8 ACKNOWLEDGMENTS GSI/LB/QAQC/TR/JFE Page 8 of 146 This series of tests was supported by the U.S. Environmental Protection Agency s (USEPA s) Great Lakes Restoration Initiative (GLRI) and the U.S. Maritime Administration. In addition, we thank the City of Superior, Wisconsin, for leasing us the land on which the GSI Facility is built. We also wish to acknowledge the administrative support of several academic and professional organizations at which GSI personnel are based. These include the Northeast-Midwest Institute, the University of Wisconsin Superior, the University of Minnesota Duluth, and AMI Consulting Engineers.

9 TABLE OF CONTENTS GSI/LB/QAQC/TR/JFE Page 9 of 146 LIST OF ACRONYMS... 3 EXECUTIVE SUMMARY... 5 ACKNOWLEDGMENTS... 8 TABLE OF CONTENTS... 9 LIST OF FIGURES LIST OF TABLES INTRODUCTION AND BACKGROUND The Testing Organization The Ballast Water Management System (BWMS) and Components JFE Intercomparison Test JFE BallastAce BWMS Status Test JFE F Panel Durability Test Roles and Responsibilities of Organizations Involved The Great Ships Initiative (GSI) Ballast Water Management System (BWMS) Developer Test Funders THE TESTING FACILITY METHODS Experimental Design Overview Challenge Conditions and Augmentation Methods Test Components and Measured Endpoints Data and Sample Collection and Analysis Methods Collection and Analysis of Operational Data Collection and Analysis of Water Chemistry/Water Quality Samples Collection and Analysis of Biological Samples Whole Effluent Toxicity (WET) and Disinfection Byproducts (DBPs) Data Processing, Storage, Verification and Validation RESULTS: JFE FILTER SYSTEM INTERCOMPARISON TEST Operational Performance... 45

10 Page 10 of Fuji Candle Filter (F Candle) Kanagawa Candle Filter (K Candle) Fuji Panel Filter (F Panel) Operational Filter Performance Comparison Solids Removal Performance and Water Quality Data Fuji Candle Filter (F Candle) Kanagawa Candle Filter (K Candle) Fuji Panel Filter (F Panel) Biological Performance Protists (Organisms 10 µm and < 50 µm) Zooplankton (Organisms 50 µm) Test Validity and Data Quality Objectives Test Validity Data Quality Indicators: Water Quality RESULTS: JFE BallastAce BALLAST WATER MANAGEMENT SYSTEM STATUS TEST Test Cycles 1, 3 and 5: F Panel Filter and NEO-CHLOR DICD BWMS Intake Measurements Retention Period Measurements Discharge Measurements Test Cycles 2, 4, and 6: F Panel and TG BallastCleaner (Low Dose) BWMS Combination Intake Measurements Retention Period Conditions Discharge Measurements Test Cycles 7 and 8: F Panel and TG BallastCleaner (High-Dose) BWMS Combination Intake Measurements Retention Period Conditions Discharge Measurements Test Validity RESULTS: JFE FUJI PANEL FILTER DURABILITY TEST Operational Data Filter Brush Arm Data

11 Page 11 of DISCUSSION CONCLUSION REFERENCES

12 LIST OF FIGURES GSI/LB/QAQC/TR/JFE Page 12 of 146 Figure 1. Location of GSI's Land-Based RDTE Facility in Superior, Wisconsin, USA Figure 2. Aerial Photo of the GSI Land-Based RDTE Facility (Source: Google Earth) Figure 3. Photo of the GSI Land-Based RDTE Facility Figure 4. Simplified Schematic of the GSI Land-Based RDTE Facility Showing Location of Sample Points, Sample Collection Tubs, Injection Points, Retention Tanks, and Treatment and Control Tracks Figure 5. Time-Dependent Operational Data from Test Cycle 3 of the JFE FS Intercomparison Test using the Candle Filter by Fuji Manufacturing Company, Ltd. (F Candle) Figure 6. Time-Dependent Operational Data from Test Cycle 3 of the JFE FS Intercomparison Test using the Candle Filter by Kanagawa Kiki Kogyo Company, Ltd. (K Candle) Figure 7. Time-Dependent Operational Data from Test Cycle 3 of the JFE FS Intercomparison Test using the Fuji Filter Manufacturing Company, Ltd. (F Panel) Figure 8. Comparison of the Average (± Standard Deviation) Differential Pressure Across Filter Types Measured During the Four Test Cycles of the JFE FS Intercomparison Test Figure 9. Comparison of the Average Ratio (%, ± Standard Deviation) of Backflush Flow Rate and Post- Treatment Flow Rate Measured Across Filter Types During the Four Test Cycles of the JFE FS Intercomparison Test Figure 10. Graph Depicting Average (± Standard Deviation) Pre- and Post-Filter Total Density of Protist Cells During Four Test Cycles of the JFE FS Intercomparison Test. Companion table shows average densities (pre- and post-filter) Figure 11. Graph Depicting Average (± Standard Error of the Mean, SEM) Pre- and Post-Filter Total Density of Macrozooplankton During Four Test Cycles of the JFE FS Intercomparison Test. Companion table shows average densities (pre- and post-filter) Figure 12. Graph Depicting Average (± Standard Error of the Mean, SEM) Pre- and Post-Filter Total Density of Microzooplankton During Four Test Cycles of the JFE FS Intercomparison Test. Companion table shows average densities (pre- and post-filter) Figure 13. Graph Depicting Average (± Standard Error of the Mean, SEM) Pre- and Post-Filter Total Density of Zooplankton (i.e., Microzooplankton plus Macrozooplankton) During Four Test Cycles of the JFE FS Intercomparison Test. Companion table shows average densities (pre- and post-filter) Figure 14. Real Time Pre- and Post-Filter Flow Rate and Pressure Data Recorded during Test Cycle 3 of the JFE BallastAce BWMS Status Test Figure 15. Real-Time Flow Rate and Pressure Data Measured Pre- and Post-Filter during Test Cycle 2 Intake of the JFE BallastAce BWMS Status Test Figure 16. Real-Time Pre- and Post-Filter Flow Rate and Pressure Data Measured During Test Cycle 8 Intake of the JFE BallastAce BWMS Status Test Figure 17. Magnified (10x) Photos of Filter Brush #1-4 Before (Left) and After (Right) the JFE F Panel Durability Test. Photos were taken in 11 sections in order to capture the entire brush

13 LIST OF TABLES GSI/LB/QAQC/TR/JFE Page 13 of 146 Table 1. Calendar for JFE FS Intercomparison Test (Four Test Cycles), BallastAce BWMS Status Test (Eight Test Cycles), and F Panel Durability Test (One Test Cycle). Note: Calendar does not incorporate the timing of analyses associated with each test cycle, which extended the test activities Table 2. Physical/Chemical and Biological Target Values for GSI Challenge Water Specific to the JFE FS Intercomparison and BallastAce BWMS Status Test Compared to Values in Ambient Duluth-Superior Harbor Water and Minimum Values Required by the ETV Protocol Table 3. The Order of Filter System Testing and Summary of Organism and Solids Injection Targets During Test Cycles 1-4 of the JFE FS Intercomparison Test Table 4. JFE BallastAce Ballast Water Management System (BWMS) Combinations Evaluated Over Eight Test Cycles during the BallastAce BWMS Status Test and Corresponding Target Flow Rates Table 5. Summary of Organism and Solids Injection Target Values Applicable to Test Cycles 1 8 of the JFE BallastAce BWMS Status Test Table 6. Operational, Water Chemistry/Quality, and Biological Data/Samples Collected per Filter System (FS) during each Test Cycle of the JFE FS Intercomparison Test Table 7. Operational, Water Chemistry/Quality, and Biological Data/Samples Collected during each Test Cycle of the JFE BallastAce Ballast Water Management System (BWMS) Status Test Table 8. Operational Data/Samples Collected during each Test Cycle of the JFE F Panel Durability Test. 44 Table 9. Test Cycles Selected for Whole Effluent Toxicity (WET) Testing and Associated Experimental Methods as Part of the JFE BallastAce Ballast Water Management System (BWMS) Status Test Table 10. Summary of Operational Measurements and Data Collected during the Four Test Cycles of the JFE FS Intercomparison Test using the Candle Filter by Fuji Manufacturing Company, Ltd. (F Candle) Table 11. Summary of Operational Measurements and Data Collected during the Four Test Cycles of the JFE FS Intercomparison Test using the Candle Filter by Kanagawa Kiki Kogyo Company, Ltd. (K Candle). 49 Table 12. Summary of Operational Measurements and Data Collected during the Four Test Cycles of the JFE FS Intercomparison Test using the Panel Filter by Fuji Filter Manufacturing Company, Ltd. (F Panel). NM = Not Measured Table 13. Summary of Water Quality Data and Solids Removal Performance of the Candle Filter by Fuji Manufacturing Company, Ltd. (F Candle) During the Four Test Cycles of the JFE FS Intercomparison Test Table 14. Summary of Water Quality Data and Solids Removal Performance of the Candle Filter by Kanagawa Kiki Kogyo Company, Ltd. (K Candle) During Four Test Cycles of the JFE FS Intercomparison Test Table 15. Summary of Water Quality Data and Solids Removal Performance of the Panel Filter by Fuji Filter Manufacturing Company, Ltd. (F Panel) During the Four Test Cycles of the JFE FS Intercomparison Test Table 16. Target Values and Results for GSI Challenge Water (Pre-Filter System) During JFE FS Intercomparison Test Table 17. Data Quality Objectives, Criteria, and Results from Water Quality Analyses during the JFE FS Intercomparison Test

14 Page 14 of 146 Table 18. Summary of Operational Measurements and Data Collected during Three Test Cycles (i.e., Test Cycles 1, 3, and 5) of the JFE BallastAce BWMS Status Test using NEO-CHLOR DICD Granules as the Active Substance. NM = Not Measured Table 19. Concentration of Total Residual Oxidants (TRO) in Grab Samples Collected Simultaneously from the Pre- and Post-Treatment Lines During Test Cycles 1, 3, and 5 Intake of the JFE BallastAce BWMS Status Test. N/A = Not Applicable. ND = Measured value was below the method detection limit Table 20. Average (± Standard Deviation, n=3) Concentration of Total Suspended Solids (TSS), Percent Transmittance (%T, in Filtered and Unfiltered Samples), Non-Purgeable Organic Carbon (NPOC), Dissolved Organic Carbon (DOC), Particulate Organic Carbon (POC), and Mineral Matter (MM) in Grab Samples Collected Simultaneously from the Pre- and Post-Treatment Line on Intake during Test Cycles 1, 3, and 5 of the of the JFE BallastAce BWMS Status Test Table 21. Average Value (±Standard Deviation, n=2) of Water Quality Parameters Measured from Pre- Treatment Sample Collection Tubs During Test Cycles 1, 3, and 5 Intake of the JFE BallastAce BWMS Status Test Table 22. Live Plankton Density (n=1 each) and Average (± Standard Deviation, n=3) Microbial Concentration in Challenge Water Samples Collected during Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test Table 23. Concentration of Total Residual Oxidants (TRO) in the Control and Treatment Retention Tanks 24 and 48 Hours after Intake during Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test Table 24. In-Situ Water Quality Parameters Measured in the Control and Treatment Retention Tanks during the 48 Hour Holding Time for Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test Table 25. Summary of Operational Measurements and Data Collected during Control Retention Tank Discharge for Test Cycles 1, 3, and 5 of the BallastAce BWMS Status Test using NEO-CHLOR DICD Granules as the Active Substance Table 26. Summary of Operational Measurements and Data Collected during Treatment Retention Tank Discharge for Test Cycles 1, 3, and 5 of the BallastAce BWMS Status Test using NEO-CHLOR DICD Granules as the Active Substance Table 27. Concentration of Total Residual Oxidants (TRO) in Grab Samples Collected During Test Cycles 1, 3, and 5 Control and Treatment Tank Discharge Operations of the JFE BallastAce BWMS Status Test. ND = Measured value was below the method detection limit Table 28. Average (± Standard Deviation, n=3) Concentration of Total Suspended Solids (TSS), Percent Transmittance (%T, in Filtered and Unfiltered Samples), Non-Purgeable Organic Carbon (NPOC), Dissolved Organic Carbon (DOC), Particulate Organic Carbon (POC), and Mineral Matter (MM) in Grab Samples Collected Sequentially from the Treatment and Control Line on Discharge during the JFE BallastAce BWMS Status Test Table 29. Water Quality Parameters Measured in Control (Sample Collection Tub #s 1 and 2) and Treatment (Sample Collection Tub #s 4-6) Sample Collection Tubs Immediately Following Discharge Operations during Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test Table 30. Live Plankton Density (Average ± Standard Deviation, Where Applicable) and Average (± Standard Deviation, n=3) Microbial Concentrations in Samples Collected During Control and Treatment Retention Tank Discharge for Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test

15 Page 15 of 146 Table 31. Results from Analysis of Selected Disinfection Byproducts in Samples Collected during Discharge of the Control and Treatment Retention Tanks in Test Cycles 1 and 5 of the JFE BallastAce BWMS Status Test. Samples were collected for analysis of disinfection byproducts only for those test cycles with Whole Effluent Toxicity testing Table 32. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Stock Solutions during Ceriodaphnia dubia and Pimephales promelas Whole Effluent Toxicity (WET) Test Associated with Test Cycle 1 of the JFE BallastAce BWMS Status Test Table 33. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Seven Day Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Test Cycle 1 of the JFE BallastAce BWMS Status Test Table 34. Average (n=10) Percent Survival and Total Number of Offspring Produced in a Three-Brood Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Treatment Discharge from Test Cycle 1 of the JFE BallastAce BWMS Status Test Table 35. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Pimephales promelas Whole Effluent Toxicity (WET) Test Associated with Test Cycle 1 of the JFE BallastAce BWMS Status Test Table 36. Pimephales promelas Average (n=4) Percent Survival and Weight per Fish after Exposure to Treatment Discharge from Test Cycle 1 of the JFE BallastAce BWMS Status Test Table 37. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Selenastrum capricornutum Whole Effluent Toxicity (WET) Test Associated with Test Cycle 1 of the JFE BallastAce BWMS Status Test Table 38. Average (n=4) Cell Density of Selenastrum capricornutum after 96 Hours Exposure to Whole Effluent from Test Cycle 1 Treatment Discharge of the JFE BallastAce BWMS Status Test Table 39. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Stock Solutions during the Ceriodaphnia dubia and Pimephales promelas Whole Effluent Toxicity (WET) Tests Associated with Test Cycle 5 of the JFE BallastAce BWMS Status Test Table 40. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Six Day Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Test Cycle 5 of the JFE BallastAce BWMS Status Test Table 41. Average (n=10) Percent Survival and Total Number of Offspring Produced in a Three-Brood Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Treatment Discharge from Test Cycle 5 of the JFE BallastAce BWMS Status Test Table 42. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Pimephales promelas Whole Effluent Toxicity (WET) Test Associated with Test Cycle 5 of the JFE BallastAce BWMS Status Test Table 43. Pimephales promelas Average (n=4) Percent Survival and Weight per Fish after Exposure to Treatment Discharge from Test Cycle 5 of the JFE BallastAce BWMS Status Test Table 44. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Selenastrum capricornutum Whole Effluent Toxicity (WET) Test Associated with Test Cycle 5 of the JFE BallastAce BWMS Status Test

16 Page 16 of 146 Table 45. Average (n=4) Cell Density of Selenastrum capricornutum after 96 Hours Exposure to Whole Effluent from Test Cycle 5 Treatment Discharge of the JFE BallastAce BWMS Status Test Table 46. Summary of Operational Measurements and Data Collected during Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test using TG BallastCleaner as the Active Substance (Low Dose/High Flow) Table 47. Concentration of Total Residual Oxidants (TRO) in Measured Grab Samples Collected Simultaneously from the Pre- and Post-Treatment Lines During Test Cycles 2, 4, and 6 Intake of the JFE BallastAce BWMS Status Test. N/A = Not Applicable. ND = Measured value was below the method detection limit Table 48. Average (± Standard Deviation, n=3) Concentration of Total Suspended Solids (TSS), Percent Transmittance (%T, in Filtered and Unfiltered Samples), Non-Purgeable Organic Carbon (NPOC), Dissolved Organic Carbon (DOC), Particulate Organic Carbon (POC), and Mineral Matter (MM) Measured in Grab Samples Collected Simultaneously from the Pre- and Post-Treatment Line on Intake During Test Cycles 2, 4, and 6 Intake of the JFE BallastAce BWMS Status Test Table 49. Average Value (±Standard Deviation, n=2) of Water Quality Parameters Measured in Pre- Treatment Sample Collection Tubs During Test Cycles 2, 4, and 6 Intake of the JFE BallastAce BWMS Status Test Table 50. Live Plankton Densities (n=1 each) and Average (± Standard Deviation, n=3) Microbial Concentration in Challenge Water Samples Collected During Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test Table 51. Concentration of Total Residual Oxidants (TRO) in the Control and Treatment Retention Tanks 24 and 48 Hours Post-Treatment during Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test. ND = Measured value was below the method detection limit Table 52. Water Quality Parameters Measured In-Situ in the Control and Treatment Retention Tanks during the 48 Hour Holding Period for Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test Table 53. Summary of Operational Measurements and Data Collected during Control Retention Tank Discharge for Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test using TG BallastCleaner as the Active Substance Table 54. Summary of Operational Measurements and Data Collected during Treatment Retention Tank Discharge for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test using TG BallastCleaner as the Active Substance Table 55. Concentration of Total Residual Oxidants (TRO) Measured in Grab Samples Collected During Test Cycles 2, 4, and 6 Control and Treatment Tank Discharge Operations Associated with the JFE BallastAce BWMS Status Test. ND = Measured value was below the method detection limit Table 56. Average (± Standard Deviation, n=3) Concentration of Total Suspended Solids (TSS), Percent Transmittance (%T, in Filtered and Unfiltered Samples), Non-Purgeable Organic Carbon (NPOC), Dissolved Organic Carbon (DOC), Particulate Organic Carbon (POC), and Mineral Matter (MM) in Grab Samples Collected Sequentially from the Treatment and Control Line on Discharge Associated with Test Cycles 2, 4 and 6 of the JFE BallastAce BWMS Status Test

17 Page 17 of 146 Table 57. Average (± Standard Deviation) Water Quality Parameters Measured in Sample Collection Tubs Immediately Following Control and Treatment Discharge Operations for Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test Table 58. Live Plankton Density (Average ± Standard Deviation, Where Applicable) and Average (± Standard Deviation, n=3) Microbial Concentrations in Samples Collected During Control and Treatment Retention Tank Discharge for Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test Table 59. Results from Analysis of Selected Disinfection Byproducts in Samples Collected during Discharge of the Control and Treatment Retention Tanks in Test Cycle 4 of the JFE BallastAce Status Test Table 61. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Stock Solutions during the Ceriodaphnia dubia and Pimephales promelas Whole Effluent Toxicity (WET) Tests Associated with Test Cycle 4 of the JFE BallastAce BWMS Status Test Table 61. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Six Day Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Test Cycle 4 of the JFE BallastAce BWMS Status Test Table 62. Average (n=10) Percent Survival and Total Number of Offspring Produced in the Three-Brood Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Treatment Discharge from Test Cycle 4 of the JFE BallastAce BWMS Status Test Table 63. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Pimephales promelas Whole Effluent Toxicity (WET) Test Associated with Test Cycle 4 of the JFE BallastAce BWMS Status Test Table 64. Pimephales promelas Average (n=4) Percent Survival and Weight per Fish after Exposure to Treatment Discharge from Test Cycle 4 of the JFE BallastAce BWMS Status Test Table 65. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Selenastrum capricornutum Whole Effluent Toxicity (WET) Test Associated with Test Cycle 4 of the JFE BallastAce BWMS Status Test Table 66. Average (n=4) Cell Density of Selenastrum capricornutum after 96 Hours Exposure to Whole Effluent from Test Cycle 4 Treatment Discharge of the JFE BallastAce BWMS Status Test Table 67. Summary of Operational Measurements and Data Collected during Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test using TG BallastCleaner as the Active Substance (High Dose/Low Flow) Table 68. Concentration of Total Residual Oxidants (TRO) and Total Residual Chlorine (TRC) Measured in Grab Samples Collected Simultaneously from the Pre- and Post-Treatment Lines During Test Cycles 7 and 8 Intake of the JFE BallastAce BWMS Status Test. N/A = Not Applicable. ND = Measured value was below the method detection limit Table 69. Average (± Standard Deviation, n=3) Concentration of Total Suspended Solids (TSS), Percent Transmittance (%T, in Filtered and Unfiltered Samples), Non-Purgeable Organic Carbon (NPOC), Dissolved Organic Carbon (DOC), Particulate Organic Carbon (POC), and Mineral Matter (MM) Measured in Grab Samples Collected Simultaneously from the Pre- and Post-Treatment Line on Intake During Test Cycles 7 and 8 Intake of the JFE BallastAce BWMS Status Test

18 Page 18 of 146 Table 70. Average Value (± Standard Deviation, n=2)of Various Water Quality Parameters Measured in the Pre-Treatment Sample Collection Tubs During Test Cycles 7 and 8 Intake of the JFE BallastAce BWMS Status Test Table 71. Live Plankton Density (n=1 each) and Average (± Standard Deviation, n=3) Microbial Concentration in Challenge Water Samples Collected During Test Cycles 7 and 8 8 of the JFE BallastAce BWMS Status Test. Values marked with an asterisk (*) did not meet TQAP requirements Table 72. Concentration of Total Residual Oxidants (TRO) and Total Residual Chlorine (TRC) in the Control and Treatment Retention Tanks 24 and 48 Hours Post-Treatment During Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test. ND = Measured value was below the method detection limit. 122 Table 73. Average (± Standard Deviation) Water Quality Parameters Measured in the Control and Treatment Retention Tanks during the 48 Hour Retention Period for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test Table 74. Summary of Operational Measurements and Data Collected during Control Retention Tank Discharge for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test using TG BallastCleaner as the Active Substance (High Dose/Low Flow) Table 75. Summary of Operational Measurements and Data Collected during Treatment Retention Tank Discharge for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test using TG BallastCleaner as the Active Substance (High Dose/Low Flow) Table 76. Concentration of Total Residual Oxidants (TRO) and Total Residual Chlorine (TRC) Measured in Grab Samples Collected During Test Cycles 7 and 8 Control and Treatment Tank Discharge Operations Associated with the JFE BallastAce BWMS Status Test. ND = Measured value was below the method detection limit Table 77. Average (± Standard Deviation, n=3) Concentration of Total Suspended Solids (TSS), Percent Transmittance (%T, in Filtered and Unfiltered Samples), Non-Purgeable Organic Carbon (NPOC), Dissolved Organic Carbon (DOC), Particulate Organic Carbon (POC), and Mineral Matter (MM) in Grab Samples Collected during Discharge of the Control and Treatment Retention Tanks for Status Test Cycles 7 and 8 Associated with Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test Table 78. Average (± Standard Deviation) Water Quality Parameters Measured in the Control and Treatment Sample Collection Tubs Immediately Following Control and Treatment Discharge Operations for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test Table 79. Live Plankton Density (Average ± Standard Deviation, Where Applicable) and Average (± Standard Deviation, n=3) Microbial Concentrations in Samples Collected During Control and Treatment Retention Tank Discharge for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test Table 80. Results from Analysis of Selected Disinfection Byproducts (DBPs) in Samples Collected during Discharge of the Control and Treatment Retention Tanks in Test Cycle 7 of the JFE BallastAce BWMS Status Test Table 81. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Stock Solutions during the Ceriodaphnia dubia and Pimephales promelas Whole Effluent Toxicity (WET) Tests Associated with Test Cycle 7 of the JFE BallastAce BWMS Status Test

19 Page 19 of 146 Table 82. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Six Day Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Test Cycle 7 of the JFE BallastAce BWMS Status Test Table 83. Average (n=10) Percent Survival and Total Number of Offspring Produced in the Three-Brood Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Treatment Discharge from Test Cycle 7 of the JFE BallastAce BWMS Status Test Table 84. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Pimephales promelas Whole Effluent Toxicity (WET) Test Associated with Test Cycle 7 of the JFE BallastAce BWMS Status Test Table 85. Pimephales promelas Average (n=4) Percent Survival and Weight per Fish after Exposure to Treatment Discharge from Test Cycle 7 of the JFE BallastAce BWMS Status Test Table 86. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Selenastrum capricornutum Whole Effluent Toxicity (WET) Test Associated with Test Cycle 7 of the JFE BallastAce BWMS Status Test Table 87. Average (n=4) Cell Density of Selenastrum capricornutum after 96 Hours Exposure to Whole Effluent from Test Cycle 7 Treatment Discharge of the JFE BallastAce BWMS Status Test Table 88. Target Values and Results for GSI Challenge Water During JFE BallastAce Ballast Water Management Status Test Table 89. Summary of Operational Data Collected during the Two Day JFE Fuji Panel Filter Durability Test Table 90. Weights of Filter Brushes Installed in Filter Brush Arms of the Fuji Panel Filter Before and After the JFE F Panel Durability Test

20 Page 20 of INTRODUCTION AND BACKGROUND This Great Ships Initiative (GSI) technical report presents findings from empirical land-based status tests in freshwater to support developer driven improvement of the JFE BallastAce Ballast Water Management System (BWMS). Three sets of tests were undertaken in September and October of 2014 at the GSI Land-Based Research, Development, Testing and Evaluation (RDTE) Facility, hereafter GSI Facility, located in the Duluth-Superior Harbor (DSH) of Lake Superior (Superior, Wisconsin, USA). The first set of tests (hereafter JFE FS Intercomparison Test) evaluated operational and biological performance of three filter system (FS) alternatives. The second set of tests evaluated operational, water chemistry/water quality, and biological performance of the prototype JFE BallastAce BWMS comprising a Fuji Panel (F Panel) FS combined with two formulations (liquid or granular) of a biocidal treatment (hereafter JFE BallastAce BWMS Status Test). The third and final set of tests involved a durability test of the F Panel FS in which operational performance was evaluated (hereafter JFE F Panel Durability Test). 1.1 The Testing Organization The testing organization, GSI, is a regional research initiative managed by the Northeast- Midwest Institute (NEMWI) devoted to ending the problem of ship-mediated invasive species in the Great Lakes-St. Lawrence Seaway System and globally. Since its establishment in 2006, GSI has provided independent performance/verification testing services to developers of BWMSs at the bench, land-based and shipboard scales. GSI performs informal status tests for systems that are in the research and development stage and formal certification/verification tests appropriate to market-ready BWMSs. NEMWI, GSI s managing entity, is a Washington, D.C-based private, non-profit, and nonpartisan research organization dedicated to the economic vitality, environmental quality, and regional equity of Northeast and Midwest states. The NEMWI directly collaborates with contracting entities, including the University of Wisconsin-Superior s (UWS s) Lake Superior Research Institute (LSRI), the University of Minnesota-Duluth (UMD s) Natural Resources Research Institute (NRRI), the University of Oregon, and AMI Consulting Engineers, to achieve GSI testing and research objectives. 1.2 The Ballast Water Management System (BWMS) and Components JFE Intercomparison Test The JFE FS Intercomparison Test involved generation of operational and biological performance information on three alternate FSs for subsequent developer evaluation. All three FSs have received type approval from the Japanese government. Specifics of the FSs are as follows:

21 Page 21 of Candle-Type Filter (K Candle) manufactured by Kanagawa Kiki Kogyo Co., Ltd. Hereafter referred to as the K Candle, this FS utilizes a notch-wire element which is manufactured by wrapping specially treated thin stainless steel wire with notches around the cylindrical FS frame. The nominal width of opening between notch wires is 50 µm. Inlet water is directed into the cylindrical FS frame and filtered water exits the outside of the frame. A backwash arm set in the bottom of the FS operates continuously and washes the filter elements using 7 % of the filtered water. When the differential pressure between the inside and outside of filter element increases to 50 kpa, intermittent backwash mode operates with 15 % of the filtered water. 2. Candle-Type Filter (F Candle) manufactured by Fuji Filter Manufacturing Co., Ltd. Hereafter referred to as the F Candle, this FS utilizes cylindrical sintered mesh with no internal frame. The nominal length of opening is 50 µm. Inlet water enters from inside of a cylinder and filtered water is discharged from the outside of the cylinder. When the differential pressure increases to 25 kpa, a backwash arm moves and the intermittent washing operation starts using 15 % of the filtered water. 3. Panel-Type Filter (F Panel) manufactured by Fuji Filter Manufacturing Co., Ltd. Hereafter referred to as the F Panel, this FS utilizes a square shaped panel made from the same sintered mesh as the two candle type FSs noted above. The nominal length of the opening is 50 µm. Two panels are set parallel and inlet water flows between the two panels and filtered water is discharged out of the panels. A backwash arm moved by an air cylinder is set between the two panels and it moves when the differential pressure increases to 25 kpa and washes all surface area of the panels with 15 % of filtered water JFE BallastAce BWMS Status Test The JFE BallastAce BWMS Status Test involved evaluation of the performance (i.e., operational, water chemistry/water quality, and biological efficacy) of the prototype JFE BallastAce BWMS comprising the F Panel FS, detailed above, combined with two formulations (liquid or granular) of a biocidal treatment, and one biocidal treatment (liquid) at two injection doses. The JFE BallastAce BWMS is a proprietary BWMS. During the JFE BallastAce BWMS Status Test, GSI tested an early prototype of the BWMS that was still under development and did not include all of the features of the planned commercially-available BWMS (e.g., the version that was tested included manual calculation of active substance/neutralizer dosing and was not automated). According to JFE Engineering, the commercially-available unit will consist of a FS, two chemical agents (i.e., a chlorine agent and a reducing agent), and Venturi tubes or a mixing plate. The market-ready JFE BallastAce BWMS is intended to operate as follows: 1. During a ballast uptake operation, the water passes through the FS, after a strainer. This operation is designed to remove most of the plankton and particulate substances larger

22 Page 22 of 146 than about 50 µm. These organisms and particles are then be discharged back into the original source water together with the backwash water. Because a chlorine agent is injected after the filtration process, the FS backwash water target is no chlorine, and no impact on the receiving environment. 2. The chlorine agent is injected into the water after filtration to react primarily with dissolved organic and inorganic matter, and act on the plankton and bacteria which have passed through the FS. This water then passesthrough the Venturi tubes or mixing plate for integration to maximize exposure of the plankton and bacteria to the chlorine agent. JFE plans to offer customers the option of using either a liquid type chlorine agent (i.e., TG BallastCleaner with the main ingredient of sodium hypochlorite) or a granular type chlorine agent (i.e., NEO-CHLOR DICD Granules, EPA Reg. No with the main ingredient of sodium dichloroisocyanurate dihydrate, DICD). 3. When the ballast water is discharged, an aqueous solution of sodium sulfite is injected into the treated ballast water to completely neutralize the chlorine in the ballast water. The neutralized/detoxified water is then discharged from the ship into the ambient water JFE F Panel Durability Test The JFE F Panel Durability Test involved evaluation of the F Panel FS component (described above in section 1.2.1) of the JFE BallastAce BWMS. 1.3 Roles and Responsibilities of Organizations Involved Roles and responsibilities for these GSI freshwater, land-based, empirical status tests were shared among GSI, the BWMS developer, and GSI funders The Great Ships Initiative (GSI) GSI was responsible for developing the Test/Quality Assurance Plan (TQAP; GSI, 2014) and subjecting the document to review by the BWMS developer prior to testing. GSI prepared and maintained the testing facility, organized the testing schedule, monitored source water conditions, supervised BWMS and component installations, supported BWMS developer commissioning exercises, and monitored the BWMS developer while they operated specific components of the BWMS. GSI was responsible for all sample collection, and sample analysis. In addition, GSI was responsible for assuring data quality, and evaluating and reporting on the performance data, maintaining security for testing activities, and assuring site safety for all personnel. Finally, GSI was responsible for subjecting the data and data analysis to BWMS developer review, and meeting as many requests as possible within the bounds of scientific and process constraints prior to publication Ballast Water Management System (BWMS) Developer The BWMS developer, JFE Engineering, was responsible for the delivery of the subject BWMS and components to the GSI Facility, for providing instructions to the GSI Engineers for proper installation of the units at the facility, for designating the installation requirements and operating conditions for the BWMS and components during the evaluations (including line pressure, flow

23 Page 23 of 146 rate, startup and shutdown procedures), and for signing off on successful commissioning outcomes. Representatives of the BWMS developer were onsite during the entire test period and operated the BWMS and components during the status test, including active substance and neutralizer dosing Test Funders This project was supported by funds from the U.S. Environmental Protection Agency s (USEPA s) Great Lakes Restoration Initiative (GLRI), and the U.S. Maritime Administration. Tests took place on land owned by the City of Superior, Wisconsin. 2 THE TESTING FACILITY Tests of the JFE BallastAce BWMS and components took place at the GSI Land-Based RDTE Facility located in the DSH of Lake Superior (Figures 1-3). Relevant features of the GSI Facility include: Control and treatment intake flows up to 340 m 3 /hour each; Highly automated flow and pressure control, monitoring and data logging; A freshwater estuary with diverse and plentiful aquatic life as a challenge water intake source (during normal testing season May to October); Capacity to amend intake challenge water to intensify challenge conditions; Validated facility sanitation before and between test cycles; High quality in-line sampling systems associated with identical 3.8 m 3 sample collection tubs; On-site laboratory space for most live analyses, additional space minutes away; and Easy plug-in connections for BWMSs.

