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Toxicity Testing Report Phillips 66 Ferndale Refinery Ferndale, Washington TOXICITY TESTING REPORT PHILLIPS 66 FERNDALE REFINERY FERNDALE, WASHINGTON Prepared for Phillips 66 Ferndale Refinery 3901 Unick Road Ferndale, Washington 98248 Prepared by EcoAnalysts, Inc. 4770 NE View Drive PO Box 216 Port Gamble, WA 98364 Submittal Date: April 14, 2017 Client Contract Reference: Contract No. 4523507907 EcoAnalysts Report ID: 032117.01 Toxicity Testing Report Phillips 66 Ferndale Refinery All testing reported herein was performed consistent with our laboratory’s quality assurance program. All results are intended to be considered in their entirety, and EcoAnalysts is not responsible for use of less than the complete report. The test results summarized in this report apply only to the sample(s) evaluated. PREPARED BY ______________________________________ Meg Pinza Program Manager ______________________________________ Brian Hester Quality Assurance Officer Authors: Jay D. Word EcoAnalysts Report #032117.01 i EcoAnalysts, Inc. Toxicity Testing Report Phillips 66 Ferndale Refinery CONTENTS 1. EXECUTIVE SUMMARY 1 2. METHODS 2 2.1 Sample Collection and Storage 2 2.2 Bioassay Testing 4 2.3 Organisms for Testing 4 2.4 Mysid, Inland Silverside, Topsmelt, and Herring Feeding 4 2.5 Water for Bioassay Testing 5 2.6 Sample Adjustment 5 2.7 Survival and Growth Tests 5 2.8 Data Management and Analysis 5 3. RESULTS 6 3.1 Pacific Herring (Clupea pallasii) Larval Chronic Test Results 6 3.2 Topsmelt (Atherinops affinis) Chronic Test Results 9 3.3 Mysid (Americamysis bahia) Chronic Test Results 12 3.4 Inland Silverside (Menidia beryllina) Chronic Test Results 15 4. QUALITY ASSURANCE/QUALITY CONTROL 18 4.1 Study Deviations 19 5. SUMMARY 20 6. REFERENCES 21 EcoAnalysts Report #032117.01 ii EcoAnalysts, Inc. Toxicity Testing Report Phillips 66 Ferndale Refinery TABLES Table 1-1. Whole Effluent Toxicity Testing Results 2 Table 2-1. Sample Conditions upon Receipt 3 Table 2-2. Biological Testing Performed 4 Table 2-3. Salinity Adjustments of Project Samples 5 Table 3-1. Endpoint Summary for Clupea pallasii Larval Chronic Test 7 Table 3-2. Statistical Results Summary for Clupea pallasii Larval Chronic Test 7 Table 3-3. Test Condition Summary for Clupea pallasii Larval Chronic Test 8 Table 3-4. Quality Assurance Summary for Clupea pallasii Larval Chronic Test 9 Table 3-5. Endpoint Summary for Atherinops affinis Chronic Test 10 Table 3-6. Statistical Results Summary for Atherinops affinis Chronic Test 10 Table 3-7. Test Condition Summary for Atherinops affinis Chronic Test 11 Table 3-8. Quality Assurance Summary for Atherinops affinis Chronic Test 12 Table 3-9. Endpoint Summary for Americamysis bahia Chronic Test 13 Table 3-10. Statistical Results Summary for Americamysis bahia Chronic Test 13 Table 3-11. Test Condition Summary for Americamysis bahia Chronic Test 14 Table 3-12. Quality Assurance Test Condition Summary for Americamysis bahia Chronic Test 15 Table 3-13. Endpoint Summary for Menidia beryllina Chronic Test 16 Table 3-14. Statistical Results Summary for Menidia beryllina Chronic Test 16 Table 3-15. Test Condition Summary for Menidia beryllina Chronic Test 17 Table 3-16. Quality Assurance Summary for Menidia beryllina Chronic Test 18 Table 5-1. Whole Effluent Toxicity Chronic Test Results Summary 20 APPENDICES Appendix A: Statistical Comparisons and Datasheets Appendix B: Chain of Custody and Sample Receipts EcoAnalysts Report #032117.01 iii EcoAnalysts, Inc. Toxicity Testing Report Phillips 66 Ferndale Refinery ACRONYMS AND ABBREVIATIONS cm: Centimeter °C: Degrees Celsius CETIS: Comprehensive Environmental Toxicity Information System; statistical software Conc.: Concentration Cu: Copper EC50: Effective Concentration that results in a 50% reduction in a sub-lethal endpoint EC25: Effective Concentration that results in a 25% reduction in a sub-lethal endpoint g: Grams LC50: Lethal Concentration that results in a 50% reduction in survival L: Liter LOEC/L: Lowest Observed Effect Concentration/Level µg: Microgram µm: Micrometer mg: Milligram mg/L: Milligrams per liter mL: Milliliter mm: Millimeter NELAP: National Environmental Laboratory Accreditation Program NOEC/L: No Observed Effect Concentration/Level NPDES: National Pollutant Discharge Elimination System PMSD: Percent Minimum Significant Different ppt: parts per thousand QM: Quality Manual SD: Standard Deviation SOP: Standard Operating Procedure TU: Toxic Units USEPA: United States Environmental Protection Agency (USEPA or EPA) WA: Washington State WET: Whole Effluent Toxicity WSPA: Washington State Petroleum Association EcoAnalysts Report #032117.01 iv EcoAnalysts, Inc. Toxicity Testing Report Phillips 66 Ferndale Refinery 1. EXECUTIVE SUMMARY EcoAnalysts’ Port Gamble Laboratory conducted whole effluent toxicity (WET) testing on an effluent sample (P66 001) collected by Whatcom Environmental Services (WES). This testing was conducted to support an Agreed Order (Holmes 2013) issued by Washington State Department of Ecology to the Western States Petroleum Association (WSPA) and Intalco Facilities. The objective of this program was to assess the potential toxicity of primary discharge water under the National Pollutant Discharge Elimination System Waste Discharge Permit (NPDES Permit No. WA0002984) to selected aquatic organisms following procedures defined within the Agreed Order. The results of the toxicity testing are contained in this report. Topsmelt (Atherinops affinis), inland silverside (Menidia beryllina), mysid (Americamysis bahia), and Pacific herring (Clupea pallasii) were exposed to the effluent using methods outlined in EPA-600-R-95- 136, EPA-821-R-02-014, and Dinnel 2008/11. All chronic tests were initiated on February 21, 2017 and terminated on February 28, 2017. All laboratory control treatments met performance acceptability standards. The reference-toxicant test results for topsmelt, mysid, inland silverside, and herring indicate the organisms were of similar sensitivity to populations of test organisms previously tested. Water quality measurements were within acceptable ranges for the all tests conducted for this larval testing suite except for minor deviations in salinity were observed in the mysid tests. These excursions for salinity were within the tolerance ranges of the test organisms and would not be expected to influence the significance of the test findings. A summary of the statistical analysis for tests conducted is provided in Table 1-1. The detailed results of the biological testing are contained in this report. EcoAnalysts Report #032117.01 1 EcoAnalysts, Inc. Toxicity Testing Report Phillips 66 Ferndale Refinery Table 1-1. Whole Effluent Toxicity Testing Results P66 001 1 2 7-Day 7-Day NOEC LOEC 3 Test LC50/EC50 LC25/EC25 TUc (%) (%) (%) (%) Herring - Clupea pallasii Survival 25 50 44.9 31.7 4 (Comparison to Lab Control) Herring - Clupea pallasii Biomass 6.25 12.5 32.6 19.0 5.3 (Comparison to Lab Control) Topsmelt - Atherinops affinis Survival 100 >100 >100 >100 1 Topsmelt - Atherinops affinis Biomass 100 >100 >100 >100 <1 Mysid - Americamysis bahia Survival 12.5 25 24.5 16.4 8 Mysid - Americamysis bahia Biomass 6.25 12.5 15.5 9.4 10.6 Inland Silverside - Menidia beryllina 100 >100 >100 >100 1 Survival Inland Silverside - Menidia beryllina 50 >100 >100 >100 <1 Biomass 1 NOEC = No Observed Effect Concentration 2 LOEC = Lowest Observed Effect Concentration 3 TUc = Chronic Toxicity Units (Survival = 100/NOEC; Growth and Biomass = 100/EC25) 2. METHODS The effluent samples were analyzed for toxicity using methods outlined in the most recently promulgated United States Environmental Protection Agency (USEPA) guidance documents (EPA/600/R- 95-136 and EPA-821-R-02-014) and relevant EcoAnalysts’ Port Gamble Laboratory standard operating procedures (SOPs). These methods are further defined through the Ecology Publication, Laboratory Guidance and Whole Effluent Toxicity Test Review Criteria (WDOE 2016). In addition, herring culturing and testing was conducted in accordance with methods outlined in Pacific Herring, Clupea pallasi, Embryo and Larval Bioassay Protocols, Summary Report for Washington Department of Ecology (Dinnel 2008) and Methods for Conducting Bioassays Using Embryos and Larvae of Pacific Herring, Clupea pallasi (Dinnel 2011). 2.1 Sample Collection and Storage Whatcom Environmental Services personnel collected grab samples of primary discharge effluent on February 20, 23 and 27, 2017. The samples were transported by courier (Thunderdog Delivery) and were received at the laboratory within seven hours after sample collection. Samples were delivered on ice, with no headspace. All samples were clear in appearance. Sample temperatures upon receipt ranged from 1.0 to 6.0°C. When the samples arrived at the testing laboratory, they were immediately recorded into the sample receipt log, salted to test salinity and stored at 4 ± 2 °C in the dark until utilized for testing purposes. Additional sample conditions are summarized in Table 2-1. EcoAnalysts Report #032117.01 2 EcoAnalysts, Inc. Toxicity Testing Report Phillips 66 Ferndale Refinery Table 2-1. Sample Conditions upon Receipt Sample P66 001 Laboratory ID P170220.01a, b, c P170223.01a, b P170227.01a Date/Time sampled 2/20/2017; 0700 2/23/2017; 0815 2/27/2017 0815 Date/Time received 2/20/2017; 1305 2/23/2017; 1330 2/27/2017 1315 Dissolved Oxygen (mg/L) 9.2 9.4 9.2 10.3 10.8 11.9 Recommended: >5.0 mg/L Temperature (°C) 6.0 5.3 5.7 4.3 3.1 1.0 Recommended: 0 – 6°C pH (units) 7.4 7.4 7.4 7.6 7.6 7.7 Recommended: 6 – 9 Salinity (ppt) 0.8 0.8 0.8 0.6 0.7 0.9 Total Free Chlorine (mg/L) 0.00
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