24 Page 24 of 146 Facility Location Figure 1. Location of GSI's Land-Based RDTE Facility in Superior, Wisconsin, USA. (Source: Google Earth). Figure 2. Aerial Photo of the GSI Land-Based RDTE Facility (Source: Google Earth).

25 Page 25 of 146 Figure 3. Photo of the GSI Land-Based RDTE Facility. The GSI Facility draws challenge water from the DSH, generally at a flow rate between m 3 /hr. This main intake flow can be augmented with solids (i.e., total suspended solids, TSS) and/or organisms (i.e., protists) at injection points A and B (Figure 4). A Y-split in the facility intake piping, just after a static mixer, simultaneously channels one half of the well-mixed flow to a treatment track and the other half to a matched control track. Thus, the facility delivers a specified flow rate in the treatment and control tracks in the range of m 3 /hour each. The treatment track directs water through a subject BWMS prior to discharging water to a 200 m 3 cylindrical retention tank, or to the harbor (Figure 4). The flow can be toggled between two installed BWMSs. Flow control valves and control system logic assure that sample flow rates are equivalent and proportional to intake and discharge flow rates throughout each operation. Flow rates are recorded by magnetic flux flow meters. Pressure readings are also recorded using pressure transducers located at multiple points throughout the facility. GSI measures and records these data, and other operational and maintenance parameters, using the facility s Programmable Logic Controller (PLC). This information is accessible by a Human Machine Interface (HMI). The HMI has a 38.1 cm color touch display and is capable of detailing valve positions, pressure from the pressure meters, and flow rates. The PLC reads, and a separate data logging computer records and saves data from all the limit switches, positioners, pressure sensors, flow meters and level indicators every five seconds for the entire duration of the operational cycle. Challenge water quality/chemistry is also monitored and recorded in the same manner using in-line temperature/ph, dissolved oxygen, turbidity and chlorophyll a sensors installed in the main piping system just prior to the BWMS.

26 Page 26 of 146 Sample water for biological analysis is generally collected continuously throughout each intake and discharge operation via several of the facility s in-line sample points (SPs). Samples for water quality/chemistry analysis are also collected from designated SPs during intake, tank retention and discharge. All SPs, with the exception of SP#15, consist of three identical sample ports spaced at regular intervals in a length of straight pipe (SP#15 consists of one sample port). Each port is fitted with a center-located elbow-shaped tube (90 o ) which samples the water. This design is based on a design developed and validated analytically by the U.S. Naval Research Laboratory in Key West, Florida (Richard et al., 2008). The design and lay-out of these replicate sample ports has also been validated empirically at GSI and shown to produce equivalent, representative and unbiased samples of water flow. On-site laboratories (Figure 4) support time sensitive analyses associated with GSI land-based tests, including live analysis of organisms 50 µm (i.e., zooplankton) and organisms 10 and < 50 µm (i.e., protists). The laboratories are climate-controlled, and have enough bench space to allow for simultaneous analysis of samples by multiple personnel. All other analyses are conducted in laboratories of LSRI on the UWS campus; approximately 5 km from the facility.

27 Page 27 of 146 Figure 4. Simplified Schematic of the GSI Land-Based RDTE Facility Showing Location of Sample Points, Sample Collection Tubs, Injection Points, Retention Tanks, and Treatment and Control Tracks.

28 3 METHODS GSI/LB/QAQC/TR/JFE Page 28 of Experimental Design Overview In total, the JFE FS Intercomparison Test, the BallastAce BWMS Status Test, and the F Panel Durability Test consisted of eight weeks of test operations, including FS and BWMS installation and commissioning (Table 1). The JFE FS Intercomparison Test took place September 2014 and comprised four test cycles (Table 1). The BallastAce BWMS Status Tests took place 15 September to 29 October 2014 and comprised eight test cycles (Table 1). The F Panel Durability Test took place October 2014 and comprised a single test cycle (Table 1). All three sets of tests took place at the GSI Facility in Superior, Wisconsin, under semi-controlled conditions and, for the JFE FS Intercomparison and BallastAce BWMS Status Test, in the context of challenge conditions stipulated in the U.S. Environmental Protection Agency (USEPA) Environmental Technology Verification (ETV) Program s Generic Protocol for the Verification of Ballast Water Treatment Technology, version 5.1 (USEPA, 2010). Table 1. Calendar for JFE FS Intercomparison Test (Four Test Cycles), BallastAce BWMS Status Test (Eight Test Cycles), and F Panel Durability Test (One Test Cycle). Note: Calendar does not incorporate the timing of analyses associated with each test cycle, which extended the test activities. Week # (Start Date) 1 (08 SEPT 2014) 2 (15 SEPT 2014) 3 (22 SEPT 2014) 4 (29 SEPT 2014) 5 (06 OCT 2014) 6 (13 OCT 2014) 7 (20 OCT 2014) 8 (27 OCT 2014) Monday Tuesday Wednesday Thursday Friday Saturday Sunday Ballast Water Management System and Components Installation and Commissioning FS Intercomparison BallastAce BWMS Status Test: Test Cycle 1 Test: Test Cycle 1 FS FS Intercomparison FS Intercomparison Intercomparison Test: Test Cycle Test: Test Cycle 4 Test: Test Cycle 2 3 BallastAce BWMS Status Test: Test Cycle 2 BallastAce BWMS Status Test: Test Cycle 3 BallastAce BWMS Status Test: Test Cycle 4 BallastAce BWMS Status Test: Test Cycle 5 BallastAce BWMS Status Test: Test Cycle 6 BallastAce BWMS Status Test: Test Cycle 8 F Panel Durability Test: Test Cycle 1 BallastAce BWMS Status Test: Test Cycle 7

29 3.1.2 Challenge Conditions and Augmentation Methods GSI/LB/QAQC/TR/JFE Page 29 of 146 All three sets of tests took place under semi-controlled conditions using source water obtained from the DSH and, for the JFE FS Intercomparison and BallastAce BWMS Status Test, in the context of challenge conditions stipulated in the ETV Program s Generic Protocol for the Verification of Ballast Water Treatment Technology, version 5.1 (USEPA, 2010). Table 2 presents target values for GSI challenge water specific to the JFE FS Intercomparison and BallastAce BWMS Status Test. Though GSI s ambient water source naturally meets many of the requirements of the ETV Protocol, to assure challenge water met the requirements listed in Table 2, GSI augmented intake water, as needed, to meet TSS minimum requirements using ISO , A2 Arizona Fine Test Dust (Powder Technology, Inc.; Burnsville, Minnesota). GSI also augmented intake water, as needed, to meet particulate organic carbon (POC) requirements using Micromate (i.e., micronized humate product for liquid suspension; Mesa Verde Resources; Placitas, New Mexico). Micromate also contributed to the total TSS concentration, while mineral matter (MM), defined as the difference between TSS and POC, was augmented indirectly through the TSS and POC augmentation. Depending on the concentration of ambient organisms 10 µm and < 50 µm, i.e., protists, in the DSH, GSI augmented intake water relative to this size class in order to meet the minimum target value detailed in Table 2. The specific injection procedure for TSS, Micromate and protists is detailed in GSI/SOP/LB/G/O/5 Procedure for Injecting Organisms and Solids into the GSI Land-Based RDTE Facility. For the JFE FS Intercomparison Test, this GSI Standard Operating Procedure (SOP) was followed for TSS and POC augmentation, though for protist augmentation the amount of concentrated protists collected from the DSH was evenly divided in proportion to expected flow through volume between the three FSs operated during each test cycle.

30 Page 30 of 146 Table 2. Physical/Chemical and Biological Target Values for GSI Challenge Water Specific to the JFE FS Intercomparison and BallastAce BWMS Status Test Compared to Values in Ambient Duluth-Superior Harbor Water and Minimum Values Required by the ETV Protocol. Parameter Target Values for JFE FS Intercomparison Test and BallastAce BWMS Status Test* Ambient Duluth-Superior Harbor (June September) ETV Generic Protocol (v. 5.1; USEPA, 2010) Temperature ( C) Salinity (ppt) < 1 < 1 < 1 for fresh water Percent (%) Transmittance Not applicable None specified Total Suspended Solids (TSS) (mg/l) Particulate Organic Matter (POM) as Particulate Organic Carbon (POC) (mg/l) Dissolved Organic Matter (DOM) as Dissolved Organic Carbon (DOC) (mg/l) > 24 1 < 1 40 Min. 24 > 4 1 < Min. 4 > Min. 6 Mineral Matter (MM) (mg/l) > 20 1 < 1-40 Min. 20 Organisms 50 µm > 100,000/m 3 100,000-3,000,000 > 100,000/m 3 (at least 5 species present across 3 phyla) Organisms 10 µm and < 50 µm > 1,000/mL ,000 > 1,000/mL (at least 5 species present across 3 phyla) Organisms < 10 µm > 1,000 MPN/mL > 500 MPN/mL > 1,000/mL (as culturable aerobic heterotrophic bacteria) * The inability to meet the target values did not invalidate a test cycle. 1 Concentrations were augmented, as needed, to achieve target values Test Components and Measured Endpoints JFE FS Intercomparison Test The JFE FS Intercomparison Test involved operation of the three alternate FSs proposed for use as part of the prototype BallastAce BWMS, i.e., the K Candle, F Candle, and F Panel FSs. Following successful installation and commissioning, the three FSs were evaluated for differential pressure (based on the difference between pre- and post-fs line pressure) and backflush water loss (based on the difference between pre- and post-fs flow rate), two parameters which help define the operational cost of running a FS as part of a BWMS and affect the ship compatibility. The three FSs were also evaluated for solids removal performance, based on the difference between pre- and post-fs TSS and POC concentrations. The FSs were assessed one at a time over the course of four test cycles (a test cycle was defined as one day of testing). The three FSs were operated once per day for a total of four runs each. A

31 Page 31 of 146 run was defined as the time each FS took to process its own nominal hourly capacity. JFE Engineering proposed that the target volume be based on the maximum flow capacity of each FS. The nominal maximum flow rate of each FS was as follows: K Candle = 360 m 3 /hour F Candle = 346 m 3 /hour F Panel = 360 m 3 /hour JFE Engineering requested that all FS testing be conducted with a target inlet pressure of 2 bar (29 psi). Due to this pressure restriction the nominal flow through rates of the FSs could not be reached with enough downstream pressure to sample reliably. The planned target flow rates were amended in order to accommodate the pressure restriction, yet still produce consistent flow control and sampling. Correspondingly, the amended target flow rates used during the JFE FS Intercomparison Test were as follows: K Candle = 308 m 3 /hour F Candle = 311 m 3 /hour F Panel = 311 m 3 /hour Table 3 summarizes the randomly-selected order of testing for each FS within a test cycle, whether organism injection was conducted, and the target concentration of Fine Test Dust and Micromate injected during each of the four test cycles. During Test Cycles 1 and 2, a single experimental mass of augmented DSH water (amended as needed to meet ETV threshold requirements) was drawn through the GSI Facility via a sea-to-sea operation, at the above specified flow rates with a target inlet pressure of 2 bar, for a period of approximately one hour. Due to a failure of the organism diaphragm injection pump at the GSI Facility, the DSH water was augmented with solids only during Test Cycles 3 and 4 (Table 3). For all four test cycles, Micromate was used to increase the POC concentration, which also increased the TSS concentration of the DSH water (Table 3). For Test Cycles 1 and 2 no addition of Fine Test Dust was needed because the TSS was increased above ETV threshold requirements using Micromate alone (Table 3). For Test Cycles 3 and 4, Fine Test Dust was needed (Table 3).

32 Page 32 of 146 Table 3. The Order of Filter System Testing and Summary of Organism and Solids Injection Targets During Test Cycles 1-4 of the JFE FS Intercomparison Test. Parameter Randomly-Selected Order of Testing Organism Injection? (YES/NO) Solids Injection: Target Additional Fine Test Dust (mg/l) Solids Injection: Target Additional Micromate (mg/l) Filter System Test Cycle 1 Test Cycle 2 Test Cycle 3 Test Cycle 4 F Candle K Candle F Panel ALL YES YES NO NO F Candle K Candle F Panel F Candle K Candle F Panel During the course of the FS runs, GSI personnel monitored the following operational parameters through the use of automated systems: differential pressure, flow rate, inlet and outlet pressure, and FS backflush volume and frequency. Maintenance or operational issues observed by GSI personnel relative to the three FSs were also documented. In addition, samples for analysis of pre- and post-fs water chemistry and biological parameters were collected and analyzed. Water chemistry endpoints comprised pre- and post-fs concentrations of TSS, percent transmittance (%T), dissolved organic carbon (DOC), and POC. Biological endpoints comprised: pre- and post-fs densities of total organisms 50 µm in preserved samples, and total organisms 10 µm and < 50 µm in preserved samples JFE BallastAce BWMS Status Test The JFE BallastAce BWMS Status Test involved evaluation of two combinations of the prototype JFE BallastAce BWMS (comprising one FS and two formulations of a secondary biocidal treatment) over eight test cycles (Table 4). All test cycles utilized the F Panel FS (Table 4). Test Cycles 1, 3, and 5 utilized NEO-CHLOR DICD granules at a target concentration of ~5 mg/l total residual oxidants (TRO) and a flow rate of 311 m 3 /hour (Table 4). Test Cycles 2, 4, and 6 utilized liquid TG BallastCleaner at a target concentration of ~5 mg/l TRO and a flow rate of 311 m 3 /hour (i.e., low dose/high flow; Table 4). Test Cycles 7 and 8 utilized TG BallastCleaner at a target TRO concentration of ~20 mg/l and a flow rate of 200 m 3 /hour (i.e., high dose/low flow; Table 4).

33 Page 33 of 146 Table 4. JFE BallastAce Ballast Water Management System (BWMS) Combinations Evaluated Over Eight Test Cycles during the BallastAce BWMS Status Test and Corresponding Target Flow Rates. * Indicates Disinfection Byproduct (DBP) and Whole Effluent Toxicity (WET) Analysis took place. Week # (Start Date) 2 (15 SEPT 2014) 4 (29 SEPT 2014) 4 (29 SEPT 2014) 5 (06 OCT 2014) 5 (06 OCT 2014) 6 (13 OCT 2014) 7 (20 OCT 2014) 8 (27 OCT 2014) Test Cycle # Target Flow Rate (m 3 /hour) Test Cycle 1* 311 F Panel Filter System Test Cycle F Panel Filter System Test Cycle F Panel Filter System Test Cycle 4* 311 F Panel Filter System Test Cycle 5* 311 F Panel Filter System Test Cycle F Panel Filter System Test Cycle 7* 200 F Panel Filter System Test Cycle F Panel Filter System BallastAce BWMS Combination NEO-CHLOR DICD (granules): Target Concentration ~5 mg/l TG BallastCleaner (liquid): Target Concentration ~5 mg/l NEO-CHLOR DICD (granules): Target Concentration ~5 mg/l TG BallastCleaner (liquid): Target Concentration ~5 mg/l NEO-CHLOR DICD (granules): Target Concentration ~5 mg/l TG BallastCleaner (liquid): Target Concentration ~5 mg/l TG BallastCleaner (liquid): Target Concentration ~20 mg/l TG BallastCleaner (liquid): Target Concentration ~20 mg/l All eight test cycles involved intake water, sourced from the DSH at a flow rate of up to 720 m 3 /hour and a pressure of 2 bar, amended as needed to meet ETV threshold requirements (Table 5), and split into two halves. One half of the flow was directed through the specific BWMS combination and into a treatment retention tank at a flow rate of 311 m 3 /hour for Test Cycles 1 6, and 200 m 3 /hour for Test Cycles 7 8, to achieve the higher target dose of active substance injection (Table 4). The other half of the flow was directed into a control retention tank. Following a two day retention period, the treated and untreated water was sequentially discharged. The treated water was discharged, following in-line neutralization, to the GSI Facility s wastewater tank 1. The untreated control water was discharged to the DSH. The duration of each intake and discharge operation was dependent upon the frequency of the FS backflush, but was approximately 33 minutes during Test Cycles 1-6 and approximately 60 minutes during Test Cycles 7 and 8. Pre-treatment intake, as well as control discharge and treatment discharge water was sampled and characterized for operational, water chemistry/water quality, and biological characteristics. GSI personnel monitored the same operational parameters, through the use of automated systems, as per the JFE FS Intercomparison Test, as well as operational parameters associated with the GSI Facility, including retention tank and sample collection tub volumes. 1 Treated discharge was held in the GSI Facility wastewater retention tank and tested for complete neutralization prior to discharge to the city sewer or back to the DSH, depending upon the active substance formulation utilized.

34 Page 34 of 146 Table 5. Summary of Organism and Solids Injection Target Values Applicable to Test Cycles 1 8 of the JFE BallastAce BWMS Status Test. Parameter Test Cycle 1* Test Cycle 2 Test Cycle 3 Test Cycle 4 Test Cycle 5 Test Cycle 6 Test Cycle 7 Test Cycle 8 Organism Injection? (YES/NO) YES, Target = 1,500 cells/ml Solids Injection: Target Additional Fine Test Dust (mg/l) Solids Injection: Recording Target Additional Error** Micromate (mg/l) *Due to operator error, the ambient DSH TSS concentration was not factored into the solids injection calculations and solids (Fine Test Dust) were overdosed. **Due to a recording error, the concentration of micromate added is not known. As part of the JFE BallastAce BWMS Status Test, four sets of whole effluent toxicity (WET) tests were conducted to determine the potential for residual toxicity of the treated discharge water. Specifically WET tests were conducted during Test Cycles 1 and 5 (i.e., when the BWMS combination utilized the granular active substance NEO-CHLOR DICD; Table 4), one WET test was conducted during Test Cycle 4 (i.e., when the BWMS combination utilized the liquid active substance TG BallastCleaner at a low dose; Table 4), and one WET test was conducted during Test Cycle 7 (i.e., when the BWMS utilized the liquid active substance TG BallastCleaner at a higher dose; Table 4). Samples for analysis of disinfection byproducts (DBPs) were also collected in association with the four test cycles in which WET was assessed. Overall, operational endpoints relative to the JFE BallastAce BWMS Status Test comprised differential pressure, flow rate, inlet and outlet pressure, FS backflush volume and frequency, sample collection tub flow rate and volume, and retention tank volume. Water chemistry endpoints measured from pre-treatment intake, and control and treatment discharge comprised concentrations of TRO, total residual chlorine (TRC), TSS, DOC, POC, and calculation of MM. Biological endpoints, measured from pre-treatment intake, and control and treatment discharge, comprised live densities of organisms 50 µm; total densities of organisms 50 µm (treatment discharge samples only); live densities of organisms 10 µm and < 50 µm; and densities of organisms < 10 µm, i.e., total culturable heterotrophic bacteria per colony forming units (CFUs) JFE F Panel Durability Test The JFE F Panel Durability Test evaluated the operational performance of an F Panel FS over a single test cycle of 16 hours duration (conducted over two, eight hour days; Table 1). During this test the flow rate was set to 200 m 3 /hour and the pressure to 2 bar. Non-amended DSH water was directed through the GSI Facility via a sea-to-sea operation and the FS s backflush mechanism was triggered every 30 seconds. The number of backflushes was the equivalent of two years of hypothetical BWMS operation on board a ship. After the test cycle was complete, the differential pressure between the inside and outside of the FS panel at the start and end of each 8 hour session was compared. Operational endpoints comprised differential pressure, flow rate, inlet and outlet pressure, FS backflush volume and frequency. Following the test, debris was rinsed from

35 Page 35 of 146 the filter brush bristles by gently hand washing each brush individually with filtered municipal water and then allowing the brushes to air dry. The cleaned and dried filter brushes were weighed on two consecutive days, and GSI compared the weight of the FS backflush brushes before and after the 16 hour test in order to quantify wear over time. Photographs of the filter brushes before and after the test were also taken. In addition, one filter brush from each of the eight filter brush arms was randomly selected for magnified photography before and after the test. 3.2 Data and Sample Collection and Analysis Methods Tables 6-8 summarize operational data, and water chemistry/water quality and biological samples collected and analyzed during the JFE FS Intercomparison Test, BallastAce BWMS Status Test, and F Panel Durability Test, respectively Collection and Analysis of Operational Data Operational data was collected continuously throughout each test cycle associated with the JFE FS Intercomparison Test, BallastAce BWMS Status Test, and F Panel Durability Test (Tables 6-8, respectively). Data was recorded by the GSI Facility s data logging computer, including data from the limit switches, positioners, pressure sensors, flow meters and level indicators. Magnetic flux flow meters (accurate to ± 2 % of reading, according to GSI s operational best practices) located on the facility s control track, treatment track, and on the discharge line measured intake and discharge flow rates. Pressure transducers located at multiple points throughout the facility measured line pressure. Following completion of each test cycle, the data was transferred to a Microsoft Excel file for subsequent analysis by GSI personnel Collection and Analysis of Water Chemistry/Water Quality Samples Water Chemistry Samples for analysis of water chemistry were collected relative to the JFE FS Intercomparison Test and BallastAce BWMS Status Test as detailed in Tables 6-7, respectively. Samples for analysis of TSS and %T were collected following the procedure outlined in GSI/SOP/LB/RA/SC/2 Procedure for Collecting Water Chemistry Samples and Data. TSS analysis was conducted according to GSI/SOP/BS/RA/C/8 Procedure for Analyzing Total Suspended Solids (TSS), Particulate Organic Matter (POM), and Mineral Matter (MM). %T analysis was conducted according to GSI/SOP/BS/RA/C/4 Procedure for Determining Percent Transmittance (%T) of Light in Water at 254 nm. Samples for analysis of DOC, used as a surrogate measure for dissolved organic matter (DOM), and POC, used as a surrogate measure for particulate organic matter (POM) and calculated as the difference between Non-Purgeable Organic Carbon (NPOC) and DOC values for a given sample, were collected consistent with the procedure outlined in GSI/SOP/LB/RA/SC/2 Procedure for Collecting Water Chemistry Samples and Data. In these tests, NPOC was used as a proxy for total organic carbon (TOC), though it may be a slight underestimate of TOC as the analytical instrument used to measure NPOC purges the sample with air to remove inorganic carbon before

36 Page 36 of 146 measuring organic carbon levels in the sample. Thus, NPOC analysis may not incorporate volatile organic carbon which may be present in the sample. Sample analysis for DOC and NPOC was conducted according to GSI/SOP/BS/RA/C/3 Procedures for Measuring Organic Carbon in Aqueous Samples except that samples were sonicated for at least 15 minutes then placed on a stir plate for manual injection into the Shimadzu Total Organic Carbon Analyzer. This modification to the analytical procedure was deemed necessary to accurately measure all of the NPOC in the samples that had been augmented. MM, defined as the difference between TSS and POM (measured as POC), was calculated for a given sample following analysis of TSS and the determination of POC based on the NPOC and DOC concentrations as described above. For analysis of TRO and TRC, applicable to the JFE BallastAce BWMS Test (Table 7), discrete grab samples were collected consistent with the procedure outlined in GSI/SOP/LB/RA/SC/2 Procedure for Collecting Water Chemistry Samples and Data. TRO and TRC analysis took place on samples as soon as possible after collection (i.e., analysis was conducted on site at the GSI Facility within five minutes of collection) to avoid sample degradation and minimize loss of chlorine due to reaction with oxidizable species in the sample. Measurements accounted for all forms of chlorine, i.e., free chlorine, hypochlorites, and chlorine bound to nitrogenous compounds. TRO analysis was conducted during Test Cycles 1-8 of the BallastAce BWMS Status Test according to GSI/SOP/BS/RA/C/2 Procedure for Determining Total Residual Oxidants (TRO) in Water. Briefly, a TRO calibration curve was prepared using standards prepared in deionized water utilizing a 65.7 mg/l chlorine stock solution. The standards, ranging in concentration from 0.50 to 4.0 mg/l, were analyzed in the same manner as described for the samples. For analysis of post-treatment intake samples from Test Cycles 7 and 8, samples were diluted, as needed, so that the calibration curve bracketed the measured sample concentration. For all samples, 10 ml aliquots of sample water (diluted as needed in Test Cycles 7 and 8) were transferred from the sample containers into 30 ml beakers. The contents of a Hach DPD Total Chlorine Reagent packet were added to each sample. The absorbance of the sample was determined using a Spectronic 20D set at a wavelength of 515 nm. The absorbance of an aliquot of each sample with no reagent added was also measured and the absorbance value subtracted from that of the sample containing the reagent in order to correct for the background absorbance of each sample. TRC analysis was conducted during Test Cycles 1 8 of the BallastAce BWMS Status Test according to GSI/SOP/BS/RA/C/6 Procedure for Analyzing Total Residual Chlorine (TRC) Concentrations in Water. Briefly, a 1,000 mg/l iodate stock solution (1,000 mg/l as chlorine) was used to prepare analytical standards, ranging in concentration from to 10.0 mg/l daily. For Test Cycles 7 and 8, a 20.0 mg/l TRC standard was added to the calibration curve in order to bracket the expected post-treatment intake concentrations. The standards were prepared in deionized water by making dilutions of the 1,000 mg/l iodate stock. Potassium iodide reagent and acetate buffer were added to the iodate containing analytical standards. For Test Cycles 7 and 8, the standards were analyzed at the same temperature as the samples (± 3 C) by storing the deionized water, iodate stock, potassium iodide reagent, and acetate buffer in a refrigerator prior to preparation. Iodate or chlorine present in the standards or samples oxidizes iodide to iodine in an acidic solution. The iodine concentration after the reaction will be equal to the iodate or chlorine concentration present before the reaction. A calibration curve plotting log of the

37 Page 37 of 146 chlorine concentration (x-axis) versus the mv response from the Residual Chlorine Electrode (yaxis) was used to determine TRC concentrations in the samples. For all sample analysis, 100 ml of sample water was transferred from the sample collection container into a 150 ml beaker, and 1.0 ml of potassium iodide reagent and 1.0 ml of acetate buffer reagent added. Analysis was conducted with a Thermo Scientific Orion Model 9770BNWP Residual Chlorine Electrode connected to an Orion Star A211 ph/ ISE/mV/ Temperature meter. In addition, a dilution of the samples was made as necessary to ensure that all samples were within the range of the calibration curve. Note: TRC results from Test Cycles 1 6 of the BallastAce BWMS Status Test will not be reported, as the temperature of the standards during analysis most likely caused the TRC concentration of the samples to be artificially high (i.e., approximately twice the expected concentration) Water Quality Specific to the BallastAce BWMS Status Test only (Table 7), water quality parameters, including temperature, dissolved oxygen, ph, turbidity, salinity, specific conductivity, and total chlorophyll, were measured using Multiparameter Sondes (YSI 6600 V2-4 Multiparameter Sondes; YSI Incorporated; Yellow Springs, Ohio) consistent with the procedure outlined in GSI/SOP/LB/RA/SC/2 Procedure for Collecting Water Chemistry Samples and Data. Measurement data were recorded on GSI/FORM/LB/C/4 - Sample Collection Tub Water Chemistry Data Collection Form, as well as internally by the Sonde. The data from the continuous measurements were exported to Microsoft Excel for subsequent analysis following completion of each test cycle. The Sondes probes were rinsed with deionized water prior to sampling, as well as calibrated prior to each test cycle according to GSI/SOP/MS/G/C/1 - Procedure for Calibration, Deployment, and Storage of YSI Multiparameter Water Quality Sondes Collection and Analysis of Biological Samples Samples for analysis of organisms were collected relative to the JFE FS Intercomparison Test and BallastAce BWMS Status Test as detailed in Tables 6-7, respectively. Specifically, samples for analysis of organisms 50 µm were collected and handled as described in GSI/SOP/LB/RA/SC/6 - Procedure for Zooplankton Sample Collection. Briefly, sample water was drawn through the relevant sample ports installed at the GSI Facility and directed into replicate 3.8 m 3 sample collection tubs via clean 3.8 cm internal diameter (ID) flexible hoses and automated flow-controlled pneumatic diaphragm valves. The water was then filtered through 35 m plankton nets and the retained organisms collected and transferred to a 1 L sample bottle. For samples collected in association with the JFE FS Intercomparison Test, the organisms were then preserved and analyzed using a modification of GSI/SOP/MS/RA/SA/2 Procedure for Zooplankton Sample Analysis. For these preserved samples, the sample volume was adjusted to ensure that there were organisms present in a single 1 ml subsample (i.e., macrozooplankton and microzooplankton were analyzed on the same slide), the entire slide was examined counting all the zooplankton present, and this procedure was repeated three times for a total of three replicate slides per sample. For samples collected in association with the BallastAce BWMS Status Test, analysis took place in accordance with GSI/SOP/MS/RA/SA/2 - Procedure for Zooplankton Sample Analysis.

38 Page 38 of 146 Samples for analysis of organisms 10 and < 50 µm were collected according to GSI/SOP/LB/RA/SC/7 - Procedure for Protist and Microbial Sample Collection Using Seep Samplers. Briefly, sample water was directed into replicate, 19 L plastic carboys via a tube branching off the main line of each sample port. A 1 L sample was then collected from each carboy and the sample, in the case of the JFE FS Intercomparison Test, preserved within 1.5 hours of sample collection by adding 10 ml Lugol s solution to the sample and mixing well by inverting several times. Preserved samples were analyzed as soon as possible following receipt of the samples by the protist taxonomists. Only those cells with intact cellular contents were counted and presumed to have been alive at the time of sample collection. In the case of samples collected in association with the BallastAce BWMS Status Test, samples were not preserved. Analysis took place according to GSI/SOP/MS/RA/SA/1 - Procedure for Protist Sample Analysis. Samples for analysis of organisms < 10 µm were collected according to GSI/SOP/LB/RA/SC/7 - Procedure for Protist and Microbial Sample Collection Using Seep Samplers. To quantify culturable, aerobic, heterotrophic bacteria, GSI analysts followed procedures detailed in GSI/SOP/BS/RA/MA/7 Procedure for Quantifying Heterotrophic Plate Counts (HPC) Using the Spread Plate Method Whole Effluent Toxicity (WET) and Disinfection Byproducts (DBPs) GSI analyzed treatment discharge samples for WET relative to Test Cycles 1, 4, 5, and 7 of the BallastAce BWMS Status Test following standard USEPA freshwater WET test methods (USEPA, 2002; Table 7). Three freshwater species were used as test organisms: the cladoceran Ceriodaphnia dubia, the fathead minnow Pimephales promelas and the green alga Selenastrum capricornutum. Samples were collected and analyzed according to the following SOPs: GSI/SOP/BS/RA/WET/1 - Procedure for Assessing Chronic Residual Toxicity of a Ballast Treatment System to Ceriodaphnia dubia; GSI/SOP/BS/RA/WET/2 - Procedure for Assessing Chronic Residual Toxicity of a Ballast Treatment System to the Fathead Minnow (Pimephales promelas), and GSI/SOP/BS/RA/WET/3 - Procedure for Assessing Chronic Residual Toxicity of a Ballast Treatment System to the Green Alga (Selenastrum capricornutum. A standard dilution series was utilized for treated and neutralized whole effluent (i.e., 0 %, 6.25 %, 12.5 %, 25 %, 50 %, and 100 %). For Test Cycles 4, 5, and 7 a Facility Control was also utilized. The Facility Control was whole effluent collected following discharge of the control retention tank, and was used to determine if the GSI Facility was a contributing factor to any toxicity resulting from the treated and neutralized discharge. In addition, commercially-purchased C. dubia were used for WET tests conducted during Test Cycles 4, 5, and 7 (Table 9). C. dubia cultured in-house were used during Test Cycle 1 (Table 9). Table 9 summarizes the experimental methods associated with each of the four sets of WET tests. Samples for analysis of DBPs were collected during the test cycles of the BallastAce BWMS Status Test that also involved analysis of WET (i.e., Test Cycles 1, 4, 5, and 7; Table 7). Samples for analysis of DBPs were stored in coolers on ice as soon as possible after collection, and subsequently transferred to the appropriate sample containers by a GSI Chemist. The samples were then preserved, based on the appropriate method, and shipped cold to ALS Environmental (Middletown, Pennsylvania) for analysis of the following DBPs: trihalomethanes, haloacetic acids, haloacetonitriles (sub-contracted; analysis conducted by Weck Laboratories, Inc.; City of Industry, California), sodium chlorate, sodium bromate, and total sodium.

39 Page 39 of 146 Table 6. Operational, Water Chemistry/Quality, and Biological Data/Samples Collected per Filter System (FS) during each Test Cycle of the JFE FS Intercomparison Test. Treatment Harbor Water (Pre-Test) Pre-Filter System Filter Systems Post-Filter System Analysis Category Water Chemistry Operational Water Chemistry Biology Operational Water Chemistry Biology Parameter Total Suspended Solids (TSS) Particulate Organic Carbon (POC) Flow Rate Pressure Total Suspended Solids (TSS) and Percent Transmittance (%T) Dissolved Organic Carbon (DOC) and Particulate Organic Carbon (POC) Sample Type Number of Samples Discrete Grab 1 Sample Volume 0.9 L - 1 L ml In-Line, Continuous Discrete Grab Discrete Grab 3 (Beginning, Middle, End*) 3 (Beginning, Middle, End*) Organisms 50 µm 1 Time-Integrated 1 3 m 3 ± 5 % Organisms 10 µm to < 50 µm 1 Backflush Volume Backflush Frequency Total Suspended Solids (TSS) and Percent Transmittance (%T) Dissolved Organic Carbon (DOC) and Particulate Organic Carbon (POC) Time-Integrated; 19 L Carboy GSI Facility: Sample Location SP#2c Various Locations Throughout Facility 0.9 L - 1 L SP#3c 100 ml -125 ml SP#3c L - 1 L Sample Collection Tub #4 via SP#3a and Tub #5 via SP#3b (as backup) Carboy via SP#3a and SP#3b (as backup) In-Line, Continuous Filter System Discrete Grab 3 (Beginning, Middle, End*) 3 (Beginning, Middle, End*) 0.9 L 1 L 100 ml -125 ml Organisms 50 µm 1 Time-Integrated 1 3 m 3 ± 5 % SP#10c Sample Collection Tub #3 via SP#10a and Tub #2 via SP#10b (as backup) Organisms 10 µm to < 50 µm 1 Time-Integrated; 19 L Carboy L 1 L Carboy via SP#10a and via SP#10b 1 Samples were preserved for analysis at a later date. *During Test Cycle 4 using the K Candle Filter, only the beginning and middle samples were collected; the duration of the test was reduced because of a very high backflush rate that caused backflush water to flood the GSI Facility during the test.

40 Page 40 of 146 Table 7. Operational, Water Chemistry/Quality, and Biological Data/Samples Collected during each Test Cycle of the JFE BallastAce Ballast Water Management System (BWMS) Status Test. Operation Treatment Harbor Water (Pre-Test) Analysis Category Water Chemistry Parameter Total Suspended Solids (TSS) Particulate Organic Carbon (POC) Sample Type Biology Organisms 10 µm to < 50 µm Discrete Grab Operational Flow Rate Inlet /outlet Pressure Retention Tank Volume Sample Collection Tub Volume Number of Samples Discrete Grab 1 In-Line, Continuous Calculated Based on Flow Rate Sample Volume 0.9 L - 1 L ml GSI Facility: Sample Location SP#2c L 1 L SP#2c 2 (1 per pond) ~50 ml Algae Pond #1 and # Various Locations Throughout Facility Water Quality Temperature, Dissolved Oxygen, ph, Turbidity, Salinity, Specific Conductivity, Total Chlorophyll Discrete (Sample Collection Tub) L 0.6 L Sample Collection Tub #4 and #5 Intake Pre-BWMS Water Chemistry Biology Total Residual Oxidants (TRO) and Total Residual Chlorine (TRC) Total Suspended Solids (TSS) and Percent Transmittance (%T) Dissolved Organic Carbon (DOC) and Particulate Organic Carbon (POC) Discrete Grab Discrete Grab Discrete Grab 4 (1, 3, 10, and 30 min.) for Test Cycle (TC) 1-6; 5 (1, 3, 10, 30, and 55 min.) for TC7 and 8 3 (Beginning, Middle, End) 3 (Beginning, Middle, End) 0.9 L 1 L SP#3c 0.9 L - 1 L 100 ml -125 ml Organisms 50 µm Time-Integrated 1 3 m 3 ± 5 % Organisms 10 µm to < 50 µm Time-Integrated; 19 L Carboy L -1 L SP#3c Sample Collection Tub #4 via SP#3a (Tub #5 via SP#3b used as backup) Carboy via SP#3a (Carboy via SP#3b used as backup)

41 Operation Discharge Treatment BWMS Post-BWMS Retention BWMS GSI Facility Treatment Discharge Analysis Category Operational/ Water Chemistry Water Chemistry Water Quality Water Chemistry Operational/ Water Chemistry Operational Water Chemistry/ Water Quality Parameter Organisms < 10 µm (Total Culturable Heterotrophic Bacteria) TRO Concentration Chemical Injection Flow Rate Ballast Water Flow Rate Differential Pressure Total Residual Oxidants (TRO) and Total Residual Chlorine (TRC) Total Suspended Solids (TSS), and Percent Transmittance (%T) Dissolved Organic Carbon (DOC) and Particulate Organic Carbon (POC) Temperature, Dissolved Oxygen, ph, Turbidity, Salinity, Specific Conductivity, Total Chlorophyll Total Residual Oxidants (TRO) and Total Residual Chlorine (TRC) TRO Concentration Ballast Water Flow Rate Flow Rate Pressure Retention Tank Volume Sample Collection Tub Volume Temperature, Dissolved Oxygen, ph, Turbidity, Salinity, Specific Conductivity, Total Chlorophyll Sample Type Time-Integrated; 19 L Carboy In-Line, Continuous Discrete Grab Continuous Measurement Discrete Grab In-Line, Continuous In-Line, Continuous Calculated Based on Flow Rate Discrete Measurement (Sample Collection Tub) Number of Samples 3 GSI/LB/QAQC/TR/JFE Page 41 of 146 Sample GSI Facility: Sample Location Volume BWMS 4 (1, 3, 10, and 30 min.) for TC1-6; 5 (1, 3, 10, 30, and 55 min.) for TC7 and 8 3 (beginning, middle and end) 3 (beginning, middle and end) Data logged every 15 minutes 2 (24 and 48 hours) 0.9 L 1 L SP# L 1 L SP# ml 125 ml N/A Measurement 0.9 L 1 L SP#15 Control and Treatment Tanks BWMS Various Locations Throughout Facility L 1 L Sample Collection Tubs #4, #5, and #6

42 Operation Treatment Control Discharge Analysis Category Biology Water Chemistry/ Water Quality Parameter Total Residual Oxidants (TRO) and Total Residual Chlorine (TRC) Total Suspended Solids (TSS) and Percent Transmittance (%T) Dissolved Organic Carbon (DOC) and Particulate Organic Carbon (POC) Disinfection Byproducts 3 : Test Cycles 1, 4, 5, and 7 Whole Effluent Toxicity (WET): Test Cycles 1, 4, 5, and 7 Sample Type Discrete Grab Discrete Grab Discrete Grab Discrete Grab Number of Samples 4 (1, 3, 10, and 25 min.) for TC1-6; 5 (1, 3, 10, 30, and 50 min.) for TC7 and 8 3 (Beginning, Middle, End) 3 (Beginning, Middle, End) 3 (Beginning, Middle, End) Time-Integrated 2 Organisms 50 µm Time-Integrated 1 Organisms 10 µm to < 50 µm Organisms < 10 µm (Total Culturable Heterotrophic Bacteria) Temperature, Dissolved Oxygen, ph, Turbidity, Salinity, Specific Conductivity, Total Chlorophyll Time-Integrated; 19 L Carboy Time-Integrated; 19 L Carboy Discrete Measurement (Sample Collection Tub) 3 GSI/LB/QAQC/TR/JFE Page 42 of 146 Sample GSI Facility: Sample Location Volume 0.9 L 1 L 0.9 L 1 L 100 ml -125 ml L 2, 19 L Carboys (38 L total) 6 m 3 ± 5 % (2 tubs with 3 m 3 /tub) 0.9 L -1 L; Composite 3 Reps L - 1 L SP#15 Sample Collection Tub #6 via SP #10a Sample Collection Tub #4 & #5 via SP#10c/b (Sample Collection Tub #6 via SP#10a used as a backup) Carboys via SP#10c/b/a L 1 L Sample Collection Tub #1 and #2 Total Suspended Solids (TSS) and 3 (Beginning, Discrete Grab 0.9 L 1 L SP#9a Percent Transmittance (%T) Middle, End) Dissolved Organic Carbon (DOC) 3 (Beginning, 100 ml -125 and Particulate Organic Carbon Discrete Grab SP#9a Middle, End) ml (POC) Total Residual Oxidants (TRO) and Discrete Grab 4 (1, 3, 10, and 0.9 L 1 L SP#9a

43 Operation Treatment After Treatment Discharge: Wastewater Tank (Test Cycle 1) After Treatment Discharge: Wastewater Tank (Test Cycles 1-8) Analysis Category Biology Water Quality/ Water Chemistry Water Quality/ Water Chemistry Parameter Total Residual Chlorine (TRC) Whole Effluent Toxicity (Facility Control): Test Cycles 4, 5, and 7 Disinfection Byproducts 3 : Test Cycles 1, 4, 5, and 7 Sample Type Number of Samples 30 min.) for TC1-6; 5 (1, 3, 10, 30, and 55 min.) for TC7 and 8 Time-Integrated 1 19 L Discrete Grab 3 (Beginning, Middle, End) Organisms 50 µm Time-Integrated 1 3 m 3 ± 5 % Organisms 10 µm to < 50 µm Organisms < 10 µm (Total Culturable Heterotrophic Bacteria) Evaluation of BWMS Impact on City of Superior Wastewater Treatment Facility* 1 Time-Integrated; 19 L Carboy Time-Integrated; 19 L Carboy 1 3 GSI/LB/QAQC/TR/JFE Page 43 of 146 Sample GSI Facility: Sample Location Volume Sample Collection Tub #2 via SP9b L SP#9a 0.9 L - 1 L Biochemical Oxygen Demand, Discrete Grab Total Suspended Solids, L 1 L Phosphorous, and ph* 2 Sample Collection Tub #1 via SP#9c (Sample Collection Tub #2 via SP#9b used as a backup) Carboy via SP#9c (Carboy via SP#9b used as a backup) L 1 L Wastewater Tank N/A - ph will be measured in ph* 1 the TSS Discrete Grab sample. Total Residual Chlorine (TRC)* L 1 L Total Suspended Solids (TSS)* L 1 L *Samples collected to meet state and/or city permitting requirements. 1 Analyzed by staff at the City of Superior Wastewater Treatment Facility. 2 Analyzed by Era Laboratories (Duluth, MN). 3 Analyzed by ALS Environmental (Middletown, PA). Discharge Monitoring Sample Point from Wastewater Storage Tank Discharge Wastewater Tank Prior to Discharge

44 Page 44 of 146 Table 8. Operational Data/Samples Collected during each Test Cycle of the JFE F Panel Durability Test. Treatment During Sea-to- Sea Operation Analysis Category GSI Facility Parameter Flow Rate Pressure Sample Type Number of Samples Sample Volume Sample Location In-Line, Continuous Various Locations Throughout Facility Pre- and Post- Test Filter Condition Filter Element Surface Damage Filter Brush Arm Weight Photograph Dry Weight (to nearest 1g) 1 Photograph per Test Session 4 (2 before and 2 after test) N/A N/A Filter element removed and photographed using a camera connected to a dissecting microscope N/A Table 9. Test Cycles Selected for Whole Effluent Toxicity (WET) Testing and Associated Experimental Methods as Part of the JFE BallastAce Ballast Water Management System (BWMS) Status Test. Test Cycle 1 (Granular #1) 4 (Liquid; Low Dose/High Flow) 5 (Granular #2) 7 (Liquid; High Dose/Low Flow Performance Control Facility Control? Ceriodaphnia dubia YES, per GSI SOPs NO CULTURED YES, per GSI SOPs YES, per GSI SOPs YES, changed C. dubia performance control water (PCW) to Moderately-Hard Water YES YES YES PURCHASED (Environmental Consulting & Testing, Inc.; Superior, WI) PURCHASED (Environmental Consulting & Testing, Inc.; Superior, WI) PURCHASED (Environmental Consulting & Testing, Inc.; Superior, WI) Test Species: Cultured or Purchased? Pimephales promelas PURCHASED (Environmental Consulting & Testing, Inc.; Superior, WI) PURCHASED (Environmental Consulting & Testing, Inc.; Superior, WI) PURCHASED (Environmental Consulting & Testing, Inc.; Superior, WI) PURCHASED (Environmental Consulting & Testing, Inc.; Superior, WI) Selenastrum capricornutum CULTURED CULTURED CULTURED CULUTRED Comments High suspended solids concentration in effluent due to operator error prior to intake operation. Purchased C. dubia were cultured in moderately-hard reconstituted water; PCW was hard reconstituted water. Purchased C. dubia were cultured in moderately-hard reconstituted water; PCW was hard reconstituted water. No comments.

45 3.3 Data Processing, Storage, Verification and Validation GSI/LB/QAQC/TR/JFE Page 45 of 146 GSI personnel recorded sample collection and analysis data by hand (using indelible ink) on preprinted data collection forms and/or in bound laboratory notebooks that were uniquely-identified and specific to the JFE BallastAce BWMS and components tests. The GSI Engineer recorded relevant information and data generated from operation of the JFE BallastAce BWMS and components in a bound laboratory notebook that was uniquely-identified (i.e., coded) and specific to the series of three tests. Completed data collection forms were secured in uniquely-identified three ring binders, specific to the JFE BallastAce BWMS and components tests. Biological and water chemistry data that were recorded by hand were manually entered into either a Microsoft Access Database that was designed, developed, and is maintained by the GSI Database Manager, or the data were entered into a Microsoft Excel spreadsheet. A percentage of biological, chemical, and operational data that was recorded by hand and entered into Microsoft Access or Excel was verified against the original raw data by the GSI Senior Quality Assurance/Quality Control (QAQC) Officer. This procedure also included verification of the accuracy of computer-generated data through hand-calculation. The percentage of verified raw data depended upon the amount of raw data that was generated, and ranged from 10 % to 100 % of the original raw data. All electronic data files are stored on the LSRI s secured Local Area Network (LAN) that can be accessed only by relevant GSI personnel. The GSI Database Manager is the single point of control for access to the LSRI LAN. The LSRI LAN is automatically backed up every 24 hours. The electronic data files are also stored on the GSI s internal SharePoint website (greatshipsinitiative.net), which acts as a secondary data backup/storage mechanism. The GSI Senior QAQC Officer is responsible for archiving and storing all original raw data applicable to the JFE BallastAce BWMS and components tests in a climate-controlled, secure archive room at the LSRI for a period seven years. 4 RESULTS: JFE FILTER SYSTEM INTERCOMPARISON TEST 4.1 Operational Performance Fuji Candle Filter (F Candle) GSI personnel did not observe any maintenance or operational issues during the four test cycles conducted using the F Candle FS. Figure 5 shows a graphical example of the flow rate and pressure (pre- and post-fs) over the entire duration of Test Cycle 3 of the JFE FS Intercomparison Test (graphs from Test Cycles 1, 2, and 4 are available on request. During Test Cycle 3 there were five backflush cycles, occurring approximately every minutes during the operation. After each backflush cycle the F Candle FS returned back to a steady state with relatively low variability in operating conditions.

46 Flow (M^3) Pressure (Bar) Flow and Pressure GSI/LB/QAQC/TR/JFE Page 46 of Time (min) Pre Filter Flow (m^3/hr) Post Filter Flow (m^3/hr) Post Filter Pressure (bar) Pre Filter Pressure (bar) Figure 5. Time-Dependent Operational Data from Test Cycle 3 of the JFE FS Intercomparison Test using the Candle Filter by Fuji Manufacturing Company, Ltd. (F Candle). Table 10 summarizes the operational measurements that were made during each of the four test cycles involving the F Candle FS, and the overall average for the JFE FS Intercomparison Test. The four test cycles ranged in duration from 67 to 74 minutes. Test Cycle 3 was slightly longer than the other three test cycles because GSI paused the operation for 7 minutes to troubleshoot the GSI Facility s Organism Diaphragm Injection System. The average pre-treatment pressure met GSI s target of 2 bar (Table 10). The differential pressure did not vary between test cycles and averaged 0.68 bar (Table 10). The post-treatment flow rate for all four test cycles was within 10 % of the GSI target of 311 m 3 /hour (Table 10). The backflush flow rate, based on the volume of backflush water collected in the backflush water tank, ranged from 1.6 m 3 /hour to 5.2 m 3 /hour, for an average of 3.1 m 3 /hour (Table 10).

47 Page 47 of 146 Table 10. Summary of Operational Measurements and Data Collected during the Four Test Cycles of the JFE FS Intercomparison Test using the Candle Filter by Fuji Manufacturing Company, Ltd. (F Candle). Parameter Units Test Cycle 1 Test Cycle 2 Test Cycle 3 Test Cycle 4 Average Date and Start Time Sep-14 09:22:20 22-Sep-14 12:17:30 24-Sep-14 09:00:40 25-Sep-14 14:38:30 Duration min Pre-Treatment Line Pressure (Average ± Std. Deviation) Post-Treatment Line Pressure (Average ± Std. Deviation) Differential Pressure (Average ± Std. Deviation) Pre-Treatment Flow Rate (Average ± Std. Deviation) Post-Treatment Flow Rate (Average ± Std. Deviation) Backflush Flow Rate (Volumetric Calculation) bar 1.98 ± ± ± ± ± 0.05 bar 1.31 ± ± ± ± ± 0.07 bar 0.67 ± ± ± ± ± 0.06 m 3 /hour 316 ± ± ± ± ± 10 m 3 /hour 307 ± ± ± ± ± 5 m 3 /hour Volume Treated (Filtered) m Kanagawa Candle Filter (K Candle) GSI personnel did not observe any maintenance or operational issues during the four test cycles of the JFE FS Intercomparison Test conducted using the K Candle FS. Figure 6 shows a graphical example of the flow rate and pressure (pre- and post-fs) over the entire duration of Test Cycle 3 (graphs from Test Cycles 1, 2, and 4 are available on request). During Test Cycle 3 there were numerous backflush cycles, starting approximately every five minutes during the first part of the operation and ending with nearly continuous backflushing. Due to the frequency of backflush cycles during this particular test cycle, the FS did not have the opportunity to return to steady-state conditions in between each backflush cycle.

48 Flow (M^3) Pressure (Bar) Flow and Pressure GSI/LB/QAQC/TR/JFE Page 48 of Time (min) Pre Filter Flow (m^3/hr) Post Filter Flow (m^3/hr) Post Filter Pressure (bar) Pre Filter Pressure (bar) Figure 6. Time-Dependent Operational Data from Test Cycle 3 of the JFE FS Intercomparison Test using the Candle Filter by Kanagawa Kiki Kogyo Company, Ltd. (K Candle). Table 11 summarizes the operational measurements that were made during each of the four test cycles involving the K Candle FS, and the overall average for the JFE FS Intercomparison Test. The test cycles ranged in duration from 69 to 35 minutes (Table 11). Test Cycle 4 was approximately half the length of the other three test cycles (Table 11). During Test Cycle 4, the K Candle FS was backflushing more water than the GSI backflush volume containment tub could accommodate. As a result, GSI truncated the test duration to one-half of the planned duration. The average pre-treatment pressure was 1.97 bar, which was acceptably close to GSI s target of 2 bar (Table 11). The differential pressure did not vary substantially between Test Cycles 1-3, but jumped to 1.03 bar during Test Cycle 4 (Table 11). The post-treatment flow rate for the first three test cycles were within 10 % of the GSI target flow rate of 309 m 3 /hour (Table 11). During Test Cycle 4, flow rates fell below the target due to the constant backflushing (Table 11). The backflush flow rate, based on the volume of backflush water collected in the backflush water tank, ranged from 31.7 m 3 /hour to as high as 63.4 m 3 /hour over the four test cycles, for an average of 40.4 m 3 /hour (Table 11).

49 Page 49 of 146 Table 11. Summary of Operational Measurements and Data Collected during the Four Test Cycles of the JFE FS Intercomparison Test using the Candle Filter by Kanagawa Kiki Kogyo Company, Ltd. (K Candle). Parameter Units Test Cycle 1 Test Cycle 2 Test Cycle 3 Test Cycle 4 Average Date and Start Time Sep-14 12:24:10 22-Sep-14 09:14:40 24-Sep-14 14:50:10 25-Sep-14 12:14:30 Duration min Pre-Treatment Line Pressure (Average ± Std. Deviation) Post-Treatment Line Pressure (Average ± Std. Deviation) Differential Pressure (Average ± Std. Deviation) Pre-Treatment Flow Rate (Average ± Std. Deviation) Post-Treatment Flow Rate (Average ± Std. Deviation) Backflush Flow Rate (Volumetric Calculation) bar 1.99 ± ± ± ± ± 0.10 bar 1.34 ± ± ± ± ± 0.14 bar 0.64 ± ± ± ± ± 0.19 m 3 /hour 355 ± ± ± ± ± 22 m 3 /hour 313 ± ± ± ± ± 22 m 3 /hour Volume Treated (Filtered) m Fuji Panel Filter (F Panel) On 18 September 2014 (i.e., after Test Cycle 1 of the JFE FS Intercomparison Test), JFE Engineering disassembled and inspected the F Panel FS. Other than this inspection event, GSI personnel did not observe any maintenance or operational issues during the remaining three test cycles conducted using the F Panel FS. Figure 7 shows a graphical example of the flow rate and pressure (pre- and post-fs) over the entire duration of Test Cycle 3 of the JFE FS Intercomparison Test (graphs from Test Cycles 1, 2, and 4 are available on request). During Test Cycle 3 there were 21 backflush cycles, occurring approximately every five minutes during the first part of the operation and ending with backflush cycles approximately every two minutes. After each backflush cycle the F Panel FS returned back to a relatively steady state with low variability in operating conditions.

50 Flow (M^3) Pressure (Bar) Flow and Pressure GSI/LB/QAQC/TR/JFE Page 50 of Time (min) Pre Filter Flow (m^3/hr) Post Filter Flow (m^3/hr) Figure 7. Time-Dependent Operational Data from Test Cycle 3 of the JFE FS Intercomparison Test using the Fuji Filter Manufacturing Company, Ltd. (F Panel). Table 12 summarizes the operational measurements that were made during each of the four test cycles of the JFE FS Intercomparison Test involving the F Panel FS, and the overall average. The test cycles ranged in duration from 63 to 70 minutes (Table 12). The average pre-treatment pressure was 1.98 bar, which met GSI s target of 2 bar (Table 12). The differential pressure did not vary substantially between test cycles and averaged 0.68 bar (Table 12). The post-treatment flow rate for all four test cycles was within 10 % of the GSI target flow rate of 311 m 3 /hour (Table 12). The backflush flow rate, which was only measured for two of the four test cycles, averaged 11 m 3 /hour (Table 12).

51 Page 51 of 146 Table 12. Summary of Operational Measurements and Data Collected during the Four Test Cycles of the JFE FS Intercomparison Test using the Panel Filter by Fuji Filter Manufacturing Company, Ltd. (F Panel). NM = Not Measured. Parameter Units Test Cycle 1 Test Cycle 2 Test Cycle 3 Test Cycle 4 Average Date and Start Time Sep-14 15:07:20 22-Sep-14 15:16:50 24-Sep-14 12:00:10 25-Sep-14 09:03:10 Duration min Pre-Treatment Line Pressure (Average ± Std. Deviation) Post-Treatment Line Pressure (Average ± Std. Deviation) bar 1.99 ± ± ± ± ± 0.04 bar 1.32 ± ± ± ± ± 0.06 Differential Pressure (Average ± Std. Deviation) Pre-Treatment Flow Rate (Average ± Std. Deviation) Post-Treatment Flow Rate (Average ± Std. Deviation) Backflush Flow Rate (Volumetric Calculation) bar 0.67 ± ± ± ± ± 0.06 m 3 /hour 320 ± ± ± ± ± 6 m 3 /hour 313 ± ± ± ± ± 4 m 3 /hour NM NM 11.0 Volume Treated (Filtered) m Operational Filter Performance Comparison Figure 8 presents the comparison of the F Candle, K Candle, and F Panel FS average differential pressures as measured during all four test cycles of the JFE FS Intercomparison Test. The F Candle and F Panel FSs had very similar differential pressure averages of approximately 0.65 bar (Figure 8). The K Candle FS had the highest differential pressure average of nearly 0.8 bar (Figure 8).

52 Page 52 of 146 Figure 8. Comparison of the Average (± Standard Deviation) Differential Pressure Across Filter Types Measured During the Four Test Cycles of the JFE FS Intercomparison Test. Figure 9 shows the comparison of the ratio (expressed as a percentage) of the backflush and posttreatment flow rates for the F Candle, K Candle, and F Panel FSs during all four test cycles of the JFE FS Intercomparison Test. The F Candle FS had the least amount of water lost to backflush with 1 % on average. The F Candle FS performed very consistently with respect to water lost to backflush, with values ranging from 0.5 % to 1.7 %. The F Panel FS performed less consistently with respect to this parameter, with approximately 3.5 % of the flow lost to backflush on average (Figure 9). The backflush volume was not measured during two of the test cycles due to operator error, therefore, the average water lost to backflush was based on n=2 rather than n=4. During Test Cycle 2, 2.6 % of the post-treatment water was lost to backflush and during Test Cycle 3, 4.5 % of the water was lost to backflush. The K Candle FS had the highest amount of water lost to backflush with 14.5 % on average (Figure 9) and a range of 10.1 % to 25.7 %.

53 Page 53 of 146 Figure 9. Comparison of the Average Ratio (%, ± Standard Deviation) of Backflush Flow Rate and Post- Treatment Flow Rate Measured Across Filter Types During the Four Test Cycles of the JFE FS Intercomparison Test. 4.3 Solids Removal Performance and Water Quality Data Fuji Candle Filter (F Candle) Table 13 summarizes the water quality data, including solids removal performance, from the four test cycles of the JFE FS Intercomparison Test utilizing the F Candle FS. Overall, the pre-treatment (i.e., pre-filter) water quality conditions were very similar during the entire test. Post-treatment water quality was very similar to pre-treatment water quality, with little to no removal of TSS, POC, or MM (Table 13). The measured concentrations of NPOC and POC concentrations in the post-treatment water were not different from the pre-treatment water (Table 13) across test cycles.

54 Page 54 of 146 Table 13. Summary of Water Quality Data and Solids Removal Performance of the Candle Filter by Fuji Manufacturing Company, Ltd. (F Candle) During the Four Test Cycles of the JFE FS Intercomparison Test. Parameter Units Test Cycle 1 Test Cycle 2 Test Cycle 3 Test Cycle 4 Pre-Treatment TSS 31.5 ± ± ± ± 1.1 mg/l Post-Treatment TSS 31.7 ± ± ± ± 0.9 TSS Removal % Pre-Treatment POC 4.8 ± ± ± ± 0.7 mg/l Post-Treatment POC 6.3 ± ± ± ± 0.6 POC Removal % Pre-Treatment MM 26.7 ± ± ± ± 1.2 mg/l Post-Treatment MM 25.5 ± ± ± ± 0.6 MM Removal % Pre-Treatment %T, 46.9 ± 0.2/ 47.8 ± 0.2/ 48.6 ± 0.2/ 48.9 ± 0.2/ Filtered/Unfiltered 39.0 ± ± ± ± 0.5 % Post-Treatment %T, 47.1 ± 0.1/ 48.1 ± 0.2/ 48.9 ± 0.2/ 49.0 ± 0.1/ Filtered/Unfiltered 39.2 ± ± ± ± 0.2 Pre-Treatment NPOC 12.0 ± ± ± ± 0.7 mg/l Post-Treatment NPOC 13.5 ± ± ± ± 0.7 Pre-Treatment DOC 7.2 ± ± ± ± 0.0 mg/l Post-Treatment DOC 7.2 ± ± ± ± Kanagawa Candle Filter (K Candle) Table 14 summarizes the water quality data and the solids removal performance from the four test cycles of the JFE FS Intercomparison Test utilizing the K Candle FS. Due to continuous backflushing during Test Cycle 3, the last set of grab samples that were collected from the pre- and post-treatment line were collected during a backflush. Test Cycle 4 was terminated after the second set of grab samples was collected; averages represent n=2. For all parameters except TSS and MM, the pre-treatment water quality conditions were very similar during all four test cycles. Pretreatment TSS ranged from 27 to 43 mg/l (Table 14). Pre-treatment MM ranged from 23 to 37 mg/l (Table 14). The K Candle FS removed up to 23 % of the TSS and 28 % of the MM in the pretreatment water over the course of four test cycles (Table 14). Similar to the F Candle FS, there was a greater concentration of NPOC and POC in the post-treatment water than in the pre-treatment water (Table 14).

55 Page 55 of 146 Table 14. Summary of Water Quality Data and Solids Removal Performance of the Candle Filter by Kanagawa Kiki Kogyo Company, Ltd. (K Candle) During Four Test Cycles of the JFE FS Intercomparison Test. Parameter Units Test Cycle 1 Test Cycle 2 Test Cycle 3** Test Cycle 4^ Pre-Treatment TSS 27.3 ± ± ± ± 17.4 mg/l Post-Treatment TSS 26.4 ± ± ± ± 2.6 TSS Removal % Pre-Treatment POC 4.5 ± ± ± 1.5*** 5.4 ± 0.6 mg/l Post-Treatment POC 6.0 ± ± ± ± 1.2 POC Removal % Pre-Treatment MM 22.8 ± ± ± 8.1*** 37.4 ± 16.8 mg/l Post-Treatment MM 20.3 ± ± ± ± 1.4 MM Removal % Pre-Treatment %T, 47.9 ± 0.8/ 47.9 ± 0.3/ 48.3 ± 0.3/ 48.4 ± 0.0/ Filtered/Unfiltered 39.8 ± ± ± ± 1.3 % Post-Treatment %T, 48.1 ± 0.5/ 47.9 ± 0.3/ 48.5 ± 0.3/ 49.0 ± 0.0/ Filtered/Unfiltered 40.0 ± ± ± ± 0.4 Pre-Treatment NPOC 11.4 ± ± ± 1.5*** 12.7 ± 0.6 mg/l Post-Treatment NPOC 13.3 ± ± ± ± 1.1 Pre-Treatment DOC 6.9 ± 0.2* 7.1 ± ± ± 0.0 mg/l Post-Treatment DOC 7.3 ± ± ± ± 0.1 *Two of the three replicate samples were refiltered and then reanalyzed. **The last set of grab samples that were collected (~60 min after the start of the operation) were collected during a backflush cycle. The filter was continuously backflushing plus backflushing due to differential pressure requirements; we were unable to collect a sample in between the differential backflush cycles as they were continuous near the end of the operation. This seems to have resulted in TSS values that were lower than the previous two samples by ~10 mg/l. ***The pre-filter sample that was collected ~30 min after the start of the operation had very high NPOC, POC, and MM values; these values were excluded as outliers potentially due to an analysis error. ^The operation was ended immediately after the second set of grab samples were collected. Due to a high backflush rate, the amount of water being pumped out of the backflush tank began to flood the GSI Facility and the operation was ended about halfway into the planned duration Fuji Panel Filter (F Panel) Table 15 summarizes the water quality data and the solids removal performance from the four test cycles of the JFE FS Intercomparison Test utilizing the F Panel FS. The pre-treatment water quality conditions were very similar during all four test cycles for all parameters measured (Table 15). The F Panel FS removed up to 1 % of the TSS and 5 % of the MM in the pre-treatment water over the course of four test cycles (Table 15). As was the case with the other two FSs tested, there was a greater concentration of NPOC and POC in the post-treatment water than in the pre-treatment water (Table 15).

56 Page 56 of 146 Table 15. Summary of Water Quality Data and Solids Removal Performance of the Panel Filter by Fuji Filter Manufacturing Company, Ltd. (F Panel) During the Four Test Cycles of the JFE FS Intercomparison Test. Parameter Units Test Cycle 1 Test Cycle 2 Test Cycle 3 Test Cycle 4 Pre-Treatment TSS 33.2 ± ± ± ± 0.4 mg/l Post-Treatment TSS 33.1 ± ± ± ± 0.4 TSS Removal % Pre-Treatment POC 5.8 ± ± ± ± 1.4 mg/l Post-Treatment POC 7.0 ± ± ± ± 0.1 POC Removal % Pre-Treatment MM 27.4 ± ± ± ± 1.6 mg/l Post-Treatment MM 26.1 ± ± ± ± 0.5 MM Removal % Pre-Treatment %T, 48.5 ± 0.4/ 48.1 ± 0.4/ 48.2 ± 0.2/ 48.2 ± 0.2/ Filtered/Unfiltered 40.5 ± ± ± ± 0.2 % Post-Treatment %T, 48.8 ± 0.0/ 47.9 ± 0.1/ 48.3 ± 0.3/ 48.3 ± 0.2/ Filtered/Unfiltered 40.4 ± ± ± ± 0.2 Pre-Treatment NPOC 12.5 ± ± ± ± 1.3 mg/l Post-Treatment NPOC 13.7 ± ± ± ± 0.1 Pre-Treatment DOC 6.7 ± ± ± ± 0.1 mg/l Post-Treatment DOC 6.7 ± ± ± ± Biological Performance Protists (Organisms 10 µm and < 50 µm) Across the four test cycles of the JFE FS Intercomparison Test, the total protist pre-fs density ranged from 1,547 cells/ml to 2,826 cells/ml (Figure 10). Although there was no organism injection during Test Cycles 3 and 4, intake densities far exceeded that of ETV requirements. Over the course of four test cycles, the F Candle FS resulted in a range of 1,761 2,805 cells/ml in post- FS samples (Figure 10). Similarly, the F Panel FS resulted in a range of 1,930 2,989 cells/ml in post-fs samples and the K Candle FS resulted in a range of 1,406 2,430 cells/ml in post-fs samples (Figure 10).

57 Page 57 of 146 Filter System F Candle K Candle F Panel Test Cycle Average Pre-Filter Density, Total Cells/mL (± Standard Deviation, n=2) Average Post-Filter Density, Total Cells/mL (± Standard Deviation, n=2) 1 2,608 (64) 2,805 (17) 2 1,856 (347) 1,998 (254) 3 1,991 (56) 1,761 (111) 4 1,806 (399) 2,070 (429) 1 2,806 (507) 2,214 (257) 2 2,305 (7) 2,430 (350) 3 1,547 (28) 1,992 (215) 4 1,601 (9) 1,406 (81) 1 2,826 (573) 2,989 (670) 2 1,843 (256) 2,473 (188) 3 2,003 (176) 1,930 (16) 4 1,764 (259) 1,954 (288) Figure 10. Graph Depicting Average (± Standard Deviation) Pre- and Post-Filter Total Density of Protist Cells During Four Test Cycles of the JFE FS Intercomparison Test. Companion table shows average densities (pre- and post-filter).

58 4.4.2 Zooplankton (Organisms 50 µm) GSI/LB/QAQC/TR/JFE Page 58 of 146 Zooplankton present in the freshwater DSH fall into two distinct size subcategories: macrozooplankton, in which all individuals are substantially 50 µm in minimum dimension; and microzooplankton, in which most individuals are 50 µm in minimum dimension and a relatively small proportion of the population, approximately 5 % in this study (data not presented), may be < 50 µm in minimum dimension. These smaller organisms (< 50 µm in minimum dimension) were not excluded from this analysis. As such, results from the JFE FS Intercomparison Test are presented as follows: macrozooplankton, microzooplankton, and total zooplankton (i.e., macrozooplankton plus microzooplankton) Macrozooplankton Only Across the four test cycles of the JFE FS Intercomparison Test, the total macrozooplankton pre-fs density ranged from 19,600 m 3 to 70,100/m 3 (Figure 11). There was a clear reduction in total macrozooplankton density in post-fs samples, total density ranged from 707/m 3 to 16,400/m 3 (Figure 11) Microzooplankton Only Across the four test cycles of the JFE FS Intercomparison Test, the total microzooplankton prefilter density ranged from 14,900/m 3 to 309,000/m 3 (Figure 12). There were two FSs during Test Cycle 3 that had pre-fs densities of microzooplankton that were quite low, i.e., 14,900/m 3 (K Candle, Figure 12) and 32,000/m 3 (F Panel, Figure 12), due to a shift in current flow in the harbor. The total microzooplankton density in post-fs samples ranged from 8,160/m 3 to as high as 313,000/m 3 (Figure 12) Total Zooplankton The total pre-fs zooplankton density ranged from 40,300/m 3 to 376,000/m 3 during the four test cycles (Figure 13). There were two FSs during Test Cycle 3 that had total zooplankton densities as low as 40,300/m 3 (i.e., K Candle, Figure 13) and 52,400/m 3 (i.e., F Panel, Figure 13) due to the low density of microzooplankton. With the exception of these two FSs during Test Cycle 3, all other test cycles had intake densities that exceeded the ETV requirements. The total zooplankton density in post-fs samples ranged from 8,860/m 3 to 314,000/m 3 (Figure 13).

59 Page 59 of 146 Filter System F Candle K Candle F Panel Test Cycle Average Pre-Filter Density, Total #/m 3 (± SEM, n=3) Average Post-Filter Density, Total #/m 3 (± SEM, n=3) 1 48,100 (5,300) 14,200 (1,240) 2 29,600 (2,580) 8,070 (2,170) 3 19,600 (2,390) 4,080 (741) 4 31,700 (4,970) 10,800 (1,860) 1 66,600 (4,390) 709 (709) 2 37,900 (3,320) 2,960 (924) 3 25,400 (1,560) 707 (237) 4 23,000 (1,770) 1,470 (658) 1 70,100 (8,580) 16,400 (2,510) 2 37,400 (7,820) 13,000 (1,620) 3 20,400 (1,280) 5,180 (1,010) 4 23,800 (1,720) 4,580 (1,030) Figure 11. Graph Depicting Average (± Standard Error of the Mean, SEM) Pre- and Post-Filter Total Density of Macrozooplankton During Four Test Cycles of the JFE FS Intercomparison Test. Companion table shows average densities (pre- and post-filter).

60 Page 60 of 146 Filter System F Candle K Candle F Panel Test Cycle Average Pre-Filter Density, Total #/m 3 (± SEM, n=3) Average Post-Filter Density, Total #/m 3 (± SEM, n=3) 1 257,000 (5,470) 245,000 (15,900) 2 145,000 (10,300) 133,000 (9,140) 3 144,000 (6,920) 168,000 (23,900) 4 165,000 (6,430) 202,000 (20,500) 1 309,000 (16,400) 313,000 (30,100) 2 193,000 (6,350) 103,000 (7,940) 3 14,900 (1,880) 8,160 (660) 4 115,000 (6,090) 109,000 (2,970) 1 270,000 (15,000) 222,000 (14,700) 2 104,000 (11,400) 87,900 (4,160) 3 32,000 (2,170) 36,500 (1,570) 4 115,000 (13,800) 54,500 (4,100) Figure 12. Graph Depicting Average (± Standard Error of the Mean, SEM) Pre- and Post-Filter Total Density of Microzooplankton During Four Test Cycles of the JFE FS Intercomparison Test. Companion table shows average densities (pre- and post-filter).

61 Page 61 of 146 Filter System F Candle K Candle F Panel Test Cycle Average Pre-Filter Density, Total #/m 3 (± SEM, n=3) Average Post-Filter Density, Total #/m 3 (± SEM, n=3) 1 305,000 (10,700) 259,000 (16,400) 2 175,000 (10,100) 141,000 (9,750) 3 164,000 (8,560) 172,000 (23,500) 4 197,000 (10,500) 212,000 (19,000) 1 376,000 (17,000) 314,000 (30,200) 2 231,000 (3,210) 106,000 (7,490) 3 40,300 (1,940) 8,860 (800) 4 138,000 (5,770) 110,000 (3,020) 1 340,000 (21,700) 238,000 (17,100) 2 142,000 (8,140) 101,000 (3,720) 3 52,400 (2,290) 41,700 (1,380) 4 139,000 (15,200) 59,100 (3,750) Figure 13. Graph Depicting Average (± Standard Error of the Mean, SEM) Pre- and Post-Filter Total Density of Zooplankton (i.e., Microzooplankton plus Macrozooplankton) During Four Test Cycles of the JFE FS Intercomparison Test. Companion table shows average densities (pre- and post-filter). 4.5 Test Validity and Data Quality Objectives Test Validity Table 16 shows the water quality and biology target values and results for pre-fs water measured during the JFE FS Intercomparison Test. The target values were met for all water quality parameters (i.e., TSS, POC, DOC, and MM) measured during the entire evaluation of the three FS

62 Page 62 of 146 tests. The minimum target value for the 10 µm and < 50 µm size class, i.e., protists, was met for all FS test cycles based on total density determined in preserved samples. For the 50 µm size class, i.e., zooplankton, the minimum target was met for all FSs except Test Cycle 3 involving the K Candle FS where total intake density was 40,300/m 3 and Test Cycle 3 involving the F Panel FS where total intake density was 53,400/m 3. Table 16. Target Values and Results for GSI Challenge Water (Pre-Filter System) During JFE FS Intercomparison Test. Parameter Total Suspended Solids (mg/l) Particulate Organic Matter as Particulate Organic Carbon (mg/l) Dissolved Organic Matter as Dissolved Organic Carbon (mg/l) Target Values for GSI Challenge Water Was Target Met for All Test Cycles? > 24 YES > 4 YES > 6 YES Mineral Matter (mg/l) > 20 YES Organisms 10 µm and < 50 µm Organisms 50 µm > 1,000/mL total cells > 100,000/m 3 total organisms YES NO; Not met for K Candle TC3 or F Panel TC3 Comments Average pre-filter values ranged from mg/l during the entire evaluation. Average pre-filter values ranged from mg/l during the entire evaluation. Average pre-filter values ranged from mg/l during the entire evaluation. Average pre-filter values ranged from mg/l during the entire evaluation. Average pre-filter values ranged from 1,547 2,826 cells/ml during the entire evaluation. Average pre-filter values ranged from 40, ,000/m 3 during the entire evaluation Data Quality Indicators: Water Quality During the JFE FS Intercomparison Test, quality control (QC) samples were collected for water quality analyses only. Therefore, GSI used the following USEPA data quality indicators (applicable to water quality analyses only) to determine compliance with the following data quality objectives: precision, bias, accuracy, comparability, sensitivity and completeness. Data quality objectives and acceptance criteria for each of these indicators are described in GSI/QAQC/QAPP/LB/1 - Quality Assurance Project Plan for Great Ships Initiative (GSI) Land-Based Tests (GSI, 2013). Results of the data quality analysis for QC samples analyzed during the JFE FS Intercomparison Test are summarized in Table 17. In regards to TSS, NPOC, DOC, POC, and %T analyses, all data quality objectives were met.

63 Page 63 of 146 Table 17. Data Quality Objectives, Criteria, and Results from Water Quality Analyses during the JFE FS Intercomparison Test. Data Quality Indicator Precision Bias, Filter Blanks Accuracy Evaluation Process/Performance Measurement Samples (10 %) were collected and analyzed in duplicate with performance measured by average relative percent difference (RPD). %T filter blanks were prepared by filtering deionized water samples (one per analysis date) using the procedure outlined in GSI/SOP/BS/RA/C/8, v.3 Sample Filtration, and analyzed using the procedure outlined in GSI/SOP/BS/RA/C/4, v.2 Sample Analysis. TSS filter blanks were prepared by filtering deionized water samples (one per analysis date) and then drying and weighing the filter following the procedure outlined in GSI/SOP/BS/RA/C/8, v.3. NPOC blanks were prepared by acidifying a volume of deionized water to 0.2 % with concentrated hydrochloric acid and analyzed following the procedure outlined in GSI/SOP/BS/RA/C/3, v.4. DOC filter blanks were prepared by filtering deionized water samples (one per analysis date) and analyzed following the procedure outlined in GSI/SOP/BS/RA/C/3, v.4. Samples (10 %) were spiked with a total organic carbon spiking solution with performance measured by average spike-recovery (SPR). Data Quality Objective < 20 % average RPD > 98 % average % T < 0.32 mg/l average TSS < 0.44 mg/l average NPOC < 0.44 mg/l average DOC 75 %-125 % average SPR. Performance Measurement Result Percentage of Samples Collected and Analyzed in Duplicate: TSS: 11% NPOC: 11% DOC: 11% %T, Filtered: 11% %T, Unfiltered: 11% Number of %T Filter Blanks Analyzed: 5 Number of TSS Filter Blanks Analyzed: 5 Number of NPOC Blanks Analyzed: 28 Number of DOC Filter Blanks Analyzed: 4 Percentage of NPOC/DOC Samples Spiked: 21% TSS: 1.0% NPOC: 6.1% DOC: 2.6% %T, Filtered: 0.2% %T, Unfiltered: 0.4% Filter blank (%T): 99.6% Filter blank (TSS): Non- Detect Blank (NPOC): 0.16 mg/l Filter blank (DOC): 0.20 mg/l NPOC/DOC: 103% Performance was measured by average percent < 20 % average D. Percentage of Analysis TSS: 7.9%

64 Data Quality Indicator Evaluation Process/Performance Measurement difference (%D) between all measured and nominal reference standard values. Data Quality Objective GSI/LB/QAQC/TR/JFE Page 64 of 146 Performance Measurement Result Days Containing a Reference Standard: TSS:100% NPOC: 100% NPOC Reference Standard: 3.4% NPOC 10 mg/l Standard: 1.5% Representativeness Comparability Completeness Sensitivity All samples were collected, handled, and analyzed in the same manner. Routine procedures were conducted according to appropriate SOPs to ensure consistency between tests. Percentage of valid (i.e., collected, handled, analyzed correctly and meeting DQOs) water chemistry samples measured out of the total number of water chemistry samples collected. Performance is measured by percent completeness (%C). The method detection limit (MDL) and limit of quantification (LOQ) for each analyte and analytical method utilized was determined annually. Not Applicable Qualitative. Not Applicable Qualitative. > 90 % C. Not Applicable All water chemistry/quality samples were collected, handled, transported and analyzed in the same manner (using the appropriate GSI SOPs). The GSI SOPs listed in Table 13 were used for all water chemistry and water quality analyses. TSS: 98% %T, Filtered: 98% %T, Unfiltered: 98% NPOC: 99% DOC: 98% POC: 97% MM: 97% TSS MDL: 0.64 mg/l; TSS LOQ: 2.12 mg/l Determined 19 May 2014 NPOC/DOC MDL: 0.13 mg/l; NPOC/DOC LOQ: 0.44 mg/l Determined 30 May 2014

65 Page 65 of RESULTS: JFE BallastAce BALLAST WATER MANAGEMENT SYSTEM STATUS TEST 5.1 Test Cycles 1, 3 and 5: F Panel Filter and NEO-CHLOR DICD BWMS Intake Measurements Operational Conditions During intake of Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test, which occurred on 15 September 2014, 02 October 2014, and 09 October 2014, respectively, the JFE BallastAce BWMS utilized the F Panel FS and NEO-CHLOR DICD Granules as the active substance formulation. The operational data measured during intake of these three test cycles are summarized in Table 18. Figure 14 shows the pre- and post-fs flow rate and pressure data in real time for Test Cycle 3 intake (real-time data from Test Cycles 1 and 5 are available on request). The average duration of the intake operation was minutes (Table 18). The pre-fs line pressure was 1.93 bar on average, which was within 3.5 % of the target value of 2 bar (Table 18). The differential pressure between the pre- and post-fs lines was 0.70 bar on average (Table 18). The pre-fs flow rate ranged from 322 to 332 m 3 /hour (Table 18). The post-fs flow rate ranged from 308 to 320 m 3 /hour, all within 10 % of the target flow rate (i.e., 311 m 3 /hour; Table 18). The backflush flow rate ranged from 9 to 15 m 3 /hour, resulting in an average of 4 % of the post-fs water lost to backflush (Table 18). The total volume of water treated was 188 m 3 on average, while the total volume of water in the control retention tank averaged 191 m 3 (Table 18). For zooplankton analysis, Sample Collection Tub #4 was used for all three test cycles and an average of 2.80 m 3 of sample water concentrated for analysis.

66 Page 66 of 146 Table 18. Summary of Operational Measurements and Data Collected during Three Test Cycles (i.e., Test Cycles 1, 3, and 5) of the JFE BallastAce BWMS Status Test using NEO-CHLOR DICD Granules as the Active Substance. NM = Not Measured. Parameter Units Test Cycle 1 Test Cycle 3 Test Cycle 5 Average Date and Start Time Sep-14 11:40:40 02-Oct-14 10:49:10 09-Oct-14 13:02:10 Duration min Pre-Treatment Line Pressure (Average ± Std. Deviation) Post-Treatment Line Pressure (Average ± Std. Deviation) Differential Pressure (Average ± Std. Deviation) Pre-Treatment Flow Rate (Average ± Std. Deviation) Post-Treatment Flow Rate (Average ± Std. Deviation) Backflush Flow Rate (Volumetric Calculation) Treatment Retention Tank Volume Control Retention Tank Volume Sample Collection Tub #4 Volume bar 1.95 ± ± ± ± 0.04 bar 1.25 ± ± ± ± 0.05 bar 0.70 ± ± ± ± 0.02 m 3 /hour 332 ± ± ± ± 6 m 3 /hour 320 ± ± ± ± 8 m 3 /hour NM NM Cannot be Calculated m ± 3 m ± 2 m ± 0.17 The real-time data in Figure 14 shows that once the set flow rate and pressure was achieved there was very low variability in pre- and post-fs flow rate and pressure during the ~ 35 minute operation. There were two backflush cycles, after which, the operational data quickly returned to a steady state condition (Figure 14).

67 Flow (M^3) Pressure (Bar) 450 Flow and Pressure GSI/LB/QAQC/TR/JFE Page 67 of Time (min) Pre Filter Flow (m^3/hr) Post Filter Flow (m^3/hr) Post Filter Pressure (bar) Pre Filter Pressure (bar) Figure 14. Real Time Pre- and Post-Filter Flow Rate and Pressure Data Recorded during Test Cycle 3 of the JFE BallastAce BWMS Status Test BWMS Active Substance Concentrations The TRO concentration measured in pre- and post-treatment grab samples collected simultaneously during Test Cycles 1, 3, and 5 intake of the JFE BallastAce BWMS Status Test are presented in Table 19. During all three test cycles, there were measurable TRO concentrations in the pretreatment intake samples with a maximum measured value of mg/l TRO, which is within the range of TRO concentrations measured in similar samples collected during previous tests at the GSI Facility. Table 19 also shows the target TRO concentration three minutes after active substance dosing, as determined manually by JFE Engineering. The target TRO concentration was based on the DOC concentration of the DSH water (data not presented), therefore, the target value varied between each test cycle. During Test Cycle 1, the BWMS active substance injection control program stopped working during the intake operation. JFE Engineering injected the active substance manually after the malfunction. As a result, the overall TRO concentration was lower than expected in post-treatment intake samples (ranging from to 5.10 mg/l TRO), however, JFE Engineering deemed the test cycle to be valid because the treatment retention tank TRO concentration 24 hours post-treatment was still sufficiently high (i.e., greater than 1.0 mg/l TRO). After Test Cycle 1, JFE Engineering repaired the active substance injection control and active substance was automatically injected for all subsequent test cycles. During Test Cycle 3, the TRO

68 Page 68 of 146 concentration in post-treatment intake samples ranged from 2.24 to 5.26 mg/l (Table 19). The TRO concentration was slightly higher overall in Test Cycle 5, ranging from 2.89 to 6.91 mg/l (Table 19). Table 19. Concentration of Total Residual Oxidants (TRO) in Grab Samples Collected Simultaneously from the Pre- and Post-Treatment Lines During Test Cycles 1, 3, and 5 Intake of the JFE BallastAce BWMS Status Test. N/A = Not Applicable. ND = Measured value was below the method detection limit. Sample Location (Pitot) Collection Time (min) JFE Target TRO (mg/l) Test Cycle 1 (TRO (mg/l) Test Cycle 3 (TRO (mg/l) Test Cycle 5 (TRO (mg/l) ND N/A Test Cycle 1 = * 5.45* * 6.91* 10 Test Cycle 3 = * 6.35* * AVERAGE Test Cycle 5 = *Reported value is above the range of the TRO calibration curve (i.e., 4 mg/l is the highest standard). Pre-Treatment (SP3c) Post-Treatment (SP15) Water Quality Conditions Grab Samples Intake water quality results from pre- and post-treatment intake samples collected simultaneously during Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test are presented in Table 20. All three test cycles met the minimum challenge water quality characteristics outlined in the ETV Protocol (Table 2). The pre-treatment TSS concentration ranged from 28.0 to 58.6 mg/l (target value was 24.0 mg/l TSS; Table 20). The DOC concentration in pre-treatment intake samples ranged from 6.8 to 8.3 mg/l (target value was 6 mg/l; Table 20); this parameter was not augmented as the DSH naturally meets the challenge water DOC criterion. The pre-treatment POC concentration ranged from 4.0 to 11.1 mg/l, which met or exceeded the target value of 4 mg/l (Table 20). Finally, the MM concentration in pre-treatment intake samples ranged from 24.0 to 47.5 mg/l (minimum target value was 20 mg/l; Table 20). During Test Cycle 1, the challenge water far exceeded the minimum concentrations for TSS, POC, and MM (Table 20); the ambient DSH TSS concentration was not taken into account when the solids injection was set up. Therefore, too much Micromate and Fine Arizona Test Dust was added to the Solids Injection System at the GSI Facility. GSI received written approval from JFE Engineering that this discrepancy did not invalidate Test Cycle 1. There was very little change in TSS concentration between the pre- and post-treatment samples. For MM, there was a slight reduction in post-treatment sample concentration compared to the pretreatment samples in Test Cycles 1 and 3, and a slight increase in Test Cycle 1. As to be expected, there was a higher %T (filtered and unfiltered) in post-treatment samples as compared to pretreatment samples. For organic carbon, however, there was an increase in NPOC, DOC, and POC

69 Page 69 of 146 concentrations in post-treatment intake samples compared to pre-treatment intake samples for all three test cycles with the exception of POC during Test Cycle 5, which remained unchanged. This increase may be due to the lack of isokinetic sampling methods for grab sample collection, which may have been exacerbated by the high rate of flow during these tests. Table 20. Average (± Standard Deviation, n=3) Concentration of Total Suspended Solids (TSS), Percent Transmittance (%T, in Filtered and Unfiltered Samples), Non-Purgeable Organic Carbon (NPOC), Dissolved Organic Carbon (DOC), Particulate Organic Carbon (POC), and Mineral Matter (MM) in Grab Samples Collected Simultaneously from the Pre- and Post-Treatment Line on Intake during Test Cycles 1, 3, and 5 of the of the JFE BallastAce BWMS Status Test. Test Cycle Sample Location (Pitot) Pre- Treatment (SP3c) Post- Treatment (SP15) Pre- Treatment (SP3c) Post- Treatment (SP15) Pre- Treatment (SP3c) Post- Treatment (SP15) TSS (mg/l) 58.6 (1.2) 57.8 (0.7) 28.0 (1.0) 28.3 (1.1) 30.3 (0.3) 31.3 (0.8) %T, Filtered/ Unfiltered 48.3 (0.1)/ 35.5 (0.3) 53.6 (0.1)/ 39.5 (0.1) 50.0 (0.1)/ 41.7 (0.5) 55.9 (0.3)/ 46.0 (0.4) 40.8 (0.2)/ 32.3 (0.1) 46.9 (0.4)/ 36.8 (0.6) NPOC (mg/l) DOC (mg/l) POC (mg/l) MM (mg/l) 17.9 (0.2) 6.8 (0.1) 11.1 (0.1) 47.5 (1.2) 21.0 (0.2) 8.7 (0.4) 12.3 (0.5) 45.5 (1.0) 10.8 (0.7) 6.8 (0.1) 4.0 (0.7) 24.0 (0.7) 13.6 (0.8) 8.1 (0.4) 5.5 (1.0) 22.8 (1.2) 13.6 (2.1) 8.3 (0.1) 5.3 (2.0) 25.0 (1.8) 15.2 (0.5) 9.9 (0.6) 5.4 (0.8) 26.0 (0.6) Sample Collection Tub Measurements The water quality data from measurements taken in the pre-treatment sample collection tubs during Test Cycles 1, 3, and 5 of the of the JFE BallastAce BWMS Status Test give a time-integrated picture of the challenge water characteristics and are presented in Table 21. The temperature ranged from to C during the three test cycles, declining over the course of the test period, which was within the range specified by the ETV Protocol (i.e., 4 to 35 C; Table 21). The turbidity measured during Test Cycle 3 (17.7 NTU) was slightly lower than Test Cycle 1 and 5 at 29.2 and 23.9 NTU, respectively (Table 21). The total chlorophyll and dissolved oxygen concentrations were also slightly lower in Test Cycle 3 compared to Test Cycle 1 and 5, but still well within the normal range for challenge water measured during similar types of tests conducted at the GSI Facility. All other parameters were very similar between all three test cycles.

70 Page 70 of 146 Table 21. Average Value (±Standard Deviation, n=2) of Water Quality Parameters Measured from Pre- Treatment Sample Collection Tubs During Test Cycles 1, 3, and 5 Intake of the JFE BallastAce BWMS Status Test. Parameter Test Cycle 1 Test Cycle 3 Test Cycle 5 Temperature ( C) ± ± ± 0.01 Specific Conductivity (ms/cm) ± ± ± Salinity (ppt) 0.09 ± ± ± 0.00 ph Turbidity (NTU) 29.2 ± ± ± 2.3 Total Chlorophyll (µg/l) 9.3 ± ± ± 0.2 Dissolved Oxygen (mg/l) 8.52 ± ± ± 0.04 Dissolved Oxygen (% Saturation) 83.7 ± ± ± Biological Conditions As shown in Table 22, Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test had live organism densities in the challenge water that exceeded the minimum criteria for challenge water total living populations specified by the ETV Land-Based Protocol (Table 2). For the largest regulated size class, nominally zooplankton, challenge water densities ranged from 136,000 to 346,000 live organisms per m 3, with Test Cycle 3 having the greatest density (Table 22). The 10 µm and < 50 µm size class, nominally protists, ranged from 1,267 to 3,899 live cells/ml in the challenge water, with Test Cycle 1 having the highest density (Table 22). The smallest regulated size class was represented by only culturable, aerobic, heterotrophic bacteria during this test. Live densities, as measured by the spread plate method, well exceeded the minimum density of 1,000/mL and ranged from 14,200 to 43,900 live bacteria per ml with Test Cycle 5 having the highest density (Table 22).

71 Page 71 of 146 Table 22. Live Plankton Density (n=1 each) and Average (± Standard Deviation, n=3) Microbial Concentration in Challenge Water Samples Collected during Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test. Regulated Size Class Parameter 50 µm Concentration (#/m 3 ) 10 µm and < 50 µm < 10 µm Concentration (cells/ml) Concentration (CFU/mL as culturable aerobic heterotrophic bacteria) TQAP Requirements Test Cycle 1 Test Cycle 3 Test Cycle 5 100,000 organisms/m 3 136, , ,000 1,000 organisms/ml 3,899 1,267 1,685 1,000/mL 14,200 (2,880) 26,800 (1,540) 43,900 (9,860) Retention Period Measurements During the 48 hour retention period associated with the JFE BallastAce BWMS Status Test, the TRO concentration in the control and treatment retention tanks was measured twice (once at 24 and once at 48 hours). Various water quality parameters were also measured every 15 minutes in both tanks and logged during retention BWMS Active Substance Concentrations As shown in Table 23, there were measurable TRO concentrations in the control retention tank during the 48 hour holding time ranging from to mg/l. Overall, these values were slightly lower than the pre-treatment intake TRO concentrations (Table 23). There was a substantial decrease in TRO concentration in the treated water during the 48 hour retention time, which indicates that there was marked chlorine demand still present in the intake water after treatment. All three test cycles had very similar TRO concentrations in the treatment retention tank at 24 and 48 hours post-treatment (Table 23). At 24 hours, the TRO concentration ranged from to mg/l (Table 23), on average this was a decrease of 89 % compared to post-treatment intake. At 48 hours, the TRO concentration ranged from to mg/l (Table 23), a 93 % decrease on average from post-treatment intake samples. Table 23. Concentration of Total Residual Oxidants (TRO) in the Control and Treatment Retention Tanks 24 and 48 Hours after Intake during Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test. Sample Location Control Retention Tank Treatment Retention Tank Collection Time (hour) Test Cycle 1 TRO (mg/l) Test Cycle 3 TRO (mg/l) Test Cycle 5 TRO (mg/l)

72 Water Quality Conditions GSI/LB/QAQC/TR/JFE Page 72 of 146 Table 24 shows the average water quality parameters measured using calibrated Sondes in the control and treatment retention tanks during the 48 hour holding time utilized during Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test. In most cases, each parameter was measured every 15 minutes during the holding period. However, during Test Cycle 3 the Sonde in the treatment retention tank was accidently set to log data every five seconds. As a result, the Sonde ran out of batteries and only logged data for approximately 31 hours of the 48 hour retention time. There were no unexpected differences in water quality measured from test cycle to test cycle. Overall, the water temperature during retention decreased from Test Cycle 1 to Test Cycle 5 (Table 24), which occurred approximately one month apart from each other during the end of the testing season. The specific conductivity, salinity, and ph increased slightly from Test Cycle 1 to Test Cycle 5 (Table 24). There were some notable, although expected, differences between the control and treatment retention tanks. The specific conductivity was slightly higher in the treatment retention tank as compared to the control retention tank, with the exception of Test Cycle 5 (Table 24). This is due to the addition of the NEO-CHLOR DICD Granules to the treated water and the subsequent increase in ions. There was also a slight decrease in ph in the treatment retention tank water as compared to the control retention tank, which is due to the formation of hypochloric and cyanuric acid upon dissolution of the NEO-CHLOR DICD Granules (Table 24). Total chlorophyll was markedly decreased in the treatment retention tank, which is due to the decrease in live protist density as a result of treatment (Table 24).

73 Page 73 of 146 Table 24. In-Situ Water Quality Parameters Measured in the Control and Treatment Retention Tanks during the 48 Hour Holding Time for Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test. Parameter Retention Tank Test Cycle 1 Test Cycle 3 Test Cycle 5 Temperature ( C) Control ± 0.23, n= ± 0.62, n= ± 0.38, n=167 Treatment ± 0.23, n= ± 0.29, n=17,387* 9.83 ± 0.38, n=165 Specific Conductivity Control ± 0.000, n= ± 0.000, n= ± 0.000, n=167 (ms/cm) Treatment ± 0.001, n= ± 0.000, n=17,387* ± 0.000, n=165 Salinity (ppt) Control 0.08 ± 0.00, n= ± 0.00, n= ± 0.00, n=167 Treatment 0.09 ± 0.00, n= ± 0.00, n=17,387* 0.10 ± 0.00, n=165 ph Control 7.38, n= , n= , n=167 Treatment 7.10, n= , n=17,387* 7.42, n=165 Turbidity (NTU) Control 24.3 ± 1.7, n= ± 1.3, n= ± 1.2, n=167 Treatment 23.5 ± 1.7, n= ± 1.2, n=17,387* 20.9 ± 1.2, n=165 Total Chlorophyll (µg/l) Control 10.1 ± 0.6, n= ± 0.6, n= ± 0.6, n=167 Treatment 4.4 ± 0.5, n= ± 0.2, n=17,387* 4.1 ± 0.2, n=165 Dissolved Oxygen Control 8.15 ± 0.09, n= ± 0.09, n= ± 0.04, n=167 (mg/l) Treatment 8.54 ± 0.01, n= ± 0.07, n=17,387* 9.65 ± 0.01, n=165 Dissolved Oxygen (% Control 79.5 ± 1.1, n= ± 1.4, n= ± 1.1, n=167 Saturation) Treatment 83.4 ± 0.4, n= ± 0.4, n=17,387* 85.2 ± 0.7, n=165 *The Sonde was set to log data every five seconds, rather than every 15 minutes as per the TQAP. Due to frequent datalogging, the Sonde ran out of batteries ~31 hours into the retention period Discharge Measurements Operational Conditions Control Discharge The operational data measured during discharge of the control retention tank for Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test are presented in Table 25. Data from all three test cycles are very similar. Control discharge occurred over an average duration of minutes; at a pressure of 1.77 bar and flow rate of 321 m 3 /hour, on average (Table 25). A total of 175 m 3 of water was discharged Zooplankton samples, all of which were collected from Sample Collection Tub #1, represented an average of 3.10 m 3 concentrated to 1 L (Table 25).

74 Page 74 of 146 Table 25. Summary of Operational Measurements and Data Collected during Control Retention Tank Discharge for Test Cycles 1, 3, and 5 of the BallastAce BWMS Status Test using NEO-CHLOR DICD Granules as the Active Substance. Parameter Units Test Cycle 1 Test Cycle 3 Test Cycle 5 Average Date and Start Time Sep-14 13:58:50 04-Oct-14 12:27:10 11-Oct-14 11:29:10 Duration min Discharge Line Pressure (Average ± Std. Deviation) Discharge Flow Rate (Average ± Std. Deviation) Volume Discharged from Retention Tank Sample Collection Tub #1 Volume bar 1.83 ± ± ± ± 0.06 m 3 /hour 325 ± ± ± ± 3 m ± 3 m ± Treatment Discharge Table 26 shows operational data measured during discharge of the treatment retention tanks for Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test. As with the control discharge data, the average values from each test cycle are very similar. The treatment discharge operation was an average of minutes in duration (Table 26). There was a slight difference in pressure, 0.49 bar on average, between the pre-neutralization line and the post-neutralization line. This difference was not as great as during intake because the FS of the BWMS was not active during discharge. The average treatment discharge flow rate was 316 m 3 /hour, and an average 182 m 3 of water from the treatment retention tank was discharged (Table 26). Zooplankton samples were collected from Sample Collection Tub #s 4 and 5, which had an average sample volume of 3.14 m 3 and 3.13 m 3, respectively (Table 26).

75 Page 75 of 146 Table 26. Summary of Operational Measurements and Data Collected during Treatment Retention Tank Discharge for Test Cycles 1, 3, and 5 of the BallastAce BWMS Status Test using NEO-CHLOR DICD Granules as the Active Substance. Parameter Units Test Cycle 1 Test Cycle 3 Test Cycle 5 Average Date and Start Time Sep-14 09:34:40 04-Oct-14 09:30:10 11-Oct-14 09:37:00 Duration min Pre-Neutralization Line Pressure (Average ± Std. bar 2.06 ± ± ± ± 0.05 Deviation) Post-Neutralization Line Pressure (Average ± Std. bar 1.55 ± ± ± ± 0.04 Deviation) Differential Pressure* (Average ± Std. Deviation) bar 0.51 ± ± ± ± 0.02 Flow Rate (Average ± Std. Deviation) m 3 /hour 318 ± ± ± ± 2 Volume Discharged from Retention Tank m ± 5 Sample Collection Tub #4 Volume m ± 0.10 Sample Collection Tub #5 Volume m ± 0.10 Sample Collection Tub #6 Volume m ± 0.07 *BWMS filter was not active during discharge BWMS Active Substance Concentrations The TRO concentration in grab samples collected throughout control and treatment tank discharge operations of the JFE BallastAce BWMS Status Test is presented in Table 27. The TRO in control discharge water ranged from below the method detection limit to mg/l (Table 27), which was in keeping with the range of TRO concentrations measured in pre-treatment water during these three test cycles. The range of TRO concentrations measured in the treatment discharge samples was only slightly higher, ranging from below the method detection limit to mg/l (Table 27). The treatment discharge water was sent to the GSI Facility s wastewater holding tank where the TRC concentration was measured; in all cases the TRC concentration was below the permitted level of mg/l (data not presented) and the water was discharged to the City of Superior Wastewater Treatment Plant (during Test Cycle 1) or the DSH (Test Cycles 3 and 5).

76 Page 76 of 146 Table 27. Concentration of Total Residual Oxidants (TRO) in Grab Samples Collected During Test Cycles 1, 3, and 5 Control and Treatment Tank Discharge Operations of the JFE BallastAce BWMS Status Test. ND = Measured value was below the method detection limit. Sample Location (Pitot) Collection Time (min) Test Cycle 1 (TRO (mg/l) Test Cycle 3 (TRO (mg/l) Test Cycle 5 (TRO (mg/l) ND Control ND (SP9c) ND ND * Treatment * (SP15) * * ND * During Test Cycle 1, all treatment discharge grab samples were collected from SP16 rather than SP Water Quality Conditions Grab Samples Table 28 shows the measured water quality data from grab samples collected throughout discharge of the control and treatment retention tanks of the JFE BallastAce BWMS Status Test. As expected, %T (both filtered and unfiltered) was higher in the treatment discharge samples than in the control discharge samples. The chlorine in the treated water continued to oxidize and break down (i.e., bleach ) the organic matter (e.g., tannic and humic acid) during retention, resulting in treatment discharge water that was more transparent than the control water.

77 Page 77 of 146 Table 28. Average (± Standard Deviation, n=3) Concentration of Total Suspended Solids (TSS), Percent Transmittance (%T, in Filtered and Unfiltered Samples), Non-Purgeable Organic Carbon (NPOC), Dissolved Organic Carbon (DOC), Particulate Organic Carbon (POC), and Mineral Matter (MM) in Grab Samples Collected Sequentially from the Treatment and Control Line on Discharge during the JFE BallastAce BWMS Status Test. Test Cycle Sample Location (Pitot) Control (SP9a) Treatment (SP16) Control (SP9a) Treatment (SP15) Control (SP9a) Treatment (SP15) TSS (mg/l) 29.8 (5.9) 40.2 (15.0) 9.5 (0.5) 11.9 (1.2) 14.5 (2.1) 15.5 (1.0) %T, Filtered/ Unfiltered 48.0 (0.2)/ 36.7 (0.5) 52.6 (0.3)/ 42.0 (0.1) 49.9 (0.0)/ 42.4 (0.2) 55.5 (0.1)/ 46.5 (0.4) 41.2 (0.4)/ 33.2 (0.1) 46.4 (0.3)/ 37.6 (0.1) NPOC (mg/l) DOC (mg/l) POC (mg/l) MM (mg/l) 13.4 (3.0) 6.8 (0.1) 6.6 (2.9) 23.2 (6.2) 16.7 (3.8) 9.0 (0.1) 7.7 (3.8) 32.5 (11.2) 8.7 (0.3) 6.9 (0.1) 1.8 (0.2) 7.7 (0.7) 10.5 (0.4) 8.3 (0.0) 2.2 (0.4) 9.6 (0.9) 11.6 (1.2) 8.2 (0.1) 3.4 (1.1) 11.1 (1.1) 12.3 (0.5) 10.0 (0.1) 2.3 (0.5) 13.2 (0.7) Sample Collection Tub Measurements Table 29 shows water quality parameters measured in the sample collection tubs associated with the JFE BallastAce BWMS Status Test using calibrated Sondes immediately following discharge of the control and treatment retention tanks. Test Cycles 1 and 5 were conducted nearly one month apart, therefore, the temperature declined ~5 C between those two test cycles (Table 29). The specific conductivity and salinity increased slightly from Test Cycle 1 to Test Cycle 5 (Table 29). Overall, the specific conductivity was higher in the treatment discharge water than the control discharge water due to the added ions from treatment with NEO-CHLOR DICD Granules and neutralization with sodium sulfite (Table 29). The total chlorophyll concentration in the control discharge was higher than in the treatment discharge due to the decreased protist density as a result of treatment (Table 29). For all other parameters, there was no discernible trend between test cycles or within a test cycle (control versus treatment; Table 29).

78 Page 78 of 146 Table 29. Water Quality Parameters Measured in Control (Sample Collection Tub #s 1 and 2) and Treatment (Sample Collection Tub #s 4-6) Sample Collection Tubs Immediately Following Discharge Operations during Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test. Parameter Sample Type Test Cycle 1 Test Cycle 3 Test Cycle 5 Temperature ( C) Specific Conductivity (ms/cm) Salinity (ppt) ph Turbidity (NTU) Total Chlorophyll (µg/l) Dissolved Oxygen (mg/l) Dissolved Oxygen (% Saturation) CONT, n= ± ± ± 0.02 TRT, n= ± ± ± 0.09 CONT, n= ± ± ± TRT, n= ± ± ± CONT, n= ± ± ± 0.00 TRT, n= ± ± ± 0.00 CONT, n= TRT, n= CONT, n= ± ± ± 0.1 TRT, n= ± ± ± 0.4 CONT, n=2 9.1 ± ± ± 0.0 TRT, n=3 5.2 ± ± ± 0.3 CONT, n= ± ± ± 0.02 TRT, n= ± ± ± 0.07 CONT, n= ± ± ± 0.2 TRT, n= ± ± ± Biological Conditions The control and treatment discharge densities of the three regulated size classes associated with JFE BallastAce BWMS Status Test are presented in Table 30; more detailed taxonomic data are available on request. The control discharge density of the 50 µm size class greatly exceeded the minimum concentration of 100 live organisms/m 3 specified in the ETV Protocol, ranging from 290,000/m 3 to 494,000/m 3 (Table 30). There was a marked decrease in treatment discharge density as compared to control discharge density for all three test cycles. Test Cycle 1 had the highest treatment discharge density, with 597 live organism/m 3 (i.e., 99.8 % reduction compared to control discharge; Table 30). Test Cycle 3 had 368 live organisms/m 3 (i.e., 99.9 % reduction compared to control discharge; Table 30) and Test Cycle 5 had 382 live organisms/m 3 (i.e., 99.9 % reduction compared to control discharge; Table 30). All three test cycles had treatment discharge densities that were well above the USCG BWDS of 10 live organisms/m 3. The control discharge density of the 10 µm and < 50 µm size class also greatly exceeded the ETV Protocol minimum required density of 100 organisms/ml; live density ranged from 637 cells/ml to 2,451 cells/ml (Table 30). There was a substantial decrease in live organism density in the treatment discharge as compared to the control discharge, with densities ranging from 0.16 cell/ml to 197 cells/ml (Table 30). Test Cycle 1 had a much higher live cell density in treatment discharge samples than Test Cycles 3 or 5 (Table 30). Of the 197 live cells/ml, 191 cells were from one colony of blue-green algae (Microcystis-like coccoid algae). The individual cells within this colony were less than 10 µm in minimum dimension but the colony itself was within the size class, which is in keeping with GSI s sizing and reporting practices for this size class of organisms. The remaining 6 live cells/ml were small flagellates (Cryptomonas/Chroomonaas-type; 5 cells/ml) and

79 Page 79 of 146 centric solitary diatom (1 cell/ml). Test Cycles 3 and 5 met the USCG BWDS for this size class of organisms. The live density of culturable, aerobic heterotrophic bacteria (i.e., < 10 µm size class) in control discharge was far greater than the minimum concentration of 500/mL specified in the ETV Protocol. The control discharge density ranged from an average of 40,600 CFU/mL to 62,300 CFU/mL (Table 30). There was a substantial decrease in heterotrophic bacteria density in the treatment discharge as compared to the control, ranging from an average of 461 CFU/mL to 2,850 CFU/mL (Table 30). There was a 97.4 % reduction in density compared to the control during Test Cycle 1. During Test Cycles 3 and 5, there was a 98.9 % and 95.4 % reduction, respectively, in comparison to control discharge densities. There is no discharge standard for heterotrophic bacteria; these densities cannot be compared to any regulation. Table 30. Live Plankton Density (Average ± Standard Deviation, Where Applicable) and Average (± Standard Deviation, n=3) Microbial Concentrations in Samples Collected During Control and Treatment Retention Tank Discharge for Test Cycles 1, 3, and 5 of the JFE BallastAce BWMS Status Test. Regulated Size Class 50 µm 10 µm and < 50 µm < 10 µm (CFU/mL as culturable aerobic heterotrophic bacteria) Maximum Concentration in Treated Discharge Test Cycle 1 Test Cycle 3 Test Cycle 5 Control Treatment Control Treatment Control Treatment < 10 organisms per m 3 290, , , < 10 organisms per ml 2, , No discharge standard for 50,500 1,300 40, ,300 2,850 heterotrophic (4,380) (111) (4,230) (235) (6,740) (2,600) bacteria Disinfection Byproducts (DBPs) Concentrations The results from analysis of selected DBPs in samples collected during Test Cycles 1 and 5 control and treatment discharge of the JFE BallastAce BWMS Status Test are presented in Table 31. Samples were collected for DBP analysis only during those test cycles that were selected for WET testing. There were elevated concentrations of all classes of DBPs in the treatment discharge as compared to the control discharge. In the control discharge samples, all of the selected DBPs were below the limit of detection with the exception of dichloroacetic acid, which was slightly elevated during Test Cycle 1, and total sodium during Test Cycle 1 and 5 (Table 31). Of all DBPs measured, the trihalomethanes had the highest concentration in treatment discharge, with an average of 214 µg/l in Test Cycle 1 and 155 µg/l in Test Cycle 5 (Table 31). Chloroform was the primary contributor and bromodichloromethane was a secondary contributor in the treatment discharge samples. Test Cycle 1 had an average of 114 µg/l total haloacetic acids in treatment discharge, while Test Cycle 5 had an average of 95 µg/l (Table 31). Dichloroacetic acid and trichloroacetic acid were the primary contributors to the total concentration of haloacetic acids in treatment discharge. The average concentration of total haloacetonitriles in treatment discharge was 41 µg/l and 37 µg/l in Test Cycle 1 and 5, respectively (Table 31); the majority of the total was from

80 Page 80 of 146 chloral hydrate. Test Cycles 1 and 5 had similar DBP results for treatment discharge samples, with the exception of the chlorate ion. During Test Cycle 1 only one of three replicates had a chlorate concentration above the limit of detection, however, during Test Cycle 5 all three replicates had a chlorate concentration above the limit of detection with an average of 51 µg/l (Table 31). Total sodium was only slightly higher in treatment discharge as compared to control discharge (Table 31). Table 31. Results from Analysis of Selected Disinfection Byproducts in Samples Collected during Discharge of the Control and Treatment Retention Tanks in Test Cycles 1 and 5 of the JFE BallastAce BWMS Status Test. Samples were collected for analysis of disinfection byproducts only for those test cycles with Whole Effluent Toxicity testing. Analyte Formula Control Average (µg/l) Test Cycle 1 Test Cycle 5 Treatment Average (µg/l) Control Average (µg/l) Treatment Average (µg/l) Bromodichloromethane CHBrCl 2 < < Bromoform CHBr 3 < 0.5 < 0.5 < 0.5 < 0.5 Chlorodibromomethane CHBr 2 Cl < < Chloroform CHCl 3 < < Total Trihalomethanes < < Bromochloroacetic acid* BrClCHCOOH < < Dibromoacetic acid CHBr 2 COOH < 1.0 < 1.0 < 1.0 < 1.0 Dichloroacetic acid CHCl 2 COOH < Monobromoacetic acid CH 2 BrCOOH < 1.0 < 1.0 < 1.0 < 1.0 Monochloroacetic acid CH 2 ClCOOH < < Trichloroacetic acid CCl 3 COOH < < Total Haloacetic Acids < ,1,1-trichloro-2-Propanone CCl 3 COCH 3 < < ,1-dichloro-2-Propanone CH 3 COCHCl 2 < < Bromochloroacetonitrile C 2 HBrClN < 0.5 < 0.5 < Bromoacetonitrile BrCH 2 CN < 0.5 < 0.5 < 0.5 < 0.5 Chloral hydrate Cl 3 CCH(OH) 2 < < Chloroacetonitrile ClCH 2 CN < 0.5 < 0.5 < 0.5 < 0.5 Chloropicrin Cl 3 CNO 2 < 0.5 < 0.5 < 0.5 < 0.5 Dibromoacetonitrile Br 2 CHCN < 0.5 < 0.5 < 0.5 < 0.5 Dichloroacetonitrile Cl 2 CHCN < < Trichloroacetonitrile Cl 3 CCN < 0.5 < 0.5 < 0.5 < 0.5 Total Haloacetonitriles < < Bromate BrO 3 - Chlorate ClO 3 - < 5.0 < 5.0 < 5.0 < 5.0 < < Sodium, Total Na *Not included in total haloacetic acids.

81 Page 81 of Whole Effluent Toxicity (WET) Treatment discharge water was collected during Test Cycles 1 and 5 of the JFE BallastAce BWMS Status Test for analysis of WET. The results are described in separate sections below Test Cycle 1 The water quality parameters measured in stock solutions prepared prior the start of Test Cycle 1 WET testing and prior to daily renewal of test water during the C. dubia and P. promelas WET tests are presented in Table 32. The temperature of the prepared stock solutions was within the acceptance range of 25 C ± 3 C in all cases (Table 32). In addition, the dissolved oxygen concentration was above the minimum value specified for P. promelas (i.e., 4.0 mg/l) in all cases (Table 32). All other water quality parameters measured (i.e., ph, conductivity, hardness, and alkalinity) were within the expected ranges for the water types measured (Table 32). There was no detectable TRO in the C. dubia or P. promelas performance control stock solutions (Table 32). The TRO concentration in the experimental control (i.e., 0 % Whole Effluent) ranged from below the limit of detection to mg/l (Table 32), which is within the range of TRO values measured historically in samples collected from the DSH. There was measurable TRO in the 100 % Whole Effluent treatment stock solutions for the entire duration of both tests; the average TRO concentration was mg/l (Table 32).

82 Treatment Group GSI/LB/QAQC/TR/JFE Page 82 of 146 Table 32. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Stock Solutions during Ceriodaphnia dubia and Pimephales promelas Whole Effluent Toxicity (WET) Test Associated with Test Cycle 1 of the JFE BallastAce BWMS Status Test. Temperature ( C) C. dubia 24.3 Performance Control 1 (23.3, 25.2) P. promelas 24.6 Performance Control 2 (24.3, 24.9) 0 % Whole 25.4 Effluent 3 (24.6, 27.2) 6.25 % Whole Effluent 12.5 % Whole Effluent 25 % Whole Effluent 50 % Whole Effluent 100 % Whole Effluent 25.8 (25.0, 26.7) 25.9 (25.1, 27.7) 25.5 (25.0, 27.3) 25.3 (24.7, 26.6) 25.3 (24.1, 26.4) Dissolved Oxygen (mg/l) 8.3 (8.0, 8.5) 6.0 (5.6, 6.6) 9.6 (8.8, 11.0) 9.0 (8.5, 9.5) 8.9 (8.5, 9.5) 8.9 (8.4, 9.3) 8.9 (8.4, 9.4) 9.1 (8.3, 10.2) ph 8.42 (8.37, 8.47) 7.21 (6.87, 7.61) 7.89 (7.86, 7.94) 7.89 (7.66, 7.97) 7.87 (7.68, 7.95) 7.76 (7.41, 7.93) 7.51 (7.24, 7.86) 7.32 (7.01, 7.71) Conductivity (µs/cm) 576 (530, 585) (142.5, 163.4) (181.7, 186.5) (184.7, 188.0) (185.2, 187.2) (186.7, 189.0) (188.0, 190.6) (189.6, 194.8) Hardness 4 (mg/l CaCO 3 ) Alkalinity 4 (mg/l CaCO 3 ) TRO (mg/l) <DL <DL * Q (<DL, Q ) 0.010* Q (<DL, Q ) 0.011* Q (<DL, Q ) 0.013* Q (<DL, Q ) 0.020* (DL, 0.033) (0.019, 0.056) 1 Hard Reconstituted Water; 2 Dechlorinated Laboratory Water; 3 Filtered Duluth-Superior Harbor Water; 4 Hardness and alkalinity were only measured on Day 0 and do not have minimum and maximum values. * Values less than the detection limit (DL) which equals mg/l were not used to calculate the average TRO value. Q Sample concentration was below the LOQ ( mg/l TRO). The water quality parameters measured in the C. dubia exposure solutions following each 24 hour renewal period are presented in Table 33. The temperature of the exposure solutions was within the acceptance range of 25 C ± 3 C during the entire seven day test. All other water quality parameters measured (i.e., ph, hardness, and alkalinity) were within the expected ranges for the water types measured (Table 33).

83 Page 83 of 146 Table 33. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Seven Day Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Test Cycle 1 of the JFE BallastAce BWMS Status Test. Treatment Group Temperature ( C) ph Hardness 3 (mg/l CaCO 3 ) Alkalinity 3 (mg/l CaCO 3 ) C. dubia Performance Control (23.6, 24.7) (8.33, 8.40) % Whole Effluent (24.1, 24.4) (8.19, 8.28) % Whole Effluent (24.2, 24.6) (8.12, 8.21) % Whole Effluent (23.8, 24.7) (8.11, 8.19) % Whole Effluent (23.5, 24.8) (8.14, 8.22) % Whole Effluent (23.9, 24.7) (8.11, 8.21) % Whole Effluent (23.7, 24.5) (8.07, 8.19) Hard Reconstituted Water; 2 Filtered Duluth-Superior Harbor Water; 3 Hardness and alkalinity are only measured on Day 6 (test termination) and do not have minimum and maximum values. Table 34 shows the survival and reproduction data from the seven day, three-brood C. dubia WET test conducted during Test Cycle 1. In order for the test results to be acceptable there must have been at least 80 % survival and an average total number of at least 15 young per female in the experimental control (0 % Whole Effluent). The WET test met these criteria with 100 % survival and 25.4 average young per female. The Performance Control is used to determine overall health of the test organisms and not test result acceptance, however, the Performance Control also met the WET test QC criteria indicating that the organisms used in this WET test were of good health. There was no effect of whole effluent on survival, with all of the treatment groups having either 90 % or 100 % adult survival (Table 34). There was no statistically significant (p<0.05) effect of whole effluent on reproduction in the 6.25 %, 12.5 %, and 25 % dilutions when compared to the experimental control. The 50 % Whole Effluent treatment had an average of 18.0 young per female, while the 100 % Whole Effluent treatment had an average of 13.9 young per female (Table 34); each of these results represents a statistically significant (p<0.05) effect of whole effluent on reproduction when compared to the experimental control. There was no Facility Control used during Test Cycle 1, which had a high concentration of suspended solids relative to all other test cycles in the JFE BallastAce BWMS Status Test. Therefore, GSI can only conclude that the reproductive effect resulting in the 50 % and 100 % Whole Effluent treatment groups is the product of treatment/neutralization and high suspended solids in the whole effluent; these effects cannot be separated out.

84 Page 84 of 146 Table 34. Average (n=10) Percent Survival and Total Number of Offspring Produced in a Three-Brood Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Treatment Discharge from Test Cycle 1 of the JFE BallastAce BWMS Status Test. Treatment Group Percent Survival ± Std. Deviation Average Total Number of Young per Female ± Std. Deviation C. dubia Performance Control 1 90 ± ± % Whole Effluent ± ± % Whole Effluent 100 ± ± % Whole Effluent 90 ± ± % Whole Effluent 90 ± ± % Whole Effluent 100 ± ± 6.2 a 100 % Whole Effluent 100 ± ± 5.2 a 1 Hard Reconstituted Water; 2 Filtered Duluth-Superior Harbor Water a The differences in the mean values of survival and average number of young per adult are statistically different compared to the Filtered Duluth-Superior Harbor Water Control (p<0.05). The water quality parameters measured in the P. promelas exposure solutions following each 24 hour renewal period are presented in Table 35. The temperature of the exposure solutions was within the acceptance range of 25 C ± 3 C during the entire seven day test. In addition, the dissolved oxygen concentration was greater than 4.0 mg/l in all cases (Table 35). All other water quality parameters measured (i.e., ph, hardness, and alkalinity) were within the expected ranges for the water types measured (Table 35).

85 Page 85 of 146 Table 35. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Pimephales promelas Whole Effluent Toxicity (WET) Test Associated with Test Cycle 1 of the JFE BallastAce BWMS Status Test. Sample ID Temperature ( C) Dissolved Oxygen (mg/l) ph Hardness 3 (mg/l CaCO 3 ) Alkalinity 3 (mg/l CaCO 3 ) P. promelas Performance Control 1 (24.5, 25.6) (5.5, 7.1) (7.50, 7.82) % Whole Effluent (24.5, 25.4) (4.9, 6.7) (7.53, 7.90) No Data % Whole Effluent (24.2, 25.0) (5.8, 7.1) (7.63, 8.00) % Whole Effluent (23.9, 25.2) (5.5, 6.8) (7.61, 7.87) % Whole Effluent (23.9, 25.1) (5.5, 6.6) (7.62, 7.85) % Whole Effluent (23.8, 24.9) (5.5, 6.9) (7.61, 7.91) % Whole Effluent (24.1, 25.1) (5.0, 6.8) (7.55, 7.70) Dechlorinated Laboratory Water; 2 Filtered Duluth-Superior Harbor Water; 3 Hardness and alkalinity are only measured on Day 7 (test termination) and do not have minimum and maximum values; 4 An air bubble appeared in the burette during titration and an endpoint could not be determined for the only sample that could be collected from this test. Table 36 shows the survival and growth data from the seven day P. promelas WET test conducted during Test Cycle 1 of the JFE BallastAce BWMS Status Test. In order for the test results to be acceptable there must have been at least 80 % survival and an average dry weight per surviving organism of at least 0.25 mg in the experimental control (0 % Whole Effluent). The WET test met these criteria with 100 % survival and mg per fish (Table 36). The Performance Control also met the WET test QC criteria indicating that the organisms used in this WET test were of good health. There was no effect of whole effluent on survival, with all of the treatment groups having 97 % to 100 % adult survival (Table 36). There was no statistically significant (p<0.05) effect of whole effluent on growth in any of the treatment groups tested.

86 Page 86 of 146 Table 36. Pimephales promelas Average (n=4) Percent Survival and Weight per Fish after Exposure to Treatment Discharge from Test Cycle 1 of the JFE BallastAce BWMS Status Test. Treatment Group Percent Survival ± Std. Deviation Mean Average Weight/Fish (mg) ± Std. Deviation P. promelas Performance Control 1 98 ± ± % Whole Effluent ± ± % Whole Effluent 100 ± ± % Whole Effluent 97 ± ± % Whole Effluent 97 ± ± % Whole Effluent 100 ± ± % Whole Effluent 97 ± ± Dechlorinated Laboratory Water; 2 Filtered Duluth-Superior Harbor Water The water quality parameters measured in the S. capricornutum exposure solutions on Day 0 and in the chemistry replicate flask every 24 hours during the 96 hour WET test are presented in Table 37. The temperature of the exposure solutions was within the acceptance range of 25 C ± 3 C during the entire seven day test (Table 37). All other water quality parameters measured (i.e., dissolved oxygen, ph, conductivity, hardness, and alkalinity) were within the expected ranges for the water types measured.

87 Page 87 of 146 Table 37. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Selenastrum capricornutum Whole Effluent Toxicity (WET) Test Associated with Test Cycle 1 of the JFE BallastAce BWMS Status Test. Temperatur Treatment Group e ( C) S. capricornutum 24.9 Performance Control 1 (24.3, 25.3) 0 % Whole Effluent (24.3, 25.1) 6.25 % Whole Effluent 12.5 % Whole Effluent 25 % Whole Effluent 50 % Whole Effluent 100 % Whole Effluent 24.7 (24.1, 25.2) 24.6 (23.9, 25.1) 24.6 (24.0, 25.1) 24.5 (23.8, 25.0) 24.5 (23.8, 25.1) Dissolved Oxygen 3 (mg/l) ph 7.85 (7.42, 10.03) 8.34 (7.95, 9.79) 8.40 (8.00, 9.77) 8.41 (8.02, 9.74) 8.43 (8.04, 9.74) 8.41 (7.99, 9.66) 8.31 (7.82, 9.63) Conductivity 3 (µs/cm) Hardness 3 (mg/l CaCO 3 ) Alkalinity 3 (mg/l CaCO 3 ) TRO (mg/l) <DL <DL USEPA Nutrient Media; 2 Filtered Duluth-Superior Harbor Water; 3 Conductivity, dissolved oxygen, hardness, and alkalinity were measured only on Day 0 and do not have minimum and maximum values. Table 38 shows the growth data from the 96 hour S. capricornutum WET test conducted during Test Cycle 1 of the JFE BallastAce BWMS Status Test. In order for the test results to be acceptable there must have been at least 1 x 10 6 cells/ml at test termination and the cell density must not have varied by more than 20 % CV among replicate flasks in the experimental control (0 % Whole Effluent). The WET test met these criteria with a cell density of 2,393,750 cells/ml and a CV of 12 % among experimental control replicates (Table 38). The Performance Control also met the WET test QC criteria indicating that the organisms were of good health. Although the highest cell density was in the 100 % Whole Effluent, there was no statistically significant effect (p<0.05) of whole effluent on growth, with average cell density ranging from 2,703,125 cells/ml to 3,856,250 cells/ml (Table 38).

88 Page 88 of 146 Table 38. Average (n=4) Cell Density of Selenastrum capricornutum after 96 Hours Exposure to Whole Effluent from Test Cycle 1 Treatment Discharge of the JFE BallastAce BWMS Status Test. Treatment Group Average Cells/mL ± Std. Deviation S. capricornutum Performance Control 1 3,309,375 ± 478,319 0% Whole Effluent 2 2,393,750 ± 296, % Whole Effluent 2,762,500 ± 222, % Whole Effluent 2,703,125 ± 566,547 25% Whole Effluent 2,771,875 ± 178,645 50% Whole Effluent 2,956,250 ± 560, % Whole Effluent 3,856,250 ± 383,038 1 USEPA Nutrient Media; 2 Filtered Duluth-Superior Harbor Water Test Cycle 5 The TRO concentration in the C. dubia Performance Control stock solution ranged from below the method detection limit to mg/l to the start of Test Cycle 5 WET testing and prior to daily renewal of test water during the C. dubia and P. promelas WET tests are presented in Table 39. The temperature of the prepared stock solutions was within the acceptance range of 25 C ± 3 C in all cases (Table 39). In addition, the dissolved oxygen concentration was above the minimum value specified for P. promelas (i.e., 4.0 mg/l) in all cases (Table 39). All other water quality parameters measured (i.e., ph, conductivity, hardness, and alkalinity) were within the expected ranges for the water types measured (Table 39). There was no detectable TRO in the P. promelas Performance Control stock solutions (Table 39). Interestingly, the TRO values in the Facility Control (i.e., control discharge water) were higher than those measured in any of the whole effluent treatment groups (i.e., treatment discharge water). However, the range of TRO concentrations measured in the Facility Control were still within the range of TRO values measured historically in samples collected from the DSH. There was measurable TRO in all of the whole effluent treatment groups for the entire duration of the C. dubia and P. promelas WET tests, ranging from as low as mg/l to mg/l overall (Table 39).

89 Treatment Group GSI/LB/QAQC/TR/JFE Page 89 of 146 Table 39. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Stock Solutions during the Ceriodaphnia dubia and Pimephales promelas Whole Effluent Toxicity (WET) Tests Associated with Test Cycle 5 of the JFE BallastAce BWMS Status Test. Temperature ( C) C. dubia 24.4 Performance Control 1 (22.8, 25.0) P. promelas 24.4 Performance Control 2 (24.0, 24.8) 25.0 Facility Control (23.8, 26.4) 0% Whole 24.3 Effluent 3 (23.9, 24.9) 6.25% Whole Effluent 12.5% Whole Effluent 25% Whole Effluent 50% Whole Effluent 100% Whole Effluent 24.4 (23.6, 25.3) 24.5 (23.7, 25.7) 24.5 (23.7, 25.7) 24.7 (23.9, 25.6) 25.3 (24.2, 27.5) Dissolved Oxygen (mg/l) 8.1 (7.5, 8.7) 6.8 (6.5, 7.3) 10.2 (9.5, 11.2) 10.6 (8.5, 11.8) 9.5 (8.4, 10.4) 9.5 (8.4, 10.3) 9.4 (8.3, 10.2) 9.4 (8.3, 10.1) 10.4 (9.6, 11.2) ph 8.43 (8.42, 8.46) 7.49 (7.39, 7.64) 7.67 (7.55, 7.79) 7.90 (7.79, 7.96) 7.92 (7.84, 7.97) 7.88 (7.74, 7.96) 7.88 (7.73, 7.97) 7.72 (7.44, 7.88) 7.60 (7.47, 7.67) Conductivity (µs/cm) 586 (580, 594) (149.8, 181.8) 221 (220, 222) 209 (207, 213) 210 (207, 211) 211 (208, 213) 214 (210, 215) 221 (219, 222) 233 (231, 234) Hardness 4 (mg/l CaCO 3 ) Alkalinity 4 (mg/l CaCO 3 ) TRO (mg/l) <DL (<DL, Q ) <DL (0.039, 0.050) 0.012* (0.006 Q, 0.022) Q (0.006 Q, 0.022) Q (0.006 Q, 0.029) (0.015 Q, 0.035) (0.021, 0.038) (0.021, 0.048) 1 Hard Reconstituted Water; 2 Dechlorinated Laboratory Water; 3 Filtered Duluth-Superior Harbor Water; 4 Hardness and alkalinity were only measured on Day 0 and do not have minimum and maximum values. * Values less than the detection limit (DL) which equals mg/l were not used to calculate the average TRO value. Q Sample concentration was below the LOQ ( mg/l TRO). The water quality parameters measured in the C. dubia exposure solutions following each 24 hour renewal period are presented in Table 40. The temperature of the exposure solutions was within the acceptance range of 25 C ± 3 C during the entire six day test (Table 40). All other water quality parameters measured (i.e., ph, hardness, and alkalinity) were within the expected ranges for the water types measured.

90 Page 90 of 146 Table 40. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Six Day Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Test Cycle 5 of the JFE BallastAce BWMS Status Test. Treatment Group Temperature ( C) ph Hardness 3 (mg/l CaCO 3 ) Alkalinity 3 (mg/l CaCO 3 ) C. dubia Performance Control (23.7, 24.4) (7.83, 8.43) Facility Control (23.8, 24.4) (8.24, 8.34) % Whole Effluent (23.8, 24.6) (8.21, 8.27) % Whole Effluent (23.2, 24.6) (8.20, 8.25) % Whole Effluent (23.8, 24.6) (8.17, 8.26) % Whole Effluent (24.0, 24.7) (8.16, 8.27) % Whole Effluent (23.5, 24.6) (8.18, 8.28) % Whole Effluent (24.0, 24.8) (8.16, 8.27) Hard Reconstituted Water; 2 Filtered Duluth-Superior Harbor Water; 3 Hardness and alkalinity were only measured on Day 6 (i.e., at test termination) and do not have minimum and maximum values. Table 41 shows the survival and reproduction data from the six day, three-brood C. dubia WET test conducted during Test Cycle 5 of the JFE BallastAce BWMS Status Test. In order for the test results to be acceptable there must have been at least 80 % survival and an average total number of at least 15 young per female in the experimental control (0 % Whole Effluent). The WET test met these criteria with 100 % survival and 22.0 average young per female (Table 41). The Performance Control, which is used to determine overall health of the test organisms and not test result acceptance, did not meet the test QC criteria. This result may be attributed to the fact that the C. dubia (purchased from Environmental Consulting and Testing, Inc.) were cultured in Moderately- Hard Reconstituted Water (specific conductivity range = µs/cm) and the Performance Control was Hard Reconstituted Water (specific conductivity range = µs/cm). Therefore, osmotic shock may have caused the low survival and reproduction in this case. Results from the Facility Control indicate that there was no statistically significant (p<0.05) effect of control discharge water on adult survival or reproduction (Table 41). In addition, there was no statistically significant (p<0.05) effect of whole effluent from treatment discharge on adult survival or reproduction when compared to the experimental control (Table 41).

91 Page 91 of 146 Table 41. Average (n=10) Percent Survival and Total Number of Offspring Produced in a Three-Brood Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Treatment Discharge from Test Cycle 5 of the JFE BallastAce BWMS Status Test. Treatment Group Percent Survival ± Std. Deviation Average Total Number of Young per Female ± Std. Deviation C. dubia Performance Control 1 60 ± ± 3.7 Facility Control 100 ± ± % Whole Effluent 2 90 ± ± % Whole Effluent 90 ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± Hard Reconstituted Water; 2 Filtered Duluth-Superior Harbor Water The water quality parameters measured in the P. promelas exposure solutions following each 24 hour renewal period are presented in Table 42. The temperature of the exposure solutions was within the acceptance range of 25 C ± 3 C during the entire seven day test (Table 42). The dissolved oxygen concentration was greater than 4.0 mg/l in all treatment groups with the exception of the 100 % Whole Effluent, which had a minimum dissolved oxygen concentration of 3.6 mg/l (Table 42). All other water quality parameters measured (i.e., ph, hardness, and alkalinity) were within the expected ranges for the water types measured (Table 42).

92 Page 92 of 146 Table 42. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Pimephales promelas Whole Effluent Toxicity (WET) Test Associated with Test Cycle 5 of the JFE BallastAce BWMS Status Test. Treatment Group Temperature ( C) Dissolved Oxygen (mg/l) ph Hardness 3 (mg/l CaCO 3 ) Alkalinity 3 (mg/l CaCO 3 ) P. promelas Performance Control 1 (23.5, 24.9) (5.9, 7.2) (7.50, 7.72) Facility Control (23.1, 24.8) (4.7, 6.8) (7.54, 7.83) % Whole Effluent (23.6, 24.6) (4.7, 6.7) (7.57, 7.86) % Whole Effluent (23.9, 25.3) (5.4, 6.5) (7.67, 7.86) % Whole Effluent (23.7, 26.1) (5.2, 6.5) (7.63, 7.80) % Whole Effluent (23.4, 25.9) (4.4, 6.4) (7.55, 7.82) % Whole Effluent (23.4, 25.3) (5.2, 6.3) (7.65, 7.78) % Whole Effluent (23.6, 25.5) (3.6, 6.2) (7.49, 7.78) Dechlorinated Laboratory Water; 2 Filtered Duluth-Superior Harbor Water; 3 Hardness and alkalinity were only measured on Day 7 (i.e., test termination) and do not have minimum and maximum values. Table 43 shows the survival and growth data from the seven day P. promelas WET test conducted during Test Cycle 5 of the JFE BallastAce BWMS Status Test. In order for the test results to be acceptable there must have been at least 80 % survival and an average dry weight per surviving organism of at least 0.25 mg in the experimental control (0 % Whole Effluent). The WET test met these criteria with 95 % survival and mg per fish (Table 43). The Performance Control also met the WET test QC criteria indicating that the organisms used in this WET test were of good health. There was no statistically significant (p<0.05) effect of control discharge water (i.e., Facility Control) on P. promelas survival and growth (Table 43). In addition, there was no statistically significant (p<0.05) effect of treatment discharge whole effluent on survival, with all of the treatment groups having 96.7 % to 100 % adult survival (Table 43). Finally, there was no statistically significant (p<0.05) effect of treatment discharge whole effluent on growth in any of the treatment groups tested.

93 Page 93 of 146 Table 43. Pimephales promelas Average (n=4) Percent Survival and Weight per Fish after Exposure to Treatment Discharge from Test Cycle 5 of the JFE BallastAce BWMS Status Test. Treatment Group Percent Survival ± Std. Deviation Mean Average Weight/Fish (mg) ± Std. Deviation P. promelas Performance Control ± ± Facility Control 100 ± ± % Whole Effluent ± ± % Whole Effluent 96.7 ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± % Whole Effluent 98.3 ± ± Dechlorinated Laboratory Water; 2 Filtered Duluth-Superior Harbor Water The water quality parameters measured in the S. capricornutum exposure solutions on Day 0 and in the chemistry replicate flask every 24 hours during the 96 hour WET test are presented in Table 44. The temperature of the exposure solutions was within the acceptance range of 25 C ± 3 C during the entire 96 hour test (Table 44). All other water quality parameters measured (i.e., dissolved oxygen, ph, conductivity, hardness, and alkalinity) were within the expected ranges for the water types measured. There was detectable concentrations of TRO in all treatment groups, with the Facility Control having the highest TRO concentration of mg/l, followed by the 50 % Whole Effluent (0.035 mg/l), and the 100 % Whole Effluent (0.029 mg/l) treatment groups (Table 44).

94 Page 94 of 146 Table 44. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Selenastrum capricornutum Whole Effluent Toxicity (WET) Test Associated with Test Cycle 5 of the JFE BallastAce BWMS Status Test. Treatment Group Temperature ( C) 24.7 S. capricornutum 24.4 Performance Control 1 (22.2, 25.3) Facility Control 24.8 (24.6, 25.0) 0 % Whole Effluent 2 (23.6, 25.2) 6.25 % Whole 24.7 Effluent (23.5, 25.3) 12.5 % Whole 24.7 Effluent (23.4, 25.0) 25 % Whole 24.7 Effluent (23.5, 25.2) 50 % Whole 24.8 Effluent (24.0, 25.2) 100 % Whole 24.9 Effluent Dissolved Oxygen 3 (mg/l) 8.1 ph 7.94 (7.54, 9.98) Conductivity 3 (µs/cm) Hardness 3 (mg/l CaCO 3 ) Alkalinity 3 (mg/l CaCO 3 ) TRO (mg/l) Q (8.05, 8.92) (8.16, 9.18) (8.17, 9.37) (8.16, 9.04) (8.16, 9.47) (8.12, 9.53) (24.6, 25.1) (7.93, 9.71) USEPA Nutrient Media; 2 Filtered Duluth-Superior Harbor Water; 3 Conductivity, dissolved oxygen, hardness, alkalinity, and TRO were measured only on Day 0 and do not have minimum and maximum values. Q Sample concentration was below the LOQ ( mg/l TRO) Q Q Q Q Table 45 shows the growth data from the 96 hour S. capricornutum WET test conducted during Test Cycle 5 of the JFE BallastAce BWMS Status Test. In order for the test results to be acceptable there must have been at least 1 x 10 6 cells/ml at test termination and the cell density must not vary by more than 20 % CV among replicate flasks in the experimental control (0 % Whole Effluent). The WET test met the criteria for cell density but did not meet the variability criteria with 25 % CV among experimental control replicates. The Performance Control met the WET test QC criteria indicating that the organisms used in this WET test were of good health. There was a reduction in cell density in the Facility Control as compared to the experimental control (0 % Whole Effluent), however, this result was not statistically significant (p<0.05). Although the highest cell density was seen in the 100 % Whole Effluent, there was no statistically significant effect (p<0.05) effect of treatment discharge whole effluent on growth, with average cell density ranging from 2,265,625 cells/ml to 3,896,875 cells/ml (Table 45).

95 Page 95 of 146 Table 45. Average (n=4) Cell Density of Selenastrum capricornutum after 96 Hours Exposure to Whole Effluent from Test Cycle 5 Treatment Discharge of the JFE BallastAce BWMS Status Test. Treatment Group Average Cells/mL ± Std. Deviation S. capricornutum Performance Control 1 3,538,000 ± 289,900 Facility Control 1,386,000 ± 187,300 0 % Whole Effluent 2 2,187,500 ± 543,427* 6.25 % Whole Effluent 2,415,625 ± 439, % Whole Effluent 2,265,625 ± 373, % Whole Effluent 2,368,750 ± 488, % Whole Effluent 2,481,250 ± 221, % Whole Effluent 3,896,875 ± 332,505 1 USEPA Nutrient Media; 2 Filtered Duluth-Superior Harbor Water; *CV=25 %, this test did not meet the criteria for variability among experimental control replicates. 5.2 Test Cycles 2, 4, and 6: F Panel and TG BallastCleaner (Low Dose) BWMS Combination Intake Measurements Operational Conditions Test Cycles 2, 4, and 6 intake of the JFE BallastAce BWMS Status Test took place 29 September 2014, 06 October 2014, and 13 October 2014, respectively. During these three test cycles, the JFE BallastAce BWMS utilized TG BallastCleaner as the active substance formulation; these test cycles were conducted at a lower dose and higher flow rate than Test Cycles 7 and 8 (reported separately). The operational data measured during intake of all three test cycles are summarized in Table 46. Figure 15 shows the pre- and post-fs flow rate and pressure data in real time for Test Cycle 2 intake (real-time data from Test Cycles 4 and 6 are available on request). The average duration of the intake operation was minutes (Table 46). The pre-treatment line pressure was 1.92 bar on average, which was within 4 % of the target value of 2 bar (Table 46). The differential pressure between the pre- and post-fs lines was 0.73 bar on average (Table 46). The pre-treatment flow rate ranged from 325 to 338 m 3 /hour (Table 46). The post-treatment flow rate ranged from 312 to 321 m 3 /hour, all within 10 % of the target flow rate (i.e., 311 m 3 /hour; Table 46). The backflush flow rate ranged from 13 to 22 m 3 /hour, for an average of 5 % of the post-treatment water lost to backflush (Table 46). The total volume of water treated was 190 m 3 on average, while the total volume of water in the control retention tank was 193 m 3 on average (Table 46). For zooplankton analysis, Sample Collection Tub #4 was used for all three test cycles and an average of 2.94 m 3 was concentrated for analysis (Table 46).

96 Page 96 of 146 Table 46. Summary of Operational Measurements and Data Collected during Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test using TG BallastCleaner as the Active Substance (Low Dose/High Flow). Parameter Units Test Cycle 2 Test Cycle 4 Test Cycle 6 Average Date and Start Time Sep-14 10:37:20 06-Oct-14 10:32:50 13-Oct-14 10:40:40 Duration min Pre-Treatment Line Pressure (Average ± Std. Deviation) Post-Treatment Line Pressure (Average ± Std. Deviation) Differential Pressure (Average ± Std. Deviation) Pre-Treatment Flow Rate (Average ± Std. Deviation) Post-Treatment Flow Rate (Average ± Std. Deviation) Backflush Flow Rate (Volumetric Calculation) Treatment Retention Tank Volume Control Retention Tank Volume Sample Collection Tub #4 Volume Sample Collection Tub #5 Volume bar 1.92 ± ± ± ± 0.03 bar 1.14 ± ± ± ± 0.05 bar 0.77 ± ± ± ± 0.04 m 3 /hour 338 ± ± ± ± 7 m 3 /hour 316 ± ± ± ± 5 m 3 /hour ± 5 m ± 3 m ± 1 m ± 0.02 m ± The real-time data in Figure 15 show that the FS was backflushing continuously. The FS did maintain flow rates and pressures in this state for the duration of the test.

97 Flow (M^3) Pressure (Bar) GSI/LB/QAQC/TR/JFE Page 97 of Flow and Pressure Time (min) Pre Filter Flow (m^3/hr) Post Filter Flow (m^3/hr) Post Filter Pressure (bar) Pre Filter Pressure (bar) Figure 15. Real-Time Flow Rate and Pressure Data Measured Pre- and Post-Filter during Test Cycle 2 Intake of the JFE BallastAce BWMS Status Test BWMS Active Substance Concentrations The TRO concentration measured in pre- and post-treatment grab samples collected simultaneously during Test Cycles 2, 4, and 6 intake are presented in Table 47. During all three test cycles, there were measurable TRO concentrations in the pre-treatment intake samples with a maximum measured value of mg/l TRO, which is within the range of TRO concentrations measured in similar samples collected during previous tests at the GSI Facility. Table 47 also shows the target TRO concentration three minutes after active substance dosing, as determined manually by JFE Engineering Corporation. The target TRO concentration was based on the DSH water DOC concentration (data not presented), therefore, the target value varied between each test cycle. During Test Cycle 2, the TRO concentration in post-treatment intake samples ranged from 1.58 to 5.23 mg/l (Table 47), while the TRO concentration in post-treatment intake samples collected during Test Cycle 4 ranged from 2.00 mg/l to 5.41 mg/l (Table 47). The TRO concentration was higher overall in Test Cycle 6, ranging from 3.53 to 6.80 mg/l (Table 47).

98 Page 98 of 146 Table 47. Concentration of Total Residual Oxidants (TRO) in Measured Grab Samples Collected Simultaneously from the Pre- and Post-Treatment Lines During Test Cycles 2, 4, and 6 Intake of the JFE BallastAce BWMS Status Test. N/A = Not Applicable. ND = Measured value was below the method detection limit. Sample Location (Pitot) Collection Time (min) JFE Target TRO (mg/l) Test Cycle 2 (TRO (mg/l) Test Cycle 4 (TRO (mg/l) Test Cycle 6 (TRO (mg/l) Pre-Treatment ND N/A (SP3c) ND ND Test Cycle 2 = 4.15* * * 4.43* 4.51* Post-Treatment 10 Test Cycle 4 = 5.23* 5.41* 3.53 (SP15) * AVERAGE Test Cycle 6 = *Reported value is above the range of the TRO calibration curve (i.e., 4 mg/l is the highest standard) Water Quality Conditions Grab Samples Intake water quality results from pre- and post-treatment samples collected simultaneously during Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test are presented in Table 48. All three test cycles met the minimum challenge water quality characteristics outlined in the ETV Protocol (USEPA, 2010). The pre-treatment TSS concentration ranged from 30.2 to 33.8 mg/l (target value was 24.0 mg/l TSS; Table 48). The DOC concentration in pre-treatment intake samples ranged from 7.1 to 8.0 mg/l (target value was 6 mg/l; Table 48); this parameter was not augmented as the DSH naturally meets the challenge water DOC criterion. The pre-treatment POC concentration ranged from 5.1 to 5.2 mg/l, which exceeded the minimum target value of 4 mg/l (Table 48). Finally, the MM concentration in pre-treatment intake samples ranged from 25.0 to 28.8 mg/l (minimum target value was 20 mg/l; Table 48). There was very little change in TSS, MM, NPOC, DOC, or POC concentrations between the preand post-treatment intake samples, with the exception of Test Cycle 4 where NPOC and POC concentrations in post-treatment samples were slightly elevated compared to pre-treatment samples (Table 48). This increase may be due to the lack of isokinetic sampling methods for grab sample collection, which may have been exacerbated by the high rate of flow during these tests. As expected, there was a higher %T (filtered and unfiltered) in post-treatment samples as compared to pre-treatment samples.

99 Page 99 of 146 Table 48. Average (± Standard Deviation, n=3) Concentration of Total Suspended Solids (TSS), Percent Transmittance (%T, in Filtered and Unfiltered Samples), Non-Purgeable Organic Carbon (NPOC), Dissolved Organic Carbon (DOC), Particulate Organic Carbon (POC), and Mineral Matter (MM) Measured in Grab Samples Collected Simultaneously from the Pre- and Post-Treatment Line on Intake During Test Cycles 2, 4, and 6 Intake of the JFE BallastAce BWMS Status Test. Test Cycle Sample Location (Pitot) Pre-Treatment (SP3c) Post-Treatment (SP15) Pre-Treatment (SP3c) Post-Treatment (SP15) Pre-Treatment (SP3c) Post-Treatment (SP15) TSS (mg/l) 30.2 (0.2) 29.2 (1.1) 30.5 (0.5) 31.1 (0.4) 33.8 (0.8) 34.8 (0.9) %T, Filtered/ Unfiltered 50.6 (0.1)/ 41.9 (0.1) 56.2 (0.9)/ 46.8 (1.2) 42.5 (0.5)/ 33.8 (0.1) 48.9 (0.4)/ 38.6 (0.5) 42.9 (0.4)/ 35.4 (0.5) 49.8 (0.4)/ 40.8 (0.7) NPOC (mg/l) DOC (mg/l) POC (mg/l) MM (mg/l) 12.2 (1.3) 7.1 (0.1) 5.1 (1.4) 25.0 (1.5) 12.4 (0.7) 7.1 (0.1) 5.3 (0.8) 24.0 (0.7) 13.0 (0.6) 7.8 (0.1) 5.2 (0.7) 25.3 (0.2) 13.8 (0.7) 7.6 (0.1) 6.2 (0.6) 24.9 (0.4) 13.1 (0.2) 8.0 (0.1) 5.1 (0.3) 28.8 (1.0) 13.7 (1.7) 8.0 (0.1) 5.7 (1.6) 29.1 (1.9) Sample Collection Tub Measurements The water quality in the pre-treatment sample collection tubs measured during Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test provide a time-integrated picture of the challenge water characteristics and are presented in Table 49. The water temperature declined over the course of the test period, ranging from 9.83 C to C, which was within the range specified by the ETV Protocol (i.e., 4 C to 35 C; USEPA, 2010). All other parameters were very similar between all three test cycles (Table 49).

100 Page 100 of 146 Table 49. Average Value (±Standard Deviation, n=2) of Water Quality Parameters Measured in Pre- Treatment Sample Collection Tubs During Test Cycles 2, 4, and 6 Intake of the JFE BallastAce BWMS Status Test. Parameter Test Cycle 2 Test Cycle 4 Test Cycle 6 Temperature ( C) ± ± ± 0.01 Specific Conductivity (ms/cm) ± ± ± Salinity (ppt) 0.10 ± ± ± 0.00 ph Turbidity (NTU) 18.7 ± ± ± 0.1 Total Chlorophyll (µg/l) 9.3 ± ± ± 0.1 Dissolved Oxygen (mg/l) 8.69 ± ± ± 0.13 Dissolved Oxygen (% Saturation) 87.2 ± ± ± Biological Conditions As shown in Table 50, Test Cycles 2, 4, and 6 had live organism densities in the challenge water that exceeded the minimum criteria for challenge water total living populations specified by the ETV Protocol (USEPA, 2010). For the largest regulated size class, nominally zooplankton, challenge water densities ranged from 177,000 to 242,000 live organisms per m 3, with Test Cycle 6 having the greatest density (Table 50). The 10 µm and < 50 µm size class, nominally protists, ranged from 1,085 to 4,027 live cells/ml in the challenge water, with Test Cycle 2 having the highest density (Table 50). The smallest regulated size class was represented by culturable, aerobic, heterotrophic bacteria. Live densities, as measured by the spread plate method, well exceeded the minimum density of 1,000/mL and ranged from 13,200 to 57,200 live bacteria per ml, with Test Cycle 4 having the highest density (Table 50). Table 50. Live Plankton Densities (n=1 each) and Average (± Standard Deviation, n=3) Microbial Concentration in Challenge Water Samples Collected During Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test. Regulated Size Class Parameter 50 µm Concentration (#/m 3 ) 10 µm and < 50 µm < 10 µm Concentration (cells/ml) Concentration (CFU/mL as culturable aerobic heterotrophic bacteria) TQAP Requirements Test Cycle 2 Test Cycle 4 Test Cycle 6 100,000 organisms/m 3 177, , ,000 1,000 organisms/ml 4,027 1,085 1,158 1,000/mL 13,200 (1,990) 57,200 (6,330) 49,900 (7,680)

101 5.2.2 Retention Period Conditions GSI/LB/QAQC/TR/JFE Page 101 of 146 During the 48 hour retention period associated with Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test, the TRO concentration in the control and treatment retention tanks was measured twice (once at 24 and once at 48 hours). Various water quality parameters were also measured every 15 minutes in both tanks and logged during retention BWMS Active Substance Concentration As shown in Table 51, there were measurable TRO concentrations in the control retention tank during the 48 hour holding time ranging from below the method detection limit to mg/l. Overall, these values were slightly lower than pre-treatment intake TRO concentrations. There was a substantial decrease in TRO concentration of the treated water during the 48 hour retention time (Table 51), which indicates that there was marked chlorine demand still present in the intake water after treatment. All three test cycles had similar TRO concentrations in the treatment retention tank at 24 and 48 hours post-treatment, with Test Cycle 2 having the lowest concentration and Test Cycle 6 having the highest concentration overall (Table 51). At 24 hours, the TRO concentration ranged from to mg/l (Table 51), on average this was a decrease of 94 % compared to post-treatment intake (Table 51). At 48 hours, the TRO concentration ranged from to mg/l, a 96 % decrease on average from post-treatment intake samples (Table 51). Table 51. Concentration of Total Residual Oxidants (TRO) in the Control and Treatment Retention Tanks 24 and 48 Hours Post-Treatment during Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test. ND = Measured value was below the method detection limit. Sample Location Control Retention Tank Treatment Retention Tank Collection Time (hour) Test Cycle 2 TRO (mg/l) Test Cycle 4 TRO (mg/l) Test Cycle 6 TRO (mg/l) 24 ND ND Water Quality Conditions Table 52 shows the average water quality parameters measured using calibrated Sondes in the control and treatment retention tanks during the 48 hour holding time utilized in Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test. Each parameter was measured every 15 minutes during the holding period, however, during Test Cycle 2 the Sonde in the control retention tank ran out of batteries ~31 hours into the retention period. There were no unexpected differences in water quality between the test cycles (Table 52). Overall, the water temperature during retention decreased from Test Cycle 2 to Test Cycle 6, which occurred approximately three weeks apart from each other during the end of the GSI Facility testing season. There were some notable, although expected, differences between the control and treatment retention tanks. The specific conductivity was slightly higher in the treatment retention tank as compared to the control retention tank (Table 52). This was due to the addition of TG

102 Page 102 of 146 BallastCleaner to the treated water and the subsequent increase in ions. Total chlorophyll was markedly decreased in the treatment retention tank, which was due to the decrease in live protist density as a result of treatment (Table 52). Table 52. Water Quality Parameters Measured In-Situ in the Control and Treatment Retention Tanks during the 48 Hour Holding Period for Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test. Parameter Retention Tank Test Cycle 2 Test Cycle 4 Test Cycle ± 0.44, ± 0.29, 9.83 ± 0.17, Control n=113* n=179 n=177 Temperature ( C) ± 0.31, 9.89 ± 0.13, Treatment ± 0.57, n=175 n=178 n= ± 0.001, ± 0.000, ± 0.000, Control Specific Conductivity n=113* n=179 n=177 (ms/cm) ± 0.000, ± 0.000, ± 0.000, Treatment n=175 n=178 n= ± 0.00, Control 0.10 ± 0.00, n=113* 0.10 ± 0.00, n=179 n=177 Salinity (ppt) 0.12 ± 0.00, Treatment 0.11 ± 0.00, n= ± 0.00, n=178 n=177 Control 7.56, n=113* 7.54, n= , n=177 ph Treatment 7.70, n= , n= , n= ± 1.2, Control 14.9 ± 1.3, n=113* 20.6 ± 1.3, n=179 n=177 Turbidity (NTU) 16.5 ± 1.3, Treatment 14.7 ± 1.0, n= ± 1.1, n=178 n= ± 0.6, Control 8.9 ± 0.7, n=113* 8.5 ± 0.5, n=179 n=177 Total Chlorophyll (µg/l) 4.4 ±0.6, Treatment 4.4 ± 0.4, n= ± 0.5, n=178 n= ± 0.02, Control 8.44 ± 0.07, n=113* 8.97 ± 0.04, n=179 Dissolved Oxygen n=177 (mg/l) 9.71 ± 0.01, Treatment 9.00 ± 0.02, n= ± 0.02, n=178 n= ± 0.4, Control 83.6 ± 1.5, n=113* 81.2 ± 0.9, n=179 Dissolved Oxygen (% n=177 Saturation) 85.9 ± 0.3, Treatment 88.5 ± 1.1, n= ± 0.5, n=178 n=177 *The Sonde ran out of batteries during the retention period and only 65 % of the retention period was logged in comparison to the treatment tank.

103 5.2.3 Discharge Measurements GSI/LB/QAQC/TR/JFE Page 103 of Operational Conditions Control Discharge The operational data measured during discharge of the control retention tank for Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test are presented in Table 53. The control discharge data from all three test cycles were very similar. Control discharge occurred over an average duration of minutes; at a pressure of 1.86 bar and flow rate of 319 m 3 /hour, on average (Table 53). A total of 174 m 3 was discharged from the control retention tank, on average (Table 53). Zooplankton samples, all of which were collected from Sample Collection Tub #1, represented an average of 3.10 m 3 concentrated to 1 L (Table 53). Table 53. Summary of Operational Measurements and Data Collected during Control Retention Tank Discharge for Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test using TG BallastCleaner as the Active Substance. Parameter Units Test Cycle 2 Test Cycle 4 Test Cycle 6 Average Date and Start Time Oct-14 13:59:00 08-Oct-14 12:33:00 15-Oct-14 12:02:40 Duration min Discharge Line Pressure (Average ± Std. Deviation) Discharge Flow Rate (Average ± Std. Deviation) Volume Discharged from Retention Tank Sample Collection Tub #1 Volume Sample Collection Tub #2 Volume bar 1.87 ± ± ± ± 0.07 m 3 /hour 315 ± ± ± ± 4 m ± 1 m ± 0.03 m ± Treatment Discharge Table 54 shows operational data measured during discharge of the treatment retention tanks for Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test. As with the control discharge data, the average values from each test cycle are very similar. The treatment discharge operation was an average of minutes in duration (Table 54). There was a slight difference in pressure, 0.50 bar on average, between the pre-neutralization line and the post-neutralization line (Table 54). This difference was not as great as during intake because the BWMS FS was not active during discharge. The average treatment discharge flow rate was 312 m 3 /hour, and an average 185 m 3 of water from the treatment retention tank was discharged (Table 54). Zooplankton samples were collected from Sample Collection Tubs #4 and #5, which had an average sample volume of 3.21 m 3 and 3.19 m 3, respectively (Table 54).

104 Page 104 of 146 Table 54. Summary of Operational Measurements and Data Collected during Treatment Retention Tank Discharge for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test using TG BallastCleaner as the Active Substance. Parameter Units Test Cycle 2 Test Cycle 4 Test Cycle 6 Average Date and Start Time Oct-14 09:39:50 08-Oct-14 09:31:30 15-Oct-14 09:34:00 Duration min Pre-Neutralization Line Pressure (Average ± Std. bar 1.96 ± ± ± ± 0.03 Deviation) Post-Neutralization Line Pressure (Average ± Std. bar 1.45 ± ± ± ± 0.02 Deviation) Differential Pressure* (Average ± Std. Deviation) bar 0.51 ± ± ± ± 0.02 Flow Rate (Average ± Std. Deviation) m 3 /hour 314 ± ± ± ± 3 Volume Discharged from Retention Tank m ± 4 Sample Collection Tub #4 Volume m ± 0.08 Sample Collection Tub #5 Volume m ± 0.09 Sample Collection Tub #6 Volume m ± 0.13 *BWMS filter was not active during discharge BWMS Active Substance Concentrations The concentration of TRO measured in grab samples collected throughout control and treatment tank discharge operations associated with Test Cycles 2, 4 and 6 of the JFE BallastAce Status Test are presented in Table 55. The concentration of TRO in control discharge water ranged from below the method detection limit to mg/l, which was in keeping with the range of TRO concentrations measured in pre-treatment water during these three test cycles (Table 55). The range of TRO concentrations measured in the treatment discharge samples was only slightly higher, ranging from below the method detection limit to mg/l (Table 55). The treatment discharge water was sent to the GSI Facility s wastewater holding tank where the TRC concentration was measured; in all cases the TRC concentration was below the permitted level of mg/l (data not presented) and the water was discharged to the DSH.

105 Page 105 of 146 Table 55. Concentration of Total Residual Oxidants (TRO) Measured in Grab Samples Collected During Test Cycles 2, 4, and 6 Control and Treatment Tank Discharge Operations Associated with the JFE BallastAce BWMS Status Test. ND = Measured value was below the method detection limit. Sample Location (Pitot) Control (SP9c) Treatment (SP15) Collection Time (min) Test Cycle 2 (TRO (mg/l) Test Cycle 4 (TRO (mg/l) Test Cycle 6 (TRO (mg/l) 1 ND ND Water Quality Conditions Grab Samples Table 56 shows the measured water quality data from grab samples collected throughout discharge of the control and treatment retention tanks associated with Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test. As expected, %T (both filtered and unfiltered) was higher in the treatment discharge samples than in the control discharge samples (Table 56). The chlorine in the treated water continued to oxidize and break down the organic matter during retention, resulting in treatment discharge water that was more transparent than the control water.

106 Page 106 of 146 Table 56. Average (± Standard Deviation, n=3) Concentration of Total Suspended Solids (TSS), Percent Transmittance (%T, in Filtered and Unfiltered Samples), Non-Purgeable Organic Carbon (NPOC), Dissolved Organic Carbon (DOC), Particulate Organic Carbon (POC), and Mineral Matter (MM) in Grab Samples Collected Sequentially from the Treatment and Control Line on Discharge Associated with Test Cycles 2, 4 and 6 of the JFE BallastAce BWMS Status Test. Test Cycle Sample Location (Pitot) Control (SP9a) Treatment (SP15) Control (SP9a) Treatment (SP15) Control (SP9a) Treatment (SP15) TSS (mg/l) 9.3 (0.7) 13.9 (1.8) 10.7 (0.5) 12.8 (1.2) 11.8 (0.4) 12.8 (1.6) %T, Filtered/ Unfiltered 50.9 (0.1)/ 43.8 (0.2) 55.0 (0.3)/ 46.0 (0.2) 42.4 (0.1)/ 34.3 (0.1) 47.2 (0.4)/ 38.7 (0.1) 42.7 (0.3)/ 36.1 (0.1) 48.4 (0.3)/ 41.8 (0.3) NPOC (mg/l) DOC (mg/l) POC (mg/l) MM (mg/l) 8.2 (0.1) 6.9 (0.1) 1.3 (0.1) 8.0 (0.8) 9.0 (0.1) 7.0 (0.1) 2.0 (0.1) 11.9 (1.7) 9.4 (0.2) 7.7 (0.1) 1.6 (0.2) 9.1 (0.4) 10.1 (0.4) 8.0 (0.1) 2.1 (0.5) 10.7 (0.7) 11.2 (0.6) 8.0 (0.1) 3.2 (0.6) 8.6 (0.2) 10.8 (0.2) 8.2 (0.2) 2.5 (0.3) 10.3 (1.9) Sample Collection Tub Measurements Table 57 shows water quality parameters measured in the sample collection tubs using calibrated Sondes immediately following discharge of the control and treatment retention tanks associated with Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test. Test Cycles 2 and 6 were conducted approximately three weeks apart; therefore, the temperature declined ~3 C between those two test cycles (Table 57). Overall, the specific conductivity and salinity were higher in the treatment discharge water than in the control discharge water due to the added ions from treatment with TG BallastCleaner and neutralization with sodium sulfite (Table 57). The total chlorophyll concentration in the control discharge was higher than in the treatment discharge due to the decreased protist density as a result of treatment (Table 57). For all other parameters, there was no discernible trend between test cycles or within a test cycle (control versus treatment; Table 57).

107 Page 107 of 146 Table 57. Average (± Standard Deviation) Water Quality Parameters Measured in Sample Collection Tubs Immediately Following Control and Treatment Discharge Operations for Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test. Parameter Sample Type Test Cycle 2 Test Cycle 4 Test Cycle 6 Temperature ( C) CONT, n= ± ± ± 0.01 TRT, n= ± ± 0.02; n=2* 9.64 ± 0.01 Specific Conductivity CONT, n= ± ± ± (ms/cm) TRT, n= ± ± 0.000; n=2* ± Salinity (ppt) CONT, n= ± ± ± 0.00 TRT, n= ± ± 0.00, n=2* 0.12 ± 0.00 ph CONT, n= TRT, n= , n=2* 7.45 Turbidity (NTU) CONT, n= ± ± ± 0.4 TRT, n= ± ± 0.1, n=2* 15.5 ± 1.2 Total Chlorophyll CONT, n=2 8.5 ± ± ± 0.1 (µg/l) TRT, n=3 4.9 ± ± 0.2, n=2* 5.1 ± 0.2 Dissolved Oxygen CONT, n= ± ± ± 0.01 (mg/l) TRT, n= ± ± 0.06, n=2* 9.87 ± 0.02 Dissolved Oxygen (% CONT, n= ± ± ± 0.1 Saturation) TRT, n= ± ± 0.6, n=2* 86.8 ± 0.2 *Water quality was not measured in Sample Collection Tub #6 because for the first four minutes of the discharge operation (~ 12 % of the operation) water was not flowing into the tub Biological Conditions The control and treatment discharge densities of the three regulated size classes associated with Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test are presented in Table 58; more detailed taxonomic data are available on request. The control discharge density of the 50 µm size class greatly exceeded the minimum concentration of 100 live organisms/m 3 specified in the ETV Protocol, ranging from 312,000/m 3 to 486,000/m 3 (Table 58). There was a marked decrease in treatment discharge density as compared to control discharge density for all three test cycles. Test Cycle 2 had an average treatment discharge density of 311 live organism/m 3 (i.e., 99.9 % reduction compared to control discharge; Table 58). Test Cycle 4 had 416 live organisms/m 3 (i.e., 99.9 % reduction compared to control discharge; Table 58) and Test Cycle 6 had 190 live organisms/m 3 (i.e., 99.9 % reduction compared to control discharge; Table 58). All three test cycles had treatment discharge densities that were well above the USCG BWDS of 10 live organisms/m 3. The control discharge density of the 10 µm and < 50 µm size class also greatly exceeded the ETV Protocol minimum required density of 100 organisms/ml; live density ranged from 773 cells/ml to 1,213 cells/ml (Table 58). There was also a substantial decrease in live organism density in the treatment discharge as compared to the control discharge, with densities ranging from 0.75 cell/ml to 1.35 cells/ml (Table 58). All three test cycles met the USCG BWDS for this size class of organisms (Table 58).

108 Page 108 of 146 The live density of culturable, aerobic heterotrophic bacteria (i.e., < 10 µm size class) in control discharge was far greater than the minimum concentration of 500/mL specified in the ETV Protocol. The control discharge density ranged from an average of 17,500 CFU/mL to 80,300 CFU/mL (Table 58). There was a substantial decrease in heterotrophic bacteria density in the treatment discharge as compared to the control, ranging from an average of 838 CFU/mL to 3,960 CFU/mL (Table 58). There was a 95.2 % reduction in density compared to the control during Test Cycle 2. During Test Cycles 4 and 6, there was a 98.7 % and 93.6 % reduction, respectively, in comparison to control discharge densities. There is no discharge standard for heterotrophic bacteria; these densities cannot be compared to any regulation. Table 58. Live Plankton Density (Average ± Standard Deviation, Where Applicable) and Average (± Standard Deviation, n=3) Microbial Concentrations in Samples Collected During Control and Treatment Retention Tank Discharge for Test Cycles 2, 4, and 6 of the JFE BallastAce BWMS Status Test. Regulated Size Class 50 µm 10 µm and < 50 µm < 10 µm (CFU/mL as culturable aerobic heterotrophic bacteria) Maximum Concentration in Treated Discharge Test Cycle 2 Test Cycle 4 Test Cycle 6 Control Treatment Control Treatment Control Treatment < 10 organisms per m 3 486, , , < 10 organisms per ml 1, , No discharge standard for 17,500 80,300 1,080 61, (459) heterotrophic (1,340) (4,510) (1,260) (1,350) 3,960 (2,700) bacteria Disinfection Byproduct s(dbps) Concentrations The results from analysis of selected DBPs in samples collected during Test Cycle 4 control and treatment discharge of the JFE BallastAce BWMS Status Test are presented in Table 59. Samples were collected for DBP analysis only during test cycles that were also selected for WET testing. There were elevated concentrations of all classes of DBPs in the treatment discharge as compared to the control discharge, with the exception of the bromate ion (Table 59). In the control discharge samples, all of the selected DBPs were below the limit of detection with the exception of total sodium (i.e., average concentration of 10.3 µg/l; Table 59). Of all DBPs measured, the chlorate ion had the highest measured concentration in treatment discharge, with an average of 238 µg/l (Table 59). It is interesting to note that the chlorate ion concentration measured in treatment discharge samples from Test Cycle 4 was over seven times higher than that of Test Cycles 1 and 5. The total trihalomethanes was the second highest class of DBPs, in terms of concentration in treatment discharge, with an average concentration of 147 µg/l (Table 59). Chloroform was the primary contributor and bromodichloromethane was a secondary contributor in the treatment discharge samples. There was an average of 117 µg/l total haloacetic acids in treatment discharge; dichloroacetic acid and trichloroacetic acid were the primary contributors to the total concentration of haloacetic acids in treatment discharge (Table 59). The average concentration of total haloacetonitriles in treatment discharge was 20 µg/l; the majority of the total was from chloral hydrate (Table 59). Total sodium was only slightly higher in treatment discharge as compared to

109 Page 109 of 146 control discharge (i.e., 14.9 µg/l in treatment discharge compared to 10.3 µg/l in control discharge; Table 59). Table 59. Results from Analysis of Selected Disinfection Byproducts in Samples Collected during Discharge of the Control and Treatment Retention Tanks in Test Cycle 4 of the JFE BallastAce Status Test. Analyte Formula Control Average (µg/l) TEST CYCLE 4 Treatment Average (µg/l) Bromodichloromethane CHBrCl 2 < Bromoform CHBr 3 < 0.5 < 0.5 Chlorodibromomethane CHBr 2 Cl < 0.5 < 0.5 Chloroform CHCl 3 < Total Trihalomethanes < Bromochloroacetic acid* BrClCHCOOH < Dibromoacetic acid CHBr 2 COOH < 1.0 < 1.0 Dichloroacetic acid CHCl 2 COOH < Monobromoacetic acid CH 2 BrCOOH < 1.0 < 1.0 Monochloroacetic acid CH 2 ClCOOH < Trichloroacetic acid CCl 3 COOH < Total Haloacetic Acids < ,1,1-trichloro-2-Propanone CCl 3 COCH 3 < ,1-dichloro-2-Propanone CH 3 COCHCl 2 < Bromochloroacetonitrile C 2 HBrClN < 0.5 < 0.5 Bromoacetonitrile BrCH 2 CN < 0.5 < 0.5 Chloral hydrate Cl 3 CCH(OH) 2 < Chloroacetonitrile ClCH 2 CN < 0.5 < 0.5 Chloropicrin Cl 3 CNO 2 < 0.5 < 0.5 Dibromoacetonitrile Br 2 CHCN < 0.5 < 0.5 Dichloroacetonitrile Cl 2 CHCN < Trichloroacetonitrile Cl 3 CCN < 0.5 < 0.5 Total Haloacetonitriles < Bromate BrO 3 - Chlorate ClO 3 - < 5.0 < 5.0 < Sodium, Total Na *Not included in total haloacetic acids.

110 Whole Effluent Toxicity (WET) GSI/LB/QAQC/TR/JFE Page 110 of 146 The water quality parameters measured in stock solutions prepared prior to the start of Test Cycle 4 WET testing and prior to daily renewal of test water during the C. dubia and P. promelas WET tests are presented in Table 60. The temperature of the prepared stock solutions was within the acceptance range of 25 C ± 3 C in all cases (Table 60). In addition, the dissolved oxygen concentration was above the minimum value specified for P. promelas (i.e., 4.0 mg/l) in all cases (Table 60). All other water quality parameters measured (i.e., ph, conductivity, hardness, and alkalinity) were within the expected ranges for the water types measured. There was no detectable TRO in the C. dubia and P. promelas Performance Control stock solutions (Table 60). The TRO values in the Facility Control (i.e., control discharge water) ranged from to mg/l (Table 60). There was measurable TRO in the 12.5 %, 25 %, 50 %, and 100 % Whole Effluent treatment groups for the entire duration of the C. dubia and P. promelas WET tests, ranging from as low as mg/l to mg/l overall (Table 60). The TRO concentration in the 0 % and 6.25 % Whole Effluent treatment groups ranged from below the method detection limit to mg/l (Table 60). Table 60. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Stock Solutions during the Ceriodaphnia dubia and Pimephales promelas Whole Effluent Toxicity (WET) Tests Associated with Test Cycle 4 of the JFE BallastAce BWMS Status Test. Treatment Group Temperature ( C) C. dubia Performance 23.3 Control 1 (22.0, 24.6) P. promelas 24.3 Performance Control 2 (23.6, 24.9) 25.8 Facility Control (23.8, 26.9) 0 % Whole Effluent (24.3, 27.0) 6.25 % Whole Effluent 12.5 % Whole Effluent 25 % Whole Effluent 50 % Whole Effluent 100 % Whole Effluent 25.5 (24.1, 26.8) 25.5 (24.2, 26.3) 25.5 (24.4, 26.6) 25.3 (24.5, 26.4) 25.5 (23.3, 26.9) Dissolved Oxygen (mg/l) 8.4 (7.8, 8.8) 6.8 (6.6, 7.0) 9.8 (9.4, 10.4) 10.1 (8.8, 10.9) 9.2 (8.5, 9.9) 9.1 (8.4, 9.9) 9.1 (8.4, 9.7) 9.1 (8.6, 9.8) 10.0 (9.6, 10.9) ph 8.49 (8.41, 8.53) 7.59 (7.52, 7.65) 7.81 (7.74, 7.85) 7.94 (7.91, 7.98) 7.97 (7.95, 8.01) 7.96 (7.87, 8.00) 7.98 (7.95, 8.00) 7.97 (7.94, 8.00) 7.88 (7.78, 7.93) Conductivity (µs/cm) 582 (576, 590) (154.5, 173.7) 212 (207, 222) 210 (207, 211) 211 (210, 211) 212 (210, 214) 216 (215, 216) 222 (221, 223) 234 (232, 235) Hardness 4 (mg/l CaCO 3 ) Alkalinity 4 (mg/l CaCO 3 ) TRO (mg/l) <DL <DL Hard Reconstituted Water; 2 Dechlorinated Laboratory Water; 3 Filtered Duluth-Superior Harbor Water; 4 Hardness and alkalinity were only measured on Day 0 and do not have minimum and maximum values. * Values less than the detection limit (DL) which equals mg/l were not used to calculate the average TRO value. Q Sample concentration was below the LOQ ( mg/l TRO) (0.023, 0.048) Q (<DL, Q ) Q (<DL, 0.019) Q (0.010 Q, 0.022) (0.017 Q, 0.032) (0.023, 0.038) (0.039, 0.054)

111 Page 111 of 146 The water quality parameters measured in the C. dubia exposure solutions following each 24 hour renewal period are presented in Table 61. The temperature of the exposure solutions was within the acceptance range of 25 C ± 3 C during the entire six day test (Table 61). All other water quality parameters measured (i.e., ph, hardness, and alkalinity) were within the expected ranges for the water types measured (Table 61). Table 61. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Six Day Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Test Cycle 4 of the JFE BallastAce BWMS Status Test. Treatment Group Temperature ( C) ph Hardness 3 (mg/l CaCO 3 ) Alkalinity 3 (mg/l CaCO 3 ) C. dubia Performance Control (23.6, 24.7) (8.36, 8.43) Facility Control (23.5, 24.5) (7.99, 8.36) % Whole Effluent (23.1, 24.5) (8.00, 8.28) % Whole Effluent (23.6, 24.2) (8.17, 8.27) % Whole Effluent (23.8, 24.2) (8.17, 8.27) % Whole Effluent (23.6, 24.3) (8.02, 8.24) % Whole Effluent (23.9, 24.3) (8.19, 8.29) % Whole Effluent (23.6, 24.0) (8.17, 8.26) Hard Reconstituted Water; 2 Filtered Duluth-Superior Harbor Water; 3 Hardness and alkalinity were only measured on Day 6 (test termination) and do not have minimum and maximum values. Table 62 shows the survival and reproduction data from the six day, three-brood C. dubia WET test conducted during Test Cycle 4 of the JFE BallastAce BWMS Status Test. In order for the test results to be acceptable there must have been at least 80 % survival and an average total number of at least 15 young per female in the experimental control (0 % Whole Effluent). The WET test met these criteria with 100 % survival and 17.7 average young per female (Table 62). The Performance Control, which is used to determine overall health of the test organisms and not test result acceptance, did not meet the test QC criteria. This result may be attributed to the fact that the C. dubia (purchased from Environmental Consulting and Testing, Inc.) were cultured in Moderately- Hard Reconstituted Water (specific conductivity range = µs/cm) and the Performance Control was Hard Reconstituted Water (specific conductivity range = µs/cm). Therefore, osmotic shock may have caused the low survival and reproduction in this case. Results from the Facility Control indicate that there was no statistically significant (p<0.05) effect of control discharge water on adult survival or reproduction. In addition, there was no statistically significant (p<0.05) effect of whole effluent from treatment discharge on adult survival or reproduction when compared to the experimental control, although, the average number of young

112 Page 112 of 146 per female was reduced in the 100 % Whole Effluent treatment group as compared to the experimental control (Table 62). Table 62. Average (n=10) Percent Survival and Total Number of Offspring Produced in the Three-Brood Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Treatment Discharge from Test Cycle 4 of the JFE BallastAce BWMS Status Test. Treatment Group Percent Survival ± Std. Deviation Average Total Number of Young per Female ± Std. Deviation C. dubia Performance Control 1 70 ± ± 3.1 Facility Control 100 ± ± % Whole Effluent ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ±4.1 1 Hard Reconstituted Water; 2 Filtered Duluth-Superior Harbor Water The water quality parameters measured in the P. promelas exposure solutions following each 24 hour renewal period are presented in Table 63. The temperature of the exposure solutions was within the acceptance range of 25 C ± 3 C during the entire seven day test (Table 63). The dissolved oxygen concentration was greater than 4.0 mg/l in all treatment groups with the exception of the 50 % and 100 % Whole Effluent, which had a minimum dissolved oxygen concentration of 3.8 mg/l (Table 63). All other water quality parameters measured (i.e., ph, hardness, and alkalinity) were within the expected ranges for the water types measured (Table 63).

113 Page 113 of 146 Table 63. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Pimephales promelas Whole Effluent Toxicity (WET) Test Associated with Test Cycle 4 of the JFE BallastAce BWMS Status Test. Treatment Group Temperature ( C) Dissolved Oxygen (mg/l) ph Hardness 3 (mg/l CaCO 3 ) Alkalinity 3 (mg/l CaCO 3 ) P. promelas Performance Control 1 (23.9, 25.5) (5.2, 7.1) (7.47, 7.89) Facility Control (24.2, 26.1) (4.2, 6.4) (7.53, 7.85) % Whole Effluent (23.9, 25.8) (4.6, 6.9) (7.56, 7.96) % Whole Effluent (23.6, 25.8) (5.0, 6.7) (7.59, 8.00) % Whole Effluent (24.0, 25.9) (4.5, 6.7) (7.55, 8.02) % Whole Effluent (24.2, 26.0) (4.4, 6.9) (7.56, 8.03) % Whole Effluent (23.9, 25.5) (3.8, 6.7) (7.53, 8.03) % Whole Effluent (23.5, 25.7) (3.8, 6.5) (7.51, 7.99) Dechlorinated Laboratory Water; 2 Filtered Duluth-Superior Harbor Water; 3 Hardness and alkalinity were only measured on Day 7 (test termination) and do not have minimum and maximum values. Table 64 shows the survival and growth data from the seven day P. promelas WET test conducted during Test Cycle 4 of the JFE BallastAce BWMS Status Test. In order for the test results to be acceptable there must have been at least 80 % survival and an average dry weight per surviving organism of at least 0.25 mg in the experimental control (0 % Whole Effluent). The WET test met these criteria with 98.3 % survival and mg per fish (Table 64). The Performance Control is used to determine overall health of the test organisms and not test result acceptance, however, the Performance Control also met the WET test QC criteria indicating that the organisms used in this WET test were of good health. There was no statistically significant (p<0.05) effect of control discharge water (i.e., Facility Control) on P. promelas survival and growth. In addition, there was no statistically significant (p<0.05) effect of treatment discharge whole effluent on survival, with all of the treatment groups having 98.3 % to 100 % adult survival (Table 64). Finally, there was no statistically significant (p<0.05) effect of treatment discharge whole effluent on growth in any of the treatment groups tested.

114 Page 114 of 146 Table 64. Pimephales promelas Average (n=4) Percent Survival and Weight per Fish after Exposure to Treatment Discharge from Test Cycle 4 of the JFE BallastAce BWMS Status Test. Treatment Group Percent Survival ± Std. Deviation Mean Average Weight/Fish (mg) ± Std. Deviation P. promelas Performance Control ± ± Facility Control 85.0 ± ± % Whole Effluent ± ± % Whole Effluent 100 ± ± % Whole Effluent 98.3 ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± % Whole Effluent 98.3 ± ± Dechlorinated Laboratory Water; 2 Filtered Duluth-Superior Harbor Water. The water quality parameters measured in the S. capricornutum exposure solutions on Day 0 and in the chemistry replicate flask every 24 hours during the 96 hour WET test are presented in Table 65. The temperature of the exposure solutions was within the acceptance range of 25 C ± 3 C during the entire 96 hour test (Table 65). All other water quality parameters measured (i.e., dissolved oxygen, ph, conductivity, hardness, and alkalinity) were within the expected ranges for the water types measured (Table 65). There were detectable concentrations of TRO in all treatment groups, with the exception of the Performance Control (Table 65). The 100 % Whole Effluent treatment group had the highest TRO concentration with mg/l (Table 65).

115 Page 115 of 146 Table 65. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Selenastrum capricornutum Whole Effluent Toxicity (WET) Test Associated with Test Cycle 4 of the JFE BallastAce BWMS Status Test. Treatment Group Temperature ( C) 24.5 S. capricornutum 24.5 Performance Control 1 (23.4, 25.1) Facility Control 24.5 (23.6, 24.9) 0 % Whole Effluent 2 (23.6, 24.9) 6.25 % Whole 24.6 Effluent (23.9, 24.9) 12.5 % Whole 24.6 Effluent (23.8, 24.8) 25 % Whole 24.6 Effluent (23.7, 24.9) 50 % Whole 24.6 Effluent (23.9, 24.8) 100 % Whole 24.6 Effluent Dissolved Oxygen 3 (mg/l) 8.7 ph 7.90 (7.49, 9.73) Conductivity 3 (µs/cm) Hardness 3 (mg/l CaCO 3 ) Alkalinity 3 (mg/l CaCO 3 ) TRO 3 (mg/l) < (8.05, 9.05) (8.21, 9.23) (8.24, 9.25) (8.26, 9.35) (8.25, 9.56) (8.24, 9.41) (23.6, 24.9) (8.15, 9.49) USEPA Nutrient Media; 2 Filtered Duluth-Superior Harbor Water; 3 Conductivity, dissolved oxygen, hardness, alkalinity, and TRO were measured only on Day 0 and do not have minimum and maximum values. Q Sample concentration was below the LOQ ( mg/l TRO). Table 66 shows the growth data from the 96 hour S. capricornutum WET test conducted during Test Cycle 4 of the JFE BallastAce BWMS Status Test. In order for the test results to be acceptable there must have been at least 1 x 10 6 cells/ml at test termination and the cell density must not have varied by more than 20 % CV among replicate flasks in the experimental control (0 % Whole Effluent). The WET test met these criteria with 2,525,000 cells/ml and 6 % CV among experimental control replicates (Table 66). The Performance Control also met the WET test QC criteria indicating that the organisms used in this WET test were of good health. There was a reduction in cell density in the Facility Control as compared to the experimental control (0 % Whole Effluent; Table 66), however, this result was not statistically significant (p<0.05). Although the highest cell density was seen in the 100 % Whole Effluent, there was no statistically significant effect (p<0.05) effect of treatment discharge whole effluent on growth, with average cell density ranging from 2,778,125 cells/ml to 3,092,708 cells/ml (Table 66).

116 Page 116 of 146 Table 66. Average (n=4) Cell Density of Selenastrum capricornutum after 96 Hours Exposure to Whole Effluent from Test Cycle 4 Treatment Discharge of the JFE BallastAce BWMS Status Test. Treatment Group Average Cells/mL ± Std. Deviation S. capricornutum Performance Control 1 3,447,000 ± 351,100 Facility Control 1,975,000 ± 388,000 0 % Whole Effluent 2 2,525,000 ± 158, % Whole Effluent 2,778,125 ± 631, % Whole Effluent 2,628,125 ± 262, % Whole Effluent 2,690,625 ± 558, % Whole Effluent 2,975,000 ± 527, % Whole Effluent 3,092,708 ± 1,447,365 1 USEPA Nutrient Media; 2 Filtered Duluth-Superior Harbor Water. 5.3 Test Cycles 7 and 8: F Panel and TG BallastCleaner (High-Dose) BWMS Combination Intake Measurements Operational Conditions Test Cycles 7 and 8 intake operations associated with the JFE BallastAce BWMS Status Test took place 22 and 27 October 2014, respectively. During these two test cycles, the JFE BallastAce BWMS utilized TG BallastCleaner as the active substance formulation; these test cycles were conducted at a higher dose and lower flow rate than Test Cycles 2, 4, and 6. The operational data measured during intake of Test Cycles 7 and 8 are summarized in Table 67. Figure 16 shows the pre- and post-fs flow rate and pressure data in real time for Test Cycle 8 intake (real-time data from Test Cycle 7 are available on request). The average duration of the intake operation was minutes (Table 67). The pre-treatment line pressure was 1.95 bar on average, which was within 3 % of the target value of 2 bar (Table 67). The differential pressure between the pre- and post-fs lines was 0.27 bar on average (Table 67). The pre-treatment flow rate was 198 m 3 /hour and 197 m 3 /hour for Test Cycles 7 and 8, respectively (Table 67). The post-treatment flow rate was 198 m 3 /hour and 199 m 3 /hour for Test Cycles 7 and 8, respectively, all within 10 % of the target flow rate (i.e., 200 m 3 /hour; Table 67). The backflush flow rate was 2 m 3 /hour and 1 m 3 /hour for Test Cycles 7 and 8, respectively (Table 67). The total volume of water treated was 191 m 3 on average, while the total volume of water in the control retention tank was 190 m 3 on average (Table 67). For zooplankton analysis, Sample Collection Tub #4 was used for both test cycles and an average of 2.77 m 3 was concentrated to 1 L (Table 67).

117 Page 117 of 146 Table 67. Summary of Operational Measurements and Data Collected during Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test using TG BallastCleaner as the Active Substance (High Dose/Low Flow). Parameter Units Test Cycle 7 Test Cycle 8 Average Date and Start Time Oct-14 10:45:50 27-Oct-14 10:24:10 Duration min Pre-Treatment Line Pressure (Average ± Std. Deviation) Post-Treatment Line Pressure (Average ± Std. Deviation) Differential Pressure (Average ± Std. Deviation) Pre-Treatment Flow Rate (Average ± Std. Deviation) Post-Treatment Flow Rate (Average ± Std. Deviation) Backflush Flow Rate (Volumetric Calculation) bar 1.96 ± ± ± 0.01 bar 1.69 ± ± ± 0.01 bar 0.27 ± ± ± 0.00 m 3 /hour 198 ± ± ± 1 m 3 /hour 198 ± ± ± 1 m 3 /hour ± 1 Treatment Retention Tank Volume m ± 2 Control Retention Tank Volume m ± 1 Sample Collection Tub #4 Volume m ± 0.01 Sample Collection Tub #5 Volume m ± The real-time data in Figure 16 shows that once the set flow rate and pressure was achieved there was very low variability in pre- and post-fs flow rate and pressure during the ~ 60 minute operation. There were eight backflush cycles, after which, the operational data quickly returned to a steady state condition (Figure 16).

118 Flow (M^3) Pressure (Bar) Flow and Pressure GSI/LB/QAQC/TR/JFE Page 118 of Time (min) Pre Filter Flow (m^3/hr) Post Filter Flow (m^3/hr) Post Filter Pressure (bar) Pre Filter Pressure (bar) Figure 16. Real-Time Pre- and Post-Filter Flow Rate and Pressure Data Measured During Test Cycle 8 Intake of the JFE BallastAce BWMS Status Test BWMS Active Substance Concentrations The TRO and TRC concentrations measured in pre- and post-treatment grab samples collected simultaneously during Test Cycles 7 and 8 intake are presented in Table 68. During Test Cycle 7 there were no measurable TRO or TRC concentrations in the pre-treatment water (Table 68). During Test Cycle 8, the TRO concentration of the pre-treatment water ranged from mg/l to mg/l (Table 68). This range is within the range of TRO concentrations historically measured in DSH. The oxidant being measured is unknown, however, it is not chlorine as there was no measurable TRC in Test Cycle 8 pre-treatment (Table 68). Table 68 also shows the target TRO concentration three minutes after active substance dosing, which was 20 mg/l for both test cycles, taking into account the DSH DOC concentration. During Test Cycle 7, the TRO (TRC) concentration in post-treatment intake samples ranged from mg/l (10.14 mg/l) to mg/l (13.82 mg/l), which was substantially lower than the JFE target TRO concentration (Table 68). According to JFE Engineering Corporation, the flow meter that was installed on the BWMS during Test Cycles 1 7 had very high variability and low accuracy. During Test Cycle 7, the flow rate as measured by the BWMS flow meter ranged from 160 m3/hour to 260 m3/hour. Since the

119 Page 119 of 146 active substance injection rate was determined by the flow rate of the BWMS (when in automatic mode), this led to an inability to meet the target TRO concentration. Therefore, during Test Cycle 8 JFE conducted a manual active substance injection, which was done at a constant rate. As a result, during Test Cycle 8, the TRO (TRC) concentration in post-treatment intake samples ranged from mg/l (17.92 mg/l) to mg/l (18.85 mg/l; Table 68). Table 68. Concentration of Total Residual Oxidants (TRO) and Total Residual Chlorine (TRC) Measured in Grab Samples Collected Simultaneously from the Pre- and Post-Treatment Lines During Test Cycles 7 and 8 Intake of the JFE BallastAce BWMS Status Test. N/A = Not Applicable. ND = Measured value was below the method detection limit. Sample Location (Pitot) Pre-Treatment (SP3c) Post-Treatment (SP15) Collection JFE TRO Target Test Cycle 7 Test Cycle 8 Time (min) (mg/l) TRO (mg/l) TRC (mg/l) TRO (mg/l) TRC (mg/l) 1 ND ND ND 3 ND ND ND 10 N/A ND ND ND 30 ND ND ND 55 ND ND ND AVERAGE Water Quality Conditions Grab Samples Intake water quality results from pre- and post-treatment intake samples collected simultaneously during Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test are presented in Table 69. Both test cycles met the minimum challenge water quality characteristics outlined in the ETV Protocol (USEPA, 2010). The pre-treatment TSS concentration was 31.3 mg/l and 32.1 mg/l in Test Cycles 7 and 8, respectively (minimum target value was 24.0 mg/l; Table 69). The pretreatment intake DOC concentration was 7.7 mg/l (Test Cycle 7) and 7.9 mg/l (Test Cycle 8; minimum target value was 6 mg/l; Table 69); this parameter was not augmented as the DSH naturally meets the challenge water DOC criterion. The pre-treatment POC concentration was 4.9 mg/l in both Test Cycles 7 and 8, which exceeded the minimum target value of 4 mg/l (Table 69). Finally, the MM concentration in pre-treatment intake samples 26.3 mg/l (Test Cycle 7) and 27.2 mg/l (Test Cycle 8; minimum target value was 20 mg/l; Table 69). There was very little change in TSS, MM, NPOC, DOC, or POC concentration between the preand post-treatment samples (Table 69). As expected, there was a higher %T (filtered and unfiltered) in post-treatment samples as compared to pre-treatment samples (Table 69).

120 Page 120 of 146 Table 69. Average (± Standard Deviation, n=3) Concentration of Total Suspended Solids (TSS), Percent Transmittance (%T, in Filtered and Unfiltered Samples), Non-Purgeable Organic Carbon (NPOC), Dissolved Organic Carbon (DOC), Particulate Organic Carbon (POC), and Mineral Matter (MM) Measured in Grab Samples Collected Simultaneously from the Pre- and Post-Treatment Line on Intake During Test Cycles 7 and 8 Intake of the JFE BallastAce BWMS Status Test. Test Cycle Sample Location (Pitot) TSS (mg/l) %T, Filtered/ Unfiltered NPOC (mg/l) DOC (mg/l) POC (mg/l) MM (mg/l) 7 Pre-Treatment (SP3c) Post-Treatment (SP15) 31.3 (0.4) 30.0 (0.1) 49.2 (5.1)/ 38.3 (0.4) 51.4 (0.5)/ 43.0 (0.4) 12.7 (0.9) 7.7 (0.1) 4.9 (0.8) 26.3 (0.4) 11.9 (0.6) 7.7 (0.1) 4.2 (0.4) 25.8 (0.5) 8 Pre-Treatment (SP3c) Post-Treatment (SP15) 32.1 (0.5) 30.7 (0.8) 46.0 (0.2)/ 38.5 (0.1) 52.4 (0.2)/ 43.7 (0.3) 12.8 (0.3) 7.9 (0.2) 4.9 (0.2) 27.2 (0.3) 12.9 (0.2) 7.7 (0.1) 5.2 (0.1) 5.6 (0.8) Sample Collection Tub Measurements The water quality data from measurements taken in the pre-treatment sample collection tubs during Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test provide a time-integrated picture of the challenge water characteristics and are presented in Table 70. The water temperature for these two test cycles, which were conducted towards the end of the GSI land-based testing season, were 9.72 C (Test Cycle 7; Table 70) and 9.96 C (Test Cycle 8; Table 70), and within the range specified by the ETV Protocol (i.e., 4 to 35 C; USEPA, 2010). All other parameters were very similar between the two test cycles, although the total chlorophyll concentration was slightly higher in pre-treatment intake during Test Cycle 8 (Table 70). Table 70. Average Value (± Standard Deviation, n=2)of Various Water Quality Parameters Measured in the Pre-Treatment Sample Collection Tubs During Test Cycles 7 and 8 Intake of the JFE BallastAce BWMS Status Test. Parameter Test Cycle 7 Test Cycle 8 Temperature ( C) 9.72 ± ± 0.04 Specific Conductivity (ms/cm) ± ± Salinity (ppt) 0.11 ± ± ph Turbidity (NTU) 18.3 ± ± 1.3 Total Chlorophyll (µg/l) 7.7 ± ± 0.0 Dissolved Oxygen (mg/l) ± ± 0.03 Dissolved Oxygen (% Saturation) 90.3 ± ± 0.1

121 Biological Conditions GSI/LB/QAQC/TR/JFE Page 121 of 146 As shown in Table 71, Test Cycles 7 and 8 had live organism densities in the challenge water that exceeded the minimum criteria for challenge water total living populations specified by the ETV Protocol, with the exception of organisms 10 µm and < 50 µm in Test Cycle 7. The challenge water density was 955 live cells/ml in this case, which was slightly lower than the minimum value of 1,000 live cells/ml (Table 71). For the largest regulated size class, nominally zooplankton, challenge water densities were 218,000 and 176,000 live organisms per m 3 in Test Cycles 7 and 8, respectively (Table 71). The 10 µm and < 50 µm size class, nominally protists, had 955 live cells/ml (Test Cycle 7; Table 71) and 1,240 cells/ml (Test Cycle 8; Table 71). The smallest regulated size class was represented by culturable, aerobic, heterotrophic bacteria during this test. Live densities, as measured by the spread plate method, well exceeded the minimum density of 1,000/mL and were 20,000 and 34,600 live bacteria per ml in Test Cycles 7 and 8, respectively (Table 71). Table 71. Live Plankton Density (n=1 each) and Average (± Standard Deviation, n=3) Microbial Concentration in Challenge Water Samples Collected During Test Cycles 7 and 8 8 of the JFE BallastAce BWMS Status Test. Values marked with an asterisk (*) did not meet TQAP requirements. Regulated Size Class Parameter TQAP Requirements Test Cycle 7 Test Cycle 8 50 µm Concentration (#/m 3 ) 100,000 organisms/m 3 218, , µm and < 50 µm < 10 µm Concentration (cells/ml) Concentration (CFU/mL as culturable aerobic heterotrophic bacteria) 1,000 organisms/ml 955* 1,240 1,000/mL 20,000 (3,560) 34,600 (9,720) Retention Period Conditions During the 48 hour retention period associated with Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test, the TRO concentration in the control and treatment retention tanks was measured twice (once at 24 and once at 48 hours). Various water quality parameters were also measured every 15 minutes in both tanks and logged during retention BWMS Active Substance Concentrations As shown in Table 72, there were measurable TRO concentrations in the control retention tank during the 48 hour holding time ranging from mg/l to mg/l. There were no detectable TRC concentrations in the control retention tank (Table 72). There was a notable decrease in TRO and TRC concentrations of the treated water during the 48 hour retention time, although this decrease was not as great as the > 90 % TRO degradation seen during the previous six test cycles.

122 Page 122 of 146 This result indicates that there was still chlorine demand present in the intake water after treatment, despite the high active substance dose. Concentrations in Test Cycle 7 were lower overall than Test Cycle 8 due to the lower initial dose in this test (Table 72). At 24 hours, the TRO (TRC) concentration was 6.19 mg/l (5.74 mg/l) in Test Cycle 7 and 8.76 mg/l (8.50 mg/l) in Test Cycle 8 (Table 72). In terms of TRO, this represented an average decrease of 53 % for Test Cycle 7 and 55 % for Test Cycle 8 compared to post-treatment intake. At 48 hours, the TRO (TRC) concentration was 4.24 mg/l (3.84 mg/l) in Test Cycle 7 and 6.70 mg/l (6.36 mg/l) in Test Cycle 8, which was an average decrease in TRO concentration of 68 % and 66 % compared to posttreatment intake samples, respectively (Table 72). Table 72. Concentration of Total Residual Oxidants (TRO) and Total Residual Chlorine (TRC) in the Control and Treatment Retention Tanks 24 and 48 Hours Post-Treatment During Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test. ND = Measured value was below the method detection limit. Sample Location Control Retention Tank Treatment Retention Tank Collection Time (hour) Test Cycle 7 Test Cycle 8 TRO (mg/l) TRC (mg/l) TRO (mg/l) TRC (mg/l) ND ND ND ND Water Quality Conditions Table 73 shows the average water quality parameters measured using calibrated Sondes in the control and treatment retention tanks during the 48 hour holding time utilized in Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test. Each parameter was measured every 15 minutes during the holding period. There were no unexpected differences in water quality measured between the two test cycles (Table 73). There were some notable, although expected, differences between the control and treatment retention tanks during both test cycles. The specific conductivity and salinity was elevated in the treatment retention tank as compared to the control retention tank (Table 73). This is due to the addition of TG BallastCleaner to the treated water and the subsequent increase in ions. Total chlorophyll was markedly decreased in the treatment retention tank, which is due to the decrease in live protist density as a result of treatment (Table 73).

123 Page 123 of 146 Table 73. Average (± Standard Deviation) Water Quality Parameters Measured in the Control and Treatment Retention Tanks during the 48 Hour Retention Period for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test. Parameter Temperature ( C) Specific Conductivity (ms/cm) Salinity (ppt) ph Turbidity (NTU) Total Chlorophyll (µg/l) Dissolved Oxygen (mg/l) Dissolved Oxygen (% Saturation) Retention Tank Test Cycle 7 Test Cycle 8 Control 9.79 ± 0.08, n= ± 0.28, n=175 Treatment 9.85 ± 0.07, n= ± 0.29, n=175 Control ± 0.000, n= ± 0.000, n=175 Treatment ± 0.001, n= ± 0.001, n=175 Control 0.11 ± 0.00, n= ± 0.00, n=175 Treatment 0.15 ± 0.00, n= ± 0.00, n=175 Control 7.50, n= , n=175 Treatment 7.72, n= , n=175 Control 15.3 ± 1.1, n= ± 1.4, n=175 Treatment 14.9 ± 1.0, n= ± 1.3, n=175 Control 7.6 ± 0.6, n= ± 0.7, n=175 Treatment 4.3 ± 0.8, n= ± 0.5, n=175 Control ± 0.03, n= ± 0.06, n=175 Treatment ± 0.02, n= ± 0.01, n=175 Control 88.8 ± 0.3, n= ± 1.1, n=175 Treatment 90.2 ± 0.1, n= ± 0.6, n= Discharge Measurements Operational Conditions Control Discharge The operational data measured during discharge of the control retention tank for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test are presented in Table 74. The control discharge operational data from both test cycles are very similar. Control discharge occurred over an average duration of minutes; at a pressure of 1.89 bar and flow rate of 199 m 3 /hour, on average (Table 74). A total of 177 m 3 was discharged from the control retention tank, on average (Table 74). Zooplankton samples, all of which were collected from Sample Tub 1, represented an average of 2.59 m 3 concentrated to 1 L (Table 74).

124 Page 124 of 146 Table 74. Summary of Operational Measurements and Data Collected during Control Retention Tank Discharge for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test using TG BallastCleaner as the Active Substance (High Dose/Low Flow). Parameter Units Test Cycle 7 Test Cycle 8 Average Date and Start Time Oct-14 11:29:10 29-Oct-14 11:28:40 Duration min Discharge Line Pressure (Average ± Std. Deviation) Discharge Flow Rate (Average ± Std. Deviation) Volume Discharged from Retention Tank Sample Collection Tub #1 Volume Sample Collection Tub #2 Volume bar 1.88 ± ± ± 0.01 m 3 /hour 199 ± ± ± 0 m ± 1 m ± 0.04 m ± Treatment Discharge Table 75 shows operational data measured during discharge of the treatment retention tanks for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test. As with the control discharge data, the average values from both test cycles are very similar to one another. The treatment discharge operation was an average of minutes in duration (Table 75). There was a slight difference in pressure, 0.19 bar on average, between the pre-neutralization line and the post-neutralization line (Table 75). This difference was not as great as during intake because the BWMS FS was not active during discharge. The average treatment discharge flow rate was 198 m 3 /hour, and an average 188 m 3 of water from the treatment retention tank was discharged (Table 75). Zooplankton samples were collected from Sample Collection Tub #s 4 and 5, which both had an average sample volume of 2.73 m 3 (Table 75).

125 Page 125 of 146 Table 75. Summary of Operational Measurements and Data Collected during Treatment Retention Tank Discharge for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test using TG BallastCleaner as the Active Substance (High Dose/Low Flow). Parameter Units Test Cycle 7 Test Cycle 8 Average Date and Start Time Oct-14 09:01:50 29-Oct-14 09:00:10 Duration min Pre-Neutralization Line Pressure (Average ± Std. bar 1.92 ± ± ± 0.01 Deviation) Post-Neutralization Line Pressure (Average ± Std. bar 1.77 ± ± ± 0.02 Deviation) Differential Pressure* (Average ± Std. Deviation) bar 0.24 ± ± ± 0.07 Flow Rate (Average ± Std. Deviation) m 3 /hour 198 ± ± ± 0 Volume Discharged from Retention Tank m ± 1 Sample Collection Tub #4 Volume m ± 0.03 Sample Collection Tub #5 Volume m ± 0.02 Sample Collection Tub #6 Volume m ± 0.04 *BWMS filter was not active during discharge BWMS Active Substance Concentrations The TRO and TRC concentrations measured in grab samples collected throughout control and treatment tank discharge operations associated with Test Cycles 7 and 8 of the JFE BallastAce Status Test are presented in Table 76. The TRO concentration in control discharge water ranged from mg/l to mg/l, which was in keeping with the range of TRO concentrations measured in pre-treatment water during these two test cycles (Table 76). There was no detectable TRO or TRC in either the control or treatment discharge water during either of these two test cycles; for treatment discharge in all cases the TRC concentration was below the permitted level of mg/l and the water was discharged from the wastewater holding tank to the DSH (Table 76). The range of TRO concentrations measured in the treatment discharge samples was overall lower than that of the control discharge samples, ranging from below the method detection limit to mg/l (Table 76).

126 Page 126 of 146 Table 76. Concentration of Total Residual Oxidants (TRO) and Total Residual Chlorine (TRC) Measured in Grab Samples Collected During Test Cycles 7 and 8 Control and Treatment Tank Discharge Operations Associated with the JFE BallastAce BWMS Status Test. ND = Measured value was below the method detection limit. Sample Location (Pitot) Control (SP9a) Treatment (SP15) Collection Test Cycle 7 Test Cycle 8 Time (min) TRO (mg/l) TRC (mg/l) TRO (mg/l) TRC (mg/l) ND ND ND ND ND ND ND ND ND ND ND ND 3 ND ND ND 10 ND ND ND 30 ND ND ND ND 50 ND ND ND ND Water Quality Measurements Grab Samples Table 77 shows the measured water quality data from grab samples collected throughout discharge of the control and treatment retention tanks associated with Test Cycles 7 and 8 of the JFE BallastAce Status Test. As expected, %T (both filtered and unfiltered) was slightly higher in the treatment discharge samples than in the control discharge samples (Table 76). The chlorine in the treated water continued to oxidize and break down the organic matter during retention, resulting in treatment discharge water that was more transparent than the control water. For all other water quality parameters measured, the results are indicative of solids settling out over the 48 hour retention time (i.e., substantially lower values than on intake), and are similar between the control and treatment discharge samples (Table 77).

127 Page 127 of 146 Table 77. Average (± Standard Deviation, n=3) Concentration of Total Suspended Solids (TSS), Percent Transmittance (%T, in Filtered and Unfiltered Samples), Non-Purgeable Organic Carbon (NPOC), Dissolved Organic Carbon (DOC), Particulate Organic Carbon (POC), and Mineral Matter (MM) in Grab Samples Collected during Discharge of the Control and Treatment Retention Tanks for Status Test Cycles 7 and 8 Associated with Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test. Test Cycle Sample Location (Pitot) TSS (mg/l) %T, Filtered/ Unfiltered NPOC (mg/l) DOC (mg/l) POC (mg/l) MM (mg/l) 7 8 Control (SP9a) 10.8 (0.1) Treatment (SP15) 10.1 (0.6) Control (SP9a) 11.1 (0.4) Treatment (SP15) 10.5 (0.8) 45.8 (0.1)/ 39.3 (0.0) 49.8 (0.1)/ 43.5 (0.1) 46.2 (0.1)/ 39.2 (0.1) 50.1 (0.4)/ 43.3 (0.1) 9.4 (0.7) 7.6 (0.1) 1.9 (0.6) 8.9 (0.7) 10.0 (0.2) 8.4 (0.1) 1.6 (0.2) 8.5 (0.8) 9.6 (0.1) 7.9 (0.2) 1.7 (0.3) 9.4 (0.6) 10.7 (0.3) 8.7 (0.2) 2.0 (0.1) 8.5 (0.7) Sample Collection Tub Measurements Table 78 shows water quality parameters measured in the sample collection tubs using calibrated Sondes immediately following discharge of the control and treatment retention tanks associated with Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test. There were slight differences in sample collection tub water quality between the two test cycles; water temperature was overall higher in Test Cycle 7 than Test Cycle 8, in general, specific conductivity, salinity, ph, and turbidity was lower in Test Cycle 7 than Test Cycle 8 (Table 78). All other parameters were similar between the two test cycles (Table 78). The specific conductivity and salinity was higher in the treatment discharge water than the control discharge water due to the added ions from treatment with TG BallastCleaner and neutralization with sodium sulfite. The total chlorophyll concentration in the control discharge was higher than in the treatment discharge due to the decreased protist density as a result of treatment. For all other parameters, there was no discernible trend between control and treatment discharge water (Table 78).

128 Page 128 of 146 Table 78. Average (± Standard Deviation) Water Quality Parameters Measured in the Control and Treatment Sample Collection Tubs Immediately Following Control and Treatment Discharge Operations for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test. Parameter Sample Type Test Cycle 7 Test Cycle 8 Temperature ( C) Specific Conductivity (ms/cm) Salinity (ppt) ph Turbidity (NTU) Total Chlorophyll (µg/l) Dissolved Oxygen (mg/l) Dissolved Oxygen (% Saturation) CONT, n= ± ± 0.00 TRT, n= ± ± 0.01 CONT, n= ± ± 0.00 TRT, n= ± ± 0.00 CONT, n= ± ± TRT, n= ± ± CONT, n= TRT, n= CONT, n= ± ± 0.6 TRT, n= ± ± 0.3 CONT, n=2 6.5 ± ± 0.1 TRT, n=3 5.7 ± ± 0.2 CONT, n= ± ±0.18 TRT, n= ± ± 0.10 CONT, n= ± ± 0.2 TRT, n= ± ± Biological Conditions The control and treatment discharge densities of the three regulated size classes associated with Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test are presented in Table 79; more detailed taxonomic data are available on request. The control discharge density of the 50 µm size class greatly exceeded the minimum concentration of 100 live organisms/m 3 specified in the ETV Protocol, with 424,000/m 3 (Test Cycle 7; Table 79) and 353,000/m 3 (Test Cycle 8; Table 79). The results from treatment discharge indicate a near-to-complete elimination of organisms in this size class; both test cycles met the USCG BWDS of less than 10 live organisms/m 3. During test Cycle 7, 0.21 m 3 of treated discharge water was analyzed revealing an average density of 0 live organism/m 3 (Table 79). A total of 0.25 m 3 of water was examined during Test Cycle 8 with an average treatment discharge density of 4 live organisms/m 3 (Table 79). The calculated live density in Test Cycle 8 treatment discharge is due to one live rotifer, in the genus Keratella that was found swimming in the concentrated sample from Sample Collection Tub #4. Given that all other Keratella observed in treatment discharge from Test Cycle 8 were dead (albeit freshly killed with internal organs intact), it is possible that this Keratella was a GSI Facility contaminant that was sampled after neutralization of the discharge. It is important to note that GSI did validate the cleanliness of the Facility prior to conducting the discharge operation for Test Cycle 8, as with all previous test cycles. The control discharge density of the 10 µm and < 50 µm size class also greatly exceeded the ETV Protocol minimum required density of 100 organisms/ml; live density was 713 cells/ml in Test Cycle 7 and 886 cells/ml in Test Cycle 8 (Table 79). There was also a substantial decrease in live organism density in the treatment discharge as compared to the control discharge, with 0.76 cell/ml

129 Page 129 of 146 and 0.23 cell/ml in Test Cycles 7 and 8, respectively (Table 79). Both test cycles met the USCG BWDS for this size class of organisms, which is less than 10 live cells/ml. The live density of culturable, aerobic heterotrophic bacteria (i.e., < 10 µm size class) in control discharge was far greater than the minimum concentration of 500/mL specified in the ETV Protocol. The control discharge density was 43,400 CFU/mL in Test Cycle 7 and 46,800 CFU/mL in Test Cycle 8 (Table 79). There was a substantial decrease in heterotrophic bacteria density in the treatment discharge as compared to the control discharge. In Test Cycle 7, the treatment discharge density was < 10 CFU/mL (i.e., a 99.9 % reduction from control discharge; Table 79). In Test Cycle 8, the density in treatment discharge was 730 CFU/mL, which was a reduction of 98.4 % compared to the control discharge (Table 79). There is no discharge standard for heterotrophic bacteria; these densities cannot be compared to any regulation. Table 79. Live Plankton Density (Average ± Standard Deviation, Where Applicable) and Average (± Standard Deviation, n=3) Microbial Concentrations in Samples Collected During Control and Treatment Retention Tank Discharge for Test Cycles 7 and 8 of the JFE BallastAce BWMS Status Test. Regulated Size Class Maximum Concentration in Treated Discharge Control Discharge 50 µm < 10 organisms per m 3 424,000 (n=1) 10 µm and < 50 µm < 10 organisms per ml 713 (n=1) < 10 µm (CFU/mL as culturable aerobic heterotrophic bacteria) No discharge standard for heterotrophic bacteria. 43,400 (13,900), n=3 Test Cycle 7 Test Cycle 8 Treatment Discharge 0 (n=2) 0.76 (n=1, composite) <10, n=3 Control Discharge 353,000 (n=1) 886 (n=1) 46,800 (11,900), n=3 Treatment Discharge 4 (n=2) 0.23 (n=1, composite) 730 (704), n=3

130 Disinfection Byproducts (DBPs) Concentrations GSI/LB/QAQC/TR/JFE Page 130 of 146 The results from analysis of selected DBPs in samples collected during Test Cycle 7 control and treatment discharge of the JFE BallastAce BWMS Status Test are presented in Table 80. Samples were collected for DBP analysis during Test Cycle 7, as this was the test cycle selected for WET testing. There were elevated concentrations of all classes of DBPs in the treatment discharge as compared to the control discharge, with the exception of the bromate ion (Table 80). In the control discharge samples, all of the selected DBPs were below the limit of detection with the exception of total sodium (i.e., average concentration of 12.9 µg/l; Table 80). Of all DBPs measured, the chlorate ion had the highest measured concentration in treatment discharge, with an average of 1410 µg/l (i.e., six times higher than in Test Cycle 4; Table 80). The total trihalomethanes was the second highest class of DBPs, in terms of concentration in treatment discharge, with an average concentration of 459 µg/l (Table 80). Chloroform was the primary contributor and bromodichloromethane was a secondary contributor in the treatment discharge samples. There was an average of 390 µg/l total haloacetic acids in treatment discharge; trichloroacetic acid and dichloroacetic acid were the primary contributors to the total concentration of haloacetic acids in treatment discharge (Table 80). The average concentration of total haloacetonitriles in treatment discharge was 66 µg/l; the majority of the total was from chloral hydrate (Table 80). Total sodium was three times higher in treatment discharge as compared to control discharge (i.e., 37.0 µg/l in treatment discharge compared to 12.9 µg/l in control discharge; Table 80). Overall, average concentrations of each class of DBPs was two to three times higher in Test Cycle 7 treatment discharge than Test Cycle 4 treatment discharge (i.e., TG BallastCleaner with low dose/high flow).

131 Page 131 of 146 Table 80. Results from Analysis of Selected Disinfection Byproducts (DBPs) in Samples Collected during Discharge of the Control and Treatment Retention Tanks in Test Cycle 7 of the JFE BallastAce BWMS Status Test. Analyte Formula Control Average (µg/l) Test Cycle 7 Treatment Average (µg/l) Bromodichloromethane CHBrCl 2 < Bromoform CHBr 3 < 0.5 < 0.5 Chlorodibromomethane CHBr 2 Cl < Chloroform CHCl 3 < Total Trihalomethanes < Bromochloroacetic acid* BrClCHCOOH < Dibromoacetic acid CHBr 2 COOH < 1.0 < 1.0 Dichloroacetic acid CHCl 2 COOH < Monobromoacetic acid CH 2 BrCOOH < 1.0 < 1.0 Monochloroacetic acid CH 2 ClCOOH < Trichloroacetic acid CCl 3 COOH < Total Haloacetic Acids < ,1,1-trichloro-2-Propanone CCl 3 COCH 3 < ,1-dichloro-2-Propanone CH 3 COCHCl 2 < Bromochloroacetonitrile C 2 HBrClN < 0.5 < 0.5 Bromoacetonitrile BrCH 2 CN < 0.5 < 0.5 Chloral hydrate Cl 3 CCH(OH) 2 < Chloroacetonitrile ClCH 2 CN < Chloropicrin Cl 3 CNO 2 < 0.5 < 0.5 Dibromoacetonitrile Br 2 CHCN < 0.5 < 0.5 Dichloroacetonitrile Cl 2 CHCN < Trichloroacetonitrile Cl 3 CCN < 0.5 < 0.5 Total Haloacetonitriles < Bromate BrO 3 - Chlorate ClO 3 - < 5.0 < 5.0 < ,410 Sodium, Total Na *Not included in total haloacetic acids.

132 Whole Effluent Toxicity (WET) GSI/LB/QAQC/TR/JFE Page 132 of 146 The water quality parameters measured in stock solutions prepared prior to the start of Test Cycle 7 WET testing and prior to daily renewal of test water during the C. dubia and P. promelas WET tests are presented in Table 81. The temperature of the prepared stock solutions was within the acceptance range of 25 C ± 3 C in all cases (Table 81). In addition, the dissolved oxygen concentration was well above the minimum value specified for P. promelas (i.e., 4.0 mg/l) in all cases (Table 81). All other water quality parameters measured (i.e., ph, conductivity, hardness, and alkalinity) were within the expected ranges for the water types measured (Table 81). The TRO concentration in the C. dubia and P. promelas Performance Control stock solutions ranged from below the method detection limit to mg/l (Table 81). The TRO values in the Facility Control (i.e., control discharge water) were the highest of all the treatment groups and ranged from to mg/l (Table 81). There was measurable TRO in the all dilutions of the whole effluent during the entire duration of the C. dubia and P. promelas WET tests, ranging from as low as mg/l to mg/l overall (Table 81). Treatment Group Table 81. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Stock Solutions during the Ceriodaphnia dubia and Pimephales promelas Whole Effluent Toxicity (WET) Tests Associated with Test Cycle 7 of the JFE BallastAce BWMS Status Test. Temperature ( C) C. dubia 24.8 Performance Control 1 (24.1, 25.7) P. promelas 24.5 Performance Control 2 (24.1, 25.3) 25.3 Facility Control (24.0, 26.7) 0 % Whole 24.9 Effluent 3 (24.1, 25.9) 6.25 % Whole Effluent 12.5 % Whole Effluent 25 % Whole Effluent 50 % Whole Effluent 100 % Whole Effluent 24.6 (23.9, 25.7) 24.6 (23.9, 25.5) 24.7 (24.2, 25.4) 24.8 (24.4, 25.7) 24.9 (24.2, 26.0) Dissolved Oxygen (mg/l) 8.1 (8.1, 8.1) 6.9 (6.4, 7.1) 10.2 (9.4, 11.0) 10.1 (8.9, 11.2) 9.3 (8.8, 10.0) 9.2 (8.6, 10.1) 9.1 (8.5, 9.8) 9.2 (8.7, 9.8) 9.8 (9.4, 10.6) ph 8.05 (7.95, 8.15) 7.58 (7.44, 7.66) 7.72 (7.67, 7.79) 7.92 (7.85,7.95) 7.89 (7.66, 8.03) 7.80 (7.55, 8.01) 7.76 (7.56, 8.01) 7.74 (7.52, 7.98) 7.73 (7.50, 7.86) Conductivity (µs/cm) 398 (396, 400) (151.3, 177.4) 235 (233, 238) 234 (201, 240) 244 (241, 249) 253 (251, 255) 267 (266, 270) 295 (293, 297) 353 (351, 355) Hardness 4 (mg/l CaCO 3 ) Alkalinity 4 (mg/l CaCO 3 ) TRO (mg/l) <DL (<DL, Q ) <DL (<DL, Q ) (0.012 Q, 0.038) Q (0.006 Q, 0.025) Q (0.009 Q, 0.019) Q (0.010 Q, 0.022) Q (0.006 Q, Q ) (0.006 Q, 0.034) Q (0.006 Q, 0.031) 1 Moderately-Hard Reconstituted Water; 2 Dechlorinated Laboratory Water; 3 Filtered Duluth-Superior Harbor Water; 4 Hardness and alkalinity were only measured on Day 0 and do not have minimum and maximum values. * Values less than the detection limit (DL) which equals mg/l were not used to calculate the average TRO value. Q Sample concentration was below the LOQ ( mg/l TRO).

133 Page 133 of 146 The water quality parameters measured in the C. dubia exposure solutions following each 24 hour renewal period are presented in Table 82. The temperature of the exposure solutions was within the acceptance range of 25 C ± 3 C during the entire six day test (Table 82). All other water quality parameters measured (i.e., ph, hardness, and alkalinity) were within the expected ranges for the water types measured (Table 82). Table 82. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Six Day Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Test Cycle 7 of the JFE BallastAce BWMS Status Test. Treatment Group Temperature ( C) ph Hardness 3 (mg/l CaCO 3 ) Alkalinity 3 (mg/l CaCO 3 ) C. dubia Performance Control (23.1, 24.2) (7.68, 8.07) Facility Control (23.2, 24.1) (8.21, 8.35) % Whole Effluent (23.5, 24.5) (8.22, 8.31) % Whole Effluent (23.7, 24.2) (8.19, 8.33) % Whole Effluent (23.3, 24.1) (8.23, 8.31) % Whole Effluent (23.8, 24.3) (8.20, 8.31) % Whole Effluent (23.9, 24.2) (8.20, 8.30) % Whole Effluent (23.2, 24.4) (8.21, 8.26) Moderately-Hard Reconstituted Water; 2 Filtered Duluth-Superior Harbor Water; 3 Hardness and alkalinity were only measured on Day 6 (test termination) and do not have minimum and maximum values. Table 83 shows the survival and reproduction data from the six day, three-brood C. dubia WET test conducted during Test Cycle 7 of the JFE BallastAce BWMS Status Test. In order for the test results to be acceptable there must have been at least 80 % survival and an average total number of at least 15 young per female in the experimental control (0 % Whole Effluent). The WET test met these criteria with 100 % survival and 17.0 average young per female (Table 83). The Performance Control, which is used to determine overall health of the test organisms and not test result acceptance, met the survival criteria but fell just short of the reproduction criteria with an average of 14.8 young per female (Table 83). Results from the Facility Control indicate that there was no statistically significant (p<0.05) effect of control discharge water on adult survival or reproduction. In addition, there was no statistically significant (p<0.05) effect of whole effluent from treatment discharge on adult survival or reproduction when compared to the experimental control, although, the average number of young per female was reduced in the 100 % Whole Effluent treatment group as compared to the experimental control.

134 Page 134 of 146 Table 83. Average (n=10) Percent Survival and Total Number of Offspring Produced in the Three-Brood Ceriodaphnia dubia Whole Effluent Toxicity (WET) Test Associated with Treatment Discharge from Test Cycle 7 of the JFE BallastAce BWMS Status Test. Treatment Group Percent Survival ± Std. Deviation Average Total Number of Young per Female ± Std. Deviation C. dubia Performance Control 1 90 ± ± 5.5 Facility Control 100 ± ± % Whole Effluent ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± % Whole Effluent 90 ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± Moderately-Hard Reconstituted Water; 2 Filtered Duluth-Superior Harbor Water The water quality parameters measured in the P. promelas exposure solutions following each 24 hour renewal period are presented in Table 84. The temperature of the exposure solutions was within the acceptance range of 25 C ± 3 C during the entire seven day test (Table 84). The dissolved oxygen concentration was greater than 4.0 mg/l in all treatment groups (Table 84). All other water quality parameters measured (i.e., ph, hardness, and alkalinity) were within the expected ranges for the water types measured (Table 84).

135 Page 135 of 146 Table 84. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Pimephales promelas Whole Effluent Toxicity (WET) Test Associated with Test Cycle 7 of the JFE BallastAce BWMS Status Test. Treatment Group Temperature ( C) Dissolved Oxygen (mg/l) ph Hardness 3 (mg/l CaCO 3 ) Alkalinity 3 (mg/l CaCO 3 ) P. promelas Performance Control 1 (23.4, 25.2) (4.8, 7.3) (7.45, 7.80) Facility Control (24.0, 24.9) (5.2, 6.8) (7.60, 7.93) % Whole Effluent (23.8, 25.0) (4.7, 6.6) (7.59, 7.97) % Whole Effluent (23.5, 24.5) (5.9, 7.3) (7.79, 8.12) % Whole Effluent (23.3, 24.5) (5.1, 7.1) (7.72, 8.11) % Whole Effluent (23.3, 24.7) (5.4, 7.1) (7.77, 8.09) % Whole Effluent (23.6, 24.5) (5.7, 7.1) (7.79, 8.11) % Whole Effluent (23.8, 24.8) (5.5, 7.0) (7.71, 8.08) Dechlorinated Laboratory Water; 2 Filtered Duluth-Superior Harbor Water; 3 Hardness and alkalinity were only measured on Day 7 (test termination) and do not have minimum and maximum values. Table 85 shows the survival and growth data from the seven day P. promelas WET test conducted during Test Cycle 7 of the JFE BallastAce Status Test. In order for the test results to be acceptable there must have been at least 80 % survival and an average dry weight per surviving organism of at least 0.25 mg in the experimental control (0 % Whole Effluent). The WET test met these criteria with 100 % survival and mg per fish (Table 85). The Performance Control is used to determine overall health of the test organisms and not test result acceptance, however, the Performance Control also met the WET test QC criteria indicating that the organisms used in this WET test were of good health. There was no statistically significant (p<0.05) effect of control discharge water (i.e., Facility Control) on P. promelas survival and growth. In addition, there was no statistically significant (p<0.05) effect of treatment discharge whole effluent on survival, with all of the treatment groups having 100 % adult survival (Table 85). Finally, there was no statistically significant (p<0.05) effect of treatment discharge whole effluent on growth in any of the treatment groups tested.

136 Page 136 of 146 Table 85. Pimephales promelas Average (n=4) Percent Survival and Weight per Fish after Exposure to Treatment Discharge from Test Cycle 7 of the JFE BallastAce BWMS Status Test. Treatment Group Percent Survival ± Std. Deviation Mean Average Weight/Fish (mg) ± Std. Deviation P. promelas Performance Control ± ± Facility Control 95 ± ± % Whole Effluent ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± % Whole Effluent 100 ± ± Dechlorinated Laboratory Water; 2 Filtered Duluth-Superior Harbor Water The water quality parameters measured in the S. capricornutum exposure solutions on Day 0 and in the chemistry replicate flask every 24 hours during the 96 hour WET test are presented in Table 86. The temperature of the exposure solutions was within the acceptance range of 25 C ± 3 C during the entire 96 hour test (Table 86). All other water quality parameters measured (i.e., dissolved oxygen, ph, conductivity, hardness, and alkalinity) were within the expected ranges for the water types measured (Table 86). There were detectable concentrations of TRO in all treatment groups, with the exception of the Performance Control (Table 86). The Facility Control had the highest TRO concentration with mg/l (Table 86). The treatment discharge whole effluent groups had a TRO range of to mg/l (Table 86).

137 Treatment Group GSI/LB/QAQC/TR/JFE Page 137 of 146 Table 86. Average Values (Minimum, Maximum) of Water Quality Parameters Measured in Exposure Solutions during the Selenastrum capricornutum Whole Effluent Toxicity (WET) Test Associated with Test Cycle 7 of the JFE BallastAce BWMS Status Test. Temperature ( C) 24.8 S. capricornutum 24.8 Performance Control 1 (24.1, 25.1) Facility Control 24.8 (23.9, 25.2) 0 % Whole Effluent 2 (23.8, 25.3) 6.25 % Whole 24.8 Effluent (23.8, 25.3) 12.5 % Whole 24.7 Effluent (23.8, 25.3) 25 % Whole 24.8 Effluent (23.8, 25.2) 50 % Whole 24.7 Effluent (23.9, 25.1) 100 % Whole 24.7 Effluent Dissolved Oxygen 3 (mg/l) 8.3 ph 7.90 (7.45, 10.37) Conductivity 3 (µs/cm) Hardness 3 (mg/l CaCO 3 ) Alkalinity 3 (mg/l CaCO 3 ) TRO 3 (mg/l) <DL (8.01, 9.10) (8.19, 9.70) (8.21, 9.56) (8.19, 9.22) (8.17, 9.48) (8.15, 9.65) (23.7, 25.0) (8.09, 9.55) 1 EPA Nutrient Media; 2 Filtered Duluth-Superior Harbor Water; 3 Conductivity, dissolved oxygen, hardness, alkalinity, and TRO were measured only on Day 0 and do not have minimum and maximum values. Q Sample concentration was below the LOQ ( mg/l TRO) Q Q Q Q Q Table 87 shows the growth data from the 96 hour S. capricornutum WET test conducted during Test Cycle 7 of the JFE BallastAce BWMS Status Test. In order for the test results to be acceptable there must have been at least 1 x 10 6 cells/ml at test termination and the cell density must not have varied by more than 20 % CV among replicate flasks in the experimental control (0 % Whole Effluent). The WET test met the criteria for cell density with 2,334,375 cells/ml, but did not meet the variability criteria with 29 % CV among experimental control replicates (Table 87). The Performance Control is used to determine overall health of the test organisms and not test result acceptance, however, the Performance Control met the WET test QC criteria indicating that the organisms used in this WET test were of good health. There was a reduction in cell density in the Facility Control as compared to the experimental control (0 % Whole Effluent), however, this result was not statistically significant (p<0.05). Although the highest cell density was seen in the 100 % Whole Effluent, there was no statistically significant effect (p<0.05) effect of treatment discharge whole effluent on growth, with average cell density ranging from 2,434,375 cells/ml to 3,771,875 cells/ml (Table 87).

138 Page 138 of 146 Table 87. Average (n=4) Cell Density of Selenastrum capricornutum after 96 Hours Exposure to Whole Effluent from Test Cycle 7 Treatment Discharge of the JFE BallastAce BWMS Status Test. Treatment Group Average Cells/mL ± Std. Deviation S. capricornutum Performance Control 1 3,788,000 ± 312,400 Facility Control 1,110,000 ± 150,600 0 % Whole Effluent 2 2,334,375 ± 666,175* 6.25 % Whole Effluent 2,434,375 ± 501, % Whole Effluent 2,543,750 ± 427, % Whole Effluent 2,675,000 ± 130, % Whole Effluent 3,484,375 ± 432, % Whole Effluent 3,771,875 ± 479,841 1 USEPA Nutrient Media; 2 Filtered Duluth-Superior Harbor Water; *Test did not meet QC criteria for variability with 29 % CV. 5.4 Test Validity Table 88 shows the water quality and biology target values and results for challenge water measured during the JFE BallastAce BWMS Status Test. The target values were met for all water quality parameters (i.e., temperature, salinity, TSS, POC, DOC, and MM) measured during the entire evaluation of the three FS tests (Table 88). For the < 10 µm size class, i.e., total culturable heterotrophic bacteria, the target value was greatly exceeded and densities ranged from 13,200 to 57,200 MPN/mL (Table 88). The minimum target value for the 10 µm and < 50 µm size class, i.e., protists, was met for all test cycles with the exception of Test Cycle 7, which feel just short of the minimum target value (i.e., 955 live cells/ml; Table 88). For the 50 µm size class, i.e., zooplankton, the minimum target was met for all eight test cycles with values ranging from 136,000 to 346,000 live organisms/m 3 (Table 88).

139 Page 139 of 146 Table 88. Target Values and Results for GSI Challenge Water During JFE BallastAce Ballast Water Management Status Test. Parameter Target Values for GSI Challenge Water Was Target Met for All Test Cycles? Temperature ( o C) 4 30 YES Salinity (PSU) 0 1 YES Total Suspended Solids (mg/l) Particulate Organic Matter as Particulate Organic Carbon (mg/l) Dissolved Organic Matter as Dissolved Organic Carbon (mg/l) > 24 YES > 4 YES > 6 YES Mineral Matter (mg/l) > 20 YES Organisms < 10 µm Organisms 10 µm and < 50 µm > 1,000 MPN/mL as culturable heterotrophic bacteria > 1,000 cells/ml YES NO; Did not meet target for Test Cycle 7. Organisms 50 µm > 100,000/m 3 YES Comments Average values ranged from during all eight test cycles. Average values ranged from during all eight test cycles. Average values ranged from during all eight test cycles. Average values ranged from during all eight test cycles. Average values ranged from during all eight test cycles. Average values ranged from during all eight test cycles. Average values ranged from 13,200 57,200 MPN/mL during all eight test cycles using the spread plate method. Values ranged from 955 4,027 live cells/ml during all eight test cycles. Values ranged from 136, ,000 live organisms/m 3 during all eight test cycles. 6.1 Operational Data 6 RESULTS: JFE FUJI PANEL FILTER DURABILITY TEST Days 1 and 2 of the JFE Fuji Panel Filter Durability Test took place October The operational data measured during the two day test cycle are summarized in Table 89. The overall duration of the test was hours, which was 2.67 hours less than the target duration of 16 hours (Table 89). The pre-treatment line pressure was 2.02 bar on average, which was within 1 % of the target value of 2 bar (Table 89). The differential pressure between the pre- and post-fs lines was 0.22 bar on average (Table 89). The average post-treatment flow rate was 203 m 3 /hour, which was within 10 % of the target flow rate (i.e., 200 m 3 /hour; Table 89). The backflush flow rate was not collected during this test. The total volume of water filtered over the two day test cycle was 2705 m 3 (Table 89).

140 Page 140 of 146 Table 89. Summary of Operational Data Collected during the Two Day JFE Fuji Panel Filter Durability Test. Parameter Units Day 1 Day 2 Average/Total Date and Start Time Oct-14 08:13:00 17-Oct-14 07:44:00 Duration min Pre-Treatment Line Pressure (Average ± Std. Deviation) Post-Treatment Line Pressure (Average ± Std. Deviation) Differential Pressure (Average ± Std. Deviation) Post-Treatment Flow Rate (Average ± Std. Deviation) (13.33 hr.) bar 2.02 ± ± ± 0.01 bar 1.80 ± ± ± 0.01 bar 0.22 ± ± ± 0.00 m 3 /hour 203 ± ± ± 0 Volume Filtered m Filter Brush Arm Data The weights of each filter brush used during the JFE F Panel Durability Test are presented in Table 90. Each filter brush was weighed prior to the start of the test, the average brush weight was g (Table 90). There was very little variability in pre-test brush weights, data ranged from g to g (Table 90). The weights from both post-test weighing days were very similar to each other, so only the data from the second post-test weighing is presented. The average post-test brush weight was g, with a range of g to g (Table 90). On average, the filter brushes weighed 4 mg less after the completion of test, indicating that brush wear was minimal (Table 90).

141 Page 141 of 146 Table 90. Weights of Filter Brushes Installed in Filter Brush Arms of the Fuji Panel Filter Before and After the JFE F Panel Durability Test. Filter Brush Arm ID Filter Brush ID Pre-Test Filter Brush Weight (g) Post Test Filter Brush Weight (g) Difference Between Pre-Test and Post-Test Weight (mg)

142 Page 142 of 146 Figure 17 shows images of Filter Brush #1-4 taken at 10x using a camera attached to a dissecting microscope. Note that randomly-selected images of brushes from the remaining seven arms are available on request. The brush was photographed in 11 sections in order to capture the entire brush. The before (left; Figure 17) and after (right; Figure 17) photos indicate that the wear was not even over the entire length of the brush. In this case, the wear appears to be greatest at one end of the brush (see sections and ; Figure 17), while the rest of the brush appears to have very little wear.

143 Page 143 of 146 Figure 17. Magnified (10x) Photos of Filter Brush #1-4 Before (Left) and After (Right) the JFE F Panel Durability Test. Photos were taken in 11 sections in order to capture the entire brush.